# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dieter Lentz' _publ_contact_author_email LENTZ@CHEMIE.FU-BERLIN.DE _publ_section_title ; Synthesis, Crystal and Molecular Structure of Alkali Metal Nonaflates ; loop_ _publ_author_name 'Dieter Lentz' 'Irene Brudgam' 'Helmut Vorbruggen' # Attachment 'CSC4F9SO3.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 737955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Caesium nonafluorobutylsulfonate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 Cs F9 O3 S' _chemical_formula_weight 432.01 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.1889(16) _cell_length_b 6.1177(19) _cell_length_c 16.787(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.195(12) _cell_angle_gamma 90.00 _cell_volume 528.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.49 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .36 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 3.828 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _exptl_special_details ; 'SADABS (Bruker-AXS) Provides only ratio of Tmin/Tmax' ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6523 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.49 _reflns_number_total 2838 _reflns_number_gt 2633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _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^)+(0.0313P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 2838 _refine_ls_number_parameters 163 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Cs1 Cs 0.43838(3) 0.72206(5) 0.081901(10) 0.02114(6) Uani 1 1 d . . . C1 C 0.0440(7) 0.2738(6) 0.2203(2) 0.0225(9) Uani 1 1 d . . . C2 C 0.1146(8) 0.0710(7) 0.2724(2) 0.0257(8) Uani 1 1 d . . . C3 C 0.2014(9) 0.1183(9) 0.3627(3) 0.0368(10) Uani 1 1 d . . . C4 C 0.2000(14) -0.0809(14) 0.4182(3) 0.0584(18) Uani 1 1 d . . . F1 F 0.2144(6) 0.4355(6) 0.24226(17) 0.0343(7) Uani 1 1 d . . . F2 F -0.1933(5) 0.3419(6) 0.23370(16) 0.0382(6) Uani 1 1 d . . . F3 F 0.3122(6) -0.0359(6) 0.24446(17) 0.0367(7) Uani 1 1 d . . . F4 F -0.0914(6) -0.0643(6) 0.26715(17) 0.0435(7) Uani 1 1 d . . . F5 F 0.4406(5) 0.2017(10) 0.37046(15) 0.0521(9) Uani 1 1 d . . . F6 F 0.0391(7) 0.2693(7) 0.38771(18) 0.0551(12) Uani 1 1 d . . . F7 F 0.3324(10) -0.2439(10) 0.3908(2) 0.0846(16) Uani 1 1 d . . . F8 F -0.0359(11) -0.1430(11) 0.4255(3) 0.100(2) Uani 1 1 d . . . F9 F 0.3193(9) -0.0260(8) 0.49078(18) 0.0769(13) Uani 1 1 d . . . O1 O 0.3089(3) 0.2200(9) 0.09845(12) 0.0220(4) Uani 1 1 d . . . O2 O -0.0964(8) 0.4230(11) 0.0783(2) 0.0263(10) Uani 1 1 d . . . O3 O -0.1004(9) 0.0280(10) 0.0945(2) 0.0258(9) Uani 1 1 d . . . S1 S 0.03803(12) 0.2290(3) 0.11076(4) 0.01753(14) Uani 1 1 d . . . 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 Cs1 0.01681(8) 0.01414(10) 0.03288(10) -0.00037(15) 0.00468(6) 0.00006(15) C1 0.0210(13) 0.020(3) 0.0265(16) -0.0011(13) 0.0045(11) 0.0026(12) C2 0.0304(18) 0.025(2) 0.0222(18) -0.0002(15) 0.0045(15) -0.0033(16) C3 0.044(2) 0.041(3) 0.0251(19) 0.0002(18) 0.0015(17) -0.004(2) C4 0.079(4) 0.062(5) 0.031(2) 0.015(3) -0.004(3) -0.003(4) F1 0.0452(18) 0.0244(18) 0.0322(14) -0.0082(12) 0.0010(12) -0.0075(14) F2 0.0300(11) 0.0495(19) 0.0373(14) 0.0010(12) 0.0132(10) 0.0151(12) F3 0.0452(18) 0.033(2) 0.0329(14) 0.0020(12) 0.0085(12) 0.0137(14) F4 0.0464(15) 0.042(2) 0.0406(15) 0.0098(13) 0.0004(12) -0.0201(14) F5 0.0465(13) 0.066(3) 0.0393(12) -0.002(2) -0.0114(10) -0.014(2) F6 0.0739(19) 0.062(4) 0.0302(12) -0.0082(15) 0.0106(12) 0.0172(18) F7 0.143(4) 0.056(4) 0.0496(18) 0.016(2) -0.006(2) 0.022(3) F8 0.098(3) 0.133(5) 0.070(3) 0.058(3) 0.007(2) -0.039(3) F9 0.113(3) 0.084(4) 0.0290(16) 0.0089(18) -0.0091(17) 0.000(3) O1 0.0167(8) 0.0193(11) 0.0308(10) -0.006(2) 0.0066(7) -0.002(2) O2 0.0214(16) 0.024(2) 0.0331(19) 0.0068(15) 0.0036(13) 0.0070(14) O3 0.0255(16) 0.019(2) 0.0323(17) -0.0041(16) 0.0033(14) -0.0096(15) S1 0.0137(2) 0.0159(4) 0.0232(3) -0.0004(7) 0.0032(2) -0.0012(7) _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 Cs1 O3 3.025(5) 1_665 ? Cs1 O2 3.036(5) 1_655 ? Cs1 O1 3.139(6) 1_565 ? Cs1 O1 3.164(6) . ? Cs1 F3 3.243(3) 1_565 ? Cs1 O2 3.270(5) 2 ? Cs1 O2 3.318(5) . ? Cs1 O3 3.393(6) 1_565 ? Cs1 O1 3.447(2) 2_655 ? Cs1 O3 3.457(4) 2 ? Cs1 F1 3.529(3) . ? Cs1 S1 3.7285(19) . ? C1 F2 1.345(4) . ? C1 F1 1.347(5) . ? C1 C2 1.536(5) . ? C1 S1 1.855(4) . ? C2 F4 1.346(5) . ? C2 F3 1.349(5) . ? C2 C3 1.553(6) . ? C3 F5 1.333(6) . ? C3 F6 1.351(6) . ? C3 C4 1.535(9) . ? C4 F8 1.302(10) . ? C4 F7 1.326(10) . ? C4 F9 1.338(7) . ? F2 Cs1 3.786(3) 1_455 ? F3 Cs1 3.243(3) 1_545 ? O1 S1 1.4472(19) . ? O1 Cs1 3.139(6) 1_545 ? O1 Cs1 3.447(2) 2_645 ? O2 S1 1.448(6) . ? O2 Cs1 3.036(5) 1_455 ? O2 Cs1 3.270(5) 2_545 ? O3 S1 1.433(6) . ? O3 Cs1 3.025(5) 1_445 ? O3 Cs1 3.393(6) 1_545 ? O3 Cs1 3.457(4) 2_545 ? S1 Cs1 3.7974(19) 1_545 ? S1 Cs1 3.8171(11) 2_545 ? 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 O3 Cs1 O2 75.53(9) 1_665 1_655 ? O3 Cs1 O1 64.50(12) 1_665 1_565 ? O2 Cs1 O1 140.01(12) 1_655 1_565 ? O3 Cs1 O1 140.31(12) 1_665 . ? O2 Cs1 O1 66.10(12) 1_655 . ? O1 Cs1 O1 152.15(6) 1_565 . ? O3 Cs1 F3 84.26(12) 1_665 1_565 ? O2 Cs1 F3 122.48(9) 1_655 1_565 ? O1 Cs1 F3 54.15(7) 1_565 1_565 ? O1 Cs1 F3 107.58(8) . 1_565 ? O3 Cs1 O2 99.66(15) 1_665 2 ? O2 Cs1 O2 124.13(8) 1_655 2 ? O1 Cs1 O2 66.91(11) 1_565 2 ? O1 Cs1 O2 109.75(11) . 2 ? F3 Cs1 O2 111.97(11) 1_565 2 ? O3 Cs1 O2 174.32(16) 1_665 . ? O2 Cs1 O2 109.4(2) 1_655 . ? O1 Cs1 O2 110.42(11) 1_565 . ? O1 Cs1 O2 43.95(11) . . ? F3 Cs1 O2 90.62(10) 1_565 . ? O2 Cs1 O2 79.96(7) 2 . ? O3 Cs1 O3 107.77(18) 1_665 1_565 ? O2 Cs1 O3 175.75(15) 1_655 1_565 ? O1 Cs1 O3 43.28(10) 1_565 1_565 ? O1 Cs1 O3 110.15(10) . 1_565 ? F3 Cs1 O3 56.01(9) 1_565 1_565 ? O2 Cs1 O3 58.48(10) 2 1_565 ? O2 Cs1 O3 67.15(7) . 1_565 ? O3 Cs1 O1 71.27(11) 1_665 2_655 ? O2 Cs1 O1 65.74(9) 1_655 2_655 ? O1 Cs1 O1 100.98(12) 1_565 2_655 ? O1 Cs1 O1 100.48(12) . 2_655 ? F3 Cs1 O1 151.63(11) 1_565 2_655 ? O2 Cs1 O1 60.41(8) 2 2_655 ? O2 Cs1 O1 113.02(9) . 2_655 ? O3 Cs1 O1 117.63(9) 1_565 2_655 ? O3 Cs1 O3 125.76(8) 1_665 2 ? O2 Cs1 O3 95.46(13) 1_655 2 ? O1 Cs1 O3 108.53(10) 1_565 2 ? O1 Cs1 O3 69.60(10) . 2 ? F3 Cs1 O3 138.02(9) 1_565 2 ? O2 Cs1 O3 42.27(8) 2 2 ? O2 Cs1 O3 57.41(11) . 2 ? O3 Cs1 O3 84.79(8) 1_565 2 ? O1 Cs1 O3 56.94(10) 2_655 2 ? O3 Cs1 F1 125.98(10) 1_665 . ? O2 Cs1 F1 93.14(10) 1_655 . ? O1 Cs1 F1 108.66(7) 1_565 . ? O1 Cs1 F1 49.98(6) . . ? F3 Cs1 F1 57.62(7) 1_565 . ? O2 Cs1 F1 128.11(10) 2 . ? O2 Cs1 F1 52.09(8) . . ? O3 Cs1 F1 82.76(10) 1_565 . ? O1 Cs1 F1 150.01(11) 2_655 . ? O3 Cs1 F1 107.61(10) 2 . ? O3 Cs1 S1 160.12(10) 1_665 . ? O2 Cs1 S1 88.42(12) 1_655 . ? O1 Cs1 S1 130.14(5) 1_565 . ? O1 Cs1 S1 22.37(4) . . ? F3 Cs1 S1 94.91(7) 1_565 . ? O2 Cs1 S1 99.04(10) 2 . ? O2 Cs1 S1 22.78(10) . . ? O3 Cs1 S1 87.79(10) 1_565 . ? O1 Cs1 S1 112.99(9) 2_655 . ? O3 Cs1 S1 66.57(10) 2 . ? F1 Cs1 S1 42.00(5) . . ? F2 C1 F1 108.0(3) . . ? F2 C1 C2 108.2(3) . . ? F1 C1 C2 109.6(3) . . ? F2 C1 S1 108.0(2) . . ? F1 C1 S1 108.0(3) . . ? C2 C1 S1 114.7(3) . . ? F4 C2 F3 108.1(4) . . ? F4 C2 C1 109.2(3) . . ? F3 C2 C1 109.3(3) . . ? F4 C2 C3 108.0(3) . . ? F3 C2 C3 106.8(3) . . ? C1 C2 C3 115.1(4) . . ? F5 C3 F6 108.5(5) . . ? F5 C3 C4 108.6(5) . . ? F6 C3 C4 107.7(4) . . ? F5 C3 C2 108.6(4) . . ? F6 C3 C2 108.4(4) . . ? C4 C3 C2 114.9(5) . . ? F8 C4 F7 110.3(7) . . ? F8 C4 F9 108.7(6) . . ? F7 C4 F9 107.7(6) . . ? F8 C4 C3 111.4(6) . . ? F7 C4 C3 110.1(5) . . ? F9 C4 C3 108.5(6) . . ? C1 F1 Cs1 115.1(2) . . ? C1 F2 Cs1 118.2(2) . 1_455 ? C2 F3 Cs1 139.1(2) . 1_545 ? S1 O1 Cs1 105.8(3) . 1_545 ? S1 O1 Cs1 101.3(3) . . ? Cs1 O1 Cs1 152.15(6) 1_545 . ? S1 O1 Cs1 127.48(11) . 2_645 ? Cs1 O1 Cs1 79.43(8) 1_545 2_645 ? Cs1 O1 Cs1 79.11(9) . 2_645 ? S1 O2 Cs1 146.4(2) . 1_455 ? S1 O2 Cs1 100.8(3) . 2_545 ? Cs1 O2 Cs1 83.81(10) 1_455 2_545 ? S1 O2 Cs1 94.7(2) . . ? Cs1 O2 Cs1 109.4(2) 1_455 . ? Cs1 O2 Cs1 126.08(11) 2_545 . ? S1 O3 Cs1 156.6(3) . 1_445 ? S1 O3 Cs1 95.0(2) . 1_545 ? Cs1 O3 Cs1 107.77(18) 1_445 1_545 ? S1 O3 Cs1 93.3(2) . 2_545 ? Cs1 O3 Cs1 80.83(9) 1_445 2_545 ? Cs1 O3 Cs1 118.02(13) 1_545 2_545 ? O3 S1 O1 114.4(3) . . ? O3 S1 O2 115.15(16) . . ? O1 S1 O2 114.1(3) . . ? O3 S1 C1 105.2(2) . . ? O1 S1 C1 104.55(14) . . ? O2 S1 C1 101.5(2) . . ? O3 S1 Cs1 160.66(18) . . ? O1 S1 Cs1 56.3(2) . . ? O2 S1 Cs1 62.5(2) . . ? C1 S1 Cs1 93.95(13) . . ? O3 S1 Cs1 62.9(2) . 1_545 ? O1 S1 Cs1 52.7(2) . 1_545 ? O2 S1 Cs1 150.06(16) . 1_545 ? C1 S1 Cs1 107.79(13) . 1_545 ? Cs1 S1 Cs1 108.76(3) . 1_545 ? O3 S1 Cs1 64.71(18) . 2_545 ? O1 S1 Cs1 114.59(9) . 2_545 ? O2 S1 Cs1 57.3(2) . 2_545 ? C1 S1 Cs1 140.35(11) . 2_545 ? Cs1 S1 Cs1 102.19(4) . 