#------------------------------------------------------------------------------ #$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/23/45/2234557.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2234557 loop_ _publ_author_name 'Zhi, Shuang' 'Zheng, Guo' 'Liu, Ying' 'Liu, Deng-Ke' _publ_section_title ; 1-(4,5,6,7-Tetrahydrothieno[3,2-c]pyridin-5-yl)-2-{4-[3-(trifluoromethyl)phenyl]piperazin-1-yl}ethanone ; _journal_coeditor_code CV5266 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1293 _journal_paper_doi 10.1107/S1600536812013591 _journal_volume 68 _journal_year 2012 _chemical_formula_iupac 'C20 H22 F3 N3 O S' _chemical_formula_moiety 'C20 H22 F3 N3 O S' _chemical_formula_sum 'C20 H22 F3 N3 O S' _chemical_formula_weight 409.47 _chemical_name_systematic ; 1-(4,5,6,7-Tetrahydrothieno[3,2-c]pyridin-5-yl)-2-{4-[3- (trifluoromethyl)phenyl]piperazin-1-yl}ethanone ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 92.985(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 32.692(6) _cell_length_b 6.3772(11) _cell_length_c 18.215(3) _cell_measurement_reflns_used 6174 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 27.9 _cell_measurement_theta_min 1.2 _cell_volume 3792.4(11) _computing_cell_refinement 'CrystalClear (Rigaku/MSC, 2005)' _computing_data_collection 'CrystalClear (Rigaku/MSC, 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC, 2005)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure (Rigaku/MSC, 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 113(2) _diffrn_detector_area_resol_mean 14.22 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator multilayer _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18550 _diffrn_reflns_theta_full 27.88 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_min 1.25 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.215 _exptl_absorpt_correction_T_max 0.9746 _exptl_absorpt_correction_T_min 0.9582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(CrystalClear; Rigaku/MSC, 2005)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 1712 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.329 _refine_diff_density_min -0.329 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 4523 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0324 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.0967 _reflns_number_gt 3449 _reflns_number_total 4523 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file cv5266.cif _cod_data_source_block I _cod_original_cell_volume 3792.5(11) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2234557 _cod_database_fobs_code 2234557 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' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity S S1 1.129431(9) 0.80354(5) 0.452757(18) 0.02545(10) Uani d . 1 1 F F1 0.76604(3) 0.73309(12) 0.07407(4) 0.0338(2) Uani d . 1 1 F F2 0.72213(2) 0.48600(13) 0.05611(5) 0.0396(2) Uani d . 1 1 F F3 0.78186(3) 0.46014(14) 0.01330(4) 0.0394(2) Uani d . 