#------------------------------------------------------------------------------ #$Date: 2025-08-19 12:52:15 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301804 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/43/2214359.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_2214359 loop_ _publ_author_name 'Lu, Hai-Hua' 'Chen, Cai-Bao' 'Hong-Ming Dong' _publ_section_title (S)-2-(1-Benzyl-5-bromo-1H-indol-3-yl)-2-hydroxy-N-methylacetamide _journal_coeditor_code OM2117 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3261 _journal_page_last o3261 _journal_paper_doi 10.1107/S1600536807025767 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'C18 H17 Br N2 O2' _chemical_formula_moiety 'C18 H17 Br N2 O2' _chemical_formula_sum 'C18 H17 Br N2 O2' _chemical_formula_weight 373.25 _chemical_name_systematic ; (S)-2-(1-Benzyl-5-bromo-1H-indol-3-yl)-2-hydroxy-N- methylacetamide ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 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 95.049(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 4.5759(6) _cell_length_b 9.4134(11) _cell_length_c 18.540(2) _cell_measurement_reflns_used 2442 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 0.00 _cell_measurement_theta_min 0.00 _cell_volume 795.51(16) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics ; SHELXTL (Sheldrick, 2001b) and PLATON (Spek, 2003) ; _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 5321 _diffrn_reflns_theta_full 27.99 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_min 2.21 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.595 _exptl_absorpt_correction_T_max 0.7814 _exptl_absorpt_correction_T_min 0.6249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2001a)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 380 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.401 _refine_diff_density_min -0.323 _refine_ls_abs_structure_details 'Flack (1983), 1456 Friedel pairs' _refine_ls_abs_structure_Flack 0.015(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 215 _refine_ls_number_reflns 3482 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.945 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0287 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.0627 _reflns_number_gt 2936 _reflns_number_total 3482 _reflns_threshold_expression I>2\s(I) _cod_data_source_file om2117.cif _cod_data_source_block 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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 795.51(17) _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2214359 _cod_database_fobs_code 2214359 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 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 Br Br1 1.14694(7) -0.31988(3) 0.737099(16) 0.06370(11) Uani d . 1 C C1 0.6534(6) 0.0039(3) 0.81575(12) 0.0391(6) Uani d . 1 H H1A 0.5425 0.0180 0.8548 0.047 Uiso calc R 1 C C2 0.8019(6) -0.1216(3) 0.80734(13) 0.0433(6) Uani d . 1 H H2 0.7932 -0.1936 0.8414 0.052 Uiso calc R 1 C C3 0.9654(6) -0.1411(3) 0.74796(13) 0.0391(5) Uani d . 1 C C4 0.9924(5) -0.0383(2) 0.69649(12) 0.0341(5) Uani d . 1 H H4 1.1062 -0.0534 0.6580 0.041 Uiso calc R 1 C C5 0.8429(5) 0.0900(2) 0.70371(11) 0.0298(5) Uani d . 1 C C6 0.6757(5) 0.1082(3) 0.76376(12) 0.0318(5) Uani d . 1 C C7 0.8163(5) 0.2179(2) 0.66256(11) 0.0317(5) Uani d . 