#------------------------------------------------------------------------------ #$Date: 2025-08-19 12:52:15 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301804 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/45/2214537.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_2214537 loop_ _publ_author_name 'Muirhead, Kirsty E. A.' 'Trembleau, Laurent' 'Harrison, William T. A.' _publ_section_title 5-Chloro-3-ethyl-N-[3-(morpholin-4-yl)propyl]-1H-indole-2-carboxamide _journal_coeditor_code BT2413 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3390 _journal_page_last o3390 _journal_paper_doi 10.1107/S1600536807031182 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'C18 H24 Cl N3 O2' _chemical_formula_moiety 'C18 H24 Cl N3 O2' _chemical_formula_sum 'C18 H24 Cl N3 O2' _chemical_formula_weight 349.85 _chemical_name_systematic ; 5-Chloro-3-ethyl-N-[3-(morpholin-4-yl)propyl]-1H-indole-2-carboxamide ; _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 _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.265(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 4.8178(3) _cell_length_b 12.1967(12) _cell_length_c 29.576(3) _cell_measurement_reflns_used 3212 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 1735.1(3) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction ; SCALEPACK and DENZO (Otwinowski & Minor, 1997), and SORTAV (Blessing, 1995) ; _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.955 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f' _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 0.0892 _diffrn_reflns_av_sigmaI/netI 0.1157 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 10192 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 3.23 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _refine_diff_density_max 1.246 _refine_diff_density_min -0.514 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 3092 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all 0.1993 _refine_ls_R_factor_gt 0.1422 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+36.1132P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3029 _refine_ls_wR_factor_ref 0.3420 _reflns_number_gt 2077 _reflns_number_total 3092 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt2413.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2214537 _cod_database_fobs_code 2214537 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_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 C C1 0.112(2) 0.1461(9) 0.6108(3) 0.027(2) Uani d . 1 C C2 -0.090(2) 0.2101(9) 0.6287(3) 0.024(2) Uani d . 