#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003451.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_2003451 loop_ _publ_author_name 'Yufit, D. S.' 'Kozhushkov, S. I.' 'de Mejere, A.' _publ_section_title trans-2-[(Dispiro[2.0.2.1]hept-7-yl)carbonyl]-3-methyl-\b-propiolactone _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 948 _journal_page_last 950 _journal_paper_doi 10.1107/S0108270194012333 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C12 H14 O3' _chemical_formula_weight 206.2 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source 'SHELXTL-Plus (Sheldrick, 1990)' _cell_angle_alpha 107.69(3) _cell_angle_beta 100.23(3) _cell_angle_gamma 73.48(3) _cell_formula_units_Z 2 _cell_length_a 8.000(4) _cell_length_b 10.162(4) _cell_length_c 7.198(2) _cell_measurement_reflns_used 20 _cell_measurement_temperature 123 _cell_measurement_theta_max 13 _cell_measurement_theta_min 12 _cell_volume 531.8(4) _diffrn_measurement_device 'Rigaku AFC-6S' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3000 _diffrn_reflns_theta_max 30 _diffrn_standards_decay_% 'not significant' _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.29 _exptl_crystal_description prism _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.34 _refine_diff_density_min -0.21 _refine_ls_goodness_of_fit_obs 2.78 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 192 _refine_ls_number_reflns 2267 _refine_ls_R_factor_obs 0.038 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s^2^(F)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.037 _reflns_number_observed 2267 _reflns_number_total 2799 _reflns_observed_criterion F>=4\s(F) _cod_data_source_file ha1129.cif _cod_data_source_block ha1129a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/\s^2^(F)' 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^(F)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2003451 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O(1) .8502(1) .6188(1) .1221(1) .029(1) O(2) .8237(1) .6871(1) -.1582(1) .026(1) O(3) .9248(1) .9567(1) .2259(1) .026(1) C(1) 1.4980(2) .9369(2) .2193(2) .026(1) C(2) 1.4177(2) .8508(2) .0288(2) .024(1) C(3) 1.3839(2) .8463(1) .2227(2) .018(1) C(4) 1.3787(2) .7436(1) .3209(2) .019(1) C(5) 1.4134(2) .5866(1) .2827(2) .027(1) C(6) 1.4938(2) .6763(2) .4691(2) .028(1) C(7) 1.2217(2) .8703(1) .3253(2) .018(1) C(8) 1.0582(2) .8611(1) .1982(2) .018(1) C(9) 1.0535(2) .7316(1) .0239(2) .018(1) C(10) .9015(2) .6676(1) .0183(2) .021(1) C(11) .9592(2) .7590(1) -.1716(2) .022(1) C(12) 1.0497(2) .6867(2) -.3544(2) .031(1) H(1.1) 1.4513(19) 1.0389(17) .2524(21) .033(4) H(1.2) 1.6224(20) .9034(15) .2547(20) .031(4) H(2.1) 1.3258(18) .9021(15) -.0473(20) .027(4) H(2.2) 1.4991(19) .7673(16) -.0449(21) .033(4) H(5.1) 1.4936(20) .5264(18) .1825(23) .042(4) H(5.2) 1.3164(19) .5445(16) .2947(21) .035(4) H(6.1) 1.4481(20) .6872(17) .5898(23) .041(4) H(6.2) 1.6181(20) .6715(16) .4790(21) .034(4) H(7) 1.2053(17) .9429(15) .4429(20) .025(4) H(9) 1.1611(17) .6607(14) .0104(18) .019(3) H(11) .8986(17) .8602(15) -.1591(19) .025(4) H(121) .9644(19) .6895(16) -.4739(22) .034(4) H(122) 1.1107(21) .5887(19) -.3544(22) .042(5) H(123) 1.1388(21) .7348(18) -.3559(23) .045(5) 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 C(10) O(2) C(11) 91.30(10) yes C(1) C(2) C(3) 58.70(10) yes C(1) C(3) C(4) 139.50(10) yes C(1) C(3) C(7) 134.50(10) yes C(4) C(3) C(7) 61.40(10) yes C(3) C(4) C(6) 136.40(10) yes C(3) C(4) C(7) 62.20(10) yes C(6) C(4) C(7) 135.40(10) yes C(4) C(6) C(5) 59.20(10) yes C(3) C(7) C(8) 116.30(10) yes O(3) C(8) C(7) 121.60(10) yes C(7) C(8) C(9) 119.90(10) yes C(8) C(9) C(11) 117.30(10) yes O(1) C(10) O(2) 127.00(10) yes O(2) C(10) C(9) 95.50(10) yes O(2) C(11) C(12) 111.80(10) yes C(2) C(1) C(3) 59.20(10) yes C(1) C(3) C(2) 62.20(10) yes C(2) C(3) C(4) 139.40(10) yes C(2) C(3) C(7) 136.00(10) yes C(3) C(4) C(5) 139.00(10) yes C(5) C(4) C(6) 61.90(10) yes C(5) C(4) C(7) 138.10(10) yes C(4) C(5) C(6) 58.80(10) yes C(3) C(7) C(4) 56.40(10) yes C(4) C(7) C(8) 122.90(10) yes O(3) C(8) C(9) 118.50(10) yes C(8) C(9) C(10) 112.30(10) yes C(10) C(9) C(11) 83.80(10) yes O(1) C(10) C(9) 137.50(10) yes O(2) C(11) C(9) 89.30(10) yes C(9) C(11) C(12) 119.00(10) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O(1) C(10) 1.193(2) yes O(2) C(10) 1.357(2) yes O(2) C(11) 1.500(2) yes O(3) C(8) 1.2210(10) yes C(1) C(2) 1.529(2) yes C(1) C(3) 1.477(2) yes C(2) C(3) 1.484(2) yes C(3) C(4) 1.440(2) yes C(3) C(7) 1.530(2) yes C(4) C(5) 1.485(2) yes C(4) C(6) 1.480(2) yes C(4) C(7) 1.519(2) yes C(5) C(6) 1.526(2) yes C(7) C(8) 1.466(2) yes C(8) C(9) 1.522(2) yes C(9) C(10) 1.524(2) yes C(9) C(11) 1.539(2) yes C(11) C(12) 1.498(2) yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 101923758