1 C C8 0.6355(5) 0.3059(3) 0.69713(12) 0.0357(5) Uani d . 1 H H8 0.5795 0.3967 0.6817 0.043 Uiso calc R 1 C C9 0.3612(5) 0.3018(3) 0.81004(12) 0.0403(5) Uani d . 1 H H9A 0.2210 0.2306 0.8225 0.048 Uiso calc R 1 H H9B 0.2518 0.3806 0.7874 0.048 Uiso calc R 1 C C10 0.5304(5) 0.3531(3) 0.87805(12) 0.0362(5) Uani d . 1 C C11 0.7243(6) 0.4648(3) 0.87613(14) 0.0482(6) Uani d . 1 H H11 0.7512 0.5078 0.8320 0.058 Uiso calc R 1 C C12 0.8776(7) 0.5135(4) 0.93757(19) 0.0689(9) Uani d . 1 H H12 1.0081 0.5887 0.9350 0.083 Uiso calc R 1 C C13 0.8399(8) 0.4520(5) 1.00341(18) 0.0757(11) Uani d . 1 H H13 0.9437 0.4858 1.0453 0.091 Uiso calc R 1 C C14 0.6496(9) 0.3411(4) 1.00709(15) 0.0733(11) Uani d . 1 H H14 0.6246 0.2985 1.0514 0.088 Uiso calc R 1 C C15 0.4936(7) 0.2922(3) 0.94434(13) 0.0545(7) Uani d . 1 H H15 0.3624 0.2173 0.9470 0.065 Uiso calc R 1 C C16 0.9457(5) 0.2509(2) 0.59302(12) 0.0352(5) Uani d . 1 H H16 1.1449 0.2120 0.5951 0.042 Uiso calc R 1 C C17 0.7595(5) 0.1810(3) 0.53065(10) 0.0338(4) Uani d . 1 C C18 0.3941(7) 0.2177(3) 0.42835(13) 0.0538(8) Uani d . 1 H H18A 0.5083 0.1786 0.3921 0.081 Uiso calc R 1 H H18B 0.2787 0.2955 0.4081 0.081 Uiso calc R 1 H H18C 0.2667 0.1457 0.4446 0.081 Uiso calc R 1 H H1 1.088(8) 0.418(4) 0.5528(18) 0.081 Uiso d . 1 H H2A 0.572(7) 0.358(3) 0.4998(16) 0.065 Uiso d . 1 N N1 0.5491(5) 0.2407(2) 0.75786(10) 0.0357(5) Uani d . 1 N N2 0.5881(5) 0.2677(2) 0.48896(11) 0.0400(5) Uani d . 1 O O1 0.9600(4) 0.40069(17) 0.58655(9) 0.0473(4) Uani d . 1 O O2 0.7673(4) 0.05083(18) 0.52216(9) 0.0470(4) 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 Br1 0.0778(2) 0.03513(14) 0.0805(2) 0.01527(16) 0.02007(15) 0.01439(16) C1 0.0485(15) 0.0387(14) 0.0309(11) -0.0056(11) 0.0081(11) 0.0018(10) C2 0.0576(16) 0.0373(14) 0.0348(12) -0.0030(12) 0.0021(11) 0.0105(10) C3 0.0440(14) 0.0296(12) 0.0428(13) 0.0029(10) -0.0012(11) 0.0021(10) C4 0.0362(12) 0.0327(12) 0.0333(11) -0.0003(9) 0.0023(10) -0.0031(9) C5 0.0320(12) 0.0310(12) 0.0260(11) -0.0047(9) 0.0010(9) -0.0029(9) C6 0.0364(14) 0.0324(13) 0.0262(11) -0.0044(10) 0.0001(10) -0.0015(10) C7 0.0372(12) 0.0282(13) 0.0295(11) -0.0015(8) 0.0017(9) -0.0013(8) C8 0.0437(14) 0.0301(12) 0.0329(12) 0.0022(10) 0.0010(10) -0.0012(10) C9 0.0381(13) 0.0436(14) 0.0400(13) 0.0040(11) 0.0082(10) -0.0024(11) C10 0.0405(13) 0.0346(13) 0.0347(12) 0.0062(10) 0.0096(10) -0.0053(10) C11 0.0534(17) 0.0466(16) 0.0447(14) -0.0031(13) 0.0046(13) -0.0055(12) C12 0.0581(19) 0.065(2) 0.081(2) -0.0043(16) -0.0046(17) -0.0260(18) C13 0.078(2) 0.086(3) 0.058(2) 0.036(2) -0.0207(18) -0.0336(19) C14 0.113(3) 0.077(3) 0.0312(15) 0.044(2) 0.0104(17) 0.0035(15) C15 0.075(2) 0.0504(17) 0.0411(15) 0.0064(16) 0.0212(14) 0.0033(13) C16 0.0404(13) 0.0287(12) 0.0371(12) -0.0001(10) 0.0070(10) 0.0034(9) C17 0.0456(11) 0.0293(10) 0.0283(9) 0.0020(13) 0.0135(9) 0.0016(12) C18 0.0660(17) 0.058(2) 0.0360(12) -0.0011(13) -0.0042(12) 0.0037(11) N1 0.0426(12) 0.0356(11) 0.0297(10) 0.0011(10) 0.0072(9) -0.0021(8) N2 0.0551(13) 0.0321(11) 0.0327(10) 0.0015(10) 0.0028(9) 0.0017(9) O1 0.0682(12) 0.0299(10) 0.0453(9) -0.0101(9) 0.0148(9) 0.0029(7) O2 0.0721(13) 0.0283(9) 0.0405(9) 0.0045(9) 0.0045(9) -0.0032(7) 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' Br Br -0.2901 2.4595 '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 C2 C1 C6 117.5(2) C2 C1 H1A 