#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/02/2010291.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_2010291 loop_ _publ_author_name 'Jasinski, Jerry P. ' 'Woudenberg, Richard C.' _publ_contact_author ; Dr. Jerry P. Jasinski Chemistry Department Keene State College 229 Main St. Keene, New Hampshire 03431 USA ; _publ_section_title ; 7-Hydroxy-4-methylcoumarin monohydrate ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1952 _journal_page_last 1953 _journal_paper_doi 10.1107/S0108270194005822 _journal_volume 50 _journal_year 1994 _chemical_formula_moiety 'C10 H8 O3, H2 O' _chemical_formula_sum 'C10 H10 O4' _chemical_formula_weight 194.19 _chemical_name_systematic ; 7-Hydroxy-4-methylcoumarin monohydrate ; _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' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 105.300(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.106(2) _cell_length_b 11.335(2) _cell_length_c 11.817(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296 _cell_measurement_theta_max 50.0 _cell_measurement_theta_min 45.0 _cell_volume 918.1(3) _computing_cell_refinement ' MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction ' TEXSAN PROCESS (Molecular Structure Corporation, 1985)' _computing_molecular_graphics ' VAXSTATION 3520 (Digital Equipment Corporation, 1990)' _computing_publication_material 'TEXSAN FINISH' _computing_structure_refinement 'TEXSAN LS' _computing_structure_solution 'MITHRIL (Gilmore, 1984)' _diffrn_ambient_temperature 296 _diffrn_measurement_device 'Rigaku AFC-6S' _diffrn_measurement_method '\w scans with profile analysis' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents XX _diffrn_reflns_av_sigmaI/netI .017 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2395 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 5.00 _diffrn_standards_decay_% -0.70 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.1023 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details \y _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.405 _exptl_crystal_description prism _exptl_crystal_F_000 408 _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.90 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.18 _refine_diff_density_min -0.18 _refine_ls_extinction_coef 8.3852E-6 _refine_ls_extinction_method 'Type 2 Gaussian isotropic (Zachariasen, 1963)' _refine_ls_goodness_of_fit_obs 1.741 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 1356 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.039 _refine_ls_shift/esd_max 0.0624 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 4F~o~^2^/\s^2^F~o~^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.045 _reflns_number_observed 1356 _reflns_number_total 2227 _reflns_observed_criterion I>3.0\s(I) _cod_data_source_file hh1047.cif _cod_data_source_block HH1047 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 24 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 4F~o~^2^/\s^2^F~o~^2^' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 4F~o~^2^/\s^2^F~o~^2^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2010291 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z 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 O1 0.0624(9) 0.0292(6) 0.0370(7) -0.0034(6) 0.0149(6) 