#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/00/2200021.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_2200021 loop_ _publ_author_name 'Czugler, M\'aty\'as' 'Bombicz, Petra' _publ_section_title ; 6,7-Dimethyl-3a,8a-dihydro-3H-8-oxacyclopenta[a]inden-5-yl benzoate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o37 _journal_page_last o38 _journal_volume 57 _journal_year 2001 _chemical_formula_sum 'C20 H18 O3' _chemical_formula_weight 306.34 _chemical_name_systematic ; 6,7-dimethyl-3a,8a-dihydro-3H-8-oxa-cyclopenta[a]inden-5-yl benzoate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 101.274(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.9964(10) _cell_length_b 18.6031(10) _cell_length_c 10.9254(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.9 _cell_measurement_theta_min 10.0 _cell_volume 1593.9(3) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_molecular_graphics 'ZORTEP (Zsolnay & Pritzkow, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .974 _diffrn_measured_fraction_theta_max .974 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71070 _diffrn_reflns_av_R_equivalents .017 _diffrn_reflns_av_sigmaI/netI .047 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 6538 _diffrn_reflns_theta_full 33.0 _diffrn_reflns_theta_max 33.0 _diffrn_reflns_theta_min 2.8 _diffrn_standards_decay_% 2 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .09 _exptl_absorpt_correction_T_max .986 _exptl_absorpt_correction_T_min .959 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(MolEN; Enraf-Nonius, 1990)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 648 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .17 _refine_diff_density_max .30 _refine_diff_density_min -.22 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .97 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 215 _refine_ls_number_reflns 6020 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .97 _refine_ls_R_factor_all .131 _refine_ls_R_factor_gt .052 _refine_ls_shift/su_max .009 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0815P)^2^+0.0559P] P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .158 _reflns_number_gt 3130 _reflns_number_total 6020 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf6004.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/a' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 1593.9(2) _cod_database_code 2200021 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 .7761(2) .08635(10) .14329(16) .0646(4) Uani d . 1 . . C H1 .8330 .0496 .1107 .077(4) Uiso calc R 1 . . H C2 .8519(2) .13357(11) .22675(15) .0708(5) Uani d . 1 . . C H2 .9681 .1332 .2603 .077(4) Uiso calc R 1 . . H C3 .7317(3) .18685(10) .26071(16) .0752(5) Uani d . 1 . . C H3B .7534 .2343 .2304 .093(4) Uiso calc R 1 . . H H3C .7411 .1890 .3505 .093(4) Uiso calc R 1 . . H C3A .5559(2) .15973(8) .19726(13) .0544(3) Uani d . 1 . . C H3A .4865 .1983 .1521 .067(3) Uiso calc R 1 . . H C3B .46054(18) .11964(7) .28143(11) .0442(3) Uani d . 1 . . C C4 .40996(18) .14021(7) .39023(11) .0461(3) Uani d . 1 . . C H4 .4305 .1864 .4222 .067(2) Uiso calc R 1 . . H C5 .32755(17) .08942(7) .44976(11) .0419(3) Uani d . 1 . . C C6 .29346(14) .01958(6) .40612(11) .0397(3) Uani d . 1 . . C C7 .34546(16) -.00099(7) .29558(11) .0418(3) Uani d . 1 . . C C7A .42922(16) .05029(7) .23805(10) .0418(3) Uani d . 1 . . C O8 .49083(13) .03627(5) .13135(8) .0532(3) Uani d . 1 . . O C8A .5893(2) .09911(8) .10792(12) .0536(3) Uani d . 1 . . C H8A .5573 .1145 .0207 .067(3) Uiso calc R 1 . . H C9 .20783(19) -.03354(8) .47702(14) .0555(4) Uani d . 1 . . C H9A .2044 -.0146 .5582 .118(3) Uiso calc R 1 . . H H9B .2707 -.0778 .4857 .118(3) Uiso calc R 1 . . H H9C .0937 -.0422 .4325 .118(3) Uiso calc R 1 . . H C10 .3153(2) -.07549(8) .24169(16) .0612(4) Uani d . 1 . . C H10A .3704 -.0803 .1716 .118(3) Uiso calc R 1 . . H H10B .1950 -.0834 .2151 .118(3) Uiso calc R 1 . . H H10C .3611 -.1103 .3041 .118(3) Uiso calc R 1 . . H O11 .28707(13) .10569(5) .56712(8) .0492(2) Uani d . 