#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003192.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_2003192 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 268 _journal_page_last 270 _publ_section_title ; (1\b,5\a,6\b)-10,10-(1,2-Ethylenedioxy)-1,5-di-methylbicyclo [4.4.0]decan-4-one ; _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Kwangyong Park' 'Dale C. Swenson' 'William J. Scott' 'David F. Wiemer' _chemical_formula_moiety 'C14 H22 O3' _chemical_formula_sum 'C14 H22 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 238.3 _cell_length_a 7.889(1) _cell_length_b 19.490(3) _cell_length_c 8.559(1) _cell_angle_alpha 90 _cell_angle_beta 101.70(1) _cell_angle_gamma 90 _cell_volume 1288.7(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.23 _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 13 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.079 _cell_measurement_temperature 295 _exptl_crystal_description 'irregular cube' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.28 _exptl_crystal_colour clear _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method ;\q-2\q scans [range (0.8 + 0.35tan\q)\%, speed 1.67-5.0\% min^-1^, background determined by the Lehman-Larson method] ; _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _diffrn_reflns_number 5325 _reflns_number_total 2622 _reflns_number_observed 1840 _reflns_observed_criterion I>2\s(I) _diffrn_reflns_av_r_equivalents '0.058 on I' _diffrn_reflns_theta_max 30 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_standards_number 4 _diffrn_standards_interval_count '400 for orientation' _diffrn_standards_interval_time '240 min for intensity' _diffrn_standards_decay_% <2.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.046 _refine_ls_wR_factor_obs 0.072 _refine_ls_goodness_of_fit_obs 1.43 _refine_ls_number_reflns 1840 _refine_ls_number_parameters 154 _refine_ls_hydrogen_treatment ; All H atoms were included in the structure-factor calculation at fixed positions with C-H = 0.95\%A. ; _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(F) + (0.04F)^2^]' _refine_ls_shift/esd_max 0.03 _refine_diff_density_max 0.22 _refine_diff_density_min -0.15 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV' _refine_ls_abs_structure_details ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O(1) 0.4615(2) 0.8721(1) 0.1527(2) 0.0978(5) O(2) 0.9159(1) 0.85509(6) 0.8481(1) 0.0504(3) O(3) 1.0664(1) 0.93121(6) 0.7265(1) 0.0598(4) C(1) 0.8336(2) 0.86594(8) 0.5612(2) 0.0404(4) C(2) 0.8426(2) 0.91508(9) 0.4218(2) 0.0531(5) C(3) 0.7603(3) 0.8857(1) 0.2588(2) 0.0655(5) C(4) 0.5842(3) 0.8565(1) 0.2549(2) 0.0613(5) C(5) 0.5703(2) 0.80745(9) 0.3882(2) 0.0550(5) C(6) 0.6438(2) 0.84245(8) 0.5514(2) 0.0422(4) C(7) 0.5260(2) 0.9009(1) 0.5847(2) 0.0552(5) C(8) 0.5950(2) 0.9355(1) 0.7431(2) 0.0632(5) C(9) 0.7778(2) 0.96122(9) 0.7524(2) 0.0588(5) C(10) 0.8976(2) 0.90382(8) 0.7212(2) 0.0432(4) C(11) 0.9534(2) 0.8043(1) 0.5562(2) 0.0617(5) C(12) 0.3883(3) 0.7788(1) 0.3735(3) 0.0865(6) C(13) 1.0684(2) 0.8728(1) 0.9620(2) 0.0599(5) C(14) 1.1795(2) 0.9087(1) 0.8675(2) 0.0585(5) H(11A) 0.9427 0.7730 0.6387 0.08* H(11B) 0.9217 0.7820 0.4556 0.08* H(11C) 1.0698 0.8197 0.5708 0.08* H(12B) 0.3858 0.7481 0.4594 0.1* H(12C) 0.3559 0.7549 0.2752 0.1* H(12A) 0.3095 0.8154 0.3766 0.1* H(2A) 0.7839 0.9563 0.4373 0.06* H(2B) 0.9607 0.9248 0.4227 0.06* H(3A) 0.7508 0.9212 0.1816 0.08* H(3B) 0.8329 0.8503 0.2328 0.08* H(5) 0.6391 0.7680 0.3808 0.06* H(6) 0.6455 0.8095 0.6334 0.05* H(7A) 0.5173 0.9340 0.5020 0.06* H(7B) 0.4144 0.8828 0.5857 0.06* H(8A) 0.5224 0.9731 0.7551 0.08* H(8B) 0.5946 0.9034 0.8265 0.08* H(9A) 0.7764 0.9962 0.6749 0.08* H(9B) 0.8202 0.9794 0.8559 0.08* H(13A) 1.0408 0.9022 1.0417 0.08* H(13B) 1.1243 0.8328 1.0107 0.08* H(14A) 1.2639 0.8782 0.8421 0.08* H(14B) 1.2356 0.9467 0.9253 0.08* 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) 0.084(1) -0.021(1) -0.0175(7) 0.134(1) 0.0257(9) 0.0615(8) O(2) 0.0471(6) -0.0133(5) -0.0007(4) 0.0532(6) 0.0088(5) 0.0465(5) O(3) 0.0438(6) -0.0178(5) -0.0006(5) 0.0679(7) 0.0188(6) 0.0630(6) C(1) 0.0381(7) 0.0013(6) 0.0084(5) 0.0387(7) 0.0039(6) 0.0443(7) C(2) 0.0488(8) -0.0091(7) 0.0106(6) 0.060(1) 0.0113(7) 0.0511(8) C(3) 0.071(1) -0.008(1) 0.0159(7) 0.081(1) 0.0105(8) 0.0461(8) C(4) 0.070(1) -0.0074(9) 0.0033(7) 0.071(1) -0.0015(8) 0.0398(8) C(5) 0.062(1) -0.0145(8) 0.0039(7) 0.0535(9) -0.0030(7) 0.0468(8) C(6) 0.0424(7) -0.0061(6) 0.0060(6) 0.0433(8) 0.0039(6) 0.0400(7) C(7) 0.0377(8) 0.0028(8) 0.0083(6) 0.069(1) -0.0006(8) 0.0581(9) C(8) 0.0555(9) 0.0128(9) 0.0163(7) 0.069(1) -0.0124(9) 0.066(1) C(9) 0.064(1) 0.0001(8) 0.0069(8) 0.0482(9) -0.0135(7) 0.0620(9) C(10) 0.0391(7) -0.0069(6) 0.0047(6) 0.0407(8) 0.0041(6) 0.0481(7) C(11) 0.0576(9) 0.0181(8) 0.0113(8) 0.060(1) -0.0040(9) 0.067(1) C(12) 0.086(1) -0.049(1) -0.0024(9) 0.103(1) -0.003(1) 0.063(1) C(13) 0.0518(9) -0.0133(8) -0.0016(7) 0.070(1) 0.0086(8) 0.0527(9) C(14) 0.0484(9) -0.0104(8) 0.0003(7) 0.068(1) 0.0008(8) 0.0549(9)