Crystal structure of ammonium 3'-azido-3'-deoxythymidine-5'-aminocarbonylphosphonate hemihydrate: an anti-HIV agent
Jasko, Maxim V.; Gurskaya, Galina V.; Kukhanova, Marina K.; Bushmarinov, Ivan S.; Acta Crystallographica Section E 70 (2014) 396–399; doi:10.1107/S1600536814022405

data_2240112
_publ_section_title
;
 Crystal structure of ammonium
 3'-azido-3'-deoxythymidine-5'-aminocarbonylphosphonate hemihydrate: an
 anti-HIV agent
;
_journal_coeditor_code           SU2792
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              396
_journal_page_last               399
_journal_paper_doi               10.1107/S1600536814022405
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'N H4 +, C11 H14 N6 O7 P -, 0.5H2 O'
_chemical_formula_moiety         'N H4 +, C11 H14 N6 O7 P -, 0.5(H2 O)'
_chemical_formula_sum            'C11 H19 N7 O7.5 P'
_chemical_formula_weight         400.30
_chemical_name_systematic
;
Ammonium
3'-azido-3'-deoxythymidine-5'-aminocarbonylphosphonate hemihydrate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5564(6)
_cell_length_b                   18.5564(6)
_cell_length_c                   10.1139(4)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.294
_cell_measurement_theta_min      2.293
_cell_volume                     3482.6(2)
_computing_cell_refinement
;
SAINT  (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47562
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.487
_diffrn_reflns_theta_min         2.195
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.290
_refine_ls_abs_structure_details
;
Flack x determined using 1919 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5322
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0415P)^2^+0.5648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                4822
_reflns_number_total             5322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2792sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        3482.6(3)
_cod_original_formula_sum        'C11 H19 N7 O7.50 P'
_cod_database_code               2240112
_cod_database_fobs_code          2240112
_shelx_hkl_checksum              75180
_shelx_res_checksum              33320