Crystal structure of 3-<i>C</i>-(<i>N</i>-benzyloxycarbonyl)aminomethyl-3-deoxy-1,2:5,6-di-<i>O</i>-isopropylidene-α-<small>D</small>-allofuranose
Rjabovs, Vitalijs; Stepanovs, Dmitrijs; Turks, Maris; Acta Crystallographica Section E 71 (2015) 1212–1215; doi:10.1107/S2056989015017582

data_2241071
_publ_section_title
;
 Crystal structure of
 3-<i>C</i>-(<i>N</i>-benzyloxycarbonyl)aminomethyl-3-deoxy-1,2:5,6-di-<i>O</i>-isopropylidene-\a-<small>D</small>-allofuranose
;
_journal_coeditor_code           SU5210
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1212
_journal_page_last               1215
_journal_paper_doi               10.1107/S2056989015017582
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C21 H29 N O7'
_chemical_formula_moiety         'C21 H29 N O7'
_chemical_formula_sum            'C21 H29 N O7'
_chemical_formula_weight         407.45
_chemical_name_systematic
;
3-<i>C</i>-(<i>N</i>-Benzyloxycarbonyl)aminomethyl-3-deoxy-1,2:5,6-di-\
<i>O</i>-isopropylidene-\a-<i>D</i>-allofuranose
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.7480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3235(3)
_cell_length_b                   5.41180(10)
_cell_length_c                   20.4381(7)
_cell_measurement_reflns_used    11906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1024.10(5)
_computing_cell_refinement
;
HKL Scalepack (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>KappaCCD Server Software</i> (Nonius, 1997)
;
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008),
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR2011 (Burla <i>et al.</i>,  2012)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5535
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.1203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                2597
_reflns_number_total             3279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su5210sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2241071
_cod_database_fobs_code          2241071