1 H H2A -0.1399 0.1994 0.6590 0.029 Uiso calc R 1 C C3 -0.224(2) 0.2917(8) 0.6014(3) 0.023(2) Uani d . 1 H H3 -0.3634 0.3375 0.6127 0.028 Uiso calc R 1 C C4 -0.142(2) 0.3021(8) 0.5575(3) 0.022(2) Uani d . 1 C C5 0.074(2) 0.2366(8) 0.5398(3) 0.022(2) Uani d . 1 C C6 0.198(2) 0.1578(9) 0.5676(3) 0.026(2) Uani d . 1 H H6 0.3415 0.1124 0.5570 0.032 Uiso calc R 1 C C7 0.1034(19) 0.2705(7) 0.4939(3) 0.016(2) Uani d . 1 C C8 -0.085(2) 0.3538(8) 0.4852(3) 0.021(2) Uani d . 1 C C9 0.281(2) 0.2097(8) 0.4623(3) 0.023(2) Uani d . 1 H H9A 0.3255 0.2590 0.4371 0.027 Uiso calc R 1 H H9B 0.4586 0.1896 0.4788 0.027 Uiso calc R 1 C C10 0.148(3) 0.1086(10) 0.4432(4) 0.041(3) Uani d . 1 H H10A 0.1087 0.0583 0.4678 0.062 Uiso calc R 1 H H10B 0.2734 0.0731 0.4227 0.062 Uiso calc R 1 H H10C -0.0263 0.1279 0.4263 0.062 Uiso calc R 1 C C11 -0.178(2) 0.4151(8) 0.4436(3) 0.018(2) Uani d . 1 C C12 -0.083(2) 0.4638(8) 0.3662(3) 0.021(2) Uani d . 1 H H12A 0.0742 0.5053 0.3544 0.025 Uiso calc R 1 H H12B -0.2397 0.5153 0.3688 0.025 Uiso calc R 1 C C13 -0.169(2) 0.3744(8) 0.3327(3) 0.024(2) Uani d . 1 H H13A -0.3204 0.3305 0.3451 0.029 Uiso calc R 1 H H13B -0.2435 0.4085 0.3041 0.029 Uiso calc R 1 C C14 0.066(2) 0.3002(9) 0.3228(3) 0.026(2) Uani d . 1 H H14A 0.2163 0.3448 0.3106 0.032 Uiso calc R 1 H H14B 0.1401 0.2671 0.3515 0.032 Uiso calc R 1 C C15 -0.048(2) 0.2544(9) 0.2446(3) 0.027(2) Uani d . 1 H H15A 0.1210 0.2943 0.2364 0.033 Uiso calc R 1 H H15B -0.2051 0.3067 0.2433 0.033 Uiso calc R 1 C C16 -0.108(2) 0.1619(9) 0.2110(3) 0.027(2) Uani d . 1 H H16A -0.2797 0.1231 0.2187 0.032 Uiso calc R 1 H H16B -0.1397 0.1928 0.1802 0.032 Uiso calc R 1 C C17 0.157(2) 0.0414(9) 0.2558(3) 0.030(2) Uani d . 1 H H17A 0.3140 -0.0111 0.2563 0.035 Uiso calc R 1 H H17B -0.0115 0.0010 0.2636 0.035 Uiso calc R 1 C C18 0.220(2) 0.1316(9) 0.2909(3) 0.026(2) Uani d . 1 H H18A 0.2460 0.0984 0.3214 0.032 Uiso calc R 1 H H18B 0.3955 0.1692 0.2841 0.032 Uiso calc R 1 N N1 -0.2339(17) 0.3725(7) 0.5236(3) 0.0200(18) Uani d . 1 H H1 -0.3660 0.4217 0.5258 0.024 Uiso calc R 1 N N2 0.0005(18) 0.4218(7) 0.4110(2) 0.0220(19) Uani d . 1 H H2 0.1733 0.4002 0.4167 0.026 Uiso calc R 1 N N3 -0.0063(17) 0.2115(7) 0.2905(2) 0.0220(19) Uani d . 1 O O1 -0.4206(13) 0.4529(6) 0.4399(2) 0.0213(15) Uani d . 1 O O2 0.1154(15) 0.0870(6) 0.2116(2) 0.0261(17) Uani d . 1 Cl Cl1 0.2751(6) 0.0473(2) 0.64686(9) 0.0329(7) Uani d . 