2_545 ? Cs1 S1 Cs1 100.92(3) 1_545 2_545 ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 C1 C2 F4 44.7(4) . . . . ? F1 C1 C2 F4 162.3(3) . . . . ? S1 C1 C2 F4 -76.0(4) . . . . ? F2 C1 C2 F3 162.9(3) . . . . ? F1 C1 C2 F3 -79.5(4) . . . . ? S1 C1 C2 F3 42.1(4) . . . . ? F2 C1 C2 C3 -76.9(4) . . . . ? F1 C1 C2 C3 40.7(5) . . . . ? S1 C1 C2 C3 162.4(3) . . . . ? F4 C2 C3 F5 163.7(5) . . . . ? F3 C2 C3 F5 47.6(6) . . . . ? C1 C2 C3 F5 -74.0(5) . . . . ? F4 C2 C3 F6 -78.7(5) . . . . ? F3 C2 C3 F6 165.2(4) . . . . ? C1 C2 C3 F6 43.6(5) . . . . ? F4 C2 C3 C4 41.8(6) . . . . ? F3 C2 C3 C4 -74.3(6) . . . . ? C1 C2 C3 C4 164.1(5) . . . . ? F5 C3 C4 F8 167.3(6) . . . . ? F6 C3 C4 F8 50.0(7) . . . . ? C2 C3 C4 F8 -70.8(7) . . . . ? F5 C3 C4 F7 -70.0(6) . . . . ? F6 C3 C4 F7 172.8(5) . . . . ? C2 C3 C4 F7 51.9(7) . . . . ? F5 C3 C4 F9 47.7(7) . . . . ? F6 C3 C4 F9 -69.6(6) . . . . ? C2 C3 C4 F9 169.6(5) . . . . ? F2 C1 F1 Cs1 -106.1(3) . . . . ? C2 C1 F1 Cs1 136.2(2) . . . . ? S1 C1 F1 Cs1 10.5(3) . . . . ? O3 Cs1 F1 C1 -165.9(3) 1_665 . . . ? O2 Cs1 F1 C1 -91.6(3) 1_655 . . . ? O1 Cs1 F1 C1 122.5(2) 1_565 . . . ? O1 Cs1 F1 C1 -36.7(2) . . . . ? F3 Cs1 F1 C1 141.4(3) 1_565 . . . ? O2 Cs1 F1 C1 47.6(3) 2 . . . ? O2 Cs1 F1 C1 20.7(2) . . . . ? O3 Cs1 F1 C1 87.3(3) 1_565 . . . ? O1 Cs1 F1 C1 -48.3(3) 2_655 . . . ? O3 Cs1 F1 C1 5.2(3) 2 . . . ? S1 Cs1 F1 C1 -7.4(2) . . . . ? F1 C1 F2 Cs1 79.4(3) . . . 1_455 ? C2 C1 F2 Cs1 -162.0(2) . . . 1_455 ? S1 C1 F2 Cs1 -37.2(3) . . . 1_455 ? F4 C2 F3 Cs1 58.0(5) . . . 1_545 ? C1 C2 F3 Cs1 -60.7(5) . . . 1_545 ? C3 C2 F3 Cs1 174.1(3) . . . 1_545 ? O3 Cs1 O1 S1 160.30(14) 1_665 . . . ? O2 Cs1 O1 S1 176.16(13) 1_655 . . . ? O1 Cs1 O1 S1 13.4(2) 1_565 . . . ? F3 Cs1 O1 S1 57.74(12) 1_565 . . . ? O2 Cs1 O1 S1 -64.31(13) 2 . . . ? O2 Cs1 O1 S1 -14.06(11) . . . . ? O3 Cs1 O1 S1 -1.70(13) 1_565 . . . ? O1 Cs1 O1 S1 -126.46(11) 2_655 . . . ? O3 Cs1 O1 S1 -77.82(12) 2 . . . ? F1 Cs1 O1 S1 59.39(11) . . . . ? O3 Cs1 O1 Cs1 -33.1(2) 1_665 . . 1_545 ? O2 Cs1 O1 Cs1 -17.26(16) 1_655 . . 1_545 ? O1 Cs1 O1 Cs1 180.0 1_565 . . 1_545 ? F3 Cs1 O1 Cs1 -135.67(15) 1_565 . . 1_545 ? O2 Cs1 O1 Cs1 102.27(17) 2 . . 1_545 ? O2 Cs1 O1 Cs1 152.5(2) . . . 1_545 ? O3 Cs1 O1 Cs1 164.89(15) 1_565 . . 1_545 ? O1 Cs1 O1 Cs1 40.12(14) 2_655 . . 1_545 ? O3 Cs1 O1 Cs1 88.76(18) 2 . . 1_545 ? F1 Cs1 O1 Cs1 -134.03(19) . . . 1_545 ? S1 Cs1 O1 Cs1 166.6(2) . . . 1_545 ? O3 Cs1 O1 Cs1 -73.30(14) 1_665 . . 2_645 ? O2 Cs1 O1 Cs1 -57.45(8) 1_655 . . 2_645 ? O1 Cs1 O1 Cs1 139.82(13) 1_565 . . 2_645 ? F3 Cs1 O1 Cs1 -175.86(6) 1_565 . . 2_645 ? O2 Cs1 O1 Cs1 62.08(9) 2 . . 2_645 ? O2 Cs1 O1 Cs1 112.34(11) . . . 2_645 ? O3 Cs1 O1 Cs1 124.70(8) 1_565 . . 2_645 ? O1 Cs1 O1 Cs1 -0.07(3) 2_655 . . 2_645 ? O3 Cs1 O1 Cs1 48.57(9) 2 . . 2_645 ? F1 Cs1 O1 Cs1 -174.22(9) . . . 2_645 ? S1 Cs1 O1 Cs1 126.40(11) . . . 2_645 ? O3 Cs1 O2 S1 -126.8(12) 1_665 . . . ? O2 Cs1 O2 S1 23.7(3) 1_655 . . . ? O1 Cs1 O2 S1 -152.89(16) 1_565 . . . ? O1 Cs1 O2 S1 13.82(13) . . . . ? F3 Cs1 O2 S1 -101.27(19) 1_565 . . . ? O2 Cs1 O2 S1 146.51(19) 2 . . . ? O3 Cs1 O2 S1 -153.6(2) 1_565 . . . ? O1 Cs1 O2 S1 94.84(19) 2_655 . . . ? O3 Cs1 O2 S1 107.65(18) 2 . . . ? F1 Cs1 O2 S1 -54.68(15) . . . . ? O3 Cs1 O2 Cs1 29.5(12) 1_665 . . 1_455 ? O2 Cs1 O2 Cs1 180.0 1_655 . . 1_455 ? O1 Cs1 O2 Cs1 3.40(13) 1_565 . . 1_455 ? O1 Cs1 O2 Cs1 170.10(17) . . . 1_455 ? F3 Cs1 O2 Cs1 55.02(11) 1_565 . . 1_455 ? O2 Cs1 O2 Cs1 -57.20(10) 2 . . 1_455 ? O3 Cs1 O2 Cs1 2.70(8) 1_565 . . 1_455 ? O1 Cs1 O2 Cs1 -108.87(12) 2_655 . . 1_455 ? O3 Cs1 O2 Cs1 -96.07(12) 2 . . 1_455 ? F1 Cs1 O2 Cs1 101.60(15) . . . 1_455 ? S1 Cs1 O2 Cs1 156.3(3) . . . 1_455 ? O3 Cs1 O2 Cs1 126.1(10) 1_665 . . 2_545 ? O2 Cs1 O2 Cs1 -83.4(2) 1_655 . . 2_545 ? O1 Cs1 O2 Cs1 100.0(2) 1_565 . . 2_545 ? O1 Cs1 O2 Cs1 -93.3(2) . . . 2_545 ? F3 Cs1 O2 Cs1 151.7(2) 1_565 . . 2_545 ? O2 Cs1 O2 Cs1 39.4(3) 2 . . 2_545 ? O3 Cs1 O2 Cs1 99.3(2) 1_565 . . 2_545 ? O1 Cs1 O2 Cs1 -12.2(3) 2_655 . . 2_545 ? O3 Cs1 O2 Cs1 0.6(2) 2 . . 2_545 ? F1 Cs1 O2 Cs1 -161.8(3) . . . 2_545 ? S1 Cs1 O2 Cs1 -107.1(3) . . . 2_545 ? Cs1 O3 S1 O1 178.7(5) 1_445 . . . ? Cs1 O3 S1 O1 11.6(2) 1_545 . . . ? Cs1 O3 S1 O1 -106.93(17) 2_545 . . . ? Cs1 O3 S1 O2 -46.3(6) 1_445 . . . ? Cs1 O3 S1 O2 146.62(17) 1_545 . . . ? Cs1 O3 S1 O2 28.1(2) 2_545 . . . ? Cs1 O3 S1 C1 64.6(6) 1_445 . . . ? Cs1 O3 S1 C1 -102.52(15) 1_545 . . . ? Cs1 O3 S1 C1 138.96(14) 2_545 . . . ? Cs1 O3 S1 Cs1 -124.5(6) 1_445 . . . ? Cs1 O3 S1 Cs1 68.4(6) 1_545 . . . ? Cs1 O3 S1 Cs1 -50.1(7) 2_545 . . . ? Cs1 O3 S1 Cs1 167.1(7) 1_445 . . 1_545 ? Cs1 O3 S1 Cs1 -118.51(15) 2_545 . . 1_545 ? Cs1 O3 S1 Cs1 -74.4(6) 1_445 . . 2_545 ? Cs1 O3 S1 Cs1 118.51(15) 1_545 . . 2_545 ? Cs1 O1 S1 O3 -13.0(2) 1_545 . . . ? Cs1 O1 S1 O3 160.55(19) . . . . ? Cs1 O1 S1 O3 75.7(4) 2_645 . . . ? Cs1 O1 S1 O2 -148.5(2) 1_545 . . . ? Cs1 O1 S1 O2 25.0(2) . . . . ? Cs1 O1 S1 O2 -59.9(4) 2_645 . . . ? Cs1 O1 S1 C1 101.49(16) 1_545 . . . ? Cs1 O1 S1 C1 -84.98(17) . . . . ? Cs1 O1 S1 C1 -169.9(3) 2_645 . . . ? Cs1 O1 S1 Cs1 -173.53(12) 1_545 . . . ? Cs1 O1 S1 Cs1 -84.9(3) 2_645 . . . ? Cs1 O1 S1 Cs1 173.53(12) . . . 1_545 ? Cs1 O1 S1 Cs1 88.7(3) 2_645 . . 1_545 ? Cs1 O1 S1 Cs1 -85.03(16) 1_545 . . 2_545 ? Cs1 O1 S1 Cs1 88.51(14) . . . 2_545 ? Cs1 O1 S1 Cs1 3.6(4) 2_645 . . 2_545 ? Cs1 O2 S1 O3 64.7(6) 1_455 . . . ? Cs1 O2 S1 O3 -30.42(19) 2_545 . . . ? Cs1 O2 S1 O3 -158.6(2) . . . . ? Cs1 O2 S1 O1 -160.1(4) 1_455 . . . ? Cs1 O2 S1 O1 104.8(2) 2_545 . . . ? Cs1 O2 S1 O1 -23.4(2) . . . . ? Cs1 O2 S1 C1 -48.3(6) 1_455 . . . ? Cs1 O2 S1 C1 -143.41(14) 2_545 . . . ? Cs1 O2 S1 C1 88.45(15) . . . . ? Cs1 O2 S1 Cs1 -136.7(6) 1_455 . . . ? Cs1 O2 S1 Cs1 128.14(15) 2_545 . . . ? Cs1 O2 S1 Cs1 143.5(2) 1_455 . . 1_545 ? Cs1 O2 S1 Cs1 48.4(5) 2_545 . . 1_545 ? Cs1 O2 S1 Cs1 -79.7(4) . . . 1_545 ? Cs1 O2 S1 Cs1 95.1(6) 1_455 . . 2_545 ? Cs1 O2 S1 Cs1 -128.14(15) . . . 2_545 ? F2 C1 S1 O3 -75.5(4) . . . . ? F1 C1 S1 O3 167.9(3) . . . . ? C2 C1 S1 O3 45.4(3) . . . . ? F2 C1 S1 O1 163.7(3) . . . . ? F1 C1 S1 O1 47.1(4) . . . . ? C2 C1 S1 O1 -75.4(4) . . . . ? F2 C1 S1 O2 44.8(4) . . . . ? F1 C1 S1 O2 -71.7(3) . . . . ? C2 C1 S1 O2 165.7(3) . . . . ? F2 C1 S1 Cs1 107.5(3) . . . . ? F1 C1 S1 Cs1 -9.0(3) . . . . ? C2 C1 S1 Cs1 -131.6(2) . . . . ? F2 C1 S1 Cs1 -141.3(2) . . . 1_545 ? F1 C1 S1 Cs1 102.1(3) . . . 1_545 ? C2 C1 S1 Cs1 -20.5(3) . . . 1_545 ? F2 C1 S1 Cs1 -7.0(4) . . . 2_545 ? F1 C1 S1 Cs1 -123.6(2) . . . 2_545 ? C2 C1 S1 Cs1 113.9(3) . . . 2_545 ? O3 Cs1 S1 O3 -105.6(8) 1_665 . . . ? O2 Cs1 S1 O3 -69.8(7) 1_655 . . . ? O1 Cs1 S1 O3 121.8(7) 1_565 . . . ? O1 Cs1 S1 O3 -66.3(7) . . . . ? F3 Cs1 S1 O3 167.7(7) 1_565 . . . ? O2 Cs1 S1 O3 54.5(6) 2 . . . ? O2 Cs1 S1 O3 87.9(6) . . . . ? O3 Cs1 S1 O3 112.1(7) 1_565 . . . ? O1 Cs1 S1 O3 -7.1(7) 2_655 . . . ? O3 Cs1 S1 O3 26.8(7) 2 . . . ? F1 Cs1 S1 O3 -166.3(7) . . . . ? O3 Cs1 S1 O1 -39.3(3) 1_665 . . . ? O2 Cs1 S1 O1 -3.51(12) 1_655 . . . ? O1 Cs1 S1 O1 -171.85(15) 1_565 . . . ? F3 Cs1 S1 O1 -125.99(11) 1_565 . . . ? O2 Cs1 S1 O1 120.81(13) 2 . . . ? O2 Cs1 S1 O1 154.2(2) . . . . ? O3 Cs1 S1 O1 178.41(12) 1_565 . . . ? O1 Cs1 S1 O1 59.21(13) 2_655 . . . ? O3 Cs1 S1 O1 93.13(13) 2 . . . ? F1 Cs1 S1 O1 -99.97(13) . . . . ? O3 Cs1 S1 O2 166.5(3) 1_665 . . . ? O2 Cs1 S1 O2 -157.7(3) 1_655 . . . ? O1 Cs1 S1 O2 34.0(2) 1_565 . . . ? O1 Cs1 S1 O2 -154.2(2) . . . . ? F3 Cs1 S1 O2 79.8(2) 1_565 . . . ? O2 Cs1 S1 O2 -33.4(2) 2 . . . ? O3 Cs1 S1 O2 24.2(2) 1_565 . . . ? O1 Cs1 S1 O2 -95.0(2) 2_655 . . . ? O3 Cs1 S1 O2 -61.06(17) 2 . . . ? F1 Cs1 S1 O2 105.8(2) . . . . ? O3 Cs1 S1 C1 65.6(3) 1_665 . . . ? O2 Cs1 S1 C1 101.35(13) 1_655 . . . ? O1 Cs1 S1 C1 -66.98(13) 1_565 . . . ? O1 Cs1 S1 C1 104.86(16) . . . . ? F3 Cs1 S1 C1 -21.12(12) 1_565 . . . ? O2 Cs1 S1 C1 -134.33(14) 2 . . . ? O2 Cs1 S1 C1 -100.9(2) . . . . ? O3 Cs1 S1 C1 -76.73(13) 1_565 . . . ? O1 Cs1 S1 C1 164.08(12) 2_655 . . . ? O3 Cs1 S1 C1 -162.00(15) 2 . . . ? F1 Cs1 S1 C1 4.89(14) . . . . ? O3 Cs1 S1 Cs1 -44.7(3) 1_665 . . 1_545 ? O2 Cs1 S1 Cs1 -8.95(7) 1_655 . . 1_545 ? O1 Cs1 S1 Cs1 -177.28(5) 1_565 . . 1_545 ? O1 Cs1 S1 Cs1 -5.43(10) . . . 1_545 ? F3 Cs1 S1 Cs1 -131.42(5) 1_565 . . 1_545 ? O2 Cs1 S1 Cs1 115.38(8) 2 . . 1_545 ? O2 Cs1 S1 Cs1 148.76(19) . . . 1_545 ? O3 Cs1 S1 Cs1 172.98(7) 1_565 . . 1_545 ? O1 Cs1 S1 Cs1 53.78(6) 2_655 . . 1_545 ? O3 Cs1 S1 Cs1 87.70(9) 2 . . 1_545 ? F1 Cs1 S1 Cs1 -105.40(9) . . . 1_545 ? O3 Cs1 S1 Cs1 -150.9(3) 1_665 . . 2_545 ? O2 Cs1 S1 Cs1 -115.09(8) 1_655 . . 2_545 ? O1 Cs1 S1 Cs1 76.58(6) 1_565 . . 2_545 ? O1 Cs1 S1 Cs1 -111.57(10) . . . 2_545 ? F3 Cs1 S1 Cs1 122.44(6) 1_565 . . 2_545 ? O2 Cs1 S1 Cs1 9.24(9) 2 . . 2_545 ? O2 Cs1 S1 Cs1 42.62(19) . . . 2_545 ? O3 Cs1 S1 Cs1 66.83(7) 1_565 . . 2_545 ? O1 Cs1 S1 Cs1 -52.36(6) 2_655 . . 2_545 ? O3 Cs1 S1 Cs1 -18.44(9) 2 . . 2_545 ? F1 Cs1 S1 Cs1 148.46(9) . . . 2_545 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.786 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.125 # Attachment 'KC4F9SO3.CIF' data_org97m _database_code_depnum_ccdc_archive 'CCDC 737956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Potasium Nonafluorobutylsulfonate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 F9 K O3 S' _chemical_formula_weight 338.