Four salt phases of theophylline
Buist, Amanda R.; Kennedy, Alan R.; Manzie, Craig; Acta Crystallographica Section C 70 (2014) 220–224; doi:10.1107/S2053229614000825

data_2019391
_publ_section_title
;
 Four salt phases of theophylline
;
_journal_coeditor_code           GZ3251
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              220
_journal_page_last               224
_journal_paper_doi               10.1107/S2053229614000825
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C7 H9 N4 O2 +, Cl1 -'
_chemical_formula_moiety         'C7 H9 N4 O2 +, Cl1 -'
_chemical_formula_sum            'C7 H9 Cl N4 O2'
_chemical_formula_weight         216.63
_chemical_name_systematic
;
1,3-Dimethyl-2,6-dioxo-7<i>H</i>-purin-9-ium bromide monohydrate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.524(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.081(3)
_cell_length_b                   4.5028(3)
_cell_length_c                   12.8256(10)
_cell_measurement_reflns_used    2617
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.6114
_cell_measurement_theta_min      3.5415
_cell_volume                     1801.3(3)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and X-SEED (Barbour, 2001)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6692
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         73.77
_diffrn_reflns_theta_min         5.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
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_refine_diff_density_max         0.480
_refine_diff_density_min         -0.256
_refine_ls_abs_structure_details 'Flack (1983), 1431 Friedel pairs'
_refine_ls_abs_structure_Flack   0.28(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3230
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+2.7204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                2966
_reflns_number_total             3230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3251sup1.cif
_cod_data_source_block           IV
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2019391