#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000148.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000148 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0107777 _journal_year 2002 _chemical_formula_sum 'C14 H28 F6 N2 O4 S2' _chemical_formula_weight 466.50 _chemical_melting_point 105 _chemical_name_systematic ; N,N,N,N-tetrakis(n-propyl)ammonium bis(trifluoromethylsulphonyl)amide ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 97.620(1) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.7417(1) _cell_length_b 22.8615(3) _cell_length_c 10.0251(1) _cell_measurement_reflns_used ? _cell_measurement_temperature 173(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 2213.0(8) _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Enraf Nonius CCD' _diffrn_measurement_method '1 deg scans in phi and omega' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 22977 _diffrn_reflns_theta_max 28.40 _diffrn_reflns_theta_min 3.26 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 326 _refine_ls_number_reflns 5483 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0464 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.0568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.1169 _reflns_number_gt 3800 _reflns_number_total 5483 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4000148 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.75188(6) 0.21636(2) 0.21813(5) 0.03898(15) Uani 1 1 d . . . F1 F 0.83783(16) 0.20655(8) -0.01760(15) 0.0801(5) Uani 1 1 d . . . O1 O 0.89169(18) 0.22130(7) 0.27900(17) 0.0623(5) Uani 1 1 d . . . N1 N 0.27036(14) 0.12400(6) 0.03933(14) 0.0265(3) Uani 1 1 d . . . C1 C 0.2503(3) 0.09279(12) 0.1699(3) 0.0328(6) Uani 0.718(3) 1 d P A 1 H1A H 0.1672 0.1095 0.2027 0.039 Uiso 0.718(3) 1 calc PR A 1 H1B H 0.2300 0.0512 0.1484 0.039 Uiso 0.718(3) 1 calc PR A 1 S2 S 0.78007(5) 0.09507(2) 0.20531(5) 0.03572(14) Uani 1 1 d . . . F2 F 0.63066(14) 0.23768(7) -0.02553(14) 0.0667(4) Uani 1 1 d . . . O2 O 0.6496(2) 0.25326(7) 0.26328(17) 0.0626(5) Uani 1 1 d . . . N2 N 0.69069(16) 0.15244(7) 0.20310(16) 0.0326(4) Uani 1 1 d . . . C2 C 0.3682(3) 0.09508(14) 0.2839(3) 0.0426(7) Uani 0.718(3) 1 d P A 1 H2A H 0.4515 0.0768 0.2547 0.051 Uiso 0.718(3) 1 calc PR A 1 H2B H 0.3905 0.1364 0.3072 0.051 Uiso 0.718(3) 1 calc PR A 1 F3 F 0.7997(2) 0.29378(8) 0.04197(19) 0.1010(7) Uani 1 1 d . . . O3 O 0.91113(16) 0.09991(8) 0.16000(16) 0.0574(4) Uani 1 1 d . . . C3 C 0.3314(3) 0.06396(12) 0.4044(2) 0.0596(7) Uani 1 1 d . . . H3A H 0.4094 0.0660 0.4768 0.089 Uiso 1 1 calc R A 1 H3B H 0.3106 0.0229 0.3816 0.089 Uiso 1 1 calc R A 1 H3C H 0.2499 0.0825 0.4342 0.089 Uiso 1 1 calc R A 1 F4 F 0.90827(19) 0.11400(8) 0.44785(15) 0.0840(5) Uani 1 1 d . . . O4 O 0.68993(17) 0.04890(7) 0.15377(19) 0.0614(5) Uani 1 1 d . . . C4 C 0.1379(2) 0.12320(12) -0.0552(3) 0.0290(6) Uani 0.718(3) 1 d P A 1 H4A H 0.1494 0.1486 -0.1328 0.035 Uiso 0.718(3) 1 calc PR A 1 H4B H 0.0645 0.1407 -0.0085 0.035 Uiso 