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0606(9) _cell_length_b 5.5530(10) _cell_length_c 16.997(3) _cell_angle_alpha 83.233(4) _cell_angle_beta 86.532(4) _cell_angle_gamma 87.185(4) _cell_volume 473.01(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 961 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 30.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .688 _exptl_absorpt_correction_T_max 1. _exptl_absorpt_process_details ? _exptl_special_details ; 'SADABS (BRUKER-AXS)' ; _diffrn_ambient_temperature 173(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 'ccd area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5886 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.51 _reflns_number_total 2796 _reflns_number_gt 2309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0357P)^2^+0.1848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2796 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 K1 K 0.02513(7) 1.24926(6) 0.08117(2) 0.01961(9) Uani 1 1 d . . . S1 S 0.47715(8) 0.76738(7) 0.09783(2) 0.01437(9) Uani 1 1 d . . . O1 O 0.6632(2) 0.6171(2) 0.05587(7) 0.0197(2) Uani 1 1 d . . . O2 O 0.5580(2) 1.0113(2) 0.10273(7) 0.0208(3) Uani 1 1 d . . . O3 O 0.2041(2) 0.7553(2) 0.07825(7) 0.0192(2) Uani 1 1 d . . . C1 C 0.4816(3) 0.6180(3) 0.20128(9) 0.0173(3) Uani 1 1 d . . . C2 C 0.3905(3) 0.7832(3) 0.26597(10) 0.0193(3) Uani 1 1 d . . . C3 C 0.3215(4) 0.6444(3) 0.34888(10) 0.0238(4) Uani 1 1 d . . . C4 C 0.3159(5) 0.8016(4) 0.41832(11) 0.0351(5) Uani 1 1 d . . . F1 F 0.7302(2) 0.5310(2) 0.21479(6) 0.0266(2) Uani 1 1 d . . . F2 F 0.3230(2) 0.42641(18) 0.20831(6) 0.0242(2) Uani 1 1 d . . . F3 F 0.5835(2) 0.93552(19) 0.27294(6) 0.0269(2) Uani 1 1 d . . . F4 F 0.1724(2) 0.91623(19) 0.24249(6) 0.0248(2) Uani 1 1 d . . . F5 F 0.5010(2) 0.4612(2) 0.36387(6) 0.0334(3) Uani 1 1 d . . . F6 F 0.0818(2) 0.5517(2) 0.34851(7) 0.0339(3) Uani 1 1 d . . . F7 F 0.5578(3) 0.8616(3) 0.43141(8) 0.0523(4) Uani 1 1 d . . . F8 F 0.1661(3) 1.0008(3) 0.40290(8) 0.0496(4) Uani 1 1 d . . . F9 F 0.2158(3) 0.6765(3) 0.48370(7) 0.0505(4) Uani 1 1 d . . . 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 K1 0.01663(18) 0.01627(17) 0.02586(18) -0.00295(13) -0.00094(13) 0.00092(13) S1 0.01158(18) 0.01385(18) 0.01795(17) -0.00277(13) -0.00149(13) -0.00032(14) O1 0.0160(6) 0.0219(6) 0.0218(6) -0.0068(4) -0.0011(4) 0.0040(5) O2 0.0221(6) 0.0158(6) 0.0250(6) -0.0031(4) -0.0005(5) -0.0044(5) O3 0.0120(5) 0.0222(6) 0.0238(6) -0.0034(5) -0.0028(4) 0.0000(5) C1 0.0165(8) 0.0141(7) 0.0215(7) -0.0015(6) -0.0030(6) 0.0001(6) C2 0.0176(8) 0.0182(8) 0.0229(7) -0.0042(6) -0.0021(6) -0.0031(6) C3 0.0242(9) 0.0257(9) 0.0217(8) -0.0022(6) -0.0012(7) -0.0035(7) C4 0.0434(13) 0.0400(12) 0.0229(9) -0.0082(8) 0.0032(8) -0.0066(10) F1 0.0197(5) 0.0337(6) 0.0259(5) -0.0028(4) -0.0064(4) 0.0101(4) F2 0.0318(6) 0.0155(5) 0.0258(5) -0.0019(4) -0.0008(4) -0.0073(4) F3 0.0296(6) 0.0261(5) 0.0273(5) -0.0079(4) -0.0010(4) -0.0132(5) F4 0.0237(5) 0.0238(5) 0.0260(5) -0.0038(4) 0.0005(4) 0.0068(4) F5 0.0398(7) 0.0326(6) 0.0258(5) 0.0035(4) -0.0045(5) 0.0046(5) F6 0.0303(6) 0.0411(7) 0.0301(6) -0.0002(5) 0.0024(5) -0.0148(5) F7 0.0529(9) 0.0760(11) 0.0344(7) -0.0236(7) -0.0050(6) -0.0219(8) F8 0.0677(10) 0.0409(8) 0.0406(7) -0.0160(6) 0.0071(7) 0.0073(7) F9 0.0671(10) 0.0620(9) 0.0215(6) -0.0032(6) 0.0093(6) -0.0120(8) _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 K1 O1 2.6895(13) 1_465 ? K1 O2 2.7491(13) 1_455 ? K1 O1 2.7797(13) 2_675 ? K1 O3 2.8509(13) . ? K1 O2 2.9676(14) . ? K1 O3 2.9885(13) 1_565 ? K1 F2 2.9917(11) 1_565 ? K1 O3 3.0145(12) 2_575 ? K1 F1 3.1672(12) 1_465 ? K1 F4 3.2266(12) . ? K1 S1 3.4310(7) . ? K1 K1 3.6929(9) 2_585 ? S1 O1 1.4398(12) . ? S1 O2 1.4471(12) . ? S1 O3 1.4475(12) . ? S1 C1 1.8547(16) . ? O1 K1 2.6895(13) 1_645 ? O1 K1 2.7797(13) 2_675 ? O2 K1 2.7491(13) 1_655 ? O3 K1 2.9885(13) 1_545 ? O3 K1 3.0145(12) 2_575 ? C1 F1 1.3484(19) . ? C1 F2 1.3535(18) . ? C1 C2 1.549(2) . ? C2 F3 1.3426(18) . ? C2 F4 1.351(2) . ? C2 C3 1.553(2) . ? C3 F6 1.341(2) . ? C3 F5 1.342(2) . ? C3 C4 1.547(3) . ? C4 F8 1.319(3) . ? C4 F7 1.322(3) . ? C4 F9 1.326(2) . ? F1 K1 3.1672(12) 1_645 ? F2 K1 2.9917(11) 1_545 ? 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 O1 K1 O2 78.05(4) 1_465 1_455 ? O1 K1 O1 95.07(4) 1_465 2_675 ? O2 K1 O1 130.75(4) 1_455 2_675 ? O1 K1 O3 152.37(4) 1_465 . ? O2 K1 O3 77.91(4) 1_455 . ? O1 K1 O3 90.39(4) 2_675 . ? O1 K1 O2 157.28(4) 1_465 . ? O2 K1 O2 124.52(4) 1_455 . ? O1 K1 O2 72.62(4) 2_675 . ? O3 K1 O2 49.21(3) . . ? O1 K1 O3 62.03(4) 1_465 1_565 ? O2 K1 O3 137.95(4) 1_455 1_565 ? O1 K1 O3 69.04(3) 2_675 1_565 ? O3 K1 O3 143.95(4) . 1_565 ? O2 K1 O3 95.41(3) . 1_565 ? O1 K1 F2 100.21(3) 1_465 1_565 ? O2 K1 F2 126.16(3) 1_455 1_565 ? O1 K1 F2 103.08(3) 2_675 1_565 ? O3 K1 F2 104.88(3) . 1_565 ? O2 K1 F2 65.51(3) . 1_565 ? O3 K1 F2 55.24(3) 1_565 1_565 ? O1 K1 O3 69.77(3) 1_465 2_575 ? O2 K1 O3 71.40(3) 1_455 2_575 ? O1 K1 O3 60.75(4) 2_675 2_575 ? O3 K1 O3 89.73(3) . 2_575 ? O2 K1 O3 117.00(3) . 2_575 ? O3 K1 O3 104.07(3) 1_565 2_575 ? F2 K1 O3 158.76(3) 1_565 2_575 ? O1 K1 F1 54.74(3) 1_465 1_465 ? O2 K1 F1 79.65(3) 1_455 1_465 ? O1 K1 F1 134.95(4) 2_675 1_465 ? O3 K1 F1 132.49(3) . 1_465 ? O2 K1 F1 121.45(3) . 1_465 ? O3 K1 F1 67.20(3) 1_565 1_465 ? F2 K1 F1 58.76(3) 1_565 1_465 ? O3 K1 F1 121.38(3) 2_575 1_465 ? O1 K1 F4 130.63(3) 1_465 . ? O2 K1 F4 83.72(3) 1_455 . ? O1 K1 F4 130.25(3) 2_675 . ? O3 K1 F4 59.27(3) . . ? O2 K1 F4 57.66(3) . . ? O3 K1 F4 111.74(3) 1_565 . ? F2 K1 F4 56.53(3) 1_565 . ? O3 K1 F4 144.06(3) 2_575 . ? F1 K1 F4 77.11(3) 1_465 . ? O1 K1 S1 175.16(3) 1_465 . ? O2 K1 S1 100.73(3) 1_455 . ? O1 K1 S1 82.15(3) 2_675 . ? O3 K1 S1 24.48(2) . . ? O2 K1 S1 24.81(2) . . ? O3 K1 S1 120.14(3) 1_565 . ? F2 K1 S1 84.32(3) 1_565 . ? O3 K1 S1 105.38(3) 2_575 . ? F1 K1 S1 129.83(2) 1_465 . ? F4 K1 S1 53.47(2) . . ? O1 K1 K1 48.57(3) 1_465 2_585 ? O2 K1 K1 109.91(3) 1_455 2_585 ? O1 K1 K1 46.51(3) 2_675 2_585 ? O3 K1 K1 130.57(3) . 2_585 ? O2 K1 K1 116.54(3) . 2_585 ? O3 K1 K1 52.35(2) 1_565 2_585 ? F2 K1 K1 107.43(3) 1_565 2_585 ? O3 K1 K1 51.72(3) 2_575 2_585 ? F1 K1 K1 96.40(3) 1_465 2_585 ? F4 K1 K1 163.86(3) . 2_585 ? S1 K1 K1 128.524(19) . 2_585 ? O1 S1 O2 115.39(7) . . ? O1 S1 O3 114.84(7) . . ? O2 S1 O3 113.82(7) . . ? O1 S1 C1 102.63(7) . . ? O2 S1 C1 104.39(7) . . ? O3 S1 C1 103.64(7) . . ? O1 S1 K1 145.71(5) . . ? O2 S1 K1 59.37(5) . . ? O3 S1 K1 54.70(5) . . ? C1 S1 K1 111.52(5) . . ? S1 O1 K1 141.43(7) . 1_645 ? S1 O1 K1 127.98(7) . 2_675 ? K1 O1 K1 84.93(4) 1_645 2_675 ? S1 O2 K1 136.12(7) . 1_655 ? S1 O2 K1 95.82(6) . . ? K1 O2 K1 124.52(4) 1_655 . ? S1 O3 K1 100.82(6) . . ? S1 O3 K1 113.72(6) . 1_545 ? K1 O3 K1 143.95(4) . 1_545 ? S1 O3 K1 129.65(7) . 2_575 ? K1 O3 K1 90.27(3) . 2_575 ? K1 O3 K1 75.93(3) 1_545 2_575 ? F1 C1 F2 107.64(13) . . ? F1 C1 C2 108.53(12) . . ? F2 C1 C2 108.59(13) . . ? F1 C1 S1 108.47(11) . . ? F2 C1 S1 108.31(10) . . ? C2 C1 S1 115.05(11) . . ? F3 C2 F4 108.37(14) . . ? F3 C2 C1 108.65(13) . . ? F4 C2 C1 108.73(13) . . ? F3 C2 C3 108.65(13) . . ? F4 C2 C3 107.89(14) . . ? C1 C2 C3 114.42(14) . . ? F6 C3 F5 108.68(15) . . ? F6 C3 C4 107.74(16) . . ? F5 C3 C4 107.48(15) . . ? F6 C3 C2 108.98(13) . . ? F5 C3 C2 109.32(15) . . ? C4 C3 C2 114.50(15) . . ? F8 C4 F7 109.25(18) . . ? F8 C4 F9 108.45(19) . . ? F7 C4 F9 108.40(17) . . ? F8 C4 C3 110.58(17) . . ? F7 C4 C3 110.81(17) . . ? F9 C4 C3 109.30(17) . . ? C1 F1 K1 116.63(9) . 1_645 ? C1 F2 K1 127.53(9) . 1_545 ? C2 F4 K1 134.04(9) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 K1 S1 O1 29.4(3) 1_465 . . . ? O2 K1 S1 O1 104.34(9) 1_455 . . . ? O1 K1 S1 O1 -25.80(11) 2_675 . . . ? O3 K1 S1 O1 82.85(11) . . . . ? O2 K1 S1 O1 -90.94(11) . . . . ? O3 K1 S1 O1 -85.95(9) 1_565 . . . ? F2 K1 S1 O1 -129.88(9) 1_565 . . . ? O3 K1 S1 O1 30.87(9) 2_575 . . . ? F1 K1 S1 O1 -170.26(9) 1_465 . . . ? F4 K1 S1 O1 178.15(9) . . . . ? K1 K1 S1 O1 -22.09(10) 2_585 . . . ? O1 K1 S1 O2 120.4(4) 1_465 . . . ? O2 K1 S1 O2 -164.73(8) 1_455 . . . ? O1 K1 S1 O2 65.14(6) 2_675 . . . ? O3 K1 S1 O2 173.78(8) . . . . ? O3 K1 S1 O2 4.98(6) 1_565 . . . ? F2 K1 S1 O2 -38.94(6) 1_565 . . . ? O3 K1 S1 O2 121.81(6) 2_575 . . . ? F1 K1 S1 O2 -79.32(6) 1_465 . . . ? F4 K1 S1 O2 -90.92(6) . . . . ? K1 K1 S1 O2 68.84(6) 2_585 . . . ? O1 K1 S1 O3 -53.4(4) 1_465 . . . ? O2 K1 S1 O3 21.49(6) 1_455 . . . ? O1 K1 S1 O3 -108.64(6) 2_675 . . . ? O2 K1 S1 O3 -173.78(8) . . . . ? O3 K1 S1 O3 -168.80(8) 1_565 . . . ? F2 K1 S1 O3 147.28(6) 1_565 . . . ? O3 K1 S1 O3 -51.97(8) 2_575 . . . ? F1 K1 S1 O3 106.90(7) 1_465 . . . ? F4 K1 S1 O3 95.30(6) . . . . ? K1 K1 S1 O3 -104.94(6) 2_585 . . . ? O1 K1 S1 C1 -145.2(4) 1_465 . . . ? O2 K1 S1 C1 -70.31(6) 1_455 . . . ? O1 K1 S1 C1 159.56(6) 2_675 . . . ? O3 K1 S1 C1 -91.80(8) . . . . ? O2 K1 S1 C1 94.42(8) . . . . ? O3 K1 S1 C1 99.40(6) 1_565 . . . ? F2 K1 S1 C1 55.47(6) 1_565 . . . ? O3 K1 S1 C1 -143.77(6) 2_575 . . . ? F1 K1 S1 C1 15.09(6) 1_465 . . . ? F4 K1 S1 C1 3.50(6) . . . . ? K1 K1 S1 C1 163.26(6) 2_585 . . . ? O2 S1 O1 K1 103.93(12) . . . 1_645 ? O3 S1 O1 K1 -120.64(11) . . . 1_645 ? C1 S1 O1 K1 -8.92(13) . . . 1_645 ? K1 S1 O1 K1 176.18(4) . . . 