1 1 O O1 0.97125(3) 1.18330(14) 0.40862(6) 0.0298(2) Uani d . 1 1 N N1 1.00374(3) 0.91401(16) 0.35494(6) 0.0198(2) Uani d . 1 1 N N2 0.92131(3) 0.71911(15) 0.37376(6) 0.0174(2) Uani d . 1 1 N N3 0.84845(3) 0.54625(15) 0.30117(5) 0.0170(2) Uani d . 1 1 C C1 1.14276(4) 1.0434(2) 0.41862(8) 0.0293(3) Uani d . 1 1 H H1 1.1687 1.1077 0.4280 0.035 Uiso calc R 1 1 C C2 1.11183(4) 1.1299(2) 0.37667(7) 0.0266(3) Uani d . 1 1 H H2 1.1137 1.2619 0.3529 0.032 Uiso calc R 1 1 C C3 1.07608(3) 1.0008(2) 0.37202(7) 0.0206(3) Uani d . 1 1 C C4 1.03599(4) 1.0538(2) 0.33102(7) 0.0238(3) Uani d . 1 1 H H4A 1.0286 1.2013 0.3408 0.029 Uiso calc R 1 1 H H4B 1.0389 1.0378 0.2775 0.029 Uiso calc R 1 1 C C5 1.01539(4) 0.69138(19) 0.35519(7) 0.0215(3) Uani d . 1 1 H H5A 1.0255 0.6524 0.3067 0.026 Uiso calc R 1 1 H H5B 0.9912 0.6036 0.3642 0.026 Uiso calc R 1 1 C C6 1.04896(4) 0.6520(2) 0.41531(7) 0.0221(3) Uani d . 1 1 H H6A 1.0372 0.6564 0.4643 0.026 Uiso calc R 1 1 H H6B 1.0612 0.5118 0.4087 0.026 Uiso calc R 1 1 C C7 1.08114(3) 0.81855(19) 0.41028(7) 0.0198(3) Uani d . 1 1 C C8 0.97449(4) 0.99396(19) 0.39714(7) 0.0194(3) Uani d . 1 1 C C9 0.94467(4) 0.84037(19) 0.42992(7) 0.0201(3) Uani d . 1 1 H H9A 0.9602 0.7426 0.4632 0.024 Uiso calc R 1 1 H H9B 0.9254 0.9193 0.4597 0.024 Uiso calc R 1 1 C C10 0.89218(4) 0.85104(19) 0.33157(7) 0.0207(3) Uani d . 1 1 H H10A 0.9069 0.9690 0.3095 0.025 Uiso calc R 1 1 H H10B 0.8721 0.9103 0.3648 0.025 Uiso calc R 1 1 C C11 0.86980(4) 0.72588(19) 0.27125(7) 0.0212(3) Uani d . 1 1 H H11A 0.8498 0.8176 0.2442 0.025 Uiso calc R 1 1 H H11B 0.8897 0.6758 0.2360 0.025 Uiso calc R 1 1 C C12 0.87583(4) 0.4201(2) 0.35010(7) 0.0240(3) Uani d . 1 1 H H12A 0.8962 0.3479 0.3206 0.029 Uiso calc R 1 1 H H12B 0.8596 0.3116 0.3744 0.029 Uiso calc R 1 1 C C13 0.89803(4) 0.55328(19) 0.40811(7) 0.0232(3) Uani d . 1 1 H H13A 0.8779 0.6166 0.4404 0.028 Uiso calc R 1 1 H H13B 0.9169 0.4642 0.4389 0.028 Uiso calc R 1 1 C C14 0.82152(3) 0.43532(18) 0.25274(6) 0.0163(2) Uani d . 1 1 C C15 0.80737(3) 0.23339(18) 0.26919(7) 0.0183(3) Uani d . 1 1 H H15 0.8172 0.1666 0.3133 0.022 Uiso calc R 1 1 C C16 0.77936(3) 0.12972(19) 0.22235(7) 0.0192(3) Uani d . 1 1 H H16 0.7707 -0.0075 0.2347 0.023 Uiso calc R 1 1 C C17 0.76363(4) 0.22165(18) 0.15800(7) 0.0193(3) Uani d . 1 1 H H17 0.7441 0.1510 0.1264 0.023 Uiso calc R 1 1 C C18 0.77749(3) 0.42091(18) 0.14144(6) 0.0179(2) Uani d . 1 1 C C19 0.80626(3) 0.52536(18) 0.18650(6) 0.0173(2) Uani d . 1 1 H H19 0.8158 0.6595 0.1724 0.021 Uiso calc R 1 1 C C20 0.76198(4) 0.5249(2) 0.07173(7) 0.0233(3) Uani d . 