1,2;5,6-Di-<i>O</i>-isopropylidene-3-<i>C</i>-nitromethyl-α-<small>D</small>-allofuranose
Zhang, Qiurong; Ke, Yu; Cheng, Weiyan; Li, Pengyun; Liu, Hongmin; Acta Crystallographica Section E 67 (2011) o1402–; doi:10.1107/S1600536811017314

data_2230280
_publ_section_title
;
 1,2;5,6-Di-<i>O</i>-isopropylidene-3-<i>C</i>-nitromethyl-\a-<small>D</small>-allofuranose
;
_journal_coeditor_code           CV5090
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1402
_journal_paper_doi               10.1107/S1600536811017314
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C13 H21 N O8'
_chemical_formula_moiety         'C13 H21 N O8'
_chemical_formula_sum            'C13 H21 N O8'
_chemical_formula_weight         319.31
_chemical_melting_point_gt       383
_chemical_melting_point_lt       384
_chemical_name_systematic
;
1,2;5,6-Di-<i>O</i>-isopropylidene-3-<i>C</i>-nitromethyl-\a-D-allofuranose
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.2581(19)
_cell_length_b                   13.2581(19)
_cell_length_c                   16.462(3)
_cell_measurement_reflns_used    398
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2
_cell_volume                     2506.0(7)
_computing_cell_refinement       'R-AXIS-IV Software (Rigaku, 1997)'
_computing_data_collection       'R-AXIS-IV Software (Rigaku, 1997)'
_computing_data_reduction        'R-AXIS-IV Software (Rigaku, 1997)'
_computing_molecular_graphics
'TEXSAN (Molecular Structure Corporation, 1992)'
_computing_publication_material
'TEXSAN (Molecular Structure Corporation, 1992)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS-IV'
_diffrn_measurement_method       'Oscillation  frames'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8380
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.9750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.260
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         1612
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0962P)^2^+1.0744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1640
_reflns_number_gt                1534
_reflns_number_total             1612
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5090.cif
_cod_data_source_block           I
_cod_database_code               2230280
_cod_database_fobs_code          2230280