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.
Pritchard, Robin G.; Stoodley, Richard J.; Yuen, Wai-Hung; Organic & biomolecular chemistry 3 (2005) 162–171; doi:10.1039/b410556g

data_7150000
_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 &amp; biomolecular chemistry'
_journal_page_first              162
_journal_page_last               171
_journal_paper_doi               10.1039/b410556g
_journal_volume                  3
_journal_year                    2005
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H31 N1 O15'
_chemical_formula_sum            'C22 H31 N O15'
_chemical_formula_weight         549.48
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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             2004-07-20T00:21:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.380(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.773(1)
_cell_length_b                   22.641(3)
_cell_length_c                   10.86(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.5
_cell_measurement_wavelength     0.71073
_cell_volume                     1369(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.020001
_diffrn_orient_matrix_UB_12      -0.00335
_diffrn_orient_matrix_UB_13      0.094061
_diffrn_orient_matrix_UB_21      -0.166928
_diffrn_orient_matrix_UB_22      -0.015986
_diffrn_orient_matrix_UB_23      -0.016465
_diffrn_orient_matrix_UB_31      0.063356
_diffrn_orient_matrix_UB_32      -0.041036
_diffrn_orient_matrix_UB_33      -0.001245
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.1336
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4176
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        -5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.9666
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         2451
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                1085
_reflns_number_total             2451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b410556g.txt
_cod_data_source_block           simon
_cod_original_cell_volume        1368.6(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7150000
_diffrn_standards_decay_corr_max 1.017
_diffrn_standards_decay_corr_min 0.919