Crystal structure of 3-deoxy-3-nitromethyl-1,2;5,6-di-<i>O</i>-isopropylidene-α-<small>D</small>-allofuranose
Lugiņina, Jevgeņija; Rjabovs, Vitālijs; Stepanovs, Dmitrijs; Acta Crystallographica Section E 72 (2016) 314–317; doi:10.1107/S2056989016001845

data_2241549
_publ_section_title
;
 Crystal structure of
 3-deoxy-3-nitromethyl-1,2;5,6-di-<i>O</i>-isopropylidene-\a-<small>D</small>-allofuranose
;
_journal_coeditor_code           SU5270
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              314
_journal_page_last               317
_journal_paper_doi               10.1107/S2056989016001845
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C13 H21 N O7'
_chemical_formula_moiety         'C13 H21 N O7'
_chemical_formula_sum            'C13 H21 N O7'
_chemical_formula_weight         303.31
_chemical_name_systematic
;
(3a<i>R</i>,5<i>S</i>,6<i>R</i>,6a<i>R</i>)-5-[(<i>R</i>)-2,2-Dimethyl-1,3-\
dioxolan-4-yl]-2,2-dimethyl-6-(nitromethyl)tetrahydrofuro[2,3-<i>d</i>][1,3]\
dioxole
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5044(2)
_cell_length_b                   12.6144(4)
_cell_length_c                   21.6348(9)
_cell_measurement_reflns_used    26214
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1502.21(10)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
KappaCCD Server Software (Nonius, 1997)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2011 (Burla <i>et al.</i>,  2012)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            4225
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.055
_diffrn_reflns_theta_min         3.230
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.3523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                2316
_reflns_number_total             4225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5270sup1.cif
_cod_data_source_block           I
_cod_database_code               2241549
_cod_database_fobs_code          2241549
_shelx_hkl_checksum              19303
_shelx_res_checksum              38087