Caffeinium bisulfate monohydrate
Jerin, C. Vincent; Athimoolam, S.; Acta Crystallographica Section E 67 (2011) o2290–; doi:10.1107/S1600536811031540

data_2231420
_publ_section_title
;
 Caffeinium bisulfate monohydrate
;
_journal_coeditor_code           BT5603
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2290
_journal_paper_doi               10.1107/S1600536811031540
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C8 H11 N4 O2 +, H S O4 -, H2 O'
_chemical_formula_moiety         'C8 H11 N4 O2 +, H O4 S -, H2 O'
_chemical_formula_sum            'C8 H14 N4 O7 S'
_chemical_formula_weight         310.29
_chemical_name_common            'Caffeinium bisulfate monohydrate'
_chemical_name_systematic
;
1,3,7-trimethyl-2,6-dioxo-7<i>H</i>-purin-9-ium  hydrogen sulfate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL/PC
_cell_angle_alpha                90.00
_cell_angle_beta                 90.788(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8296(10)
_cell_length_b                   6.2879(6)
_cell_length_c                   21.340(2)
_cell_measurement_reflns_used    2986
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.14
_cell_volume                     1318.8(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2001)'
_computing_data_collection       '<i>SMART</i> (Bruker, 2001)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2001)'
_computing_molecular_graphics    '<i>PLATON</i> (Spek, 2009)'
_computing_publication_material  '<i>SHELXTL/PC</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXTL/PC</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXTL/PC</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11981
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      1.550(10)
_exptl_crystal_density_method
'flotation technique using a liquid-mixture of xylene and bromoform'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.377
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXTL/PC</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2317
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0659P)^2^+0.5199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                2200
_reflns_number_total             2317
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5603.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231420
_cod_database_fobs_code          2231420