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.01591(16) 0.0367(2) 0.02358(18) 0.00031(13) -0.00047(12) -0.00149(14) F1 0.0528(5) 0.0192(4) 0.0272(4) -0.0012(3) -0.0169(4) 0.0034(3) F2 0.0294(4) 0.0463(5) 0.0411(5) -0.0079(4) -0.0182(4) 0.0124(4) F3 0.0558(5) 0.0456(5) 0.0166(4) 0.0109(4) 0.0013(4) -0.0002(4) O1 0.0313(5) 0.0203(5) 0.0382(6) 0.0007(4) 0.0039(4) -0.0036(4) N1 0.0175(5) 0.0211(5) 0.0205(5) -0.0011(4) -0.0016(4) 0.0002(4) N2 0.0159(5) 0.0179(5) 0.0180(5) -0.0004(4) -0.0035(4) 0.0012(4) N3 0.0172(5) 0.0158(5) 0.0175(5) -0.0016(4) -0.0039(4) 0.0039(4) C1 0.0185(6) 0.0419(8) 0.0278(7) -0.0089(6) 0.0047(5) -0.0034(6) C2 0.0240(6) 0.0319(7) 0.0245(7) -0.0068(6) 0.0067(5) -0.0006(6) C3 0.0184(6) 0.0268(6) 0.0166(6) -0.0019(5) 0.0026(5) -0.0033(5) C4 0.0221(6) 0.0272(7) 0.0220(6) -0.0042(5) -0.0006(5) 0.0030(5) C5 0.0198(6) 0.0220(6) 0.0224(7) 0.0009(5) -0.0014(5) -0.0057(5) C6 0.0202(6) 0.0205(6) 0.0253(7) 0.0019(5) -0.0014(5) -0.0020(5) C7 0.0160(6) 0.0256(6) 0.0176(6) 0.0004(5) -0.0005(5) -0.0049(5) C8 0.0178(6) 0.0220(6) 0.0179(6) 0.0004(5) -0.0056(5) -0.0009(5) C9 0.0190(6) 0.0227(6) 0.0184(6) -0.0001(5) -0.0016(5) -0.0022(5) C10 0.0221(6) 0.0159(6) 0.0236(7) -0.0005(5) -0.0046(5) 0.0021(5) C11 0.0236(6) 0.0178(6) 0.0215(6) -0.0050(5) -0.0062(5) 0.0054(5) C12 0.0275(6) 0.0179(6) 0.0256(7) -0.0021(5) -0.0096(5) 0.0072(5) C13 0.0238(6) 0.0232(6) 0.0216(6) -0.0037(5) -0.0073(5) 0.0066(5) C14 0.0135(5) 0.0172(6) 0.0181(6) 0.0019(4) 0.0015(4) 0.0003(5) C15 0.0171(5) 0.0179(6) 0.0198(6) 0.0012(5) 0.0010(5) 0.0028(5) C16 0.0187(6) 0.0153(6) 0.0240(6) -0.0010(4) 0.0042(5) 0.0007(5) C17 0.0185(6) 0.0191(6) 0.0201(6) -0.0006(5) -0.0003(5) -0.0043(5) C18 0.0190(6) 0.0192(6) 0.0156(6) 0.0022(4) -0.0002(5) -0.0006(5) C19 0.0183(5) 0.0152(6) 0.0182(6) -0.0003(4) 0.0003(5) 0.0017(5) C20 0.0284(7) 0.0209(7) 0.0197(6) -0.0021(5) -0.0053(5) -0.0021(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 S1 C7 91.82(6) C8 N1 C4 118.63(11) C8 N1 C5 123.45(10) C4 N1 C5 113.49(10) C10 N2 C13 107.61(9) C10 N2 C9 111.45(9) C13 N2 C9 110.30(10) C14 N3 C11 117.15(10) C14 N3 C12 116.58(10) C11 N3 C12 111.56(9) C2 C1 S1 111.82(10) C2 C1 H1 124.1 S1 C1 H1 124.1 C1 C2 C3 112.56(12) C1 C2 H2 123.7 C3 C2 H2 123.7 C7 C3 C2 112.61(11) C7 C3 C4 121.55(11) C2 C3 C4 125.83(12) N1 C4 C3 109.61(10) N1 C4 H4A 109.7 C3 C4 H4A 109.7 N1 C4 H4B 109.7 C3 C4 H4B 109.7 H4A C4 H4B 108.2 N1 C5 C6 109.69(10) N1 C5 H5A 109.7 C6 C5 H5A 109.7 N1 C5 H5B 109.7 C6 C5 H5B 109.7 H5A C5 H5B 108.2 C7 C6 C5 108.60(11) C7 C6 H6A 110.0 C5 C6 H6A 110.0 C7 C6 H6B 110.0 C5 C6 H6B 110.0 H6A C6 H6B 108.4 C3 C7 C6 124.64(11) C3 C7 S1 111.19(9) C6 C7 S1 124.17(10) O1 C8 N1 122.29(12) O1 C8 C9 120.06(11) N1 C8 C9 117.65(11) N2 C9 C8 112.71(10) N2 C9 H9A 109.0 C8 C9 H9A 109.0 N2 C9 H9B 109.0 C8 C9 H9B 109.0 H9A C9 H9B 107.8 N2 C10 C11 110.82(10) N2 C10 H10A 109.5 C11 C10 H10A 109.5 N2 C10 H10B 109.5 C11 C10 H10B 109.5 H10A C10 H10B 108.1 N3 C11 C10 111.36(10) N3 C11 H11A 109.4 C10 C11 H11A 109.4 N3 C11 H11B 109.4 C10 C11 H11B 109.4 H11A C11 H11B 108.0 N3 C12 C13 111.82(10) N3 C12 H12A 109.3 C13 C12 H12A 109.3 N3 C12 H12B 109.3 C13 C12 H12B 109.3 H12A C12 H12B 107.9 N2 C13 C12 110.42(10) N2 C13 H13A 109.6 C12 C13 H13A 109.6 N2 C13 H13B 109.6 C12 C13 H13B 109.6 H13A C13 H13B 108.1 C19 C14 N3 121.12(10) C19 C14 C15 116.85(10) N3 C14 C15 121.99(10) C16 C15 C14 121.31(11) C16 C15 