121.3 C6 C1 H1A 121.3 C1 C2 C3 120.4(2) C1 C2 H2 119.8 C3 C2 H2 119.8 C4 C3 C2 122.9(2) C4 C3 Br1 119.02(18) C2 C3 Br1 118.10(18) C3 C4 C5 117.9(2) C3 C4 H4 121.1 C5 C4 H4 121.1 C4 C5 C6 118.8(2) C4 C5 C7 134.2(2) C6 C5 C7 107.0(2) N1 C6 C1 129.9(2) N1 C6 C5 107.5(2) C1 C6 C5 122.6(2) C8 C7 C5 106.69(19) C8 C7 C16 125.3(2) C5 C7 C16 127.91(19) C7 C8 N1 110.1(2) C7 C8 H8 125.0 N1 C8 H8 125.0 N1 C9 C10 113.0(2) N1 C9 H9A 109.0 C10 C9 H9A 109.0 N1 C9 H9B 109.0 C10 C9 H9B 109.0 H9A C9 H9B 107.8 C11 C10 C15 118.0(2) C11 C10 C9 120.7(2) C15 C10 C9 121.3(2) C12 C11 C10 121.3(3) C12 C11 H11 119.3 C10 C11 H11 119.3 C11 C12 C13 120.3(3) C11 C12 H12 119.9 C13 C12 H12 119.9 C14 C13 C12 119.8(3) C14 C13 H13 120.1 C12 C13 H13 120.1 C13 C14 C15 119.6(3) C13 C14 H14 120.2 C15 C14 H14 120.2 C10 C15 C14 121.0(3) C10 C15 H15 119.5 C14 C15 H15 119.5 O1 C16 C7 107.67(18) O1 C16 C17 113.1(2) C7 C16 C17 109.08(18) O1 C16 H16 109.0 C7 C16 H16 109.0 C17 C16 H16 109.0 O2 C17 N2 123.8(2) O2 C17 C16 120.3(2) N2 C17 C16 116.0(2) N2 C18 H18A 109.5 N2 C18 H18B 109.5 H18A C18 H18B 109.5 N2 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C8 N1 C6 108.7(2) C8 N1 C9 126.5(2) C6 N1 C9 124.8(2) C17 N2 C18 122.7(2) C17 N2 H2A 121(2) C18 N2 H2A 116(2) C16 O1 H1 106(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C3 1.895(2) C1 C2 1.378(4) C1 C6 1.386(3) C1 H1A 0.9300 C2 C3 1.397(4) C2 H2 0.9300 C3 C4 1.372(3) C4 C5 1.400(3) C4 H4 0.9300 C5 C6 1.416(3) C5 C7 1.425(3) C6 N1 1.375(3) C7 C8 1.369(3) C7 C16 1.498(3) C8 N1 1.371(3) C8 H8 0.9300 C9 N1 1.467(3) C9 C10 1.500(3) C9 H9A 0.9700 C9 H9B 0.9700 C10 C11 1.378(4) C10 C15 1.380(3) C11 C12 1.363(4) C11 H11 0.9300 C12 C13 1.376(5) C12 H12 0.9300 C13 C14 1.365(5) C13 H13 0.9300 C14 C15 1.389(5) C14 H14 0.9300 C15 H15 0.9300 C16 O1 1.418(3) C16 C17 1.524(3) C16 H16 0.9800 C17 O2 1.236(4) C17 N2 1.331(3) C18 N2 1.448(3) C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 N2 H2A 0.87(3) O1 H1 0.91(4) 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 N2 H2A O1 . 0.87(3) 2.32(3) 2.682(3) 105(2) C18 H18C O1 2_646 0.96 2.57 3.395(3) 143.7 N2 H2A O2 2_656 0.87(3) 2.40(3) 3.119(3) 139(3) O1 H1 O2 2_756 0.91(4) 2.02(4) 2.839(2) 149(3) 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 -0.5(4) C1 C2 C3 C4 1.3(4) C1 C2 C3 Br1 -176.7(2) C2 C3 C4 C5 -1.4(4) Br1 C3 C4 C5 176.59(17) C3 C4 C5 C6 0.8(3) C3 C4 C5 C7 -179.7(2) C2 C1 C6 N1 178.8(2) C2 C1 C6 C5 0.0(4) C4 C5 C6 N1 -179.2(2) C7 C5 C6 N1 1.2(2) C4 C5 C6 C1 -0.1(3) C7 C5 C6 C1 -179.7(2) C4 C5 C7 C8 179.5(2) C6 C5 C7 C8 -1.0(3) C4 C5 C7 C16 2.1(4) C6 C5 C7 C16 -178.3(2) C5 C7 C8 N1 0.4(3) C16 C7 C8 N1 177.8(2) N1 C9 C10 C11 65.1(3) N1 C9 C10 C15 -116.1(3) C15 C10 C11 C12 0.5(4) C9 C10 C11 C12 179.4(3) C10 C11 C12 C13 -0.3(5) C11 C12 C13 C14 0.4(5) C12 C13 C14 C15 -0.6(5) C11 C10 C15 C14 -0.7(4) C9 C10 C15 C14 -179.5(2) C13 C14 C15 C10 0.7(4) C8 C7 C16 O1 25.1(3) C5 C7 C16 O1 -158.0(2) C8 C7 C16 C17 -97.9(3) C5 C7 C16 C17 78.9(3) O1 C16 C17 O2 167.5(2) C7 C16 C17 O2 -72.7(3) O1 C16 C17 N2 -14.3(3) C7 C16 C17 N2 105.5(2) C7 C8 N1 C6 0.4(3) C7 C8 N1 C9 178.4(2) C1 C6 N1 C8 -180.0(2) C5 C6 N1 C8 -1.0(2) C1 C6 N1 C9 1.9(4) C5 C6 N1 C9 -179.1(2) C10 C9 N1 C8 -101.6(3) C10 C9 N1 C6 76.2(3) O2 C17 N2 C18 -0.7(3) C16 C17 N2 C18 -178.8(2) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 21184733 2 PubChem 139072535