#------------------------------------------------------------------------------ #$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005695.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_2005695 loop_ _publ_author_name 'Shaw, J. P.' 'Tan, E. W.' 'Blackman, A. G.' _publ_contact_author ; Allan Blackman Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; _publ_section_title ; Methyl 2-Benzoyloxy-3-oxo-3-phenylpropanoate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2883 _journal_page_last 2885 _journal_paper_doi 10.1107/S0108270196008323 _journal_volume 52 _journal_year 1996 _chemical_formula_moiety 'C17 H14 O5' _chemical_formula_sum 'C17 H14 O5' _chemical_formula_weight 298.28 _chemical_name_systematic ' Methyl 2-benzoyloxy-3-oxo-3-phenylpropanoate' _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 SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 93.14(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.070(2) _cell_length_b 12.824(3) _cell_length_c 18.457(5) _cell_measurement_reflns_used 27 _cell_measurement_temperature 151(2) _cell_measurement_theta_max 14 _cell_measurement_theta_min 5 _cell_volume 1434.6(7) _computing_cell_refinement SHELXTL-Plus _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1991)' _computing_data_reduction SHELXTL-Plus _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method '\w scans' _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 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 2260 _diffrn_reflns_theta_max 24.00 _diffrn_reflns_theta_min 2.21 _diffrn_standards_decay_% <2 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 624 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.150 _refine_diff_density_min -0.153 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.831 _refine_ls_goodness_of_fit_obs 0.993 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 2245 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.831 _refine_ls_restrained_S_obs 0.993 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_obs 0.0332 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0291P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0665 _refine_ls_wR_factor_obs 0.0627 _reflns_number_observed 1470 _reflns_number_total 2245 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ta1103.cif _cod_data_source_block epox _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0291P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0291P)^2^] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1434.5(6) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2005695 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_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 0.0256(8) 0.0255(8) 0.0398(9) -0.0004(6) 0.0114(7) 0.0038(6) O2 0.0359(8) 0.0220(8) 0.0531(10) 0.0018(7) 0.0154(7) 0.0008(7) O3 0.0239(7) 0.0242(7) 0.0311(8) 0.0008(6) 0.0112(6) 0.0010(6) O4 0.0275(8) 0.0388(9) 0.0384(9) 0.0041(7) -0.0033(7) -0.0038(7) O5 0.0314(8) 0.0212(8) 0.0421(9) 0.0015(7) 0.0100(7) -0.0009(7) C8 0.0394(13) 0.0208(11) 0.0358(13) 0.0029(10) 0.0122(10) -0.0004(10) C6 0.0297(12) 0.0229(11) 0.0262(11) -0.0016(9) 0.0063(9) -0.0035(9) C11 0.0246(11) 0.0238(11) 0.0217(10) -0.0029(10) -0.0002(9) 0.0008(9) C3 0.0202(11) 0.0236(11) 0.0268(11) 0.0018(8) 0.0069(9) 0.0008(9) C4 0.0240(11) 0.0231(11) 0.0273(11) -0.0028(9) 0.0039(9) 0.0031(9) C5 0.0235(11) 0.0208(11) 0.0230(11) -0.0027(8) 0.0058(9) 0.0008(9) C12 0.0239(11) 0.0249(11) 0.0188(10) 0.0004(9) 0.0030(9) -0.0001(8) C13 0.0292(12) 0.0252(11) 0.0267(12) -0.0042(9) 0.0054(9) -0.0019(9) C17 0.0279(11) 0.0237(11) 0.0245(11) 0.0012(9) 0.0013(9) 0.0011(9) C1 0.0311(12) 0.0324(12) 0.0454(13) -0.0063(10) 0.0107(10) 0.0129(10) C16 0.0291(12) 0.0328(13) 0.0264(12) -0.0021(10) 0.0074(9) 0.0039(10) C7 0.0275(12) 0.0268(11) 0.0357(13) -0.0007(10) 0.0041(10) 0.0038(10) C9 0.0505(15) 0.0286(12) 0.0273(12) 0.0001(11) 