#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/74/2007443.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_2007443 loop_ _publ_author_name 'Eilers, Frank' 'Bach, Thorsten' 'Fr\"ohlich, Roland' _publ_section_title ; 9-Methyl-8,11,12-trioxatricyclo[7.2.1.0^2,7^]dodeca-2,4,6-trien-10-one ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1011 _journal_page_last 1013 _journal_paper_doi 10.1107/S0108270198001528 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'C10 H8 O4' _chemical_formula_sum 'C10 H8 O4' _chemical_formula_weight 192.16 _chemical_name_systematic ; 9-Methyl-8,11,12-trioxatricyclo[7.2.1.0^2,7^]dodeca-2,4,6-trien-10-one ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.8380(10) _cell_length_b 7.2310(10) _cell_length_c 20.5480(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 223(2) _cell_measurement_theta_max 46.44 _cell_measurement_theta_min 40.34 _cell_volume 867.4(2) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1996)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 223(2) _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0104 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 1068 _diffrn_reflns_theta_max 74.26 _diffrn_reflns_theta_min 4.30 _diffrn_standards_decay_% 2.7 _diffrn_standards_interval_count 250 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_type 'empirical via \y scan data (Fair, 1990)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_meas ? _exptl_crystal_description plate _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.192 _refine_diff_density_min -0.139 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.2(4) _refine_ls_extinction_coef 0.0160(14) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.132 _refine_ls_goodness_of_fit_obs 1.139 _refine_ls_hydrogen_treatment ; H atoms calculated and refined as riding atoms with U = 1.2(1.5) \\times U~host~ ; _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 1068 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.132 _refine_ls_restrained_S_obs 1.139 _refine_ls_R_factor_all 0.031 _refine_ls_R_factor_obs .031 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.1854P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.090 _refine_ls_wR_factor_obs .090 _reflns_number_observed 1051 _reflns_number_total 1068 _reflns_observed_criterion I>2sigma(I) _[local]_cod_data_source_file jz1270.cif _[local]_cod_data_source_block I _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 ; _cod_database_code 2007443 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -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 C1 .0298(8) .0291(8) .0333(8) .0007(8) .0027(7) -.0015(7) C2 .0374(10) .0329(9) .0414(9) .0008(9) -.0045(9) -.0054(8) C3 .0644(13) .0353(10) .0323(9) .0053(11) -.0069(10) -.0040(8) C4 .0593(13) .0367(10) .0371(9) .0041(11) .0137(10) .0005(8) C5 .0346(10) .0332(9) .0479(10) .0013(8) .0084(9) -.0012(8) C6 .0288(8) .0314(9) .0362(9) .0022(8) -.0005(8) -.0029(7) O7 .0355(7) .0471(8) .0354(6) -.0055(7) .0049(5) -.0003(6) C8 .0460(10) .0416(11) .0323(10) .0038(10) .0006(9) .0022(8) O8 .0434(8) .0443(8) .0403(7) .0085(8) -.0065(6) .0020(6) C9 .0585(12) .0437(11) .0252(8) .0069(12) -.0009(9) .0004(8) O9 .0827(13) .0544(9) .0396(7) .0232(11) .0131(9) .0010(7) O10 .0561(9) .0406(7) .0378(7) -.0049(7) -.0049(7) -.0075(6) C10 .0350(9) .0448(11) .0414(10) -.0014(9) -.0053(8) -.0033(9) C11 .077(2) .0530(13) .0431(11) .0065(15) .0123(12) .0123(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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol C1 1.1406(3) 1.0338(2) .80369(8) .0307(4) Uani d . 