#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2202346.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_2202346 loop_ _publ_author_name 'Wang, Jian-Feng' 'Lin, Xin' 'Huang, Yao-Jian' 'Su, Wen-Jin' 'Zhao, Yu-Fen' 'Ng, Seik Weng' _publ_section_title ; 7-Methoxy-4,6-dimethyl-3H-isobenzofuran-1-one ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1235 _journal_page_last o1236 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'C11 H12 O3' _chemical_formula_moiety 'C11 H12 O3' _chemical_formula_sum 'C11 H12 O3' _chemical_formula_weight 192.21 _chemical_name_systematic ; 7-Methoxy-4,6-dimethyl-3H-isobenzofuran-1-one ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.5508(7) _cell_length_b 12.6160(10) _cell_length_c 10.1223(9) _cell_measurement_reflns_used 1595 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 21.8 _cell_measurement_theta_min 2.6 _cell_volume 964.26(15) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device_type 'Bruker APEX 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 0.070 _diffrn_reflns_av_sigmaI/netI 0.025 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 12924 _diffrn_reflns_theta_full 25.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.6 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type none _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 408 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.15 _refine_diff_density_min -0.26 _refine_ls_abs_structure_details 'Calculation of Flack parameter suppressed by MERG 4' _refine_ls_abs_structure_Flack 0 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 897 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.13 _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_gt 0.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1P)^2^+0.1111P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.151 _refine_ls_wR_factor_ref 0.156 _reflns_number_gt 840 _reflns_number_total 897 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6316.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'None' changed to 'none' 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 964.27(15) _cod_database_code 2202346 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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 O1 0.3423(5) 0.9901(2) 0.4999(4) 0.0670(10) Uani d . 1 O O2 0.2527(5) 0.9312(3) 0.3053(4) 0.0690(10) Uani d . 1 O O3 0.2614(4) 0.6788(2) 0.3127(4) 0.0550(10) Uani d . 1 O C1 0.3061(6) 0.9115(4) 0.4148(5) 0.0520(10) Uani d . 1 C C2 0.3997(8) 0.9475(4) 0.6241(5) 0.0600(10) Uani d . 1 C C3 0.3990(5) 0.8311(3) 0.6058(4) 0.0400(10) Uani d . 1 C C4 0.4399(5) 0.7506(4) 0.6960(5) 0.0410(10) Uani d . 1 C C5 0.4198(6) 0.6486(4) 0.6492(4) 0.0430(10) Uani d . 1 C C6 0.3643(5) 0.6247(3) 0.5223(4) 0.0420(10) Uani d . 1 C C7 0.3257(6) 0.7049(4) 0.4340(5) 0.0430(10) Uani d . 1 C C8 0.3440(6) 0.8101(3) 0.4787(5) 0.0440(10) Uani d . 1 C C9 0.4964(7) 0.7760(4) 0.8333(5) 0.0560(10) Uani d . 1 C C10 0.3463(7) 0.5103(3) 0.4784(6) 0.0590(10) Uani d . 1 C C11 0.3633(8) 0.7076(5) 0.2007(6) 0.068(2) Uani d . 