2-<i>N</i>-Benzyl-2,6-dideoxy-2,6-imino-3,4-<i>O</i>-isopropylidene-3-<i>C</i>-methyl-<small>D</small>-allononitrile
Ayers, Benjamin J.; Jenkinson, Sarah F.; Fleet, George W. J.; Thompson, Amber L.; Acta Crystallographica Section E 68 (2012) o1474–; doi:10.1107/S1600536812016273

data_2234732
_publ_section_title
;
 2-<i>N</i>-Benzyl-2,6-dideoxy-2,6-imino-3,4-<i>O</i>-isopropylidene-3-<i>C</i>-methyl-<small>D</small>-allononitrile
;
_journal_coeditor_code           LH5456
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1474
_journal_paper_doi               10.1107/S1600536812016273
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C17 H22 N2 O3'
_chemical_formula_moiety         'C17 H22 N2 O3'
_chemical_formula_sum            'C17 H22 N2 O3'
_chemical_formula_weight         302.37
_chemical_name_systematic
;
2-<i>N</i>-Benzyl-2,6-dideoxy-2,6-imino-3,4-<i>O</i>-isopropylidene-
3-<i>C</i>-methyl-<i>D</i>-allononitrile
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5647(3)
_cell_length_b                   10.0019(4)
_cell_length_c                   18.7031(7)
_cell_measurement_reflns_used    1959
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1602.17(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7953
_diffrn_reflns_theta_full        26.923
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         5.179
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.22
_refine_ls_extinction_coef       28E1(11)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9711
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2082
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.0002994
_refine_ls_shift/su_mean         0.0000299
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + (0.07P)^2^ + 0.23P], where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1064
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                1808
_reflns_number_total             2082
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5456.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2234732
_cod_database_fobs_code          2234732