Methyl 2-Aza-2-deoxy-4,6-di-<i>O</i>-methyl-2-<i>N</i>-(<i>p</i>-nitrophenylamino)-β-<small>D</small>-<i>erythro</i>-hexopyranosid-3-ulose
Bernardinelli, Gérald; Tronchet, Jeannine F.; Tronchet, Jean M.J.; Acta Crystallographica Section C 53 (1997) 950–951; doi:10.1107/S0108270197002345

data_2006313
_publ_contact_author
; Dr G\'erald Bernardinelli
  Laboratoire de Cristallographie
  Universit\'e de Gen\`eve
  24 Quai E. Ansermet
  CH - 1211 GENEVE 4
  Switzerland
;
_publ_section_title
;Methyl
 2-Aza-2-deoxy-4,6-di-<i>O</i>-methyl-2-<i>N</i>-(<i>p</i>-nitrophenylamino)-\b-<small>D</small>-<i>erythro</i>-hexopyranosid-3-ulose
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              950
_journal_page_last               951
_journal_paper_doi               10.1107/S0108270197002345
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C14 H19 N3 O7'
_chemical_formula_structural     'C14 H19 N3 O7'
_chemical_formula_sum            'C14 H19 N3 O7'
_chemical_formula_weight         341.3
_chemical_melting_point          420.00(11)
_chemical_name_systematic
;
Methyl 2-aza-2-deoxy-4,6-di-O-methyl-2-N-(p-nitrophenylamino)-\b-D-erythro-
hexopyranosid-3-ulose.
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 104.238(5)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   21.5740(10)
_cell_length_b                   4.5576(9)
_cell_length_c                   17.039(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.5
_cell_measurement_theta_min      5.5
_cell_volume                     1623.9(4)
_computing_cell_refinement       'xtal LATCON (Hall, Flack & Stewart, 1992)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'xtal REFCAL, LSABS SORTRF (Blanc & Schwarzenbach, 1991)'
_computing_molecular_graphics    'xtal ORTEP'
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    'MULTAN87 (Main et al., 1987)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       Enraf-Nonius_CAD4_diffractometer
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         Sealed-off_tube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.084
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2491
_diffrn_reflns_theta_max         54
_diffrn_reflns_theta_min         4.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   Analytical_integration
_exptl_absorpt_process_details   'xtal LSABS (Blanc & Schwarzenbach, 1991)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'fine needle elongated along b'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.333
_refine_ls_abs_structure_details Flack_XABS_refined
_refine_ls_abs_structure_Flack   0.5(1.0)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.172
_refine_ls_goodness_of_fit_obs   2.342
_refine_ls_hydrogen_treatment
'H atoms in calculated positions with U~iso~ = 0.050'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1804
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.120
_refine_ls_R_factor_obs          .076
_refine_ls_shift/esd_max         0.09
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/\s^2^(F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.083
_refine_ls_wR_factor_obs         .074
_reflns_number_observed          1371
_reflns_number_total             2403
_reflns_observed_criterion       'refl observed if F > 4.0 sigma(F)'
_cod_data_source_file            ha1186.cif
_cod_data_source_block           JTRO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '419.9 - 420.11' was changed to
'420.00(11)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '419.9 - 420.11' was changed to
'420.00(11)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/\s^2^(F^2^)' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/\s^2^(F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_Hall     C_2y
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2006313