#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003336.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003336 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 700 _journal_page_last 703 _publ_section_title ; Two Highly Substituted Methylenecyclopropanes ; _chemical_formula_sum 'C12 H20 O2' _chemical_formula_weight 196.3 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' '-x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 12.398(2) _cell_length_b 10.057(1) _cell_length_c 10.177(1) _cell_angle_alpha 90.00 _cell_angle_beta 109.65(1) _cell_angle_gamma 90.00 _cell_volume 1194.9(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.3 _cell_measurement_theta_max 27.7 _exptl_absorpt_coefficient_mu 0.072 _cell_measurement_temperature 293(2) _exptl_crystal_description 'needle' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w-2\q scan' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2512 _reflns_number_total 2294 _reflns_number_observed 1308 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 'linear correction for 51% intensity decay' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0511 _refine_ls_wR_factor_obs 0.0799 _refine_ls_wR_factor_all 0.4120 _refine_ls_goodness_of_fit_obs 1.17 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1308 _refine_ls_number_parameters 132 _refine_ls_hydrogen_treatment ; H atoms riding, C-H 0.96\%A, O---H refxyzU ; _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0034F^2^]' _refine_ls_shift/esd_max 0.02 _refine_diff_density_max 0.20 _refine_diff_density_min -0.17 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 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 O(1) 1 0.9029(2) 0.2365(2) 0.5143(2) 0.047(1) O(2) 1 0.8935(2) 0.0961(2) 0.7834(2) 0.054(1) C(1) 1 0.8347(2) 0.2623(2) 0.5989(2) 0.041(1) C(2) 1 0.8545(3) 0.3947(2) 0.6761(3) 0.057(1) C(3) 1 0.7544(3) 0.3725(2) 0.5520(3) 0.050(1) C(4) 1 0.6589(3) 0.4163(3) 0.4622(4) 0.075(1) C(5) 1 1.0208(3) 0.2132(4) 0.5894(3) 0.078(2) C(6) 1 0.8010(2) 0.1422(2) 0.6659(2) 0.042(1) C(7) 1 0.7599(2) 0.0249(2) 0.5662(2) 0.042(1) C(8) 1 0.7112(3) -0.0860(3) 0.6328(3) 0.057(1) C(9) 1 0.6759(3) -0.2072(3) 0.5375(3) 0.068(1) C(10) 1 0.5921(3) -0.1703(3) 0.3952(3) 0.066(1) C(11) 1 0.6386(3) -0.0585(3) 0.3300(3) 0.059(1) C(12) 1 0.6721(2) 0.0622(3) 0.4265(2) 0.047(1) H(2A) 1 0.902(3) 0.148(3) 0.865(4) 0.100(12) H(2B) 1 0.9141 0.4514 0.6677 0.075(2) H(2C) 1 0.8432 0.3979 0.7648 0.075(2) H(4A) 1 0.6137 0.3593 0.3884 0.075(2) H(4B) 1 0.6339 0.5054 0.4697 0.075(2) H(5A) 1 1.0604 0.1965 0.5247 0.075(2) H(5B) 1 1.0531 0.2901 0.6445 0.075(2) H(5C) 1 1.0284 0.1376 0.6494 0.075(2) H(6A) 1 0.7396 0.1680 0.6980 0.075(2) H(7A) 1 0.8255 -0.0106 0.5483 0.075(2) H(8A) 1 0.6458 -0.0530 0.6530 0.075(2) H(8B) 1 0.7677 -0.1122 0.7194 0.075(2) H(9A) 1 0.6414 -0.2719 0.5803 0.075(2) H(9B) 1 0.7428 -0.2467 0.5264 0.075(2) H(10A) 1 0.5207 -0.1435 0.4046 0.075(2) H(10B) 1 0.5778 -0.2468 0.3354 0.075(2) H(11A) 1 0.5811 -0.0326 0.2440 0.075(2) H(11B) 1 0.7041 -0.0895 0.3087 0.075(2) H(12A) 1 0.7036 0.1296 0.3832 0.075(2) H(12B) 1 0.6052 0.0983 0.4408 0.075(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O(1) 0.042(1) -0.000(1) 0.018(1) 0.063(1) 0.001(1) 0.040(1) O(2) 0.060(1) 0.001(1) 0.011(1) 0.063(1) 0.011(1) 0.035(1) C(1) 0.041(1) -0.007(1) 0.016(1) 0.048(1) -0.004(1) 0.037(1) C(2) 0.070(2) -0.013(1) 0.026(2) 0.050(2) -0.012(1) 0.054(2) C(3) 0.058(2) -0.000(1) 0.023(1) 0.042(1) 0.005(1) 0.052(2) C(4) 0.081(2) -0.002(2) 0.016(2) 0.051(2) 0.019(2) 0.083(2) C(5) 0.049(2) 0.015(2) 0.028(2) 0.119(3) 0.012(2) 0.071(2) C(6) 0.042(1) 0.001(1) 0.017(1) 0.049(1) 0.007(1) 0.036(1) C(7) 0.044(1) -0.000(1) 0.019(1) 0.042(1) 0.005(1) 0.043(1) C(8) 0.067(2) 0.005(1) 0.019(2) 0.051(2) -0.001(1) 0.054(2) C(9) 0.085(2) 0.002(2) 0.034(2) 0.047(2) -0.009(2) 0.077(2) C(10) 0.076(2) -0.017(2) 0.032(2) 0.060(2) -0.019(2) 0.069(2) C(11) 0.064(2) -0.013(1) 0.021(1) 0.066(2) -0.018(2) 0.049(2) C(12) 0.051(2) -0.003(1) 0.019(1) 0.048(1) -0.005(1) 0.043(1)