#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2200204.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_2200204 loop_ _publ_author_name 'Wallet, Jean-Claude' 'Espinosa, Enrique' 'Molins, Elies' 'Miravitlles, Carlos' _publ_section_title ; 2',6'-Dimethoxyflavone--bromoacetic acid (1/1) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o174 _journal_page_last o175 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C17 H14 O4, C2 H3 Br O2' _chemical_formula_moiety 'C17 H14 O4, C2 H3 Br O2' _chemical_formula_sum 'C19 H17 Br O6' _chemical_formula_weight 421.24 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 86.560(10) _cell_angle_beta 78.560(10) _cell_angle_gamma 76.30(2) _cell_formula_units_Z 2 _cell_length_a 7.6630(10) _cell_length_b 9.6930(10) _cell_length_c 12.8770(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.51 _cell_measurement_theta_min 8.46 _cell_volume 910.71(19) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'PLUTON93 (Spek, 1993)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .997 _diffrn_measured_fraction_theta_max .997 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled \w/2\q' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0646 _diffrn_reflns_av_sigmaI/netI .2166 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2993 _diffrn_reflns_theta_full 23.70 _diffrn_reflns_theta_max 23.70 _diffrn_reflns_theta_min 2.94 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.289 _exptl_absorpt_correction_T_max .913 _exptl_absorpt_correction_T_min .440 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 428 _exptl_crystal_size_max .66 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .04 _refine_diff_density_max .650 _refine_diff_density_min -.662 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .955 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 2760 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .955 _refine_ls_R_factor_all .2508 _refine_ls_R_factor_gt .0747 _refine_ls_shift/su_max .006 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1319P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .2485 _reflns_number_gt 1072 _reflns_number_total 2760 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob6023.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 910.71(17) _cod_database_code 2200204 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _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_type_symbol Br1 .9559(3) .26096(14) .36870(11) .1161(9) Uani d . 1 Br O1 .4596(8) .8299(6) .9302(5) .0437(18) Uani d . 1 O O4 .7735(10) .4825(6) .7659(5) .064(2) Uani d . 1 O O2' .6078(11) .9965(7) .6770(6) .067(2) Uani d . 1 O O6' .0975(10) .8764(7) .8903(6) .061(2) Uani d . 1 O O121 .8240(12) .4156(8) .5732(6) .081(3) Uani d . 1 O H121 .844(16) .439(13) .652(11) .122 Uiso d . 1 H O122 .6331(11) .6031(8) .5214(6) .082(3) Uani d . 1 O C2 .4654(12) .8183(9) .8257(7) .037(2) Uani d . 