Crystal structure of 4,6-dimethyl-2-[(2,3,4,6-tetra-<i>O</i>-acetyl-β-<small>D</small>-galactopyranosyl)sulfanyl]pyrimidine
Abu-Zaied, Mamdouh A.; Elgemeie, Galal H.; Jones, Peter G.; Acta Crystallographica Section E 75 (2019) 1820–1823; doi:10.1107/S205698901901449X

data_2243183
_publ_section_title
;
 Crystal structure of
 4,6-dimethyl-2-[(2,3,4,6-tetra-<i>O</i>-acetyl-\b-<small>D</small>-galactopyranosyl)sulfanyl]pyrimidine
;
_journal_coeditor_code           HB7861
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1820
_journal_page_last               1823
_journal_paper_doi               10.1107/S205698901901449X
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C20 H26 N2 O9 S'
_chemical_formula_moiety         'C20 H26 N2 O9 S'
_chemical_formula_sum            'C20 H26 N2 O9 S'
_chemical_formula_weight         470.49
_chemical_name_systematic
4,6-Dimethyl-2-[(2,3,4,6-tetra-<i>O</i>-acetyl-\b-<i>D</i>-galactopyranosyl)sulfanyl]pyrimidine
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 91.3762(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4868(2)
_cell_length_b                   8.6444(2)
_cell_length_c                   11.5561(2)
_cell_measurement_reflns_used    34705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.8870
_cell_measurement_theta_min      2.5140
_cell_volume                     1147.15(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            107162
_diffrn_reflns_theta_full        31.500
_diffrn_reflns_theta_max         32.573
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.211
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3355 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.003(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         7825
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                7530
_reflns_number_total             7825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7861sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1147.14(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2243183
_cod_database_fobs_code          2243183
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              83660
_shelx_res_checksum              89488