2-Methoxy-3-methyl-6-oxo-4-(2,3,4-tri-<i>O</i>-acetyl-β-<small>D</small>-xylopyranosylamino)-1,6-dihydropyrimidine-5-carbaldehyde 0.065-hydrate and 2-methylsulfanyl-6-oxo-4-(2,3,4-tri-<i>O</i>-acetyl-β-<small>D</small>-xylopyranosylamino)-1,6-dihydropyrimidine-5-carbaldehyde: hydrogen-bonded structures in one or three dimensions
Cobo, Justo; Nogueras, Manuel; de la Torre, José M.; Glidewell, Christopher; Acta Crystallographica Section C 65 (2009) o321–o325; doi:10.1107/S0108270109019374

data_2017185
_publ_section_title
;2-Methoxy-3-methyl-6-oxo-4-(2,3,4-tri-<i>O</i>-acetyl-\b-<small>D</small>-xylopyranosylamino)-1,6-dihydropyrimidine-5-carbaldehyde
 0.065-hydrate and
 2-methylsulfanyl-6-oxo-4-(2,3,4-tri-<i>O</i>-acetyl-\b-<small>D</small>-xylopyranosylamino)-1,6-dihydropyrimidine-5-carbaldehyde:
 hydrogen-bonded structures in one or three dimensions
;
_journal_coeditor_code           GG3202
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o321
_journal_page_last               o325
_journal_paper_doi               10.1107/S0108270109019374
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C17 H21 N3 O9 S'
_chemical_formula_moiety         'C17 H21 N3 O9 S'
_chemical_formula_sum            'C17 H21 N3 O9 S'
_chemical_formula_weight         443.44
_chemical_name_systematic        1,6-dihydropyrimidine-5-carbaldehyde
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.92940(10)
_cell_length_b                   10.7415(2)
_cell_length_c                   26.4825(5)
_cell_measurement_reflns_used    4481
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.32
_cell_volume                     1971.15(6)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>,  2000)'
_computing_data_collection       'COLLECT (Hooft, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12812
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.451
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_coef       0.039(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   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4482
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.0098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                4065
_reflns_number_total             4482
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3202.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2017185
_cod_database_fobs_code          2017185