#------------------------------------------------------------------------------ #$Date$ #$Revision$ #$URL$ #------------------------------------------------------------------------------ # # 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_2218176 loop_ _publ_author_name 'Choi, Hong Dae' 'Seo, Pil Ja' 'Son, Byeng Wha' 'Lee, Uk' _publ_section_title ; 7-Bromo-2-methyl-1-(phenylsulfonyl)naphtho[2,1-b]furan ; _journal_coeditor_code JH2063 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o944 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac 'C19 H13 Br O3 S' _chemical_formula_moiety 'C19 H13 Br O3 S' _chemical_formula_sum 'C19 H13 Br O3 S' _chemical_formula_weight 401.26 _chemical_melting_point_gt 483 _chemical_melting_point_lt 484 _chemical_name_systematic ; 7-Bromo-2-methyl-1-(phenylsulfonyl)naphtho[2,1-b]furan ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 107.4290(10) _cell_angle_beta 93.6780(10) _cell_angle_gamma 90.417(2) _cell_formula_units_Z 2 _cell_length_a 7.8583(7) _cell_length_b 8.0025(7) _cell_length_c 13.2780(10) _cell_measurement_reflns_used 4679 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.19 _cell_measurement_theta_min 2.60 _cell_volume 794.72(12) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 10.0 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker SMART CCD' _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 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 6371 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.61 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.732 _exptl_absorpt_correction_T_max 0.571 _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2000)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 404 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.436 _refine_diff_density_min -0.354 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 218 _refine_ls_number_reflns 3084 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0233 _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^)+(0.0451P)^2^+0.2317P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.0782 _reflns_number_gt 2874 _reflns_number_total 3084 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file jh2063.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Br 0.56455(3) 0.99911(3) 0.696889(17) 0.03340(10) Uani d . 1 S S 0.82852(6) 0.36218(7) 0.16782(4) 0.02320(13) Uani d . 1 O O1 0.91789(19) 0.0602(2) 0.34760(12) 0.0280(3) Uani d . 1 O O2 0.9034(2) 0.5362(2) 0.20422(12) 0.0303(3) Uani d . 1 O O3 0.8886(2) 0.2407(2) 0.07411(12) 0.0330(4) Uani d . 1 C C1 0.8504(3) 0.2648(3) 0.26930(16) 0.0228(4) Uani d . 1 C C2 0.8191(2) 0.3362(3) 0.38127(16) 0.0216(4) Uani d . 1 C C3 0.7591(2) 0.4950(3) 0.45075(16) 0.0212(4) Uani d . 1 C C4 0.7119(3) 0.6446(3) 0.42140(17) 0.0248(4) Uani d . 1 H H4 0.7201 0.6435 0.3501 0.030 Uiso calc R 1 C C5 0.6545(3) 0.7918(3) 0.49309(17) 0.0265(4) Uani d . 1 H H5 0.6230 0.8911 0.4717 0.032 Uiso calc R 1 C C6 0.6432(3) 0.7931(3) 0.59824(17) 0.0245(4) Uani d . 1 C C7 0.6885(3) 0.6539(3) 0.63190(17) 0.0256(4) Uani d . 1 H H7 0.6804 0.6593 0.7039 0.031 Uiso calc R 1 C C8 0.7476(3) 0.5013(3) 0.55938(16) 0.0229(4) Uani d . 