Isostructurality and the conformational role of the 2′,3′-moieties in the diversity of lamivudine crystal forms probed in halide salts
Tenorio Clavijo, Juan Carlos; Guimarães, Freddy Fernandes; Ellena, Javier; Martins, Felipe Terra; CrystEngComm 17 (2015) 5187–; doi:10.1039/C4CE02373K

data_7219135
_publ_section_title
;
 Isostructurality and the conformational role of the
 2&#x2032;,3&#x2032;-moieties in the diversity of lamivudine crystal forms
 probed in halide salts
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5187
_journal_paper_doi               10.1039/C4CE02373K
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C8 H12 N3 O3 S, F2 H'
_chemical_formula_sum            'C8 H13 F2 N3 O3 S'
_chemical_formula_weight         269.27
_chemical_name_common            Lamivudine_Hydrofluoride
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-11-05T17:03:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-11-06 deposited with the CCDC.
2014-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.35980(10)
_cell_length_b                   12.0206(4)
_cell_length_c                   8.6306(3)
_cell_measurement_reflns_used    2175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     538.22(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.002546
_diffrn_orient_matrix_UB_12      -0.083175
_diffrn_orient_matrix_UB_13      -0.001278
_diffrn_orient_matrix_UB_21      0.142312
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      0.100351
_diffrn_orient_matrix_UB_31      -0.129983
_diffrn_orient_matrix_UB_32      -0.001629
_diffrn_orient_matrix_UB_33      0.065249
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2207
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2189
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.1551P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.074
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                2094
_reflns_number_total             2189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02373k1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7219133--7219137.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7219135
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.968