1_645 ? O2 S1 O1 K1 -39.10(10) . . . 2_675 ? O3 S1 O1 K1 96.33(9) . . . 2_675 ? C1 S1 O1 K1 -151.95(7) . . . 2_675 ? K1 S1 O1 K1 33.15(13) . . . 2_675 ? O1 S1 O2 K1 -16.65(12) . . . 1_655 ? O3 S1 O2 K1 -152.53(9) . . . 1_655 ? C1 S1 O2 K1 95.17(10) . . . 1_655 ? K1 S1 O2 K1 -158.07(11) . . . 1_655 ? O1 S1 O2 K1 141.43(6) . . . . ? O3 S1 O2 K1 5.55(7) . . . . ? C1 S1 O2 K1 -106.75(6) . . . . ? O1 K1 O2 S1 -169.13(7) 1_465 . . . ? O2 K1 O2 S1 18.31(10) 1_455 . . . ? O1 K1 O2 S1 -109.64(6) 2_675 . . . ? O3 K1 O2 S1 -3.40(5) . . . . ? O3 K1 O2 S1 -175.67(6) 1_565 . . . ? F2 K1 O2 S1 136.58(6) 1_565 . . . ? O3 K1 O2 S1 -66.87(6) 2_575 . . . ? F1 K1 O2 S1 117.80(5) 1_465 . . . ? F4 K1 O2 S1 71.97(5) . . . . ? K1 K1 O2 S1 -125.36(5) 2_585 . . . ? O1 K1 O2 K1 -7.44(13) 1_465 . . 1_655 ? O2 K1 O2 K1 180.0 1_455 . . 1_655 ? O1 K1 O2 K1 52.06(5) 2_675 . . 1_655 ? O3 K1 O2 K1 158.29(7) . . . 1_655 ? O3 K1 O2 K1 -13.98(6) 1_565 . . 1_655 ? F2 K1 O2 K1 -61.73(5) 1_565 . . 1_655 ? O3 K1 O2 K1 94.82(5) 2_575 . . 1_655 ? F1 K1 O2 K1 -80.50(6) 1_465 . . 1_655 ? F4 K1 O2 K1 -126.34(6) . . . 1_655 ? S1 K1 O2 K1 161.69(10) . . . 1_655 ? K1 K1 O2 K1 36.34(6) 2_585 . . 1_655 ? O1 S1 O3 K1 -141.98(6) . . . . ? O2 S1 O3 K1 -5.85(8) . . . . ? C1 S1 O3 K1 106.90(6) . . . . ? O1 S1 O3 K1 48.60(9) . . . 1_545 ? O2 S1 O3 K1 -175.27(6) . . . 1_545 ? C1 S1 O3 K1 -62.52(7) . . . 1_545 ? K1 S1 O3 K1 -169.43(8) . . . 1_545 ? O1 S1 O3 K1 -42.51(11) . . . 2_575 ? O2 S1 O3 K1 93.62(9) . . . 2_575 ? C1 S1 O3 K1 -153.63(8) . . . 2_575 ? K1 S1 O3 K1 99.47(8) . . . 2_575 ? O1 K1 O3 S1 171.59(6) 1_465 . . . ? O2 K1 O3 S1 -158.40(6) 1_455 . . . ? O1 K1 O3 S1 69.83(6) 2_675 . . . ? O2 K1 O3 S1 3.44(5) . . . . ? O3 K1 O3 S1 16.59(12) 1_565 . . . ? F2 K1 O3 S1 -33.82(6) 1_565 . . . ? O3 K1 O3 S1 130.58(7) 2_575 . . . ? F1 K1 O3 S1 -94.85(6) 1_465 . . . ? F4 K1 O3 S1 -68.56(5) . . . . ? K1 K1 O3 S1 95.63(6) 2_585 . . . ? O1 K1 O3 K1 -24.99(13) 1_465 . . 1_545 ? O2 K1 O3 K1 5.02(7) 1_455 . . 1_545 ? O1 K1 O3 K1 -126.76(7) 2_675 . . 1_545 ? O2 K1 O3 K1 166.86(10) . . . 1_545 ? O3 K1 O3 K1 180.0 1_565 . . 1_545 ? F2 K1 O3 K1 129.59(7) 1_565 . . 1_545 ? O3 K1 O3 K1 -66.01(7) 2_575 . . 1_545 ? F1 K1 O3 K1 68.56(9) 1_465 . . 1_545 ? F4 K1 O3 K1 94.86(8) . . . 1_545 ? S1 K1 O3 K1 163.41(12) . . . 1_545 ? K1 K1 O3 K1 -100.95(8) 2_585 . . 1_545 ? O1 K1 O3 K1 41.01(9) 1_465 . . 2_575 ? O2 K1 O3 K1 71.02(3) 1_455 . . 2_575 ? O1 K1 O3 K1 -60.75(4) 2_675 . . 2_575 ? O2 K1 O3 K1 -127.14(5) . . . 2_575 ? O3 K1 O3 K1 -114.00(7) 1_565 . . 2_575 ? F2 K1 O3 K1 -164.40(3) 1_565 . . 2_575 ? O3 K1 O3 K1 0.0 2_575 . . 2_575 ? F1 K1 O3 K1 134.57(4) 1_465 . . 2_575 ? F4 K1 O3 K1 160.86(4) . . . 2_575 ? S1 K1 O3 K1 -130.58(7) . . . 2_575 ? K1 K1 O3 K1 -34.95(4) 2_585 . . 2_575 ? O1 S1 C1 F1 35.59(12) . . . . ? O2 S1 C1 F1 -85.16(12) . . . . ? O3 S1 C1 F1 155.42(10) . . . . ? K1 S1 C1 F1 -147.50(9) . . . . ? O1 S1 C1 F2 -80.97(12) . . . . ? O2 S1 C1 F2 158.28(11) . . . . ? O3 S1 C1 F2 38.86(13) . . . . ? K1 S1 C1 F2 95.94(11) . . . . ? O1 S1 C1 C2 157.33(12) . . . . ? O2 S1 C1 C2 36.58(13) . . . . ? O3 S1 C1 C2 -82.84(12) . . . . ? K1 S1 C1 C2 -25.76(13) . . . . ? F1 C1 C2 F3 47.45(17) . . . . ? F2 C1 C2 F3 164.19(13) . . . . ? S1 C1 C2 F3 -74.26(15) . . . . ? F1 C1 C2 F4 165.19(13) . . . . ? F2 C1 C2 F4 -78.06(16) . . . . ? S1 C1 C2 F4 43.49(16) . . . . ? F1 C1 C2 C3 -74.14(17) . . . . ? F2 C1 C2 C3 42.60(18) . . . . ? S1 C1 C2 C3 164.15(12) . . . . ? F3 C2 C3 F6 160.99(14) . . . . ? F4 C2 C3 F6 43.71(18) . . . . ? C1 C2 C3 F6 -77.42(18) . . . . ? F3 C2 C3 F5 -80.36(17) . . . . ? F4 C2 C3 F5 162.36(13) . . . . ? C1 C2 C3 F5 41.23(18) . . . . ? F3 C2 C3 C4 40.3(2) . . . . ? F4 C2 C3 C4 -77.01(18) . . . . ? C1 C2 C3 C4 161.86(16) . . . . ? F6 C3 C4 F8 -70.4(2) . . . . ? F5 C3 C4 F8 172.66(16) . . . . ? C2 C3 C4 F8 51.0(2) . . . . ? F6 C3 C4 F7 168.33(16) . . . . ? F5 C3 C4 F7 51.4(2) . . . . ? C2 C3 C4 F7 -70.3(2) . . . . ? F6 C3 C4 F9 48.9(2) . . . . ? F5 C3 C4 F9 -68.0(2) . . . . ? C2 C3 C4 F9 170.34(17) . . . . ? F2 C1 F1 K1 71.73(13) . . . 1_645 ? C2 C1 F1 K1 -170.92(9) . . . 1_645 ? S1 C1 F1 K1 -45.27(12) . . . 1_645 ? F1 C1 F2 K1 -114.97(11) . . . 1_545 ? C2 C1 F2 K1 127.71(11) . . . 1_545 ? S1 C1 F2 K1 2.12(16) . . . 1_545 ? F3 C2 F4 K1 68.10(16) . . . . ? C1 C2 F4 K1 -49.83(17) . . . . ? C3 C2 F4 K1 -174.44(9) . . . . ? O1 K1 F4 C2 -156.53(12) 1_465 . . . ? O2 K1 F4 C2 135.12(13) 1_455 . . . ? O1 K1 F4 C2 -5.00(14) 2_675 . . . ? O3 K1 F4 C2 55.47(12) . . . . ? O2 K1 F4 C2 -2.99(12) . . . . ? O3 K1 F4 C2 -85.38(13) 1_565 . . . ? F2 K1 F4 C2 -83.22(13) 1_565 . . . ? O3 K1 F4 C2 89.43(13) 2_575 . . . ? F1 K1 F4 C2 -144.10(13) 1_465 . . . ? S1 K1 F4 C2 26.79(12) . . . . ? K1 K1 F4 C2 -76.41(16) 2_585 . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.533 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.074 # Attachment 'KC4F9SO3_CH3CN.CIF' data_vorma _database_code_depnum_ccdc_archive 'CCDC 737957' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Potasium nonafluorobutylsulfonate acetonitril solvate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H3 F9 K N O3 S' _chemical_formula_weight 379.25 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' K K 0.2009 0.2494 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.493(2) _cell_length_b 8.5886(15) _cell_length_c 30.962(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.036(19) _cell_angle_gamma 90.00 _cell_volume 2514.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 879 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .7 _exptl_crystal_size_mid .55 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15250 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 30.54 _reflns_number_total 3813 _reflns_number_gt 3071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _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^)+(0.0977P)^2^+1.9274P] 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 3813 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 K1 K 0.76127(5) 0.27263(6) 0.752079(14) 0.03053(14) Uani 1 1 d . . . C1 C 0.50152(19) 0.0206(2) 0.62580(6) 0.0203(3) Uani 1 1 d . . . C2 C 0.3524(2) 0.0139(2) 0.60138(6) 0.0221(3) Uani 1 1 d . . . C3 C 0.3512(2) -0.0061(3) 0.55156(7) 0.0330(5) Uani 1 1 d . . . C4 C 0.2041(3) 0.0025(3) 0.52603(8) 0.0439(6) Uani 1 1 d . . . C1L C 0.5218(3) 0.5132(3) 0.67517(9) 0.0360(5) Uani 1 1 d . . . C2L C 0.4292(3) 0.5218(3) 0.63558(9) 0.0425(6) Uani 1 1 d . . . H2L1 H 0.3675 0.6099 0.6368 0.064 Uiso 1 1 calc R . . H2L2 H 0.3738 0.4283 0.6323 0.064 Uiso 1 1 calc R . . H2L3 H 0.4847 0.5328 0.6113 0.064 Uiso 1 1 calc R . . F1 F 0.56693(13) 0.14975(16) 0.61321(4) 0.0346(3) Uani 1 1 d . . . F2 F 0.57629(13) -0.10389(16) 0.61384(4) 0.0336(3) Uani 1 1 d . . . F3 F 0.28308(14) 0.14505(16) 0.60907(5) 0.0385(3) Uani 1 1 d . . . F4 F 0.28045(13) -0.10609(17) 0.61638(4) 0.0365(3) Uani 1 1 d . . . F5 F 0.4322(2) 0.1018(3) 0.53572(5) 0.0665(6) Uani 1 1 d . . . F6 F 0.4044(2) -0.1467(2) 0.54301(5) 0.0652(6) Uani 1 1 d . . . F7 F 0.1456(2) 0.1389(3) 0.53051(7) 0.0858(7) Uani 1 1 d . . . F8 F 0.1193(2) -0.1033(3) 0.53895(7) 0.0832(7) Uani 1 1 d . . . F9 F 0.2174(2) -0.0181(3) 0.48430(5) 0.0705(6) Uani 1 1 d . . . N1L N 0.5957(3) 0.5080(3) 0.70587(9) 0.0534(6) Uani 1 1 d . . . O1 O 0.65862(16) 0.03867(18) 0.69748(5) 0.0312(3) Uani 1 1 d . . . O2 O 0.42522(18) 0.1552(2) 0.69511(5) 0.0384(4) Uani 1 1 d . . . O3 O 0.45311(18) -0.12677(19) 0.69676(5) 0.0347(4) Uani 1 1 d . . . S1 S 0.50850(5) 0.02191(6) 0.685504(14) 0.02175(14) Uani 1 1 d . . . 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 K1 0.0349(3) 0.0297(2) 0.0275(2) 0.00013(15) 0.00557(17) -0.00948(17) C1 0.0174(8) 0.0230(8) 0.0208(8) -0.0004(6) 0.0035(6) -0.0007(6) C2 0.0186(8) 0.0261(9) 0.0217(8) 0.0002(6) 0.0023(6) 0.0006(6) C3 0.0275(10) 0.0472(12) 0.0240(9) -0.0016(8) 0.0001(8) 0.0012(8) C4 0.0377(13) 0.0621(16) 0.0299(11) -0.0005(10) -0.0088(10) 0.0000(11) C1L 0.0293(11) 0.0290(10) 0.0498(13) -0.0027(9) 0.0045(10) -0.0014(8) C2L 0.0338(12) 0.0462(13) 0.0465(14) -0.0023(10) -0.0019(10) 0.0020(10) F1 0.0326(6) 0.0400(7) 0.0308(6) 0.0096(5) 0.0010(5) -0.0172(5) F2 0.0271(6) 0.0425(7) 0.0310(6) -0.0111(5) 0.0015(5) 0.0141(5) F3 0.0324(7) 0.0379(7) 0.0436(7) -0.0102(6) -0.0054(5) 0.0162(5) F4 0.0284(6) 0.0431(7) 0.0372(7) 0.0094(5) -0.0017(5) -0.0153(5) F5 0.0573(10) 0.1123(16) 0.0294(7) 0.0150(9) 0.0014(7) -0.0383(11) F6 0.0693(12) 0.0800(13) 0.0433(9) -0.0303(8) -0.0120(8) 0.0347(10) F7 0.0844(14) 0.0948(16) 0.0697(13) -0.0135(11) -0.0413(11) 0.0467(13) F8 0.0607(12) 0.1224(19) 0.0611(11) 0.0202(12) -0.0260(9) -0.0466(13) F9 0.0631(12) 0.1175(18) 0.0280(8) -0.0055(8) -0.0131(7) -0.0010(11) N1L 0.0457(14) 0.0542(14) 0.0584(15) 0.0041(11) -0.0072(12) -0.0026(10) O1 0.0244(7) 0.0431(9) 0.0251(7) -0.0010(6) -0.0039(5) -0.0032(6) O2 0.0431(9) 0.0410(9) 0.0317(8) -0.0097(7) 0.0074(7) 0.0137(7) O3 0.0406(9) 0.0369(8) 0.0267(7) 0.0077(6) 0.0038(6) -0.0104(7) S1 0.0214(2) 0.0257(2) 0.0182(2) -0.00090(14) 0.00216(16) -0.00037(16) _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 K1 O2 2.7078(17) 2_656 ? K1 O3 2.7466(17) 3 ? K1 O1 2.7487(16) . ? K1 O1 2.8337(16) 4_656 ? K1 N1L 2.865(3) . ? K1 N1L 2.897(3) 4_646 ? K1 O3 3.1391(19) 4_656 ? K1 S1 3.5148(8) 4_656 ? K1 S1 3.7115(9) . ? K1 K1 4.3010(7) 4_656 ? K1 K1 4.3010(7) 4_646 ? K1 K1 4.5457(14) 2_756 ? C1 F1 1.346(2) . ? C1 F2 1.353(2) . ? C1 C2 1.546(3) . ? C1 S1 1.8440(19) . ? C2 F3 1.337(2) . ? C2 F4 1.341(2) . ? C2 C3 1.551(3) . ? C3 F5 1.326(3) . ? C3 F6 1.344(3) . ? C3 C4 1.545(3) . ? C4 F8 1.300(4) . ? C4 F7 1.309(3) . ? C4 F9 1.321(3) . ? C1L N1L 1.131(4) . ? C1L C2L 1.446(4) . ? C2L H2L1 0.9600 . ? C2L H2L2 0.9600 . ? C2L H2L3 0.9600 . ? N1L K1 2.897(3) 4_656 ? O1 S1 1.4479(16) . ? O1 K1 2.8337(16) 4_646 ? O2 S1 1.4374(16) . ? O2 K1 2.7078(16) 2_656 ? O3 S1 1.4356(16) . ? O3 K1 2.7466(16) 3_445 ? O3 K1 3.1391(19) 4_646 ? S1 K1 3.5148(8) 4_646 ? 