1 C C9 0.7963(3) 0.3570(3) 0.59591(17) 0.0265(4) Uani d . 1 H H9 0.7877 0.3654 0.6683 0.032 Uiso calc R 1 C C10 0.8549(3) 0.2078(3) 0.52932(17) 0.0269(5) Uani d . 1 H H10 0.8883 0.1115 0.5533 0.032 Uiso calc R 1 C C11 0.8634(3) 0.2034(3) 0.42350(17) 0.0241(4) Uani d . 1 C C12 0.9097(3) 0.0997(3) 0.25436(18) 0.0265(4) Uani d . 1 C C13 0.6075(3) 0.3813(3) 0.14109(15) 0.0238(4) Uani d . 1 C C14 0.5417(3) 0.5444(3) 0.14748(17) 0.0294(5) Uani d . 1 H H14 0.6117 0.6475 0.1741 0.035 Uiso calc R 1 C C15 0.3714(3) 0.5544(4) 0.11432(19) 0.0372(6) Uani d . 1 H H15 0.3246 0.6649 0.1178 0.045 Uiso calc R 1 C C16 0.2704(3) 0.4035(4) 0.07638(19) 0.0404(6) Uani d . 1 H H16 0.1546 0.4108 0.0531 0.049 Uiso calc R 1 C C17 0.3368(3) 0.2418(4) 0.0720(2) 0.0395(6) Uani d . 1 H H17 0.2657 0.1392 0.0473 0.047 Uiso calc R 1 C C18 0.5066(3) 0.2292(3) 0.10354(17) 0.0310(5) Uani d . 1 H H18 0.5533 0.1183 0.0995 0.037 Uiso calc R 1 C C19 0.9685(3) -0.0435(3) 0.1644(2) 0.0379(6) Uani d . 1 H H19A 0.9215 -0.0285 0.0975 0.057 Uiso calc R 1 H H19B 0.9292 -0.1568 0.1697 0.057 Uiso calc R 1 H H19C 1.0933 -0.0395 0.1665 0.057 Uiso calc R 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 Br 0.04740(16) 0.02425(14) 0.02669(14) 0.00861(10) 0.00501(10) 0.00413(9) S 0.0219(2) 0.0270(3) 0.0203(2) 0.00089(19) 0.00223(19) 0.0063(2) O1 0.0319(8) 0.0226(8) 0.0282(8) 0.0070(6) -0.0002(6) 0.0061(6) O2 0.0302(8) 0.0308(8) 0.0310(8) -0.0054(6) 0.0006(6) 0.0116(7) O3 0.0325(8) 0.0402(10) 0.0247(8) 0.0068(7) 0.0088(6) 0.0058(7) C1 0.0225(10) 0.0231(10) 0.0213(10) 0.0004(8) -0.0009(8) 0.0052(8) C2 0.0205(9) 0.0222(10) 0.0218(10) -0.0009(8) -0.0013(8) 0.0065(8) C3 0.0191(9) 0.0224(10) 0.0218(10) -0.0016(7) -0.0017(7) 0.0067(8) C4 0.0300(11) 0.0240(10) 0.0215(10) 0.0013(8) 0.0002(8) 0.0086(8) C5 0.0331(11) 0.0215(10) 0.0254(11) 0.0017(8) -0.0008(9) 0.0083(8) C6 0.0278(10) 0.0207(10) 0.0227(10) 0.0015(8) 0.0013(8) 0.0031(8) C7 0.0297(11) 0.0265(11) 0.0208(10) -0.0003(9) 0.0024(8) 0.0070(8) C8 0.0231(10) 0.0233(10) 0.0225(10) -0.0010(8) -0.0007(8) 0.0075(8) C9 0.0291(11) 0.0290(11) 0.0239(10) 0.0002(9) 0.0005(8) 0.0119(9) C10 0.0285(11) 0.0255(11) 0.0298(11) 0.0030(8) -0.0018(9) 0.0140(9) C11 0.0231(10) 0.0202(10) 0.0269(11) 0.0016(8) -0.0017(8) 0.0047(8) C12 0.0239(10) 0.0276(11) 0.0262(10) 0.0025(8) -0.0014(8) 0.0059(9) C13 0.0236(10) 0.0322(12) 0.0162(9) 0.0012(8) 0.0026(8) 0.0080(8) C14 0.0333(11) 0.0326(12) 0.0209(10) 0.0051(9) 0.0016(9) 0.0060(9) C15 0.0355(12) 0.0495(15) 0.0257(11) 0.0166(11) 0.0050(9) 0.0091(11) C16 0.0230(11) 0.0736(19) 0.0263(12) 0.0053(11) 0.0022(9) 0.0172(12) C17 0.0310(12) 0.0577(17) 0.0314(12) -0.0138(11) -0.0041(10) 0.0174(12) C18 0.0332(12) 0.0355(13) 0.0261(11) -0.0044(10) -0.0010(9) 0.0128(10) C19 0.0454(14) 0.0306(13) 0.0327(13) 0.0122(10) 0.0012(11) 0.0022(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br C6 1.908(2) S O2 1.4378(16) S O3 1.4400(16) S C1 1.748(2) S C13 1.767(2) O1 C12 1.364(3) O1 C11 1.372(3) C1 C12 1.366(3) C1 C2 1.462(3) C2 C11 1.379(3) C2 C3 1.432(3) C3 C4 1.410(3) C3 C8 1.437(3) C4 C5 1.375(3) C4 H4 0.9500 C5 C6 1.402(3) C5 H5 0.9500 C6 C7 1.360(3) C7 C8 1.413(3) C7 H7 0.9500 C8 