2',3'-Didehydro-3'-deoxythymidine <i>N</i>-methyl-2-pyrrolidone solvate (D4T·NMPO)
Viterbo, Davide; Milanesio, Marco; Pomés Hernández, Ramón; Rodríguez Tanty, Chryslaine; Colás González, Ivan; Sablón Carrazana, Marquiza; Duque Rodríguez, Julio; Acta Crystallographica Section C 56 (2000) 580–581; doi:10.1107/S0108270100001451

data_2010926
_publ_section_title
;
2',3'-Didehydro-3'-deoxythymidine <i>N</i>-methyl-2-pyrrolidone 
solvate (D4T&#x00B7;NMPO)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              580
_journal_page_last               581
_journal_paper_doi               10.1107/S0108270100001451
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C10 H12 N2 O4 , C5 H9 N O'
_chemical_formula_sum            'C15 H21 N3 O5'
_chemical_formula_weight         323.35
_chemical_name_common
;
2',3'-didehydro-2',3'-O-dideoxythymidine (D4T)
1-methylpyrrolidone (NMPO) solvate
;
_chemical_name_systematic
;
1-(2',3'-dideoxy-\b-D-glycero-pent-2-enofuranosyl)thimine
1-methylpyrrolidone
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4710(10)
_cell_length_b                   13.9880(10)
_cell_length_c                   15.739(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      12
_cell_volume                     1644.8(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics
'SHELXTL/IRIS (Sheldrick, 1990) and MOLDRAW (Ugliengo et al., 1993)'
_computing_publication_material
;
 PARST (Nardelli, 1995), PARSTCIF (Nardelli, 1991) and SHELXL97
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_max .988
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0133
_diffrn_reflns_av_sigmaI/netI    .0407
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2807
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          .65
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .35
_refine_diff_density_max         .26
_refine_diff_density_min         -.41
_refine_ls_abs_structure_details
; The absolute configuration was assumed
to agree with the known chirality of
D4T (Gurskaya et al., 1991; Harte et al., 1991;
Van Roey et al., 1993).
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .998
_refine_ls_R_factor_all          .0992
_refine_ls_R_factor_gt           .0584
_refine_ls_shift/su_max          .006
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0936P)^2^+0.0334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1553
_reflns_number_gt                1674
_reflns_number_total             2619
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1454.cif
_cod_data_source_block           I
_cod_depositor_comments
;
Automatic conversion scripts had previously changed 
'_atom_site_refinement_flags' tag values 'd' into 'D' as recommended by 
'cif_core.dic' version 2.4.1. However, manual inspection revealed that the 
underlying problem was actually related to a wrong tag names inside the 
atom site loop. The following changes were performed to resolve the problem: 

* '_atom_site_refinement_flags' tag was changed to '_atom_site_calc_flag'
* '_atom_site_calc_flag' tag was changed to '_atom_site_site_symmetry_order'
* '_atom_site_disorder_group' tag was changed to 
  '_atom_site_refinement_flags_posn'

Antanas Vaitkus,
2015-02-19
;
_cod_database_code               2010926