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 O2 K1 O3 176.45(5) 2_656 3 ? O2 K1 O1 83.33(5) 2_656 . ? O3 K1 O1 93.73(5) 3 . ? O2 K1 O1 97.21(5) 2_656 4_656 ? O3 K1 O1 85.96(5) 3 4_656 ? O1 K1 O1 172.70(4) . 4_656 ? O2 K1 N1L 101.84(7) 2_656 . ? O3 K1 N1L 80.29(7) 3 . ? O1 K1 N1L 93.40(6) . . ? O1 K1 N1L 79.35(6) 4_656 . ? O2 K1 N1L 75.05(7) 2_656 4_646 ? O3 K1 N1L 102.52(7) 3 4_646 ? O1 K1 N1L 80.20(6) . 4_646 ? O1 K1 N1L 107.00(6) 4_656 4_646 ? N1L K1 N1L 173.11(7) . 4_646 ? O2 K1 O3 112.30(5) 2_656 4_656 ? O3 K1 O3 68.74(5) 3 4_656 ? O1 K1 O3 139.06(5) . 4_656 ? O1 K1 O3 47.30(4) 4_656 4_656 ? N1L K1 O3 118.00(6) . 4_656 ? N1L K1 O3 68.85(6) 4_646 4_656 ? O2 K1 S1 107.62(4) 2_656 4_656 ? O3 K1 S1 74.75(4) 3 4_656 ? O1 K1 S1 162.40(4) . 4_656 ? O1 K1 S1 23.36(3) 4_656 4_656 ? N1L K1 S1 97.60(5) . 4_656 ? N1L K1 S1 89.23(5) 4_646 4_656 ? O3 K1 S1 24.08(3) 4_656 4_656 ? O2 K1 S1 72.19(4) 2_656 . ? O3 K1 S1 105.54(4) 3 . ? O1 K1 S1 19.49(3) . . ? O1 K1 S1 154.56(4) 4_656 . ? N1L K1 S1 80.35(6) . . ? N1L K1 S1 92.81(5) 4_646 . ? O3 K1 S1 158.07(3) 4_656 . ? S1 K1 S1 177.813(19) 4_656 . ? O2 K1 K1 110.88(4) 2_656 4_656 ? O3 K1 K1 72.62(4) 3 4_656 ? O1 K1 K1 134.22(4) . 4_656 ? O1 K1 K1 38.89(3) 4_656 4_656 ? N1L K1 K1 42.01(5) . 4_656 ? N1L K1 K1 144.77(5) 4_646 4_656 ? O3 K1 K1 77.22(3) 4_656 4_656 ? S1 K1 K1 55.610(14) 4_656 4_656 ? S1 K1 K1 122.32(2) . 4_656 ? O2 K1 K1 67.22(4) 2_656 4_646 ? O3 K1 K1 109.23(4) 3 4_646 ? O1 K1 K1 40.33(3) . 4_646 ? O1 K1 K1 146.29(4) 4_656 4_646 ? N1L K1 K1 131.74(6) . 4_646 ? N1L K1 K1 41.44(5) 4_646 4_646 ? O3 K1 K1 109.17(3) 4_656 4_646 ? S1 K1 K1 130.66(2) 4_656 4_646 ? S1 K1 K1 51.396(13) . 4_646 ? K1 K1 K1 173.61(2) 4_656 4_646 ? O2 K1 K1 136.34(4) 2_656 2_756 ? O3 K1 K1 42.69(4) 3 2_756 ? O1 K1 K1 106.45(4) . 2_756 ? O1 K1 K1 78.20(4) 4_656 2_756 ? N1L K1 K1 119.38(6) . 2_756 ? N1L K1 K1 65.39(6) 4_646 2_756 ? O3 K1 K1 36.39(3) 4_656 2_756 ? S1 K1 K1 56.090(16) 4_656 2_756 ? S1 K1 K1 125.588(18) . 2_756 ? K1 K1 K1 92.652(12) 4_656 2_756 ? K1 K1 K1 92.652(12) 4_646 2_756 ? F1 C1 F2 107.80(15) . . ? F1 C1 C2 108.37(14) . . ? F2 C1 C2 108.45(14) . . ? F1 C1 S1 107.96(12) . . ? F2 C1 S1 107.79(12) . . ? C2 C1 S1 116.18(13) . . ? F3 C2 F4 108.19(16) . . ? F3 C2 C1 108.98(15) . . ? F4 C2 C1 109.36(15) . . ? F3 C2 C3 108.02(16) . . ? F4 C2 C3 107.44(16) . . ? C1 C2 C3 114.66(17) . . ? F5 C3 F6 108.3(2) . . ? F5 C3 C4 107.8(2) . . ? F6 C3 C4 106.3(2) . . ? F5 C3 C2 109.66(18) . . ? F6 C3 C2 108.96(17) . . ? C4 C3 C2 115.5(2) . . ? F8 C4 F7 108.2(3) . . ? F8 C4 F9 108.8(2) . . ? F7 C4 F9 107.6(2) . . ? F8 C4 C3 111.4(2) . . ? F7 C4 C3 111.2(2) . . ? F9 C4 C3 109.5(2) . . ? N1L C1L C2L 178.9(3) . . ? C1L C2L H2L1 109.5 . . ? C1L C2L H2L2 109.5 . . ? H2L1 C2L H2L2 109.5 . . ? C1L C2L H2L3 109.5 . . ? H2L1 C2L H2L3 109.5 . . ? H2L2 C2L H2L3 109.5 . . ? C1L N1L K1 136.0(2) . . ? C1L N1L K1 125.3(2) . 4_656 ? K1 N1L K1 96.55(8) . 4_656 ? S1 O1 K1 121.20(9) . . ? S1 O1 K1 105.75(8) . 4_646 ? K1 O1 K1 100.78(5) . 4_646 ? S1 O2 K1 145.31(10) . 2_656 ? S1 O3 K1 135.09(10) . 3_445 ? S1 O3 K1 92.79(8) . 4_646 ? K1 O3 K1 100.92(5) 3_445 4_646 ? O3 S1 O2 116.01(11) . . ? O3 S1 O1 113.55(10) . . ? O2 S1 O1 114.50(10) . . ? O3 S1 C1 104.85(9) . . ? O2 S1 C1 103.91(9) . . ? O1 S1 C1 101.85(9) . . ? O3 S1 K1 63.13(7) . 4_646 ? O2 S1 K1 134.28(7) . 4_646 ? O1 S1 K1 50.89(6) . 4_646 ? C1 S1 K1 120.89(6) . 4_646 ? O3 S1 K1 127.88(7) . . ? O2 S1 K1 76.31(7) . . ? O1 S1 K1 39.31(6) . . ? C1 S1 K1 121.66(6) . . ? K1 S1 K1 72.994(18) 4_646 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 C1 C2 F3 -56.2(2) . . . . ? F2 C1 C2 F3 -172.99(15) . . . . ? S1 C1 C2 F3 65.47(18) . . . . ? F1 C1 C2 F4 -174.31(14) . . . . ? F2 C1 C2 F4 68.92(19) . . . . ? S1 C1 C2 F4 -52.61(19) . . . . ? F1 C1 C2 C3 65.0(2) . . . . ? F2 C1 C2 C3 -51.8(2) . . . . ? S1 C1 C2 C3 -173.34(14) . . . . ? F3 C2 C3 F5 69.3(2) . . . . ? F4 C2 C3 F5 -174.22(18) . . . . ? C1 C2 C3 F5 -52.4(2) . . . . ? F3 C2 C3 F6 -172.30(17) . . . . ? F4 C2 C3 F6 -55.8(2) . . . . ? C1 C2 C3 F6 66.0(2) . . . . ? F3 C2 C3 C4 -52.7(3) . . . . ? F4 C2 C3 C4 63.8(2) . . . . ? C1 C2 C3 C4 -174.44(19) . . . . ? F5 C3 C4 F8 178.2(2) . . . . ? F6 C3 C4 F8 62.2(3) . . . . ? C2 C3 C4 F8 -58.8(3) . . . . ? F5 C3 C4 F7 -60.9(3) . . . . ? F6 C3 C4 F7 -176.9(2) . . . . ? C2 C3 C4 F7 62.1(3) . . . . ? F5 C3 C4 F9 57.8(3) . . . . ? F6 C3 C4 F9 -58.2(3) . . . . ? C2 C3 C4 F9 -179.2(2) . . . . ? C2L C1L N1L K1 -116(17) . . . . ? C2L C1L N1L K1 44(17) . . . 4_656 ? O2 K1 N1L C1L -88.7(3) 2_656 . . . ? O3 K1 N1L C1L 88.4(3) 3 . . . ? O1 K1 N1L C1L -4.8(3) . . . . ? O1 K1 N1L C1L 176.1(3) 4_656 . . . ? N1L K1 N1L C1L -26.3(4) 4_646 . . . ? O3 K1 N1L C1L 147.9(3) 4_656 . . . ? S1 K1 N1L C1L 161.4(3) 4_656 . . . ? S1 K1 N1L C1L -19.3(3) . . . . ? K1 K1 N1L C1L 163.2(4) 4_656 . . . ? K1 K1 N1L C1L -18.7(4) 4_646 . . . ? K1 K1 N1L C1L 106.2(3) 2_756 . . . ? O2 K1 N1L K1 108.14(8) 2_656 . . 4_656 ? O3 K1 N1L K1 -74.75(7) 3 . . 4_656 ? O1 K1 N1L K1 -167.97(8) . . . 4_656 ? O1 K1 N1L K1 12.92(7) 4_656 . . 4_656 ? N1L K1 N1L K1 170.55(19) 4_646 . . 4_656 ? O3 K1 N1L K1 -15.26(10) 4_656 . . 4_656 ? S1 K1 N1L K1 -1.74(8) 4_656 . . 4_656 ? S1 K1 N1L K1 177.50(8) . . . 4_656 ? K1 K1 N1L K1 178.08(3) 4_646 . . 4_656 ? K1 K1 N1L K1 -56.93(9) 2_756 . . 4_656 ? O2 K1 O1 S1 53.68(10) 2_656 . . . ? O3 K1 O1 S1 -128.34(10) 3 . . . ? O1 K1 O1 S1 -41.0(2) 4_656 . . . ? N1L K1 O1 S1 -47.86(11) . . . . ? N1L K1 O1 S1 129.59(11) 4_646 . . . ? O3 K1 O1 S1 170.30(8) 4_656 . . . ? S1 K1 O1 S1 -176.56(5) 4_656 . . . ? K1 K1 O1 S1 -59.08(12) 4_656 . . . ? K1 K1 O1 S1 116.00(12) 4_646 . . . ? K1 K1 O1 S1 -169.85(8) 2_756 . . . ? O2 K1 O1 K1 -62.32(5) 2_656 . . 4_646 ? O3 K1 O1 K1 115.67(5) 3 . . 4_646 ? O1 K1 O1 K1 -157.01(19) 4_656 . . 4_646 ? N1L K1 O1 K1 -163.85(7) . . . 4_646 ? N1L K1 O1 K1 13.59(7) 4_646 . . 4_646 ? O3 K1 O1 K1 54.30(8) 4_656 . . 4_646 ? S1 K1 O1 K1 67.44(13) 4_656 . . 4_646 ? S1 K1 O1 K1 -116.00(12) . . . 4_646 ? K1 K1 O1 K1 -175.08(3) 4_656 . . 4_646 ? K1 K1 O1 K1 74.15(5) 2_756 . . 4_646 ? K1 O3 S1 O2 -20.07(17) 3_445 . . . ? K1 O3 S1 O2 -128.59(8) 4_646 . . . ? K1 O3 S1 O1 115.66(13) 3_445 . . . ? K1 O3 S1 O1 7.14(9) 4_646 . . . ? K1 O3 S1 C1 -134.03(11) 3_445 . . . ? K1 O3 S1 C1 117.45(7) 4_646 . . . ? K1 O3 S1 K1 108.52(12) 3_445 . . 4_646 ? K1 O3 S1 K1 72.57(14) 3_445 . . . ? K1 O3 S1 K1 -35.95(9) 4_646 . . . ? K1 O2 S1 O3 28.7(2) 2_656 . . . ? K1 O2 S1 O1 -106.65(18) 2_656 . . . ? K1 O2 S1 C1 143.15(16) 2_656 . . . ? K1 O2 S1 K1 -48.2(2) 2_656 . . 4_646 ? K1 O2 S1 K1 -97.10(17) 2_656 . . . ? K1 O1 S1 O3 -121.66(10) . . . . ? K1 O1 S1 O3 -8.21(11) 4_646 . . . ? K1 O1 S1 O2 14.75(13) . . . . ? K1 O1 S1 O2 128.20(9) 4_646 . . . ? K1 O1 S1 C1 126.19(9) . . . . ? K1 O1 S1 C1 -120.36(7) 4_646 . . . ? K1 O1 S1 K1 -113.45(10) . . . 4_646 ? K1 O1 S1 K1 113.45(10) 4_646 . . . ? F1 C1 S1 O3 -173.10(13) . . . . ? F2 C1 S1 O3 -56.89(15) . . . . ? C2 C1 S1 O3 64.99(15) . . . . ? F1 C1 S1 O2 64.69(15) . . . . ? F2 C1 S1 O2 -179.10(13) . . . . ? C2 C1 S1 O2 -57.22(15) . . . . ? F1 C1 S1 O1 -54.55(14) . . . . ? F2 C1 S1 O1 61.66(14) . . . . ? C2 C1 S1 O1 -176.46(13) . . . . ? F1 C1 S1 K1 -105.82(12) . . . 4_646 ? F2 C1 S1 K1 10.38(15) . . . 4_646 ? C2 C1 S1 K1 132.27(11) . . . 