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 C1 0.031(6) 0.020(6) 0.030(6) -0.001(5) -0.008(5) 0.003(5) C2 0.032(6) 0.029(6) 0.011(4) 0.001(5) 0.002(4) -0.001(4) C3 0.021(5) 0.022(6) 0.026(5) -0.002(4) 0.007(4) -0.010(4) C4 0.027(6) 0.019(5) 0.021(5) -0.010(4) 0.001(4) 0.000(4) C5 0.023(5) 0.025(6) 0.017(5) -0.005(4) 0.000(4) -0.002(4) C6 0.035(6) 0.024(6) 0.020(5) -0.001(5) 0.001(4) 0.001(4) C7 0.026(5) 0.008(5) 0.013(4) -0.006(4) 0.003(4) -0.005(3) C8 0.025(5) 0.020(5) 0.019(5) -0.004(4) 0.006(4) -0.005(4) C9 0.038(6) 0.015(5) 0.015(4) 0.002(4) 0.000(4) 0.000(4) C10 0.050(8) 0.033(7) 0.042(7) -0.003(6) 0.016(6) -0.015(6) C11 0.027(6) 0.011(5) 0.014(4) 0.002(4) -0.005(4) -0.005(4) C12 0.029(5) 0.016(5) 0.017(5) 0.007(4) 0.005(4) 0.003(4) C13 0.029(6) 0.022(6) 0.021(5) 0.005(5) -0.004(4) -0.002(4) C14 0.037(6) 0.029(6) 0.012(4) 0.002(5) 0.000(4) -0.006(4) C15 0.034(6) 0.027(6) 0.021(5) -0.003(5) 0.003(4) 0.004(4) C16 0.033(6) 0.031(6) 0.016(5) 0.008(5) 0.000(4) 0.000(4) C17 0.041(7) 0.014(5) 0.034(6) 0.002(5) 0.003(5) -0.001(5) C18 0.025(6) 0.027(6) 0.027(5) 0.011(5) 0.002(4) 0.009(5) N1 0.020(4) 0.017(4) 0.024(4) 0.008(4) 0.006(3) 0.002(3) N2 0.028(5) 0.026(5) 0.011(4) 0.005(4) -0.003(3) -0.004(3) N3 0.031(5) 0.024(5) 0.011(4) 0.005(4) 0.000(3) -0.004(3) O1 0.019(4) 0.023(4) 0.021(3) 0.002(3) 0.000(3) 0.000(3) O2 0.038(4) 0.022(4) 0.019(3) 0.003(3) 0.005(3) -0.004(3) Cl1 0.0442(16) 0.0303(15) 0.0239(12) 0.0014(13) -0.0005(11) 0.0092(12) 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' Cl Cl 0.1484 0.1585 '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 C6 C1 C2 123.8(10) C6 C1 Cl1 119.0(9) C2 C1 Cl1 117.1(8) C1 C2 C3 119.3(9) C1 C2 H2A 120.4 C3 C2 H2A 120.4 C4 C3 C2 117.1(9) C4 C3 H3 121.5 C2 C3 H3 121.5 N1 C4 C3 130.0(10) N1 C4 C5 107.0(8) C3 C4 C5 122.9(9) C6 C5 C4 118.1(9) C6 C5 C7 134.5(10) C4 C5 C7 107.5(8) C1 C6 C5 118.8(10) C1 C6 H6 120.6 C5 C6 H6 120.6 C8 C7 C5 106.7(8) C8 C7 C9 130.0(8) C5 C7 C9 122.6(8) C7 C8 N1 109.5(8) C7 C8 C11 133.7(9) N1 C8 C11 116.4(8) C10 C9 C7 113.4(9) C10 C9 H9A 108.9 C7 C9 H9A 108.9 C10 C9 H9B 108.9 C7 C9 H9B 108.9 H9A C9 H9B 107.7 C9 C10 H10A 109.5 C9 C10 H10B 109.5 H10A C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 O1 C11 N2 123.4(8) O1 C11 C8 119.7(9) N2 C11 C8 116.8(8) N2 C12 C13 113.2(8) N2 C12 H12A 108.9 C13 C12 H12A 108.9 N2 C12 H12B 108.9 C13 C12 H12B 108.9 H12A C12 H12B 107.8 C14 C13 C12 112.4(8) C14 C13 H13A 109.1 C12 C13 H13A 109.1 C14 C13 H13B 109.1 C12 C13 H13B 109.1 H13A C13 H13B 107.9 N3 C14 C13 114.8(8) N3 C14 H14A 108.6 C13 C14 H14A 108.6 N3 C14 H14B 108.6 C13 C14 H14B 108.6 H14A C14 H14B 107.6 N3 C15 C16 110.7(9) N3 C15 H15A 109.5 C16 C15 H15A 109.5 N3 C15 H15B 109.5 C16 C15 H15B 109.5 H15A C15 H15B 108.1 O2 C16 C15 110.7(8) O2 C16 H16A 109.5 C15 C16 H16A 109.5 O2 C16 H16B 109.5 C15 