1 . . O O12 .10692(15) .19461(6) .49072(9) .0662(3) Uani d . 1 . . O C13 .17338(16) .15775(6) .57653(11) .0408(3) Uani d . 1 . . C C14 .14310(15) .16360(6) .70628(11) .0382(2) Uani d . 1 . . C C15 .04804(19) .22128(7) .73546(13) .0510(3) Uani d . 1 . . C H15 .0048 .2548 .6744 .067(2) Uiso calc R 1 . . H C16 .0174(2) .22905(9) .85491(14) .0617(4) Uani d . 1 . . C H16 -.0451 .2681 .8744 .067(2) Uiso calc R 1 . . H C17 .0794(2) .17900(9) .94495(13) .0589(4) Uani d . 1 . . C H17 .0582 .1841 1.0252 .067(2) Uiso calc R 1 . . H C18 .1728(2) .12130(8) .91680(12) .0538(3) Uani d . 1 . . C H18 .2142 .0875 .9780 .067(2) Uiso calc R 1 . . H C19 .20536(17) .11335(7) .79753(12) .0452(3) Uani d . 1 . . C H19 .2688 .0744 .7788 .067(2) 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 C1 .0676(10) .0669(10) .0656(9) .0013(8) .0284(8) .0013(8) C2 .0680(10) .0845(12) .0632(10) -.0166(9) .0207(8) .0069(9) C3 .1016(14) .0658(10) .0679(10) -.0321(10) .0406(10) -.0094(8) C3A .0759(10) .0441(7) .0499(7) .0013(7) .0282(7) .0079(6) C3B .0562(7) .0385(6) .0406(6) .0043(5) .0165(5) .0042(5) C4 .0619(8) .0354(6) .0446(6) .0039(6) .0188(6) -.0012(5) C5 .0483(7) .0433(6) .0364(5) .0093(5) .0140(5) .0009(5) C6 .0355(6) .0421(6) .0424(6) .0036(5) .0099(5) .0032(5) C7 .0403(6) .0416(6) .0434(6) -.0002(5) .0084(5) -.0033(5) C7A .0474(7) .0451(6) .0344(5) .0033(5) .0114(5) -.0024(5) O8 .0683(6) .0546(6) .0417(5) -.0038(5) .0230(4) -.0079(4) C8A .0699(9) .0569(8) .0386(6) -.0020(7) .0219(6) .0037(6) C9 .0531(8) .0520(8) .0672(9) -.0010(6) .0262(7) .0083(7) C10 .0666(9) .0502(8) .0702(10) -.0145(7) .0214(8) -.0183(7) O11 .0620(6) .0508(5) .0385(4) .0172(4) .0194(4) .0037(4) O12 .0805(8) .0724(7) .0483(6) .0334(6) .0189(5) .0146(5) C13 .0435(6) .0385(6) .0421(6) .0017(5) .0123(5) .0000(5) C14 .0400(6) .0366(5) .0394(5) -.0011(5) .0110(4) -.0030(5) C15 .0580(8) .0459(7) .0504(7) .0093(6) .0140(6) -.0017(6) C16 .0731(10) .0570(9) .0600(8) .0125(8) .0258(7) -.0121(7) C17 .0699(10) .0675(9) .0434(7) -.0039(8) .0208(6) -.0100(7) C18 .0638(9) .0580(8) .0403(6) -.0017(7) .0118(6) .0040(6) C19 .0506(7) .0422(6) .0444(6) .0037(5) .0133(5) .0017(5) 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 . 1.324(2) yes C1 C8A . 1.487(2) ? C2 C3 . 1.478(3) yes C3 C3A . 1.526(2) ? C3A C3B . 1.5024(18) ? C3A C8A . 1.548(2) yes C3B C7A . 1.3804(17) yes C3B C4 . 1.3824(17) ? C4 C5 . 1.3848(17) ? C5 C6 . 1.3925(17) ? C5 O11 . 1.4151(14) yes C6 C7 . 1.4051(16) ? C6 C9 . 1.5009(17) ? C7 C7A . 1.3850(17) ? C7 C10 . 1.5067(19) ? C7A O8 . 1.3762(13) yes O8 C8A . 1.4597(17) yes O11 C13 . 1.3459(14) yes O12 C13 . 1.1986(14) yes C13 C14 . 1.4880(16) ? C14 C19 . 1.3862(17) ? C14 C15 . 1.3877(17) ? C15 C16 . 1.3816(19) ? C16 C17 . 1.375(2) ? C17 C18 . 1.376(2) ? C18 C19 . 1.3858(17) ? 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' 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 C8A 111.98(16) ? C1 C2 C3 112.64(17) yes C2 C3 C3A 104.53(14) ? C3B C3A C3 114.75(12) yes C3B C3A C8A 101.25(11) ? C3 C3A C8A 105.66(13) ? C7A C3B C4 119.34(12) ? C7A C3B C3A 109.48(11) ? C4 C3B C3A 131.12(12) yes C3B C4 C5 117.46(12) ? C4 C5 C6 123.71(11) ? C4 C5 O11 119.59(11) ? C6 C5 O11 116.47(11) ? C5 C6 C7 118.51(11) ? C5 C6 C9 121.07(11) ? C7 C6 C9 120.39(11) ? C7A C7 C6 116.95(11) ? C7A C7 C10 120.73(11) ? C6 C7 C10 122.32(12) ? O8 C7A C3B 113.38(11) yes O8 C7A C7 122.61(11) yes C3B C7A C7 124.01(11) ? C7A O8 C8A 106.95(9) ? O8 C8A C1 112.05(12) yes O8 C8A C3A 107.90(10) ? C1 C8A C3A 103.93(13) ? C13 O11 C5 120.04(9) yes O12 C13 O11 123.69(11) yes O12 C13 C14 124.99(11) ? O11 C13 C14 111.31(10) ? C19 C14 C15 119.48(11) ? C19 C14 C13 122.24(11) ? C15 C14 C13 118.28(11) ? C16 C15 C14 120.28(13) ? C17 C16 C15 119.95(13) ? C16 C17 C18 120.26(13) ? C17 C18 C19 120.22(13) ? C18 C19 C14 119.81(12) ? _cod_database_fobs_code 2200021 _journal_paper_doi 10.1107/S1600536800018821