4_646 ? F1 C1 S1 K1 -17.63(15) . . . . ? F2 C1 S1 K1 98.58(12) . . . . ? C2 C1 S1 K1 -139.54(11) . . . . ? O2 K1 S1 O3 -41.50(10) 2_656 . . . ? O3 K1 S1 O3 135.65(12) 3 . . . ? O1 K1 S1 O3 81.31(13) . . . . ? O1 K1 S1 O3 -109.88(12) 4_656 . . . ? N1L K1 S1 O3 -147.35(11) . . . . ? N1L K1 S1 O3 31.82(11) 4_646 . . . ? O3 K1 S1 O3 64.12(17) 4_656 . . . ? S1 K1 S1 O3 -127.1(4) 4_656 . . . ? K1 K1 S1 O3 -145.37(9) 4_656 . . . ? K1 K1 S1 O3 33.20(9) 4_646 . . . ? K1 K1 S1 O3 93.30(9) 2_756 . . . ? O2 K1 S1 O2 70.99(6) 2_656 . . . ? O3 K1 S1 O2 -111.87(8) 3 . . . ? O1 K1 S1 O2 -166.21(12) . . . . ? O1 K1 S1 O2 2.60(11) 4_656 . . . ? N1L K1 S1 O2 -34.86(9) . . . . ? N1L K1 S1 O2 144.30(10) 4_646 . . . ? O3 K1 S1 O2 176.60(11) 4_656 . . . ? S1 K1 S1 O2 -14.6(4) 4_656 . . . ? K1 K1 S1 O2 -32.88(7) 4_656 . . . ? K1 K1 S1 O2 145.69(7) 4_646 . . . ? K1 K1 S1 O2 -154.22(7) 2_756 . . . ? O2 K1 S1 O1 -122.81(11) 2_656 . . . ? O3 K1 S1 O1 54.33(11) 3 . . . ? O1 K1 S1 O1 168.81(10) 4_656 . . . ? N1L K1 S1 O1 131.34(11) . . . . ? N1L K1 S1 O1 -49.49(11) 4_646 . . . ? O3 K1 S1 O1 -17.19(13) 4_656 . . . ? S1 K1 S1 O1 151.6(4) 4_656 . . . ? K1 K1 S1 O1 133.32(10) 4_656 . . . ? K1 K1 S1 O1 -48.11(10) 4_646 . . . ? K1 K1 S1 O1 11.99(10) 2_756 . . . ? O2 K1 S1 C1 169.06(8) 2_656 . . . ? O3 K1 S1 C1 -13.79(8) 3 . . . ? O1 K1 S1 C1 -68.13(12) . . . . ? O1 K1 S1 C1 100.68(11) 4_656 . . . ? N1L K1 S1 C1 63.21(9) . . . . ? N1L K1 S1 C1 -117.62(9) 4_646 . . . ? O3 K1 S1 C1 -85.32(11) 4_656 . . . ? S1 K1 S1 C1 83.5(4) 4_656 . . . ? K1 K1 S1 C1 65.19(7) 4_656 . . . ? K1 K1 S1 C1 -116.24(7) 4_646 . . . ? K1 K1 S1 C1 -56.14(7) 2_756 . . . ? O2 K1 S1 K1 -74.70(4) 2_656 . . 4_646 ? O3 K1 S1 K1 102.44(4) 3 . . 4_646 ? O1 K1 S1 K1 48.11(10) . . . 4_646 ? O1 K1 S1 K1 -143.09(8) 4_656 . . 4_646 ? N1L K1 S1 K1 179.45(6) . . . 4_646 ? N1L K1 S1 K1 -1.38(6) 4_646 . . 4_646 ? O3 K1 S1 K1 30.92(9) 4_656 . . 4_646 ? S1 K1 S1 K1 -160.3(4) 4_656 . . 4_646 ? K1 K1 S1 K1 -178.57(3) 4_656 . . 4_646 ? K1 K1 S1 K1 60.098(16) 2_756 . . 4_646 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.624 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.079 # Attachment 'Lic4F9SO3.CIF' data_orgvorlm _database_code_depnum_ccdc_archive 'CCDC 737958' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Lithium nonafluorobtylsulfonate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 F9 Li O4 S' _chemical_formula_weight 350.09 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' Li Li -0.0003 0.0001 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.323(5) _cell_length_b 5.580(5) _cell_length_c 17.527(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 97.885(5) _cell_angle_gamma 90.000(5) _cell_volume 1193.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.54 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .63 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (BRUKER-AXS)' _exptl_special_details ; 'SADABS (BRUKER-AXS) The ratio of Tmin/Tmax is provided by the program' ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13968 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.54 _reflns_number_total 3605 _reflns_number_gt 3069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _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^)+(0.0401P)^2^+0.3808P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3605 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Li1 Li 0.54469(15) 0.2646(3) 0.34693(11) 0.0219(4) Uani 1 1 d . . . C1 C 0.78565(8) 0.8124(2) 0.28828(6) 0.0200(2) Uani 1 1 d . . . C2 C 0.87098(8) 0.74663(19) 0.35864(6) 0.0199(2) Uani 1 1 d . . . C3 C 0.98755(8) 0.8471(2) 0.35406(7) 0.0216(2) Uani 1 1 d . . . C4 C 1.07994(10) 0.7351(2) 0.41166(8) 0.0299(3) Uani 1 1 d . . . C1L C 0.39832(10) 0.4262(3) 0.46252(8) 0.0360(3) Uani 1 1 d . . . H1L H 0.3680 0.3437 0.5035 0.043 Uiso 1 1 calc R . . H2L H 0.3444 0.4216 0.4167 0.043 Uiso 1 1 calc R . . C2L C 0.42249(12) 0.6821(3) 0.48547(8) 0.0378(3) Uani 1 1 d . . . H4L H 0.4487 0.7670 0.4433 0.045 Uiso 1 1 calc R . . H3L H 0.3558 0.7598 0.4963 0.045 Uiso 1 1 calc R . . F1 F 0.79835(6) 1.04356(14) 0.26973(5) 0.03171(18) Uani 1 1 d . . . F2 F 0.80468(6) 0.67634(16) 0.22824(4) 0.03456(19) Uani 1 1 d . . . F3 F 0.83682(6) 0.83174(15) 0.42297(4) 0.03226(18) Uani 1 1 d . . . F4 F 0.87766(6) 0.50701(13) 0.36393(5) 0.03330(18) Uani 1 1 d . . . F5 F 0.98768(6) 1.08298(13) 0.36827(5) 0.03105(17) Uani 1 1 d . . . F6 F 1.01311(6) 0.81188(15) 0.28284(4) 0.03006(17) Uani 1 1 d . . . F7 F 1.05446(8) 0.73911(18) 0.48238(5) 0.0448(2) Uani 1 1 d . . . F8 F 1.10065(7) 0.51202(15) 0.39303(6) 0.0438(2) Uani 1 1 d . . . F9 F 1.17113(6) 0.86212(18) 0.41042(6) 0.0496(3) Uani 1 1 d . . . O1 O 0.64006(7) 0.53188(15) 0.33517(6) 0.02747(19) Uani 1 1 d . . . O2 O 0.58523(7) 0.79044(18) 0.22471(5) 0.0312(2) Uani 1 1 d . . . O3 O 0.61820(7) 0.95820(15) 0.35322(5) 0.02684(18) Uani 1 1 d . . . O1L O 0.49641(7) 0.30705(17) 0.44761(5) 0.02862(19) Uani 1 1 d . . . S1 S 0.64153(2) 0.76818(5) 0.302144(16) 0.01942(7) Uani 1 1 d . . . 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 Li1 0.0215(8) 0.0214(9) 0.0226(9) -0.0011(7) 0.0026(7) 0.0006(7) C1 0.0180(4) 0.0227(5) 0.0195(5) 0.0008(4) 0.0032(4) 0.0001(4) C2 0.0182(4) 0.0193(5) 0.0220(5) 0.0011(4) 0.0026(4) 0.0000(4) C3 0.0187(4) 0.0202(5) 0.0256(5) -0.0012(4) 0.0024(4) -0.0007(4) C4 0.0216(5) 0.0281(6) 0.0378(7) 0.0014(5) -0.0039(5) -0.0009(4) C1L 0.0217(5) 0.0578(9) 0.0289(7) -0.0127(6) 0.0049(5) 0.0003(5) C2L 0.0383(7) 0.0483(8) 0.0250(6) -0.0044(6) -0.0019(5) 0.0198(6) F1 0.0250(3) 0.0284(4) 0.0411(4) 0.0165(3) 0.0023(3) -0.0030(3) F2 0.0255(3) 0.0532(5) 0.0256(4) -0.0140(3) 0.0055(3) 0.0029(3) F3 0.0250(3) 0.0515(5) 0.0208(4) -0.0033(3) 0.0047(3) 0.0002(3) F4 0.0246(3) 0.0195(4) 0.0535(5) 0.0094(3) -0.0024(3) -0.0008(3) F5 0.0295(3) 0.0185(3) 0.0440(5) -0.0026(3) 0.0011(3) -0.0031(3) F6 0.0236(3) 0.0389(4) 0.0292(4) -0.0019(3) 0.0088(3) -0.0023(3) F7 0.0434(5) 0.0573(6) 0.0305(4) 0.0044(4) -0.0064(4) 0.0044(4) F8 0.0316(4) 0.0306(4) 0.0657(6) -0.0015(4) -0.0055(4) 0.0113(3) F9 0.0223(4) 0.0500(6) 0.0714(6) 0.0119(5) -0.0112(4) -0.0109(3) O1 0.0225(4) 0.0207(4) 0.0389(5) 0.0053(3) 0.0033(3) -0.0032(3) O2 0.0213(4) 0.0435(5) 0.0270(5) 0.0036(4) -0.0030(3) -0.0009(3) O3 0.0241(4) 0.0243(4) 0.0329(5) -0.0015(3) 0.0069(3) 0.0060(3) O1L 0.0278(4) 0.0360(5) 0.0223(4) -0.0053(4) 0.0041(3) 0.0038(3) S1 0.01513(11) 0.01964(13) 0.02337(14) 0.00145(9) 0.00218(9) 0.00027(8) _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 Li1 O2 1.900(2) 2_645 ? Li1 O1 1.927(2) . ? Li1 O3 1.931(3) 1_545 ? Li1 O1L 1.953(2) . ? C1 F2 1.3439(14) . ? C1 F1 1.3448(17) . ? C1 C2 1.5509(15) . ? C1 S1 1.8418(13) . ? C2 F4 1.3421(17) . ? C2 F3 1.3432(14) . ? C2 C3 1.5544(16) . ? C3 F5 1.3393(17) . ? C3 F6 1.3431(14) . ? C3 C4 1.5463(17) . ? C4 F7 1.3200(18) . ? C4 F8 1.3205(18) . ? C4 F9 1.3314(15) . ? C1L O1L 1.4346(16) . ? C1L C2L 1.502(2) . ? C1L H1L 0.9700 . ? C1L H2L 0.9700 . ? C2L O1L 1.4341(16) 3_666 ? C2L H4L 0.9700 . ? C2L H3L 0.9700 . ? O1 S1 1.4411(14) . ? O2 S1 1.4424(10) . ? O2 Li1 1.900(2) 2_655 ? O3 S1 1.4418(11) . ? O3 Li1 1.931(3) 1_565 ? O1L C2L 1.4341(16) 3_666 ? 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 O2 Li1 O1 109.97(11) 2_645 . ? O2 Li1 O3 116.82(11) 2_645 1_545 ? O1 Li1 O3 113.78(11) . 1_545 ? O2 Li1 O1L 104.74(10) 2_645 . ? O1 Li1 O1L 105.58(10) . . ? O3 Li1 O1L 104.75(10) 1_545 . ? F2 C1 F1 108.29(10) . . ? F2 C1 C2 108.48(9) . . ? F1 C1 C2 109.28(9) . . ? F2 C1 S1 107.62(7) . . ? F1 C1 S1 107.86(7) . . ? C2 C1 S1 115.10(8) . . ? F4 C2 F3 108.52(10) . . ? F4 C2 C1 108.60(9) . . ? F3 C2 C1 109.12(9) . . ? F4 C2 C3 108.34(9) . . ? F3 C2 C3 108.30(9) . . ? C1 C2 C3 113.84(9) . . ? F5 C3 F6 108.81(9) . . ? F5 C3 C4 107.10(10) . . ? F6 C3 C4 107.57(10) . . ? F5 C3 C2 108.81(9) . . ? F6 C3 C2 109.35(9) . . ? C4 C3 C2 115.04(10) . . ? F7 C4 F8 109.10(12) . . ? F7 C4 F9 108.43(11) . . ? F8 C4 F9 107.80(12) . . ? F7 C4 C3 110.94(11) . . ? F8 C4 C3 111.70(11) . . ? F9 C4 C3 108.75(11) . . ? O1L C1L C2L 110.38(11) . . ? O1L C1L H1L 109.6 . . ? C2L C1L H1L 109.6 . . ? O1L C1L H2L 109.6 . . ? C2L C1L H2L 109.6 . . ? H1L C1L H2L 108.1 . . ? O1L C2L C1L 110.44(11) 3_666 . ? O1L C2L H4L 109.6 3_666 . ? C1L C2L H4L 109.6 . . ? O1L C2L H3L 109.6 3_666 . ? C1L C2L H3L 109.6 . . ? H4L C2L H3L 108.1 . . ? S1 O1 Li1 142.42(8) . . ? S1 O2 Li1 150.26(9) . 2_655 ? S1 O3 Li1 138.39(9) . 1_565 ? C2L O1L C1L 109.97(10) 3_666 . ? C2L O1L Li1 118.67(10) 3_666 . ? C1L O1L Li1 126.14(10) . . ? O1 S1 O3 114.13(7) . . ? O1 S1 O2 115.20(6) . . ? O3 S1 O2 114.19(6) . . ? O1 S1 C1 103.94(5) . . ? O3 S1 C1 105.16(5) . . ? O2 S1 C1 102.26(5) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 C1 C2 F4 -45.92(12) . . . . ? F1 C1 C2 F4 -163.80(9) . . . . ? S1 C1 C2 F4 74.69(11) . . . . ? F2 C1 C2 F3 -164.04(9) . . . . ? F1 C1 C2 F3 78.08(11) . . . . ? S1 C1 C2 F3 -43.43(12) . . . . ? F2 C1 C2 C3 74.86(13) . . . . ? F1 C1 C2 C3 -43.02(12) . . . . ? S1 C1 C2 C3 -164.54(8) . . . . ? F4 C2 C3 F5 -164.58(9) . . . . ? F3 C2 C3 F5 -47.06(12) . . . . ? C1 C2 C3 F5 74.50(12) . . . . ? F4 C2 C3 F6 76.70(12) . . . . ? F3 C2 C3 F6 -165.78(9) . . . . ? C1 C2 C3 F6 -44.22(13) . . . . ? F4 C2 C3 C4 -44.44(13) . . . . ? F3 C2 C3 C4 73.07(13) . . . . ? C1 C2 C3 C4 -165.37(10) . . . . ? F5 C3 C4 F7 70.21(13) . . . . ? F6 C3 C4 F7 -172.97(10) . . . . ? C2 C3 C4 F7 -50.86(14) . . . . ? F5 C3 C4 F8 -167.82(10) . . . . ? F6 C3 C4 F8 -51.00(13) . . . . ? C2 C3 C4 F8 71.11(15) . . . . ? F5 C3 C4 F9 -48.97(14) . . . . ? F6 C3 C4 F9 67.86(13) . . . . ? C2 C3 C4 F9 -170.03(10) . . . . ? O1L C1L C2L O1L -58.17(16) . . . 3_666 ? O2 Li1 O1 S1 16.5(2) 2_645 . . . ? O3 Li1 O1 S1 149.69(11) 1_545 . . . ? O1L Li1 O1 S1 -96.00(15) . . . . ? C2L C1L O1L C2L 57.90(17) . . . 3_666 ? C2L C1L O1L Li1 -95.92(14) . . . . ? O2 Li1 O1L C2L -174.67(11) 2_645 . . 