Chiral Hydroxylamines. I. 1-(<i>N</i>-Benzyl-<i>N</i>-hydroxyamino)-1-deoxy-2,3-<i>O</i>-isopropylidene-1-(1-methylimidazol-2-yl)-<small>D</small>-<i>threo</i>-triitol
Merino, P.; Merchan, F. L.; Tejero, T.; Acta Crystallographica Section C 51 (1995) 2400–2401; doi:10.1107/S0108270195006962

data_2004098
_publ_section_title
;Chiral Hydroxylamines. I.
 1-(<i>N</i>-Benzyl-<i>N</i>-hydroxyamino)-1-deoxy-2,3-<i>O</i>-isopropylidene-1-(1-methylimidazol-2-yl)-<small>D</small>-<i>threo</i>-triitol
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2400
_journal_page_last               2401
_journal_paper_doi               10.1107/S0108270195006962
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C17 H23 N3 O3'
_chemical_formula_sum            'C17 H23 N3 O3'
_chemical_formula_weight         317.38
_chemical_melting_point          376
_chemical_name_systematic
;
N-Benzyl-1-deoxy-1-(hydroxyamino)-2,3-O-diisopropylidene-1-
(N-methylimidazol-2-yl)-D-threo-triitol.
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.388(2)
_cell_length_b                   10.527(2)
_cell_length_c                   19.730(4)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.656
_cell_measurement_theta_min      6.623
_cell_volume                     1742.2(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990b)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'Profile data from 2\q/\w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1822
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        3.70
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       'Transparent block'
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.147
_refine_ls_extinction_coef       0.0103(17)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    'H atoms refined as riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         1659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0524P)^2^ + 0.5028P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1251
_refine_ls_wR_factor_obs         0.1027
_reflns_number_observed          1120
_reflns_number_total             1659
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk1141.cif
_cod_data_source_block           gly3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2004098