0.0040(10) -0.0063(10) C2 0.0236(11) 0.0261(12) 0.0259(11) 0.0002(10) 0.0040(9) -0.0015(9) C10 0.0330(12) 0.0279(12) 0.0303(12) -0.0007(10) 0.0007(10) 0.0006(10) C15 0.0310(12) 0.0385(13) 0.0293(12) 0.0041(11) 0.0100(10) -0.0037(10) C14 0.0366(13) 0.0243(11) 0.0332(12) 0.0019(10) 0.0101(10) -0.0041(10) loop_ _atom_site_label _atom_site_occupancy _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_refinement_flags _atom_site_type_symbol O1 1 -0.4124(2) 0.48828(9) 0.89600(7) 0.0300(3) Uani d . O O2 1 -0.1443(2) 0.38118(10) 0.86161(8) 0.0365(4) Uani d . O O3 1 0.0746(2) 0.53973(9) 0.80772(7) 0.0260(3) Uani d . O O4 1 0.1160(2) 0.61582(10) 0.94630(7) 0.0351(4) Uani d . O O5 1 0.1079(2) 0.70868(10) 0.77920(7) 0.0313(4) Uani d . O C8 1 -0.5010(3) 0.86417(15) 0.98486(11) 0.0316(5) Uani d . C H8 1 -0.5981(3) 0.91322(15) 1.00216(11) 0.038 Uiso calc R H C6 1 -0.4142(3) 0.73463(14) 0.89817(11) 0.0261(5) Uani d . C H6 1 -0.4528(3) 0.69714(14) 0.85624(11) 0.031 Uiso calc R H C11 1 0.1704(3) 0.61984(15) 0.77371(10) 0.0234(4) Uani d . C C3 1 -0.1168(3) 0.56736(14) 0.84473(10) 0.0234(5) Uani d . C H3 1 -0.2201(3) 0.60561(14) 0.81187(10) 0.028 Uiso calc R H C4 1 -0.0566(3) 0.63397(14) 0.91217(10) 0.0247(5) Uani d . C C5 1 -0.2122(3) 0.71606(14) 0.93523(10) 0.0223(4) Uani d . C C12 1 0.3554(3) 0.58501(14) 0.73089(10) 0.0224(4) Uani d . C C13 1 0.4065(3) 0.47992(15) 0.72300(10) 0.0269(5) Uani d . C H13 1 0.3189(3) 0.42917(15) 0.74305(10) 0.032 Uiso calc R H C17 1 0.4844(3) 0.66015(15) 0.69954(10) 0.0253(5) Uani d . C H17 1 0.4494(3) 0.73036(15) 0.70412(10) 0.030 Uiso calc R H C1 1 -0.5392(3) 0.40056(15) 0.92035(11) 0.0360(5) Uani d . C H1A 1 -0.6769(9) 0.4250(2) 0.9372(6) 0.054 Uiso calc R H H1B 1 -0.4577(9) 0.3656(6) 0.9592(5) 0.054 Uiso calc R H H1C 1 -0.5673(17) 0.3529(5) 0.8808(2) 0.054 Uiso calc R H C16 1 0.6648(3) 0.6311(2) 0.66151(10) 0.0292(5) Uani d . C H16 1 0.7510(3) 0.6816(2) 0.64057(10) 0.035 Uiso calc R H C7 1 -0.5585(3) 0.80844(15) 0.92314(11) 0.0299(5) Uani d . C H7 1 -0.6936(3) 0.82020(15) 0.89824(11) 0.036 Uiso calc R H C9 1 -0.2982(3) 0.8473(2) 1.02144(11) 0.0354(5) Uani d . C H9 1 -0.2586(3) 0.8861(2) 1.06270(11) 0.042 Uiso calc R H C2 1 -0.2211(3) 0.4662(2) 0.86771(10) 0.0251(5) Uani d . C C10 1 -0.1552(3) 0.77348(14) 0.99697(11) 0.0304(5) Uani d . C H10 1 -0.0201(3) 0.76218(14) 1.02196(11) 0.037 Uiso calc R H C15 1 0.7161(3) 0.5264(2) 0.65479(10) 0.0326(5) Uani d . C H15 1 0.8378(3) 0.5066(2) 0.62957(10) 0.039 Uiso calc R H C14 1 0.5869(3) 0.4512(2) 0.68546(10) 0.0311(5) Uani d . C H14 1 0.6220(3) 0.3810(2) 0.68071(10) 0.037 Uiso calc R H 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' 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 C1 116.54(15) yes C11 O3 C3 114.62(14) yes C7 C8 C9 120.0(2) no C7 C6 C5 120.6(2) no O5 C11 O3 122.2(2) yes O5 C11 C12 125.6(2) yes O3 C11 C12 112.2(2) yes O3 C3 C2 106.60(14) yes O3 C3 C4 111.26(15) yes C2 C3 C4 109.51(14) yes O4 C4 C5 121.9(2) yes O4 C4 C3 118.3(2) yes C5 C4 C3 119.8(2) yes C10 C5 C6 119.2(2) no C10 C5 C4 118.5(2) yes C6 C5 C4 122.4(2) yes C17 C12 C13 119.6(2) no C17 C12 C11 118.4(2) yes C13 C12 C11 121.9(2) yes C14 C13 C12 120.0(2) no C16 C17 C12 120.3(2) no C17 C16 C15 119.6(2) no C8 C7 C6 119.7(2) no C10 C9 C8 120.4(2) no O2 C2 O1 125.9(2) yes O2 C2 C3 125.8(2) yes O1 C2 C3 108.4(2) yes C9 C10 C5 120.1(2) no C14 C15 C16 120.3(2) no C13 C14 C15 120.2(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 1.330(2) yes O1 C1 1.448(2) yes O2 C2 1.193(2) yes O3 C11 1.352(2) yes O3 C3 1.424(2) yes O4 C4 1.215(2) yes O5 C11 1.207(2) yes C8 C7 1.373(3) no C8 C9 1.389(3) no C6 C7 1.385(3) no C6 C5 1.392(3) no C11 C12 1.477(2) yes C3 C2 1.515(3) yes C3 C4 1.537(3) yes C4 C5 1.492(2) yes C5 C10 1.385(3) no C12 C17 1.388(2) no C12 C13 1.392(2) no C13 C14 1.378(2) no C17 C16 1.383(2) no C16 C15 1.386(3) no C9 C10 1.377(3) no C15 C14 1.384(3) no