A synthetic intermediate of enantiopure <i>N</i>-protected β-hydroxyvaline, (2<i>R</i>)-2-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)amino]-3-methylbutane-1,3-diol
Oku, Hiroyuki; Naito, Ryo; Yamada, Keiichi; Katakai, Ryoichi; Acta Crystallographica Section E 60 (2004) o2462–o2464; doi:10.1107/S1600536804030363

data_2204718
_publ_section_title
;A synthetic intermediate of enantiopure <i>N</i>-protected \b-hydroxyvaline,
 (2<i>R</i>)-2-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)amino]-3-methylbutane-1,3-diol
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2462
_journal_page_last               o2464
_journal_paper_doi               10.1107/S1600536804030363
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C10 H21 N O4 '
_chemical_formula_moiety         'C10 H21 N O4 '
_chemical_formula_sum            'C10 H21 N O4'
_chemical_formula_weight         219.28
_chemical_name_systematic
;
(2R)-2-N-(tert-Butoxycarbonyl)-Amino-3-Methyl-1,3-Butanediol
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.833(8)
_cell_length_b                   18.994(17)
_cell_length_c                   6.713(8)
_cell_measurement_reflns_used    8702
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      66.6
_cell_measurement_theta_min      4.5
_cell_volume                     1254(2)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection
'RAPID-AUTO (RIGAKU/MSC & Rigaku Corporation, 2003)'
_computing_data_reduction
;
CrystalStructure (RIGAKU/MSC & Rigaku Corporation, 2003)
;
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  CrystalStructure
_computing_structure_refinement  'CRYSTALS (Watkin et al., 1996)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9780
_diffrn_measured_fraction_theta_max 0.9780
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10309
_diffrn_reflns_theta_full        68.12
_diffrn_reflns_theta_max         68.12
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1318
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.007Fo^2^ + \s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                965
_reflns_number_total             1318
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            is6014.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C10 H21 N O4 '
_cod_database_code               2204718