3_666 ? O1 Li1 O1L C2L -58.57(14) . . . 3_666 ? O3 Li1 O1L C2L 61.84(14) 1_545 . . 3_666 ? O2 Li1 O1L C1L -22.88(16) 2_645 . . . ? O1 Li1 O1L C1L 93.23(14) . . . . ? O3 Li1 O1L C1L -146.36(11) 1_545 . . . ? Li1 O1 S1 O3 90.23(15) . . . . ? Li1 O1 S1 O2 -44.76(15) . . . . ? Li1 O1 S1 C1 -155.78(14) . . . . ? Li1 O3 S1 O1 -144.88(12) 1_565 . . . ? Li1 O3 S1 O2 -9.42(13) 1_565 . . . ? Li1 O3 S1 C1 101.86(12) 1_565 . . . ? Li1 O2 S1 O1 59.22(19) 2_655 . . . ? Li1 O2 S1 O3 -75.75(19) 2_655 . . . ? Li1 O2 S1 C1 171.23(18) 2_655 . . . ? F2 C1 S1 O1 73.55(10) . . . . ? F1 C1 S1 O1 -169.81(8) . . . . ? C2 C1 S1 O1 -47.53(9) . . . . ? F2 C1 S1 O3 -166.20(8) . . . . ? F1 C1 S1 O3 -49.56(9) . . . . ? C2 C1 S1 O3 72.72(10) . . . . ? F2 C1 S1 O2 -46.64(10) . . . . ? F1 C1 S1 O2 70.00(9) . . . . ? C2 C1 S1 O2 -167.72(8) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.461 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.050 # Attachment 'NaC4F9SO3_new.CIF' data_orgvor5 _database_code_depnum_ccdc_archive 'CCDC 737959' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Sodium Nonafluorobutylsulfonate hydrate' ; _chemical_name_common "'Sodium Nonafluorobutylsulfonate hydrate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H2 F9 Na O4 S' _chemical_formula_weight 340.11 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' Na Na 0.0362 0.0249 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.165(5) _cell_length_b 5.634(5) _cell_length_c 11.085(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 100.122(5) _cell_angle_gamma 90.000(5) _cell_volume 1055.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 25.14 _exptl_crystal_description platelett _exptl_crystal_colour colorless _exptl_crystal_size_max .3 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8136 _diffrn_reflns_av_R_equivalents 0.1737 _diffrn_reflns_av_sigmaI/netI 0.1497 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.14 _reflns_number_total 1874 _reflns_number_gt 862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _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^)+(0.1417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1874 _refine_ls_number_parameters 180 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1689 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2639 _refine_ls_wR_factor_gt 0.2173 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.002 _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 Na1 Na 0.41701(8) 0.6567(2) 1.02596(11) 0.0266(4) Uani 1 1 d . . . S1 S 0.37404(6) 0.82828(14) 0.71333(7) 0.0225(2) Uani 1 1 d . . . O1 O 0.39214(15) 0.8738(3) 0.84308(19) 0.0247(7) Uani 1 1 d . . . O2 O 0.39484(16) 1.0147(4) 0.6371(2) 0.0350(7) Uani 1 1 d . . . O3 O 0.39742(16) 0.5931(4) 0.6806(2) 0.0297(7) Uani 1 1 d . . . O1W O 0.44507(15) 0.3410(3) 0.90306(19) 0.0274(7) Uani 1 1 d D . . F1 F 0.24374(15) 0.6480(5) 0.7515(2) 0.0619(8) Uani 1 1 d . . . F2 F 0.24054(14) 1.0289(5) 0.7251(2) 0.0600(8) Uani 1 1 d . . . F3 F 0.23325(18) 1.0010(5) 0.4919(2) 0.0819(11) Uani 1 1 d . . . F4 F 0.26286(16) 0.6366(5) 0.4943(2) 0.0830(10) Uani 1 1 d . . . F5 F 0.1319(2) 0.4987(7) 0.5541(3) 0.1172(14) Uani 1 1 d . . . F6 F 0.10206(17) 0.8467(8) 0.6069(3) 0.1149(15) Uani 1 1 d . . . F7 F 0.0830(2) 0.9920(8) 0.3772(3) 0.1216(16) Uani 1 1 d . . . F8 F 0.01830(17) 0.6961(8) 0.3936(3) 0.1055(14) Uani 1 1 d . . . F9 F 0.12614(16) 0.6742(6) 0.3200(2) 0.0794(11) Uani 1 1 d . . . C1 C 0.2648(2) 0.8235(6) 0.6843(3) 0.0308(11) Uani 1 1 d . . . C2 C 0.2252(2) 0.7934(7) 0.5515(3) 0.0383(12) Uani 1 1 d . . . C3 C 0.1387(3) 0.7415(10) 0.5280(4) 0.0583(16) Uani 1 1 d . . . C4 C 0.0913(3) 0.7466(11) 0.4054(5) 0.073(2) Uani 1 1 d . . . H1W H 0.4239(10) 0.2125(18) 0.908(3) 0.058(13) Uiso 1 1 d D . . H2W H 0.4472(15) 0.414(3) 0.8402(9) 0.025(9) Uiso 1 1 d D . . 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 Na1 0.0541(8) 0.0173(6) 0.0106(6) -0.0011(5) 0.0117(6) 0.0021(6) S1 0.0439(5) 0.0150(3) 0.0100(4) 0.0008(3) 0.0084(4) -0.0021(4) O1 0.0471(14) 0.0163(10) 0.0094(11) -0.0046(9) 0.0011(11) -0.0042(10) O2 0.0625(16) 0.0255(11) 0.0197(12) 0.0128(10) 0.0144(12) -0.0090(12) O3 0.0570(15) 0.0191(10) 0.0127(11) -0.0041(10) 0.0050(11) 0.0086(11) O1W 0.0559(15) 0.0128(10) 0.0145(11) 0.0028(10) 0.0088(11) -0.0016(11) F1 0.0608(15) 0.0883(17) 0.0387(13) 0.0311(12) 0.0146(12) -0.0230(14) F2 0.0646(15) 0.0741(15) 0.0411(13) -0.0262(12) 0.0089(12) 0.0301(13) F3 0.094(2) 0.106(2) 0.0418(15) 0.0278(16) 0.0013(16) -0.0280(18) F4 0.0598(17) 0.137(2) 0.0473(14) -0.0557(15) -0.0050(14) 0.0194(17) F5 0.100(2) 0.127(2) 0.115(3) 0.040(2) -0.009(2) -0.046(2) F6 0.0494(17) 0.248(4) 0.0492(16) -0.040(2) 0.0141(15) 0.006(2) F7 0.103(3) 0.162(3) 0.088(2) 0.001(3) -0.015(2) 0.029(3) F8 0.0436(16) 0.215(4) 0.0555(18) 0.011(2) 0.0035(15) -0.028(2) F9 0.0594(17) 0.142(3) 0.0349(14) -0.0223(16) 0.0041(14) -0.0079(18) C1 0.041(2) 0.0294(17) 0.0245(19) -0.0001(16) 0.0120(17) 0.0063(18) C2 0.045(2) 0.055(2) 0.0171(19) -0.0054(18) 0.0115(18) -0.004(2) C3 0.054(3) 0.092(3) 0.033(2) -0.003(2) 0.019(2) -0.004(3) C4 0.056(3) 0.120(4) 0.047(3) 0.010(3) 0.020(3) 0.010(3) _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. The O1W H distances were constraint using DFIX 0.82 0.02. ; 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 Na1 O3 2.288(3) 4_566 ? Na1 O2 2.292(3) 4_576 ? Na1 O1W 2.341(3) . ? Na1 O1 2.342(3) . ? Na1 O1W 2.360(3) 3_667 ? Na1 Na1 3.485(3) 3_667 ? Na1 H2W 2.600(16) . ? S1 O2 1.432(3) . ? S1 O1 1.440(2) . ? S1 O3 1.449(3) . ? S1 C1 1.847(4) . ? O2 Na1 2.292(3) 4_575 ? O3 Na1 2.288(3) 4_565 ? O1W Na1 2.360(3) 3_667 ? O1W H1W 0.817(12) . ? O1W H2W 0.814(12) . ? F1 C1 1.326(4) . ? F2 C1 1.336(4) . ? F3 C2 1.362(5) . ? F4 C2 1.321(5) . ? F5 C3 1.408(7) . ? F6 C3 1.306(6) . ? F7 C4 1.419(7) . ? F8 C4 1.269(6) . ? F9 C4 1.273(6) . ? C1 C2 1.519(5) . ? C2 C3 1.490(6) . ? C3 C4 1.457(6) . ? 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 O3 Na1 O2 91.94(11) 4_566 4_576 ? O3 Na1 O1W 92.34(10) 4_566 . ? O2 Na1 O1W 175.40(11) 4_576 . ? O3 Na1 O1 160.29(11) 4_566 . ? O2 Na1 O1 91.23(10) 4_576 . ? O1W Na1 O1 85.29(10) . . ? O3 Na1 O1W 91.40(9) 4_566 3_667 ? O2 Na1 O1W 93.90(9) 4_576 3_667 ? O1W Na1 O1W 84.33(9) . 3_667 ? O1 Na1 O1W 107.78(10) . 3_667 ? O3 Na1 Na1 92.52(9) 4_566 3_667 ? O2 Na1 Na1 135.71(10) 4_576 3_667 ? O1W Na1 Na1 42.37(7) . 3_667 ? O1 Na1 Na1 98.72(9) . 3_667 ? O1W Na1 Na1 41.96(6) 3_667 3_667 ? O3 Na1 H2W 110.2(3) 4_566 . ? O2 Na1 H2W 157.9(3) 4_576 . ? O1W Na1 H2W 18.0(3) . . ? O1 Na1 H2W 67.7(3) . . ? O1W Na1 H2W 86.5(6) 3_667 . ? Na1 Na1 H2W 47.1(5) 3_667 . ? O2 S1 O1 115.22(14) . . ? O2 S1 O3 114.47(16) . . ? O1 S1 O3 113.11(13) . . ? O2 S1 C1 105.01(16) . . ? O1 S1 C1 102.17(16) . . ? O3 S1 C1 105.10(16) . . ? S1 O1 Na1 138.26(13) . . ? S1 O2 Na1 172.60(18) . 4_575 ? S1 O3 Na1 146.50(14) . 4_565 ? Na1 O1W Na1 95.67(9) . 3_667 ? Na1 O1W H1W 119(2) . . ? Na1 O1W H1W 114.5(13) 3_667 . ? Na1 O1W H2W 99.3(12) . . ? Na1 O1W H2W 95.1(18) 3_667 . ? H1W O1W H2W 126(3) . . ? F1 C1 F2 108.9(3) . . ? F1 C1 C2 110.0(3) . . ? F2 C1 C2 108.2(3) . . ? F1 C1 S1 106.4(2) . . ? F2 C1 S1 107.2(2) . . ? C2 C1 S1 116.0(3) . . ? F4 C2 F3 104.0(3) . . ? F4 C2 C3 110.0(4) . . ? F3 C2 C3 105.5(3) . . ? F4 C2 C1 111.5(3) . . ? F3 C2 C1 108.0(3) . . ? C3 C2 C1 116.9(4) . . ? F6 C3 F5 103.7(4) . . ? F6 C3 C4 111.0(4) . . ? F5 C3 C4 99.0(4) . . ? F6 C3 C2 112.1(4) . . ? F5 C3 C2 105.8(4) . . ? C4 C3 C2 122.4(4) . . ? F8 C4 F9 115.8(4) . . ? F8 C4 F7 97.8(4) . . ? F9 C4 F7 100.9(4) . . ? F8 C4 C3 118.2(5) . . ? F9 C4 C3 115.4(4) . . ? F7 C4 C3 104.1(4) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Na1 -155.8(2) . . . . ? O3 S1 O1 Na1 -21.5(3) . . . . ? C1 S1 O1 Na1 91.0(2) . . . . ? O3 Na1 O1 S1 -64.1(4) 4_566 . . . ? O2 Na1 O1 S1 -163.3(2) 4_576 . . . ? O1W Na1 O1 S1 19.7(2) . . . . ? O1W Na1 O1 S1 102.2(2) 3_667 . . . ? Na1 Na1 O1 S1 60.0(2) 3_667 . . . ? O1 S1 O2 Na1 -61.0(13) . . . 4_575 ? O3 S1 O2 Na1 165.3(12) . . . 4_575 ? C1 S1 O2 Na1 50.5(13) . . . 4_575 ? O2 S1 O3 Na1 -33.1(4) . . . 4_565 ? O1 S1 O3 Na1 -167.8(3) . . . 4_565 ? C1 S1 O3 Na1 81.5(3) . . . 4_565 ? O3 Na1 O1W Na1 -91.17(10) 4_566 . . 3_667 ? O2 Na1 O1W Na1 67.5(13) 4_576 . . 3_667 ? O1 Na1 O1W Na1 108.43(10) . . . 3_667 ? O1W Na1 O1W Na1 0.0 3_667 . . 3_667 ? O2 S1 C1 F1 178.5(2) . . . . ? O1 S1 C1 F1 -60.9(3) . . . . ? O3 S1 C1 F1 57.4(3) . . . . ? O2 S1 C1 F2 -65.1(3) . . . . ? O1 S1 C1 F2 55.5(3) . . . . ? O3 S1 C1 F2 173.8(2) . . . . ? O2 S1 C1 C2 55.8(3) . . . . ? O1 S1 C1 C2 176.4(3) . . . . ? O3 S1 C1 C2 -65.3(3) . . . . ? F1 C1 C2 F4 -80.1(4) . . . . ? F2 C1 C2 F4 161.0(3) . . . . ? S1 C1 C2 F4 40.6(4) . . . . ? F1 C1 C2 F3 166.2(3) . . . . ? F2 C1 C2 F3 47.4(4) . . . . ? S1 C1 C2 F3 -73.0(4) . . . . ? F1 C1 C2 C3 47.6(5) . . . . ? F2 C1 C2 C3 -71.3(5) . . . . ? S1 C1 C2 C3 168.3(3) . . . . ? F4 C2 C3 F6 162.5(4) . . . . ? F3 C2 C3 F6 -85.9(5) . . . . ? C1 C2 C3 F6 34.1(6) . . . . ? F4 C2 C3 F5 50.2(4) . . . . ? F3 C2 C3 F5 161.8(3) . . . . ? C1 C2 C3 F5 -78.3(5) . . . . ? F4 C2 C3 C4 -61.7(6) . . . . ? F3 C2 C3 C4 49.9(6) . . . . ? C1 C2 C3 C4 169.9(5) . . . . ? F6 C3 C4 F8 -45.0(7) . . . . ? F5 C3 C4 F8 63.5(6) . . . . ? C2 C3 C4 F8 178.8(5) . . . . ? F6 C3 C4 F9 171.7(5) . . . . ? F5 C3 C4 F9 -79.8(6) . . . . ? C2 C3 C4 F9 35.5(8) . . . . ? F6 C3 C4 F7 62.1(6) . . . . ? F5 C3 C4 F7 170.6(4) . . . . ? C2 C3 C4 F7 -74.