#------------------------------------------------------------------------------ #$Date: 2009-11-18 15:56:34 +0100 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003275.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_2003275 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 515 _journal_page_last 517 _publ_section_title ; 5-Fluoro-8,8-dimethyl-7-oxa-3,9-diazabicyclo[4.3.0]nona-1,6-dien-2,4-dione (C~8~H~7~FN~2~O~3~): A Novel Product from Pyrolysis of N-Isopropylidene-O-tetrafluoro-4-pyridylhydroxylamine in Glass ; _chemical_formula_moiety 'C8 H7 F1 N2 O3' _chemical_formula_sum 'C8 H7 F N2 O3' _[local]_cod_chemical_formula_sum_orig 'C8 H7 F1 N2 O3' _chemical_formula_structural 'C8 H7 F1 N2 O3' _chemical_formula_weight 198.15 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 25.171(3) _cell_length_b 5.245(1) _cell_length_c 15.557(2) _cell_angle_alpha 90 _cell_angle_beta 121.92(2) _cell_angle_gamma 90 _cell_volume 1743(1) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 24.0 _exptl_absorpt_coefficient_mu 0.1229 _cell_measurement_temperature 296 _exptl_crystal_description 'needle' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_size_rad ? _exptl_crystal_colour 'black' _chemical_compound_source 'synthesis' _diffrn_measurement_device 'CAD-4' _diffrn_measurement_method '\w/2theta scans' _exptl_absorpt_correction_type none _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _diffrn_reflns_number 3258 _reflns_number_total 1729 _reflns_number_observed 842 _reflns_observed_criterion 'I>2\s(I)' _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not significant' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0414 _refine_ls_wR_factor_obs 0.0270 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 1.947 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 842 _refine_ls_number_parameters 156 _refine_ls_hydrogen_treatment ;All H atoms located from \DF maps and isotropically refined ; _refine_ls_weighting_scheme sigma _refine_ls_shift/esd_max 0.0512 _refine_diff_density_max 0.19375 _refine_diff_density_min -0.16216 _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef ' 2.1 (1) x 10^-7^ ' loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'International Tables' 0.002 0.002 H 'International Tables' 0.000 0.000 F 'International Tables' 0.014 0.010 N 'International Tables' 0.004 0.003 O 'International Tables' 0.008 0.006 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? ##;MSC/AFC (Molecular Structure Corporation, 1988) ##; ##;TEXSAN: PROCESS (Molecular Structure Corporation, 1985) ##; ##;TEXSAN: LS (Molecular Structure Corporation, 1985) ##; ##;TEXSAN: FINISH (Molecular Structure Corporation, 1985). Literature ##surveyed using CSSR (1984) ##; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv F2 0.40884(9) 1.0681(4) 0.5073(1) 0.057(1) O3 0.3120(1) 0.9505(5) 0.5275(2) 0.058(1) O5 0.25261(10) 0.2664(4) 0.3191(2) 0.053(1) O9 0.42552(9) 0.7240(4) 0.3740(2) 0.046(1) N4 0.2831(1) 0.6113(6) 0.4218(2) 0.043(1) N7 0.3582(1) 0.3720(5) 0.2954(2) 0.041(1) C1 0.3811(1) 0.7164(6) 0.3964(2) 0.036(1) C2 0.3726(2) 0.8654(7) 0.4570(2) 0.039(1) C3 0.3210(2) 0.8184(7) 0.4719(3) 0.041(1) C5 0.2877(2) 0.4414(7) 0.3581(2) 0.040(2) C6 0.3418(2) 0.5008(6) 0.3473(2) 0.034(1) C8 0.4123(2) 0.5021(7) 0.3049(2) 0.042(1) C10 0.4693(2) 0.3342(9) 0.3556(4) 0.057(2) C11 0.3960(2) 0.610(1) 0.2045(3) 0.065(2) H4 0.253(1) 0.592(6) 0.430(2) 0.05(1) H10A 0.480(1) 0.252(7) 0.427(2) 0.08(1) H10B 0.505(1) 0.432(6) 0.367(2) 0.05(1) H10C 0.463(2) 0.204(7) 0.314(2) 0.08(1) H11A 0.387(2) 0.483(7) 0.161(3) 0.07(1) H11B 0.357(2) 0.724(8) 0.176(3) 0.13(2) H11C 0.433(2) 0.709(6) 0.218(3) 0.08(1) 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 F2 0.064(1) -0.018(1) 0.038(1) 0.049(1) -0.017(1) 0.064(1) O3 0.071(2) -0.012(1) 0.048(1) 0.060(2) -0.021(2) 0.062(2) O5 0.049(2) -0.018(1) 0.031(1) 0.054(2) -0.016(1) 0.059(2) O9 0.046(1) -0.007(1) 0.035(1) 0.048(2) -0.004(1) 0.056(2) N4 0.041(2) -0.009(2) 0.030(2) 0.051(2) -0.008(2) 0.048(2) N7 0.042(2) 0.000(2) 0.023(1) 0.042(2) -0.006(1) 0.041(2) C1 0.033(2) 0.000(2) 0.019(2) 0.039(2) 0.004(2) 0.036(2) C2 0.040(2) -0.009(2) 0.021(2) 0.035(2) -0.005(2) 0.041(2) C3 0.045(2) -0.001(2) 0.022(2) 0.042(2) 0.002(2) 0.036(2) C5 0.039(2) -0.004(2) 0.019(2) 0.042(3) -0.002(2) 0.037(2) C6 0.030(2) 0.002(2) 0.014(2) 0.036(2) 0.001(2) 0.031(2) C8 0.042(2) -0.002(2) 0.025(2) 0.047(2) -0.006(2) 0.041(2) C10 0.042(3) 0.013(2) 0.035(3) 0.061(3) 0.007(3) 0.075(3) C11 0.069(3) 0.003(3) 0.038(3) 0.086(4) 0.004(3) 0.050(3)