H15 119.3 C14 C15 H15 119.3 C17 C16 C15 121.54(11) C17 C16 H16 119.2 C15 C16 H16 119.2 C16 C17 C18 117.41(11) C16 C17 H17 121.3 C18 C17 H17 121.3 C19 C18 C17 122.05(11) C19 C18 C20 118.61(10) C17 C18 C20 119.32(11) C18 C19 C14 120.80(11) C18 C19 H19 119.6 C14 C19 H19 119.6 F1 C20 F3 106.27(11) F1 C20 F2 106.51(10) F3 C20 F2 106.27(10) F1 C20 C18 112.62(10) F3 C20 C18 112.34(10) F2 C20 C18 112.35(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C1 1.7161(14) S1 C7 1.7241(12) F1 C20 1.3350(14) F2 C20 1.3420(14) F3 C20 1.3407(15) O1 C8 1.2309(15) N1 C8 1.3571(15) N1 C4 1.4644(16) N1 C5 1.4699(16) N2 C10 1.4591(15) N2 C13 1.4624(15) N2 C9 1.4651(15) N3 C14 1.4047(15) N3 C11 1.4617(15) N3 C12 1.4695(15) C1 C2 1.3528(19) C1 H1 0.9500 C2 C3 1.4288(17) C2 H2 0.9500 C3 C7 1.3606(18) C3 C4 1.5124(17) C4 H4A 0.9900 C4 H4B 0.9900 C5 C6 1.5301(17) C5 H5A 0.9900 C5 H5B 0.9900 C6 C7 1.5013(17) C6 H6A 0.9900 C6 H6B 0.9900 C8 C9 1.5254(17) C9 H9A 0.9900 C9 H9B 0.9900 C10 C11 1.5153(16) C10 H10A 0.9900 C10 H10B 0.9900 C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.5114(17) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13A 0.9900 C13 H13B 0.9900 C14 C19 1.4041(16) C14 C15 1.4059(16) C15 C16 1.3865(17) C15 H15 0.9500 C16 C17 1.3854(17) C16 H16 0.9500 C17 C18 1.3877(17) C17 H17 0.9500 C18 C19 1.3860(16) C18 C20 1.4973(17) C19 H19 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C6 H6A O1 5_776 0.99 2.56 3.4709(17) 153.1 C13 H13B O1 1_545 0.99 2.60 3.3607(16) 133.4 C16 H16 Cg 4_645 0.95 2.61 3.3641(13) 136 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 C7 S1 C1 C2 -0.21(11) S1 C1 C2 C3 0.45(15) C1 C2 C3 C7 -0.53(17) C1 C2 C3 C4 178.54(12) C8 N1 C4 C3 108.44(12) C5 N1 C4 C3 -48.79(14) C7 C3 C4 N1 14.37(17) C2 C3 C4 N1 -164.62(12) C8 N1 C5 C6 -87.88(13) C4 N1 C5 C6 68.10(13) N1 C5 C6 C7 -46.98(13) C2 C3 C7 C6 -179.84(11) C4 C3 C7 C6 1.05(19) C2 C3 C7 S1 0.36(14) C4 C3 C7 S1 -178.75(10) C5 C6 C7 C3 15.39(17) C5 C6 C7 S1 -164.84(9) C1 S1 C7 C3 -0.09(10) C1 S1 C7 C6 -179.89(11) C4 N1 C8 O1 8.89(18) C5 N1 C8 O1 163.72(11) C4 N1 C8 C9 -171.93(10) C5 N1 C8 C9 -17.10(16) C10 N2 C9 C8 -69.20(13) C13 N2 C9 C8 171.33(9) O1 C8 C9 N2 119.78(12) N1 C8 C9 N2 -59.42(14) C13 N2 C10 C11 -61.83(13) C9 N2 C10 C11 177.12(10) C14 N3 C11 C10 170.67(10) C12 N3 C11 C10 -51.32(14) N2 C10 C11 N3 57.59(13) C14 N3 C12 C13 -170.23(10) C11 N3 C12 C13 51.50(14) C10 N2 C13 C12 61.50(13) C9 N2 C13 C12 -176.74(10) N3 C12 C13 N2 -57.23(14) C11 N3 C14 C19 -18.70(16) C12 N3 C14 C19 -154.62(11) C11 N3 C14 C15 163.73(11) C12 N3 C14 C15 27.81(16) C19 C14 C15 C16 -0.63(17) N3 C14 C15 C16 177.05(11) C14 C15 C16 C17 -1.02(18) C15 C16 C17 C18 1.02(17) C16 C17 C18 C19 0.64(17) C16 C17 C18 C20 178.81(11) C17 C18 C19 C14 -2.33(18) C20 C18 C19 C14 179.49(10) N3 C14 C19 C18 -175.44(10) C15 C14 C19 C18 2.25(17) C19 C18 C20 F1 -23.30(16) C17 C18 C20 F1 158.47(11) C19 C18 C20 F3 96.66(13) C17 C18 C20 F3 -81.57(14) C19 C18 C20 F2 -143.58(11) C17 C18 C20 F2 38.19(16)