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.109 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.139 # Attachment 'RbC4F9SO3.CIF' data_rbtf _database_code_depnum_ccdc_archive 'CCDC 737960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Rubidium nonafluorobutylsulfonate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 F9 O3 Rb S' _chemical_formula_weight 384.57 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.0346(18) _cell_length_b 5.8254(19) _cell_length_c 33.361(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.21(3) _cell_angle_gamma 90.00 _cell_volume 976.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 867 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 30.45 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .25 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 5.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .508 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (BRUKER-AXS)' _exptl_special_details ; 'The ratio of minimum and max transmission is provided by the program' ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14785 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.52 _reflns_number_total 2962 _reflns_number_gt 2315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _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^)+(0.0525P)^2^+15.7807P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2962 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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 Rb1 Rb 0.64054(12) 1.02095(10) 0.21149(2) 0.0191(2) Uani 1 1 d . . . C1 C 0.1772(14) 0.5756(13) 0.1424(2) 0.0200(14) Uani 1 1 d . . . C2 C 0.2294(14) 0.3638(12) 0.1158(2) 0.0191(13) Uani 1 1 d . . . C3 C 0.2717(17) 0.4195(16) 0.0710(3) 0.0282(17) Uani 1 1 d . . . C4 C 0.245(2) 0.2152(18) 0.0424(3) 0.038(2) Uani 1 1 d . . . F1 F 0.3432(9) 0.7473(8) 0.13274(14) 0.0246(10) Uani 1 1 d . . . F2 F -0.0752(9) 0.6475(9) 0.13412(15) 0.0278(10) Uani 1 1 d . . . F3 F 0.4479(9) 0.2539(8) 0.13067(15) 0.0270(10) Uani 1 1 d . . . F4 F 0.0188(10) 0.2218(9) 0.11710(15) 0.0311(11) Uani 1 1 d . . . F5 F 0.5148(11) 0.5104(10) 0.06862(16) 0.0367(12) Uani 1 1 d . . . F6 F 0.0907(12) 0.5792(11) 0.05826(16) 0.0403(13) Uani 1 1 d . . . F7 F -0.0029(15) 0.1457(15) 0.0376(2) 0.068(2) Uani 1 1 d . . . F8 F 0.3985(17) 0.0424(12) 0.0563(2) 0.0596(19) Uani 1 1 d . . . F9 F 0.3257(16) 0.2750(13) 0.00687(18) 0.0562(18) Uani 1 1 d . . . O1 O 0.0985(10) 0.7276(9) 0.21327(17) 0.0232(11) Uani 1 1 d . . . O2 O 0.5098(9) 0.5207(9) 0.20419(16) 0.0189(10) Uani 1 1 d . . . O3 O 0.0934(10) 0.3116(9) 0.20320(16) 0.0202(10) Uani 1 1 d . . . S1 S 0.2238(3) 0.5262(3) 0.19675(5) 0.0144(3) Uani 1 1 d . . . 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 Rb1 0.0154(3) 0.0101(3) 0.0319(4) 0.0000(3) 0.0016(2) 0.0000(2) C1 0.017(3) 0.020(3) 0.024(4) 0.001(3) 0.000(3) 0.001(2) C2 0.017(3) 0.017(3) 0.023(4) 0.000(3) -0.001(3) -0.004(2) C3 0.028(4) 0.034(4) 0.022(4) 0.001(3) 0.001(3) -0.004(3) C4 0.047(5) 0.041(5) 0.025(5) -0.006(4) 0.003(4) -0.007(4) F1 0.023(2) 0.024(2) 0.027(2) 0.0070(18) 0.0046(18) -0.0018(17) F2 0.020(2) 0.034(3) 0.029(3) 0.000(2) -0.0028(18) 0.0107(19) F3 0.023(2) 0.027(2) 0.030(3) 0.000(2) 0.0008(18) 0.0095(18) F4 0.030(2) 0.032(3) 0.032(3) -0.008(2) 0.009(2) -0.012(2) F5 0.035(3) 0.044(3) 0.032(3) 0.006(2) 0.009(2) -0.007(2) F6 0.047(3) 0.046(3) 0.027(3) 0.008(2) -0.004(2) 0.007(3) F7 0.066(4) 0.092(6) 0.046(4) -0.032(4) 0.009(3) -0.044(4) F8 0.100(6) 0.038(3) 0.042(4) -0.011(3) 0.018(4) 0.010(4) F9 0.083(5) 0.065(5) 0.022(3) -0.010(3) 0.014(3) -0.010(4) O1 0.020(2) 0.022(3) 0.027(3) -0.010(2) -0.001(2) 0.006(2) O2 0.0116(19) 0.017(2) 0.028(3) -0.003(2) 0.0015(17) -0.0039(18) O3 0.016(2) 0.023(3) 0.022(3) 0.006(2) -0.0002(18) -0.0045(19) S1 0.0111(6) 0.0118(7) 0.0205(8) 0.0000(6) 0.0016(5) 0.0000(5) _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 Rb1 O3 2.866(5) 1_665 ? Rb1 O1 2.868(5) 1_655 ? Rb1 O2 2.992(5) 1_565 ? Rb1 O2 2.994(5) . ? Rb1 O1 3.088(6) 2 ? Rb1 F3 3.124(5) 1_565 ? Rb1 O1 3.223(6) . ? Rb1 O3 3.232(5) 1_565 ? Rb1 O2 3.233(5) 2_655 ? Rb1 F1 3.353(5) . ? Rb1 O3 3.369(6) 2 ? Rb1 S1 3.5827(19) . ? C1 F2 1.352(8) . ? C1 F1 1.354(8) . ? C1 C2 1.551(10) . ? C1 S1 1.839(8) . ? C2 F3 1.344(8) . ? C2 F4 1.347(8) . ? C2 C3 1.553(11) . ? C3 F5 1.340(10) . ? C3 F6 1.354(10) . ? C3 C4 1.528(13) . ? C4 F7 1.314(12) . ? C4 F9 1.320(11) . ? C4 F8 1.336(13) . ? F3 Rb1 3.124(5) 1_545 ? O1 S1 1.455(5) . ? O1 Rb1 2.868(5) 1_455 ? O1 Rb1 3.088(6) 2_545 ? O2 S1 1.448(5) . ? O2 Rb1 2.992(5) 1_545 ? O2 Rb1 3.233(5) 2_645 ? O3 S1 1.434(5) . ? O3 Rb1 2.866(5) 1_445 ? O3 Rb1 3.232(5) 1_545 ? O3 Rb1 3.369(6) 2_545 ? S1 Rb1 3.6319(19) 1_545 ? S1 Rb1 3.656(2) 2_545 ? 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 O3 Rb1 O1 73.20(16) 1_665 1_655 ? O3 Rb1 O2 65.78(14) 1_665 1_565 ? O1 Rb1 O2 138.98(15) 1_655 1_565 ? O3 Rb1 O2 137.69(14) 1_665 . ? O1 Rb1 O2 66.08(14) 1_655 . ? O2 Rb1 O2 153.39(17) 1_565 . ? O3 Rb1 O1 101.34(15) 1_665 2 ? O1 Rb1 O1 124.40(10) 1_655 2 ? O2 Rb1 O1 65.98(14) 1_565 2 ? O2 Rb1 O1 110.58(14) . 2 ? O3 Rb1 F3 82.55(14) 1_665 1_565 ? O1 Rb1 F3 119.15(15) 1_655 1_565 ? O2 Rb1 F3 56.69(13) 1_565 1_565 ? O2 Rb1 F3 107.24(14) . 1_565 ? O1 Rb1 F3 114.58(13) 2 1_565 ? O3 Rb1 O1 173.74(15) 1_665 . ? O1 Rb1 O1 111.35(18) 1_655 . ? O2 Rb1 O1 109.57(13) 1_565 . ? O2 Rb1 O1 45.82(13) . . ? O1 Rb1 O1 79.79(11) 2 . ? F3 Rb1 O1 91.38(14) 1_565 . ? O3 Rb1 O3 111.17(17) 1_665 1_565 ? O1 Rb1 O3 173.88(15) 1_655 1_565 ? O2 Rb1 O3 45.63(13) 1_565 1_565 ? O2 Rb1 O3 108.69(13) . 1_565 ? O1 Rb1 O3 59.75(14) 2 1_565 ? F3 Rb1 O3 58.44(13) 1_565 1_565 ? O1 Rb1 O3 63.96(13) . 1_565 ? O3 Rb1 O2 71.75(14) 1_665 2_655 ? O1 Rb1 O2 65.41(14) 1_655 2_655 ? O2 Rb1 O2 100.24(14) 1_565 2_655 ? O2 Rb1 O2 100.18(15) . 2_655 ? O1 Rb1 O2 60.73(13) 2 2_655 ? F3 Rb1 O2 151.46(13) 1_565 2_655 ? O1 Rb1 O2 113.83(14) . 2_655 ? O3 Rb1 O2 119.63(13) 1_565 2_655 ? O3 Rb1 F1 121.86(14) 1_665 . ? O1 Rb1 F1 93.21(14) 1_655 . ? O2 Rb1 F1 108.20(13) 1_565 . ? O2 Rb1 F1 52.21(13) . . ? O1 Rb1 F1 130.16(13) 2 . ? F3 Rb1 F1 55.03(12) 1_565 . ? O1 Rb1 F1 54.63(13) . . ? O3 Rb1 F1 80.86(13) 1_565 . ? O2 Rb1 F1 151.49(12) 2_655 . ? O3 Rb1 O3 127.82(10) 1_665 2 ? O1 Rb1 O3 94.91(15) 1_655 2 ? O2 Rb1 O3 109.59(13) 1_565 2 ? O2 Rb1 O3 68.33(14) . 2 ? O1 Rb1 O3 44.26(13) 2 2 ? F3 Rb1 O3 141.26(12) 1_565 2 ? O1 Rb1 O3 57.04(14) . 2 ? O3 Rb1 O3 85.71(11) 1_565 2 ? O2 Rb1 O3 57.60(13) 2_655 2 ? F1 Rb1 O3 109.14(12) . 2 ? O3 Rb1 S1 157.67(12) 1_665 . ? O1 Rb1 S1 89.27(12) 1_655 . ? O2 Rb1 S1 130.34(10) 1_565 . ? O2 Rb1 S1 23.30(9) . . ? O1 Rb1 S1 99.98(10) 2 . ? F3 Rb1 S1 94.58(10) 1_565 . ? O1 Rb1 S1 23.95(9) . . ? O3 Rb1 S1 85.41(10) 1_565 . ? O2 Rb1 S1 113.90(10) 2_655 . ? F1 Rb1 S1 43.76(8) . . ? O3 Rb1 S1 66.10(10) 2 . ? F2 C1 F1 108.0(6) . . ? F2 C1 C2 108.5(6) . . ? F1 C1 C2 109.0(6) . . ? F2 C1 S1 108.4(5) . . ? F1 C1 S1 107.7(5) . . ? C2 C1 S1 115.1(5) . . ? F3 C2 F4 108.9(6) . . ? F3 C2 C1 109.2(6) . . ? F4 C2 C1 108.1(6) . . ? F3 C2 C3 107.6(6) . . ? F4 C2 C3 108.1(6) . . ? C1 C2 C3 114.9(6) . . ? F5 C3 F6 108.1(7) . . ? F5 C3 C4 108.5(7) . . ? F6 C3 C4 107.7(7) . . ? F5 C3 C2 108.4(6) . . ? F6 C3 C2 108.7(7) . . ? C4 C3 C2 115.2(7) . . ? F7 C4 F9 108.1(8) . . ? F7 C4 F8 109.6(9) . . ? F9 C4 F8 108.1(9) . . ? F7 C4 C3 111.4(8) . . ? F9 C4 C3 109.6(8) . . ? F8 C4 C3 109.9(8) . . ? C1 F1 Rb1 114.8(4) . . ? C2 F3 Rb1 137.3(4) . 1_545 ? S1 O1 Rb1 146.9(3) . 1_455 ? S1 O1 Rb1 101.0(3) . 2_545 ? Rb1 O1 Rb1 84.24(14) 1_455 2_545 ? S1 O1 Rb1 92.0(2) . . ? Rb1 O1 Rb1 111.35(18) 1_455 . ? Rb1 O1 Rb1 126.20(18) 2_545 . ? S1 O2 Rb1 104.3(2) . 1_545 ? S1 O2 Rb1 101.8(2) . . ? Rb1 O2 Rb1 153.39(17) 1_545 . ? S1 O2 Rb1 129.6(3) . 2_645 ? Rb1 O2 Rb1 79.81(12) 1_545 2_645 ? Rb1 O2 Rb1 79.77(12) . 2_645 ? S1 O3 Rb1 154.5(3) . 1_445 ? S1 O3 Rb1 94.3(2) . 1_545 ? Rb1 O3 Rb1 111.17(17) 1_445 1_545 ? S1 O3 Rb1 89.8(3) . 2_545 ? Rb1 O3 Rb1 79.32(12) 1_445 2_545 ? Rb1 O3 Rb1 117.01(16) 1_545 2_545 ? O3 S1 O2 114.5(3) . . ? O3 S1 O1 115.7(3) . . ? O2 S1 O1 113.6(3) . . ? O3 S1 C1 104.5(3) . . ? O2 S1 C1 104.1(3) . . ? O1 S1 C1 102.3(3) . . ? O3 S1 Rb1 161.9(2) . . ? O2 S1 Rb1 54.9(2) . . ? O1 S1 Rb1 64.0(2) . . ? C1 S1 Rb1 92.9(2) . . ? O3 S1 Rb1 62.5(2) . 1_545 ? O2 S1 Rb1 53.0(2) . 1_545 ? O1 S1 Rb1 149.5(2) . 1_545 ? C1 S1 Rb1 107.5(2) . 1_545 ? Rb1 S1 Rb1 107.69(5) . 1_545 ? O3 S1 Rb1 67.1(2) . 2_545 ? O2 S1 Rb1 113.4(2) . 2_545 ? O1 S1 Rb1 56.0(2) . 2_545 ? C1 S1 Rb1 141.7(2) . 2_545 ? Rb1 S1 Rb1 102.07(5) . 2_545 ? Rb1 S1 Rb1 101.13(5) 1_545 2_545 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.177 _refine_diff_density_min -2.991 _refine_diff_density_rms 0.217