C9 1.425(3) C9 C10 1.359(3) C9 H9 0.9500 C10 C11 1.401(3) C10 H10 0.9500 C12 C19 1.487(3) C13 C14 1.388(3) C13 C18 1.390(3) C14 C15 1.392(3) C14 H14 0.9500 C15 C16 1.383(4) C15 H15 0.9500 C16 C17 1.385(4) C16 H16 0.9500 C17 C18 1.386(3) C17 H17 0.9500 C18 H18 0.9500 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2 S O3 118.45(10) O2 S C1 109.45(10) O3 S C1 107.55(10) O2 S C13 107.64(10) O3 S C13 106.29(10) C1 S C13 106.88(10) C12 O1 C11 107.28(17) C12 C1 C2 107.30(19) C12 C1 S 122.87(17) C2 C1 S 129.79(16) C11 C2 C3 118.02(18) C11 C2 C1 104.08(18) C3 C2 C1 137.90(19) C4 C3 C2 125.47(19) C4 C3 C8 117.87(19) C2 C3 C8 116.67(19) C5 C4 C3 121.8(2) C5 C4 H4 119.1 C3 C4 H4 119.1 C4 C5 C6 118.9(2) C4 C5 H5 120.5 C6 C5 H5 120.5 C7 C6 C5 122.2(2) C7 C6 Br 119.45(16) C5 C6 Br 118.36(16) C6 C7 C8 119.7(2) C6 C7 H7 120.1 C8 C7 H7 120.1 C7 C8 C9 119.17(19) C7 C8 C3 119.49(19) C9 C8 C3 121.34(19) C10 C9 C8 121.4(2) C10 C9 H9 119.3 C8 C9 H9 119.3 C9 C10 C11 116.5(2) C9 C10 H10 121.8 C11 C10 H10 121.8 O1 C11 C2 111.29(18) O1 C11 C10 122.57(19) C2 C11 C10 126.1(2) O1 C12 C1 110.04(19) O1 C12 C19 113.40(19) C1 C12 C19 136.5(2) C14 C13 C18 121.4(2) C14 C13 S 119.76(17) C18 C13 S 118.51(17) C13 C14 C15 119.0(2) C13 C14 H14 120.5 C15 C14 H14 120.5 C16 C15 C14 120.0(2) C16 C15 H15 120.0 C14 C15 H15 120.0 C15 C16 C17 120.5(2) C15 C16 H16 119.7 C17 C16 H16 119.7 C16 C17 C18 120.3(2) C16 C17 H17 119.9 C18 C17 H17 119.9 C17 C18 C13 118.9(2) C17 C18 H18 120.6 C13 C18 H18 120.6 C12 C19 H19A 109.5 C12 C19 H19B 109.5 H19A C19 H19B 109.5 C12 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 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 O2 S C1 C12 -131.89(18) O3 S C1 C12 -2.0(2) C13 S C1 C12 111.81(19) O2 S C1 C2 45.6(2) O3 S C1 C2 175.49(18) C13 S C1 C2 -70.7(2) C12 C1 C2 C11 -0.1(2) S C1 C2 C11 -177.90(16) C12 C1 C2 C3 180.0(2) S C1 C2 C3 2.2(4) C11 C2 C3 C4 178.60(19) C1 C2 C3 C4 -1.5(4) C11 C2 C3 C8 -1.0(3) C1 C2 C3 C8 178.9(2) C2 C3 C4 C5 179.6(2) C8 C3 C4 C5 -0.8(3) C3 C4 C5 C6 0.2(3) C4 C5 C6 C7 0.5(3) C4 C5 C6 Br 179.61(16) C5 C6 C7 C8 -0.6(3) Br C6 C7 C8 -179.70(15) C6 C7 C8 C9 179.35(19) C6 C7 C8 C3 0.0(3) C4 C3 C8 C7 0.7(3) C2 C3 C8 C7 -179.67(18) C4 C3 C8 C9 -178.63(19) C2 C3 C8 C9 1.0(3) C7 C8 C9 C10 -179.6(2) C3 C8 C9 C10 -0.3(3) C8 C9 C10 C11 -0.4(3) C12 O1 C11 C2 0.2(2) C12 O1 C11 C10 179.8(2) C3 C2 C11 O1 179.89(17) C1 C2 C11 O1 0.0(2) C3 C2 C11 C10 0.3(3) C1 C2 C11 C10 -179.6(2) C9 C10 C11 O1 -179.10(19) C9 C10 C11 C2 0.4(3) C11 O1 C12 C1 -0.3(2) C11 O1 C12 C19 178.94(19) C2 C1 C12 O1 0.2(2) S C1 C12 O1 178.21(14) C2 C1 C12 C19 -178.7(3) S C1 C12 C19 -0.7(4) O2 S C13 C14 5.9(2) O3 S C13 C14 -121.94(17) C1 S C13 C14 123.41(17) O2 S C13 C18 179.40(16) O3 S C13 C18 51.54(19) C1 S C13 C18 -63.10(19) C18 C13 C14 C15 -0.7(3) S C13 C14 C15 172.57(17) C13 C14 C15 C16 0.4(3) C14 C15 C16 C17 0.7(4) C15 C16 C17 C18 -1.4(4) C16 C17 C18 C13 1.1(4) C14 C13 C18 C17 0.0(3) S C13 C18 C17 -173.39(17) 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 C7 H7 Cg1 2_666 0.95 2.85 3.764(3) 161.2 C4 H4 O2 . 0.95 2.44 3.226(3) 140.2 C16 H16 O3 1_455 0.95 2.56 3.257(3) 130.3 C19 H19A O3 . 0.98 2.28 2.926(3) 122.4