0.718(3) 1 calc PR A 1 F5 F 0.70954(18) 0.07619(8) 0.44555(17) 0.0855(5) Uani 1 1 d . . . C5 C 0.0885(3) 0.06425(14) -0.1083(3) 0.0383(7) Uani 0.718(3) 1 d P A 1 H5A H 0.1587 0.0473 -0.1600 0.046 Uiso 0.718(3) 1 calc PR A 1 H5B H 0.0801 0.0379 -0.0314 0.046 Uiso 0.718(3) 1 calc PR A 1 F6 F 0.87745(18) 0.02380(7) 0.39630(16) 0.0798(5) Uani 1 1 d . . . C6 C -0.0485(2) 0.06648(12) -0.1972(2) 0.0553(6) Uani 1 1 d . . . H6A H -0.0743 0.0270 -0.2295 0.083 Uiso 1 1 calc R A 1 H6B H -0.0409 0.0921 -0.2742 0.083 Uiso 1 1 calc R A 1 H6C H -0.1195 0.0818 -0.1459 0.083 Uiso 1 1 calc R A 1 C7 C 0.3172(3) 0.18715(11) 0.0683(3) 0.0322(6) Uani 0.718(3) 1 d P A 1 H7A H 0.4086 0.1866 0.1249 0.039 Uiso 0.718(3) 1 calc PR A 1 H7B H 0.3297 0.2063 -0.0179 0.039 Uiso 0.718(3) 1 calc PR A 1 C8 C 0.2186(5) 0.22375(17) 0.1382(4) 0.0477(9) Uani 0.718(3) 1 d P A 1 H8A H 0.1244 0.2200 0.0882 0.057 Uiso 0.718(3) 1 calc PR A 1 H8B H 0.2162 0.2078 0.2296 0.057 Uiso 0.718(3) 1 calc PR A 1 C9 C 0.2543(5) 0.28571(11) 0.1497(3) 0.1003(13) Uani 1 1 d . . . H9A H 0.1855 0.3063 0.1952 0.150 Uiso 1 1 calc R A 1 H9B H 0.2552 0.3023 0.0597 0.150 Uiso 1 1 calc R A 1 H9C H 0.3461 0.2901 0.2020 0.150 Uiso 1 1 calc R A 1 C10 C 0.3877(3) 0.09259(12) -0.0211(3) 0.0296(6) Uani 0.718(3) 1 d P A 1 H10A H 0.4743 0.0970 0.0419 0.036 Uiso 0.718(3) 1 calc PR A 1 H10B H 0.3657 0.0503 -0.0274 0.036 Uiso 0.718(3) 1 calc PR A 1 C11 C 0.4143(3) 0.11369(16) -0.1587(3) 0.0377(7) Uani 0.718(3) 1 d P A 1 H11A H 0.3308 0.1067 -0.2245 0.045 Uiso 0.718(3) 1 calc PR A 1 H11B H 0.4323 0.1563 -0.1551 0.045 Uiso 0.718(3) 1 calc PR A 1 C12 C 0.5340(3) 0.08319(13) -0.2037(3) 0.0626(7) Uani 1 1 d . . . H12A H 0.5479 0.0974 -0.2932 0.094 Uiso 1 1 calc R A 1 H12B H 0.5161 0.0410 -0.2078 0.094 Uiso 1 1 calc R A 1 H12C H 0.6173 0.0910 -0.1400 0.094 Uiso 1 1 calc R A 1 C13 C 0.7550(2) 0.23960(11) 0.0438(2) 0.0501(6) Uani 1 1 d . . . C14 C 0.8205(3) 0.07662(11) 0.3842(2) 0.0514(6) Uani 1 1 d . . . C1' C 0.3366(9) 0.0999(3) 0.1677(7) 0.0315(16) Uani 0.282(3) 1 d P A 2 H1'1 H 0.4186 0.1244 0.1981 0.038 Uiso 0.282(3) 1 calc PR A 2 H1'2 H 0.3712 0.0604 0.1494 0.038 Uiso 0.282(3) 1 calc PR A 2 C2' C 0.2545(8) 0.0947(3) 0.2827(7) 0.0392(18) Uani 0.282(3) 1 d P A 2 H2'1 H 0.1682 0.0729 0.2524 0.047 Uiso 0.282(3) 1 calc PR A 2 H2'2 H 0.2281 0.1343 0.3097 0.047 Uiso 0.282(3) 1 calc PR A 2 C4' C 0.1509(6) 0.0817(3) -0.0213(7) 0.0261(15) Uani 0.282(3) 1 d P A 2 H4'1 H 0.1912 0.0422 -0.0286 0.031 Uiso 0.282(3) 1 calc PR A 2 H4'2 H 0.0830 0.0790 0.0437 0.031 Uiso 0.282(3) 1 calc PR A 2 C5' C 0.0726(7) 0.0977(4) -0.1580(8) 0.0358(17) Uani 0.282(3) 1 d P A 2 H5'1 H 0.0493 0.1398 -0.1571 0.043 Uiso 0.282(3) 1 calc PR A 2 H5'2 H 0.1354 0.0919 -0.2269 0.043 Uiso 0.282(3) 1 calc PR A 2 C7' C 0.1963(7) 0.1831(3) 0.0621(7) 0.0273(15) Uani 0.282(3) 1 d P A 2 H7'1 H 0.1525 0.1980 -0.0261 0.033 Uiso 0.282(3) 1 calc PR A 2 H7'2 H 0.1215 0.1756 0.1179 0.033 Uiso 0.282(3) 1 calc PR A 2 C8' C 0.2896(10) 0.2296(4) 0.1289(10) 