C16 H16B 109.5 H16A C16 H16B 108.1 O2 C17 C18 110.8(8) O2 C17 H17A 109.5 C18 C17 H17A 109.5 O2 C17 H17B 109.5 C18 C17 H17B 109.5 H17A C17 H17B 108.1 N3 C18 C17 110.6(8) N3 C18 H18A 109.5 C17 C18 H18A 109.5 N3 C18 H18B 109.5 C17 C18 H18B 109.5 H18A C18 H18B 108.1 C4 N1 C8 109.3(8) C4 N1 H1 125.4 C8 N1 H1 125.4 C11 N2 C12 121.7(8) C11 N2 H2 119.2 C12 N2 H2 119.2 C15 N3 C18 108.1(8) C15 N3 C14 110.8(8) C18 N3 C14 109.5(8) C16 O2 C17 109.4(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C6 1.375(14) C1 C2 1.377(15) C1 Cl1 1.763(10) C2 C3 1.412(14) C2 H2A 0.9500 C3 C4 1.385(13) C3 H3 0.9500 C4 N1 1.374(12) C4 C5 1.432(14) C5 C6 1.381(14) C5 C7 1.434(12) C6 H6 0.9500 C7 C8 1.376(14) C7 C9 1.499(13) C8 N1 1.397(12) C8 C11 1.487(13) C9 C10 1.487(15) C9 H9A 0.9900 C9 H9B 0.9900 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 O1 1.253(11) C11 N2 1.333(12) C12 N2 1.455(11) C12 C13 1.516(14) C12 H12A 0.9900 C12 H12B 0.9900 C13 C14 1.494(14) C13 H13A 0.9900 C13 H13B 0.9900 C14 N3 1.472(12) C14 H14A 0.9900 C14 H14B 0.9900 C15 N3 1.456(12) C15 C16 1.522(14) C15 H15A 0.9900 C15 H15B 0.9900 C16 O2 1.413(12) C16 H16A 0.9900 C16 H16B 0.9900 C17 O2 1.425(12) C17 C18 1.531(15) C17 H17A 0.9900 C17 H17B 0.9900 C18 N3 1.463(12) C18 H18A 0.9900 C18 H18B 0.9900 N1 H1 0.8800 N2 H2 0.8800 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 N1 H1 O1 3_466 0.88 2.13 2.945(10) 153 N2 H2 O1 1_655 0.88 2.13 2.895(10) 144 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 C6 C1 C2 C3 1.1(17) Cl1 C1 C2 C3 178.9(8) C1 C2 C3 C4 0.3(15) C2 C3 C4 N1 179.5(10) C2 C3 C4 C5 -1.8(15) N1 C4 C5 C6 -179.3(9) C3 C4 C5 C6 1.8(15) N1 C4 C5 C7 -0.5(11) C3 C4 C5 C7 -179.5(9) C2 C1 C6 C5 -1.1(17) Cl1 C1 C6 C5 -178.9(8) C4 C5 C6 C1 -0.3(15) C7 C5 C6 C1 -178.7(11) C6 C5 C7 C8 179.2(11) C4 C5 C7 C8 0.7(11) C6 C5 C7 C9 7.3(18) C4 C5 C7 C9 -171.2(9) C5 C7 C8 N1 -0.7(11) C9 C7 C8 N1 170.4(9) C5 C7 C8 C11 -172.5(11) C9 C7 C8 C11 -1.4(18) C8 C7 C9 C10 -91.6(13) C5 C7 C9 C10 78.3(12) C7 C8 C11 O1 150.4(11) N1 C8 C11 O1 -20.9(13) C7 C8 C11 N2 -26.3(16) N1 C8 C11 N2 162.4(9) N2 C12 C13 C14 -65.2(11) C12 C13 C14 N3 179.8(8) N3 C15 C16 O2 -60.3(11) O2 C17 C18 N3 58.3(11) C3 C4 N1 C8 178.9(10) C5 C4 N1 C8 0.0(11) C7 C8 N1 C4 0.5(11) C11 C8 N1 C4 173.8(8) O1 C11 N2 C12 -6.7(14) C8 C11 N2 C12 169.9(8) C13 C12 N2 C11 -94.2(11) C16 C15 N3 C18 57.2(11) C16 C15 N3 C14 177.2(9) C17 C18 N3 C15 -56.3(11) C17 C18 N3 C14 -177.1(8) C13 C14 N3 C15 73.0(11) C13 C14 N3 C18 -167.9(9) C15 C16 O2 C17 60.0(11) C18 C17 O2 C16 -59.2(11) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 21123970 2 PubChem 139072624