Chiral Hydroxylamines. V. (2<i>S</i>,3<i>S</i>)-<i>N</i>-Benzyl-<i>N</i>-[3-(<i>tert</i>-butoxycarbonylamino)-2-butyl]hydroxylamine
Merino, Pedro; Merchan, Francisco L.; Tejero, Tomas; Lanaspa, Ana; Acta Crystallographica Section C 54 (1998) 85–86; doi:10.1107/S0108270197013267

data_2006944
_publ_section_title
;Chiral Hydroxylamines. V.
 (2<i>S</i>,3<i>S</i>)-<i>N</i>-Benzyl-<i>N</i>-[3-(<i>tert</i>-butoxycarbonylamino)-2-butyl]hydroxylamine
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              85
_journal_page_last               86
_journal_paper_doi               10.1107/S0108270197013267
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'C16 H26 N2 O3'
_chemical_formula_weight         294.39
_chemical_melting_point          397
_chemical_name_systematic
;
 (2S,3S)-N-Benzyl-N-[3-(tert-butoxycarbonylamino)-2-butyl]hydroxylamine
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.0
_cell_angle_beta                 94.57(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   6.358(5)
_cell_length_b                   10.463(5)
_cell_length_c                   12.842(5)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.025
_cell_measurement_theta_min      10.099
_cell_volume                     851.6(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2349
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        7.24
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.235
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         1749
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_obs          .0505
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0889P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1481
_refine_ls_wR_factor_obs         .1292
_reflns_number_gt                1458
_reflns_number_total             1841
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1318.cif
_cod_data_source_block           ala3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '397 K' was changed to '397' - the
value should be numeric and without a unit designator.

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 '397 K' was changed to '397' - the
value should be numeric and without a unit designator.

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 'calc w =
1/[\s^2^(Fo^2^)+(0.0889P)^2^] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0889P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2006944