1 C H2a 0.3194 0.9679 0.6944 0.072 Uiso calc R 1 H H2b 0.5177 0.9724 0.6457 0.072 Uiso calc R 1 H H5 0.4450 0.5927 0.7061 0.051 Uiso calc R 1 H H9a 0.3940 0.7906 0.8865 0.084 Uiso calc R 1 H H9b 0.5723 0.8371 0.8323 0.084 Uiso calc R 1 H H9C 0.5595 0.7168 0.8698 0.084 Uiso calc R 1 H H10a 0.2270 0.4975 0.4498 0.088 Uiso calc R 1 H H10b 0.3742 0.4642 0.5509 0.088 Uiso calc R 1 H H10c 0.4264 0.4969 0.4067 0.088 Uiso calc R 1 H H11a 0.3037 0.6848 0.1219 0.102 Uiso calc R 1 H H11b 0.4775 0.6743 0.2057 0.102 Uiso calc R 1 H H11c 0.3778 0.7832 0.1987 0.102 Uiso calc R 1 H 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 0.101(3) 0.038(2) 0.062(2) 0.005(2) 0.003(2) 0.007(2) O2 0.089(3) 0.062(2) 0.056(2) 0.014(2) -0.001(2) 0.023(2) O3 0.062(2) 0.063(2) 0.042(2) -0.011(2) -0.004(2) -0.002(2) C1 0.056(3) 0.048(3) 0.052(3) 0.004(2) 0.008(2) 0.011(2) C2 0.077(3) 0.050(3) 0.052(3) -0.002(2) 0.005(2) -0.007(2) C3 0.043(2) 0.038(2) 0.040(2) 0.000(2) 0.005(2) -0.005(2) C4 0.038(2) 0.047(2) 0.038(2) 0.002(2) 0.009(2) 0.003(2) C5 0.045(2) 0.047(3) 0.036(2) 0.005(2) 0.002(2) 0.014(2) C6 0.044(2) 0.038(2) 0.043(3) -0.001(2) 0.005(2) 0.002(2) C7 0.043(2) 0.053(3) 0.034(2) -0.002(2) 0.001(2) 0.001(2) C8 0.047(2) 0.043(2) 0.042(3) -0.001(2) 0.004(2) 0.006(2) C9 0.069(3) 0.058(3) 0.042(3) 0.001(2) -0.004(2) 0.001(2) C10 0.080(3) 0.043(2) 0.054(3) -0.005(2) -0.001(3) -0.003(2) C11 0.083(4) 0.083(4) 0.039(3) -0.006(3) 0.003(3) -0.003(3) 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 0.0000 '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 0.0000 '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 C1 O1 C2 110.3(4) yes C7 O3 C11 117.7(3) yes O2 C1 O1 120.4(5) yes O2 C1 C8 130.7(5) yes O1 C1 C8 108.8(4) yes O1 C2 C3 105.2(4) yes C8 C3 C4 122.4(4) yes C8 C3 C2 108.0(4) yes C4 C3 C2 129.6(5) yes C5 C4 C3 115.3(4) yes C5 C4 C9 123.6(5) yes C3 C4 C9 121.1(4) yes C4 C5 C6 123.7(4) yes C7 C6 C5 120.3(4) yes C7 C6 C10 119.3(4) yes C5 C6 C10 120.4(4) yes O3 C7 C6 118.8(4) yes O3 C7 C8 123.5(4) yes C6 C7 C8 117.5(4) yes C3 C8 C7 120.7(4) yes C3 C8 C1 107.7(4) yes C7 C8 C1 131.5(4) yes O1 C2 H2a 110.7 no C3 C2 H2a 110.7 no O1 C2 H2b 110.7 no C3 C2 H2b 110.7 no H2a C2 H2b 108.8 no C4 C5 H5 118.1 no C6 C5 H5 118.1 no C4 C9 H9a 109.5 no C4 C9 H9b 109.5 no H9a C9 H9b 109.5 no C4 C9 H9C 109.5 no H9a C9 H9C 109.5 no H9b C9 H9C 109.5 no C6 C10 H10a 109.5 no C6 C10 H10b 109.5 no H10a C10 H10b 109.5 no C6 C10 H10c 109.5 no H10a C10 H10c 109.5 no H10b C10 H10c 109.5 no O3 C11 H11a 109.5 no O3 C11 H11b 109.5 no H11a C11 H11b 109.5 no O3 C11 H11c 109.5 no H11a C11 H11c 109.5 no H11b C11 H11c 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 1.342(6) yes O1 C2 1.434(7) yes O2 C1 1.205(6) yes O3 C7 1.361(6) yes O3 C11 1.418(7) yes C1 C8 1.462(6) yes C2 C3 1.480(7) yes C3 C8 1.377(7) yes C3 C4 1.400(7) yes C4 C5 1.381(7) yes C4 C9 1.489(7) yes C5 C6 1.385(6) yes C6 C7 1.381(6) yes C6 C10 1.515(6) yes C7 C8 1.409(6) yes C2 H2a 0.97 no C2 H2b 0.97 no C5 H5 0.93 no C9 H9a 0.96 no C9 H9b 0.96 no C9 H9C 0.96 no C10 H10a 0.96 no C10 H10b 0.96 no C10 H10c 0.96 no C11 H11a 0.96 no C11 H11b 0.96 no C11 H11c 0.96 no 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 _geom_torsion_publ_flag C2 O1 C1 O2 178.7(5) no C2 O1 C1 C8 -1.8(5) no C1 O1 C2 C3 1.2(5) no O1 C2 C3 C8 -0.1(5) no O1 C2 C3 C4 -178.5(4) no C8 C3 C4 C5 -0.5(6) no C2 C3 C4 C5 177.6(4) no C8 C3 C4 C9 -179.1(4) no C2 C3 C4 C9 -0.9(7) no C3 C4 C5 C6 0.3(6) no C9 C4 C5 C6 178.8(4) no C4 C5 C6 C7 0.1(6) no C4 C5 C6 C10 179.8(4) no C11 O3 C7 C6 -118.2(5) no C11 O3 C7 C8 66.4(6) no C5 C6 C7 O3 -176.1(4) no C10 C6 C7 O3 4.3(6) no C5 C6 C7 C8 -0.4(6) no C10 C6 C7 C8 180.0(4) no C4 C3 C8 C7 0.3(6) no C2 C3 C8 C7 -178.2(4) no C4 C3 C8 C1 177.6(4) no C2 C3 C8 C1 -0.9(5) no O3 C7 C8 C3 175.7(4) no C6 C7 C8 C3 0.2(6) no O3 C7 C8 C1 -0.9(8) no C6 C7 C8 C1 -176.4(5) no O2 C1 C8 C3 -178.9(5) no O1 C1 C8 C3 1.7(5) no O2 C1 C8 C7 -1.9(9) no O1 C1 C8 C7 178.6(4) no