1 . C C2 1.0376(3) 1.0004(3) .74463(9) .0372(4) Uani d . 1 . C H2 .8937(3) .9425(3) .74253(9) .045 Uiso calc R 1 . H C3 1.1500(4) 1.0538(3) .68827(9) .0440(5) Uani d . 1 . C H3 1.0798(4) 1.0339(3) .64770(9) .053 Uiso calc R 1 . H C4 1.3644(4) 1.1362(3) .69079(10) .0444(5) Uani d . 1 . C H4 1.4392(4) 1.1709(3) .65218(10) .053 Uiso calc R 1 . H C5 1.4673(4) 1.1669(3) .75034(10) .0386(4) Uani d . 1 . C H5 1.6125(4) 1.2228(3) .75228(10) .046 Uiso calc R 1 . H C6 1.3572(3) 1.1155(3) .80712(9) .0322(4) Uani d . 1 . C O7 1.0268(2) .9817(2) .85995(6) .0393(4) Uani d . 1 . O C8 1.1450(4) 1.0199(3) .91985(9) .0400(5) Uani d . 1 . C O8 1.3813(3) .9872(2) .91259(7) .0427(4) Uani d . 1 . O C9 1.1400(4) 1.2310(3) .92953(8) .0425(5) Uani d . 1 . C O9 .9928(4) 1.3241(2) .95272(7) .0589(5) Uani d . 1 . O O10 1.3361(3) 1.2977(2) .90417(7) .0448(4) Uani d . 1 . O C10 1.4498(4) 1.1406(3) .87410(9) .0404(5) Uani d . 1 . C H10 1.6183(4) 1.1557(3) .87385(9) .048 Uiso calc R 1 . H C11 1.0404(5) .9073(4) .97256(11) .0576(7) Uani d . 1 . C H11A 1.121(2) .931(2) 1.0131(2) .086 Uiso calc R 1 . H H11B 1.052(3) .7772(4) .9616(5) .086 Uiso calc R 1 . H H11C .8804(11) .941(2) .9774(7) .086 Uiso calc R 1 . H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 C1 O7 118.6(2) ? C2 C1 C6 120.9(2) ? O7 C1 C6 120.4(2) ? C1 C2 C3 118.8(2) ? C2 C3 C4 121.0(2) ? C5 C4 C3 119.6(2) ? C4 C5 C6 120.1(2) ? C5 C6 C1 119.4(2) ? C5 C6 C10 125.3(2) ? C1 C6 C10 115.2(2) ? C1 O7 C8 115.59(15) yes O8 C8 O7 110.3(2) ? O8 C8 C11 112.8(2) ? O7 C8 C11 108.8(2) ? O8 C8 C9 101.5(2) ? O7 C8 C9 107.0(2) ? C11 C8 C9 116.2(2) ? C8 O8 C10 101.8(2) yes O9 C9 O10 124.4(2) ? O9 C9 C8 128.7(2) ? O10 C9 C8 106.8(2) ? C9 O10 C10 105.8(2) yes O8 C10 O10 104.18(15) ? O8 C10 C6 108.5(2) ? O10 C10 C6 108.8(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . 1.376(3) ? C1 O7 . 1.386(2) yes C1 C6 . 1.397(3) yes C2 C3 . 1.386(3) ? C3 C4 . 1.387(3) ? C4 C5 . 1.381(3) ? C5 C6 . 1.383(3) ? C6 C10 . 1.490(3) yes O7 C8 . 1.438(2) yes C8 O8 . 1.407(3) yes C8 C11 . 1.486(3) ? C8 C9 . 1.539(3) yes O8 C10 . 1.420(3) yes C9 O9 . 1.191(3) yes C9 O10 . 1.347(3) yes O10 C10 . 1.454(3) yes 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 O7 C1 C2 C3 179.4(2) C6 C1 C2 C3 -1.7(3) C1 C2 C3 C4 1.3(3) C2 C3 C4 C5 -0.5(3) C3 C4 C5 C6 0.1(3) C4 C5 C6 C1 -0.5(3) C4 C5 C6 C10 179.8(2) C2 C1 C6 C5 1.3(3) O7 C1 C6 C5 -179.8(2) C2 C1 C6 C10 -179.0(2) O7 C1 C6 C10 -0.1(2) C2 C1 O7 C8 179.7(2) C6 C1 O7 C8 0.8(2) C1 O7 C8 O8 -38.4(2) C1 O7 C8 C11 -162.7(2) C1 O7 C8 C9 71.1(2) O7 C8 O8 C10 73.4(2) C11 C8 O8 C10 -164.8(2) C9 C8 O8 C10 -39.8(2) O8 C8 C9 O9 -160.4(2) O7 C8 C9 O9 84.0(2) C11 C8 C9 O9 -37.6(3) O8 C8 C9 O10 21.8(2) O7 C8 C9 O10 -93.8(2) C11 C8 C9 O10 144.5(2) O9 C9 O10 C10 -172.7(2) C8 C9 O10 C10 5.3(2) C8 O8 C10 O10 44.8(2) C8 O8 C10 C6 -71.0(2) C9 O10 C10 O8 -30.8(2) C9 O10 C10 C6 84.8(2) C5 C6 C10 O8 -144.2(2) C1 C6 C10 O8 36.2(2) C5 C6 C10 O10 103.1(2) C1 C6 C10 O10 -76.6(2)