2-<i>C</i>-Azidomethyl-2-deoxy-3,4-<i>O</i>-isopropylidene-<small>D</small>-ribono-1,5-lactone
Punzo, Francesco; Watkin, David J.; Jenkinson, Sarah F.; da Cruz, Filipa P.; Fleet, George W. J.; Acta Crystallographica Section E 62 (2006) o321–o323; doi:10.1107/S1600536805041632

data_2207820
_publ_section_title
2-<i>C</i>-Azidomethyl-2-deoxy-3,4-<i>O</i>-isopropylidene-<small>D</small>-ribono-1,5-lactone
_journal_coeditor_code           LH2002
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o321
_journal_page_last               o323
_journal_paper_doi               10.1107/S1600536805041632
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C9 H13 N3 O4'
_chemical_formula_moiety         'C9 H13 N3 O4'
_chemical_formula_sum            'C9 H13 N3 O4'
_chemical_formula_weight         227.22
_chemical_name_systematic
;
2-C-Azidomethyl-2-deoxy-3,4-O-isopropylidene-D-ribono-1,5-lactone
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 91.6306(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6145(2)
_cell_length_b                   11.1194(4)
_cell_length_c                   15.0252(8)
_cell_measurement_reflns_used    2605
_cell_measurement_temperature    250
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     1104.65(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      250
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5623
_diffrn_reflns_theta_full        26.303
_diffrn_reflns_theta_max         29.890
_diffrn_reflns_theta_min         5.178
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.52
_refine_ls_extinction_coef       10E1(2)
_refine_ls_extinction_method     'Larson (1970), eq. 22'
_refine_ls_goodness_of_fit_ref   1.0765
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3275
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000084
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince,
1982)
w = 1/[A~0~T~0~(x)+A~1~T~1~(x) ... +A~n-1~T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x = F~calc~/F~max~
Method = Robust Weighting (Prince, 1982)
W = w[1-(\dF/6\sF)^2^]^2^, A~i~ are 38.7 61.9 38.9 16.8 3.80
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1288
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                1944
_reflns_number_total             3275
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2002.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2207820