0.039(2) Uani 0.282(3) 1 d P A 2 H8'1 H 0.3258 0.2139 0.2187 0.047 Uiso 0.282(3) 1 calc PR A 2 H8'2 H 0.3695 0.2315 0.0776 0.047 Uiso 0.282(3) 1 calc PR A 2 C10' C 0.3679(6) 0.1346(3) -0.0609(7) 0.0273(15) Uani 0.282(3) 1 d P A 2 H10C H 0.4449 0.1594 -0.0186 0.033 Uiso 0.282(3) 1 calc PR A 2 H10D H 0.3186 0.1567 -0.1376 0.033 Uiso 0.282(3) 1 calc PR A 2 C11' C 0.4284(7) 0.0796(4) -0.1146(8) 0.0353(17) Uani 0.282(3) 1 d P A 2 H11C H 0.4672 0.0559 -0.0358 0.042 Uiso 0.282(3) 1 calc PR A 2 H11D H 0.3502 0.0569 -0.1624 0.042 Uiso 0.282(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0494(3) 0.0329(3) 0.0323(3) -0.0026(2) -0.0034(2) -0.0079(2) F1 0.0701(10) 0.1233(14) 0.0516(9) 0.0279(9) 0.0252(8) 0.0245(10) O1 0.0605(11) 0.0603(11) 0.0570(10) 0.0079(8) -0.0262(8) -0.0258(8) N1 0.0269(8) 0.0242(7) 0.0291(8) 0.0022(6) 0.0057(6) -0.0025(6) C1 0.0312(16) 0.0346(15) 0.0335(15) 0.0080(12) 0.0076(12) -0.0030(13) S2 0.0331(3) 0.0369(3) 0.0369(3) -0.0027(2) 0.0041(2) 0.0060(2) F2 0.0523(8) 0.0953(11) 0.0474(8) 0.0182(8) -0.0128(7) 0.0013(8) O2 0.0916(13) 0.0409(9) 0.0557(10) -0.0138(8) 0.0109(9) 0.0115(9) N2 0.0279(8) 0.0304(8) 0.0397(9) -0.0022(7) 0.0049(7) -0.0013(6) C2 0.0380(18) 0.0528(18) 0.0357(16) 0.0094(14) 0.0007(13) -0.0082(14) F3 0.1274(16) 0.0740(11) 0.0951(13) 0.0420(10) -0.0090(12) -0.0456(11) O3 0.0424(9) 0.0787(12) 0.0553(10) 0.0096(9) 0.0221(8) 0.0180(8) C3 0.0650(16) 0.0740(17) 0.0388(12) 0.0157(12) 0.0033(11) 0.0023(13) F4 0.1058(13) 0.0917(12) 0.0459(8) 0.0073(8) -0.0218(9) -0.0070(10) O4 0.0618(11) 0.0332(8) 0.0826(12) -0.0123(8) -0.0149(9) 0.0041(7) C4 0.0236(12) 0.0296(16) 0.0336(14) 0.0026(12) 0.0029(10) 0.0008(10) F5 0.0925(12) 0.1005(13) 0.0729(11) 0.0352(9) 0.0460(10) 0.0269(10) C5 0.0329(15) 0.0340(17) 0.0460(19) 0.0025(15) -0.0022(13) -0.0019(13) F6 0.1032(13) 0.0678(10) 0.0683(10) 0.0225(8) 0.0111(9) 0.0414(9) C6 0.0402(12) 0.0730(17) 0.0499(13) -0.0127(12) -0.0043(10) -0.0043(12) C7 0.0362(16) 0.0269(14) 0.0335(14) -0.0012(11) 0.0053(11) -0.0081(11) C8 0.050(2) 0.040(2) 0.053(2) -0.0121(16) 0.010(2) 0.0022(19) C9 0.220(4) 0.0329(14) 0.0555(17) -0.0063(12) 0.045(2) 0.0017(19) C10 0.0230(12) 0.0306(15) 0.0354(14) 0.0012(12) 0.0049(10) 0.0032(10) C11 0.0383(16) 0.0396(18) 0.0364(16) -0.0012(15) 0.0095(12) -0.0025(13) C12 0.0465(14) 0.093(2) 0.0524(14) -0.0030(14) 0.0210(11) 0.0031(13) C13 0.0508(14) 0.0527(14) 0.0441(12) 0.0138(11) -0.0036(11) -0.0101(11) C14 0.0551(14) 0.0531(14) 0.0471(13) 0.0123(11) 0.0105(12) 0.0121(11) C1' 0.032(4) 0.031(4) 0.031(4) 0.005(3) 0.001(3) 0.000(3) C2' 0.045(5) 0.041(4) 0.030(4) 0.002(3) 0.000(3) -0.011(3) C4' 0.027(3) 0.020(3) 0.033(4) -0.001(3) 0.010(3) -0.005(2) C5' 0.037(4) 0.036(4) 0.035(4) -0.001(4) 0.003(3) -0.005(3) C7' 0.032(4) 0.021(3) 0.030(3) -0.002(3) 0.008(3) 0.003(2) C8' 0.041(5) 0.032(4) 0.045(5) -0.008(3) 0.007(4) -0.003(4) C10' 0.024(3) 0.026(4) 0.034(3) 0.002(3) 0.010(3) -0.003(3) C11' 0.035(4) 0.029(4) 0.042(4) 0.002(3) 0.008(3) -0.002(3)