0.0032(5) O2 0.1130(10) 0.0415(9) 0.0494(9) -0.0024(9) 0.0251(9) -0.0002(7) O11 0.1120(10) 0.0327(7) 0.0562(9) -0.0145(8) 0.0253(9) -0.0024(6) O13 0.0709(10) 0.0395(8) 0.0464(8) -0.0110(7) 0.0074(7) -0.0040(6) C2 0.0650(10) 0.0338(10) 0.0430(10) -0.0043(9) 0.0207(10) -0.0051(8) C3 0.0570(10) 0.0410(10) 0.0376(10) -0.0047(9) 0.0157(9) -0.0084(8) C4 0.0430(10) 0.0420(10) 0.0356(9) 0.0028(8) 0.0146(8) -0.0007(8) C5 0.0480(10) 0.0366(10) 0.0410(10) 0.0037(9) 0.0119(9) 0.0110(8) C6 0.0520(10) 0.0285(9) 0.0510(10) -0.0007(8) 0.0144(9) 0.0051(8) C7 0.0430(10) 0.0337(9) 0.0428(10) 0.0002(8) 0.0125(8) -0.0027(8) C8 0.0470(10) 0.0348(9) 0.0318(9) 0.0038(8) 0.0121(8) 0.0033(7) C9 0.0399(10) 0.0282(8) 0.0381(9) 0.0020(7) 0.0161(8) 0.0028(7) C10 0.0390(10) 0.0341(9) 0.0342(9) 0.0041(8) 0.0129(8) 0.0036(7) C12 0.068(2) 0.0620(10) 0.0360(10) 0.0000(10) 0.0080(10) 0.0050(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom O1 0.8319(2) 0.16979(9) 0.50906(10) 0.0425 Uani ? ? O2 0.5273(3) 0.0770(2) 0.86030(10) 0.0673 Uani ? ? O11 0.9597(3) 0.33960(10) 0.57580(10) 0.0663 Uani ? ? O13 0.5438(2) -0.18880(10) 0.34400(10) 0.0538 Uani ? ? C2 0.9316(3) 0.2374(2) 0.6005(2) 0.0459 Uani ? ? C3 0.9940(3) 0.1842(2) 0.7135(2) 0.0448 Uani ? ? C4 0.9563(3) 0.0707(2) 0.7328(2) 0.0394 Uani ? ? C5 0.7975(3) -0.1184(2) 0.6422(2) 0.0419 Uani ? ? C6 0.6975(3) -0.1787(2) 0.5453(2) 0.0438 Uani ? ? C7 0.6437(3) -0.1239(2) 0.4363(2) 0.0396 Uani ? ? C8 0.6915(3) -0.0070(2) 0.4257(2) 0.0374 Uani ? ? C9 0.7905(3) 0.05290(10) 0.5247(2) 0.0343 Uani ? ? C10 0.8483(3) 0.00090(10) 0.63550(10) 0.0353 Uani ? ? C12 1.0253(4) 0.0161(2) 0.8518(2) 0.0564 Uani ? ? H2A 0.524(4) 0.005(3) 0.873(2) 0.089(9) Uani ? ? H2B 0.498(4) 0.110(3) 0.921(3) 0.100(10) Uani ? ? H3 1.070(3) 0.233(2) 0.774(2) 0.046(5) Uani ? ? H5 0.837(2) -0.157(2) 0.717(2) 0.051(5) Uani ? ? H6 0.664(3) -0.260(2) 0.549(2) 0.049(5) Uani ? ? H8 0.658(3) 0.032(2) 0.352(2) 0.047(5) Uani ? ? H12A 1.116(3) -0.049(2) 0.853(2) 0.081(8) Uani ? ? H12B 0.916(4) -0.011(2) 0.878(2) 0.084(8) Uani ? ? H12C 1.100(3) 0.073(2) 0.907(2) 0.072(7) Uani ? ? H13 0.522(3) -0.147(2) 0.279(2) 0.077(8) Uani ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.002 0.002 International_Tables_Vol_IV_Table_2.2B H 0.000 0.000 International_Tables_Vol_IV_Table_2.2B O 0.008 0.006 International_Tables_Vol_IV_Table_2.2B loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -1 0 1 3 -1 2 -1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 O1 C9 121.30(10) yes O1 C2 O11 115.3(2) yes O1 C2 C3 118.2(2) yes O11 C2 C3 126.5(2) yes C2 C3 C4 122.5(2) yes C3 C4 C10 118.6(2) yes C3 C4 C12 121.6(2) yes C10 C4 C12 119.8(2) yes C6 C5 C10 121.3(2) yes C5 C6 C7 120.7(2) yes O13 C7 C6 117.6(2) yes O13 C7 C8 122.6(2) yes C6 C7 C8 119.9(2) yes C7 C8 C9 118.6(2) yes O1 C9 C8 116.10(10) yes O1 C9 C10 120.70(10) yes C8 C9 C10 123.30(10) yes C4 C10 C5 125.0(2) yes C4 C10 C9 118.8(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 . . 1.362(2) yes O1 C9 . . 1.380(2) yes O11 C2 . . 1.223(2) yes O13 C7 . . 1.352(2) yes C2 C3 . . 1.424(3) yes C3 C4 . . 1.346(2) yes C4 C10 . . 1.439(2) yes C4 C12 . . 1.496(3) yes C5 C6 . . 1.362(2) yes C5 C10 . . 1.407(2) yes C6 C7 . . 1.390(2) yes C7 C8 . . 1.382(2) yes C8 C9 . . 1.374(2) yes C9 C10 . . 1.395(2) yes