1 C C3 .5688(12) .7072(9) .7686(7) .042(3) Uani d . 1 C H3 .5710 .7073 .6962 .051 Uiso calc R 1 H C4 .6758(13) .5885(9) .8162(7) .040(3) Uani d . 1 C C5 .7635(13) .4939(10) .9879(8) .047(3) Uani d . 1 C H5 .8357 .4116 .9546 .057 Uiso calc R 1 H C6 .7540(15) .5101(11) 1.0935(8) .062(3) Uani d . 1 C H6 .8214 .4399 1.1316 .075 Uiso calc R 1 H C7 .6440(15) .6308(11) 1.1439(8) .066(3) Uani d . 1 C H7 .6353 .6394 1.2164 .079 Uiso calc R 1 H C8 .5480(15) .7375(11) 1.0897(8) .059(3) Uani d . 1 C H8 .4768 .8196 1.1238 .070 Uiso calc R 1 H C9 .5596(14) .7204(9) .9810(7) .045(3) Uani d . 1 C C10 .6667(13) .5989(10) .9299(7) .043(3) Uani d . 1 C C11 .7951(16) .4398(12) .3927(9) .080(4) Uani d . 1 C H11A .8501 .5085 .3482 .119 Uiso calc R 1 H H11B .6839 .4370 .3685 .119 Uiso calc R 1 H C12 .7427(15) .4937(12) .5016(8) .055(3) Uani d . 1 C C21 .6876(16) 1.0748(13) .5943(10) .086(4) Uani d . 1 C H21A .6490 1.0598 .5302 .130 Uiso calc R 1 H H21B .8184 1.0446 .5847 .130 Uiso calc R 1 H H21C .6504 1.1739 .6111 .130 Uiso calc R 1 H C61 -.0955(14) .8867(13) .9198(9) .077(4) Uani d . 1 C H61A -.1545 .9781 .9499 .115 Uiso calc R 1 H H61B -.1179 .8138 .9710 .115 Uiso calc R 1 H H61C -.1434 .8753 .8582 .115 Uiso calc R 1 H C1' .3504(14) .9426(9) .7804(8) .042(3) Uani d . 1 C C2' .4210(16) 1.0271(10) .7014(8) .047(3) Uani d . 1 C C3' .311(2) 1.1358(11) .6567(9) .067(3) Uani d . 1 C H3' .3611 1.1940 .6050 .080 Uiso calc R 1 H C4' .131(2) 1.1573(11) .6883(11) .080(4) Uani d . 1 C H4' .0565 1.2289 .6551 .097 Uiso calc R 1 H C5' .0500(16) 1.0789(12) .7675(10) .070(3) Uani d . 1 C H5' -.0764 1.1005 .7893 .084 Uiso calc R 1 H C6' .1587(15) .9663(10) .8153(8) .051(3) Uani d . 1 C 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 .1754(19) .0781(10) .0628(9) .0120(9) .0079(10) -.0172(7) O1 .047(5) .048(4) .031(4) .005(3) -.014(3) -.004(3) O4 .086(6) .052(4) .034(4) .023(4) -.010(4) -.005(3) O2' .067(6) .064(5) .065(5) -.019(4) -.003(4) .031(4) O6' .047(5) .068(5) .063(5) -.003(4) -.010(4) .000(4) O121 .110(7) .072(5) .038(4) .040(5) -.030(5) -.009(4) O122 .096(6) .065(5) .064(5) .028(5) -.021(5) -.003(4) C2 .039(6) .038(5) .038(6) -.006(5) -.020(5) .002(4) C3 .051(7) .040(5) .027(5) .009(5) -.011(5) .004(4) C4 .044(6) .040(5) .029(5) .000(5) -.005(5) .006(4) C5 .045(7) .048(5) .044(7) .003(5) -.015(5) .012(5) C6 .068(8) .071(7) .049(7) -.006(6) -.030(6) .019(6) C7 .082(9) .074(8) .036(6) .000(7) -.023(6) .008(6) C8 .075(9) .062(7) .040(6) -.013(6) -.014(6) -.010(5) C9 .055(7) .045(6) .031(6) -.001(5) -.011(5) .002(5) C10 .032(6) .065(6) .030(5) .001(5) -.015(5) .001(5) C11 .083(9) .085(8) .056(7) .031(7) -.032(7) -.019(6) C12 .048(7) .067(7) .046(7) -.006(6) -.012(6) -.004(6) C21 .072(9) .093(9) .096(11) -.031(8) -.015(8) .018(8) C61 .025(7) .123(10) .078(9) -.015(7) .007(6) -.031(8) C1' .042(7) .038(5) .043(6) .006(5) -.015(5) -.007(5) C2' .052(8) .045(6) .044(6) -.005(6) -.019(6) .005(5) C3' .082(10) .052(7) .063(8) -.001(7) -.028(8) .013(6) C4' .101(12) .046(7) .092(10) .014(8) -.057(10) .014(7) C5' .047(8) .075(8) .083(9) .011(7) -.026(7) -.008(7) C6' .051(8) .050(6) .050(7) .005(6) -.022(6) -.013(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -2 3 -3 1 4 0 2 5 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 O1 C9 118.3(6) C2' O2' C21 117.0(9) C6' O6' C61 118.9(9) C3 C2 O1 123.2(8) C3 C2 C1' 123.6(8) O1 C2 C1' 113.1(7) C2 C3 C4 121.7(8) O4 C4 C3 123.7(8) O4 C4 C10 120.9(8) C3 C4 C10 115.4(8) C6 C5 C10 120.6(9) C5 C6 C7 119.9(9) C8 C7 C6 121.4(10) C7 C8 C9 118.2(9) O1 C9 C10 123.0(8) O1 C9 C8 116.0(8) C10 C9 C8 121.0(9) C9 C10 C5 118.8(9) C9 C10 C4 118.4(8) C5 C10 C4 122.8(8) C12 C11 Br1 118.2(8) O122 C12 O121 123.2(10) O122 C12 C11 120.3(11) O121 C12 C11 116.4(9) C2' C1' C6' 119.7(9) C2' C1' C2 122.8(10) C6' C1' C2 117.3(9) C3' C2' O2' 124.0(11) C3' C2' C1' 121.6(11) O2' C2' C1' 114.2(9) C4' C3' C2' 118.8(12) C3' C4' C5' 123.2(11) C4' C5' C6' 119.6(12) O6' C6' C5' 126.0(11) O6' C6' C1' 117.0(9) C5' C6' C1' 117.0(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C11 1.876(10) O1 C2 1.348(10) O1 C9 1.369(10) O4 C4 1.249(10) O2' C2' 1.367(11) O2' C21 1.396(12) O6' C6' 1.351(12) O6' C61 1.433(11) O121 C12 1.316(12) O122 C12 1.192(11) C2 C3 1.337(11) C2 C1' 1.478(12) C3 C4 1.428(12) C4 C10 1.461(13) C5 C6 1.364(14) C5 C10 1.384(12) C6 C7 1.381(14) C7 C8 1.362(14) C8 C9 1.402(13) C9 C10 1.383(12) C11 C12 1.472(14) C1' C2' 1.375(13) C1' C6' 1.415(13) C2' C3' 1.360(14) C3' C4' 1.327(16) C4' C5' 1.373(17) C5' C6' 1.398(15) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O121 H121 O4 1.09(14) 1.51(14) 2.534(9) 152(11) C3 H3 O122 .93 2.44 3.305(12) 156 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 C9 O1 C2 C3 -2.4(14) C9 O1 C2 C1' 179.4(9) O1 C2 C3 C4 2.8(15) C1' C2 C3 C4 -179.1(9) C2 C3 C4 O4 179.7(9) C2 C3 C4 C10 -1.2(15) C10 C5 C6 C7 1.3(17) C5 C6 C7 C8 -2.1(19) C6 C7 C8 C9 1.7(18) C2 O1 C9 C10 .3(14) C2 O1 C9 C8 -179.7(9) C7 C8 C9 O1 179.5(10) C7 C8 C9 C10 -.5(17) O1 C9 C10 C5 179.8(9) C8 C9 C10 C5 -.2(16) O1 C9 C10 C4 1.1(16) C8 C9 C10 C4 -178.8(9) C6 C5 C10 C9 -.2(16) C6 C5 C10 C4 178.4(10) O4 C4 C10 C9 178.5(9) C3 C4 C10 C9 -.7(14) O4 C4 C10 C5 -.1(16) C3 C4 C10 C5 -179.3(9) Br1 C11 C12 O122 -175.8(9) Br1 C11 C12 O121 4.7(16) C3 C2 C1' C2' -59.5(14) O1 C2 C1' C2' 118.7(10) C3 C2 C1' C6' 115.3(11) O1 C2 C1' C6' -66.5(11) C21 O2' C2' C3' -5.9(15) C21 O2' C2' C1' 177.5(9) C6' C1' C2' C3' 1.4(15) C2 C1' C2' C3' 176.0(9) C6' C1' C2' O2' 178.1(8) C2 C1' C2' O2' -7.2(13) O2' C2' C3' C4' -178.6(11) C1' C2' C3' C4' -2.2(17) C2' C3' C4' C5' 3(2) C3' C4' C5' C6' -3.0(19) C61 O6' C6' C5' 5.3(14) C61 O6' C6' C1' -173.4(8) C4' C5' C6' O6' -176.7(10) C4' C5' C6' C1' 2.0(16) C2' C1' C6' O6' 177.5(9) C2 C1' C6' O6' 2.6(12) C2' C1' C6' C5' -1.3(14) C2 C1' C6' C5' -176.2(9)