#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100681.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_1100681 _publ_section_title ; The Structure of 2-Amino-2-deoxyascorbic acid and 2-Amino-2-deoxyerythorbic acid ; loop_ _publ_author_name 'Tokiko Imai' 'Yokoyama Yoshihiro' 'Akiko Sekine' 'Hidediro Uekusa' 'Yuji Ohashi' _chemical_name_common 'Scorbamic acid' _chemical_formula_sum 'C6 H9 N O5' _chemical_formula_weight 175.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.8162(6) _cell_length_b 16.9420(15) _cell_length_c 4.8651(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 726.67(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3092 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.51 _exptl_crystal_description prism _exptl_crystal_colour 'clear yellow' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS CS Imaging Plate' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3092 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.51 _reflns_number_total 1543 _reflns_number_gt 1459 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.2257P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.6(16) _refine_ls_number_reflns 1543 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.88499(16) 0.44673(8) 0.7717(4) 0.0316(4) Uani 1 1 d . . . O2 O 1.12075(18) 0.47637(10) 0.6256(4) 0.0396(4) Uani 1 1 d . . . O3 O 0.93622(19) 0.31463(9) 1.3340(4) 0.0371(4) Uani 1 1 d . . . O4 O 0.75352(17) 0.28253(8) 0.7412(4) 0.0346(4) Uani 1 1 d . . . H4 H 0.8159 0.2985 0.6291 0.052 Uiso 1 1 calc R . . O5 O 0.44540(17) 0.34613(9) 0.6640(5) 0.0434(5) Uani 1 1 d . . . H5 H 0.4670 0.2991 0.6672 0.065 Uiso 1 1 calc R . . N1 N 1.2319(2) 0.37311(11) 1.0878(5) 0.0339(5) Uani 1 1 d . . . H1A H 1.2351 0.3279 1.1811 0.051 Uiso 1 1 calc R . . H1B H 1.2659 0.4121 1.1936 0.051 Uiso 1 1 calc R . . H1C H 1.2899 0.3692 0.9387 0.051 Uiso 1 1 calc R . . C1 C 1.0407(2) 0.44040(11) 0.7866(5) 0.0288(5) Uani 1 1 d . . . C2 C 1.0774(2) 0.38943(12) 1.0067(5) 0.0282(4) Uani 1 1 d . . . C3 C 0.9500(2) 0.36199(11) 1.1371(5) 0.0287(4) Uani 1 1 d . . . C4 C 0.8174(2) 0.40243(12) 0.9953(5) 0.0298(5) Uani 1 1 d . . . H4A H 0.7715 0.4398 1.1247 0.036 Uiso 1 1 calc R . . C5 C 0.6939(2) 0.34731(12) 0.8899(5) 0.0296(5) Uani 1 1 d . . . H5A H 0.6405 0.3260 1.0504 0.035 Uiso 1 1 calc R . . C6 C 0.5782(2) 0.39172(12) 0.7168(6) 0.0333(5) Uani 1 1 d . . . H6A H 0.5495 0.4399 0.8115 0.040 Uiso 1 1 calc R . . H6B H 0.6244 0.4065 0.5433 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0268(7) 0.0240(6) 0.0440(10) 0.0068(6) -0.0006(7) -0.0014(5) O2 0.0336(8) 0.0380(9) 0.0471(10) 0.0153(8) -0.0032(8) -0.0102(6) O3 0.0405(8) 0.0313(7) 0.0395(10) 0.0083(6) 0.0128(7) 0.0058(6) O4 0.0325(7) 0.0209(6) 0.0503(10) -0.0020(6) 0.0143(8) -0.0019(6) O5 0.0279(7) 0.0314(7) 0.0708(14) -0.0016(8) -0.0051(9) -0.0013(6) N1 0.0274(8) 0.0266(8) 0.0478(13) 0.0046(7) -0.0052(9) -0.0032(6) C1 0.0262(9) 0.0221(8) 0.0380(13) 0.0010(7) -0.0019(9) -0.0036(7) C2 0.0256(9) 0.0248(8) 0.0343(12) 0.0047(8) -0.0006(8) -0.0003(8) C3 0.0294(9) 0.0198(8) 0.0368(12) -0.0016(7) 0.0029(9) 0.0013(7) C4 0.0269(9) 0.0220(9) 0.0405(13) 0.0001(9) 0.0044(9) 0.0018(7) C5 0.0234(8) 0.0246(9) 0.0407(13) 0.0005(8) 0.0078(9) -0.0004(7) C6 0.0263(9) 0.0267(9) 0.0470(14) 0.0007(9) 0.0038(9) -0.0003(8) _cod_database_code 1100681