data_7150001 loop_ _publ_author_name 'Pritchard, Robin G.' 'Stoodley, Richard J.' 'Yuen, Wai-Hung' _publ_section_title ; Studies related to carba-pyranoses: synthesis of acetylated derivatives of 4-amino-2,4-dideoxy-3-O-(beta-D-glucopyranosyl)-beta-L-(and beta-D-) altrocarba-pyranose from a D-glucose template. ; _journal_issue 1 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 162 _journal_page_last 171 _journal_volume 3 _journal_year 2005 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C4 H5 N1 O4' _chemical_formula_sum 'C4 H5 N O4' _chemical_formula_weight 131.09 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_creation_date 2004-07-20T01:14:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 96.99(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.356(2) _cell_length_b 6.688(2) _cell_length_c 16.787(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.2 _cell_measurement_theta_min 9.2 _cell_measurement_wavelength 0.71073 _cell_volume 596.9(4) _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measured_fraction_theta_full 0.836 _diffrn_measured_fraction_theta_max 0.836 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_unetI/netI 0.0329 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 987 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.44 _diffrn_source 'Enraf Nonius FR590' _diffrn_standards_decay_% -3 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_T_max 0.9803 _exptl_absorpt_correction_T_min 0.9611 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 272 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.19 _refine_diff_density_min -0.141 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 90 _refine_ls_number_reflns 878 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.146 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0534 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.2347P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.1404 _reflns_number_gt 621 _reflns_number_total 878 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b410556g.txt _[local]_cod_data_source_block tom96y _cod_database_code 7150001 #BEGIN Tags that were not found in dictionaries: _diffrn_standards_decay_corr_max 1.01 _diffrn_standards_decay_corr_min 0.943 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.1496(4) 0.1599(3) 0.42302(12) 0.0613(7) Uani 1 1 d . . . O2 O 0.5209(6) 0.2451(4) 0.48988(14) 0.0693(8) Uani 1 1 d . . . O3 O -0.1138(5) 0.4165(4) 0.67225(13) 0.0713(8) Uani 1 1 d . . . O4 O 0.2231(5) 0.5610(4) 0.72791(14) 0.0836(9) Uani 1 1 d . . . N1 N 0.1090(6) 0.4578(4) 0.67540(14) 0.0548(8) Uani 1 1 d . . . C1 C 0.2973(8) 0.2320(5) 0.48607(17) 0.0488(9) Uani 1 1 d . . . C2 C 0.1457(8) 0.2924(5) 0.54976(17) 0.0500(9) Uani 1 1 d . . . C3 C 0.2531(7) 0.3869(5) 0.61290(17) 0.0513(9) Uani 1 1 d . . . C4 C 0.2745(7) 0.0982(6) 0.35490(18) 0.0714(11) Uani 1 1 d . . . H4A H 0.1517 0.0489 0.3131 0.107 Uiso 0.5 1 calc PR . . H4B H 0.3936 -0.0056 0.3713 0.107 Uiso 0.5 1 calc PR . . H4C H 0.3606 0.2105 0.3353 0.107 Uiso 0.5 1 calc PR . . H4D H 0.4522 0.1203 0.3667 0.107 Uiso 0.5 1 calc PR . . H4E H 0.2103 0.1748 0.3085 0.107 Uiso 0.5 1 calc PR . . H4F H 0.2433 -0.0413 0.3444 0.107 Uiso 0.5 1 calc PR . . H2 H -0.024(7) 0.265(5) 0.5433(17) 0.050(10) Uiso 1 1 d . . . H3 H 0.428(7) 0.410(5) 0.6230(19) 0.061(11) Uiso 1 1 d . . . 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 0.0642(17) 0.0760(15) 0.0428(11) -0.0071(11) 0.0037(10) -0.0026(13) O2 0.0545(19) 0.0899(19) 0.0640(15) -0.0133(13) 0.0089(11) -0.0033(15) O3 0.0632(19) 0.0938(19) 0.0588(14) -0.0059(12) 0.0150(12) -0.0065(16) O4 0.095(2) 0.094(2) 0.0582(15) -0.0282(14) -0.0030(14) -0.0051(16) N1 0.067(2) 0.0567(17) 0.0402(14) 0.0006(12) 0.0023(13) 0.0016(17) C1 0.055(3) 0.0475(18) 0.0436(16) 0.0034(13) 0.0043(15) -0.0032(18) C2 0.054(3) 0.0509(19) 0.0448(17) 0.0077(14) 0.0038(15) -0.0060(18) C3 0.050(3) 0.057(2) 0.0466(17) -0.0013(15) 0.0045(15) -0.0026(18) C4 0.091(3) 0.076(2) 0.0485(18) -0.0101(17) 0.0122(18) 0.005(2) 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 0 1 0 2 1 0 1 3 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C4 116.3(3) . . ? O3 N1 O4 124.0(3) . . ? O3 N1 C3 119.8(3) . . ? O4 N1 C3 116.2(3) . . ? O2 C1 O1 124.3(3) . . ? O2 C1 C2 125.3(3) . . ? O1 C1 C2 110.4(3) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2 121.5(19) . . ? C1 C2 H2 118.9(19) . . ? C2 C3 N1 121.6(4) . . ? C2 C3 H3 124(2) . . ? N1 C3 H3 114.7(19) . . ? O1 C4 H4A 109.5 . . ? O1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C4 H4D 109.5 . . ? H4A C4 H4D 141.1 . . ? H4B C4 H4D 56.3 . . ? H4C C4 H4D 56.3 . . ? O1 C4 H4E 109.5 . . ? H4A C4 H4E 56.3 . . ? H4B C4 H4E 141.1 . . ? H4C C4 H4E 56.3 . . ? H4D C4 H4E 109.5 . . ? O1 C4 H4F 109.5 . . ? H4A C4 H4F 56.3 . . ? H4B C4 H4F 56.3 . . ? H4C C4 H4F 141.1 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.332(4) . ? O1 C4 1.453(4) . ? O2 C1 1.195(4) . ? O3 N1 1.220(3) . ? O4 N1 1.223(3) . ? N1 C3 1.455(4) . ? C1 C2 1.475(5) . ? C2 C3 1.306(4) . ? C2 H2 0.92(3) . ? C3 H3 0.94(3) . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C4 H4D 0.96 . ? C4 H4E 0.96 . ? C4 H4F 0.96 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 O1 C1 O2 -1.3(5) . . . . ? C4 O1 C1 C2 178.8(3) . . . . ? O2 C1 C2 C3 7.5(5) . . . . ? O1 C1 C2 C3 -172.6(3) . . . . ? C1 C2 C3 N1 177.0(3) . . . . ? O3 N1 C3 C2 5.3(5) . . . . ? O4 N1 C3 C2 -173.2(3) . . . . ?