Theobrominium perchlorate dibenzo-18-crown-6 3.25-hydrate
Kulikov, Vladislav; Meyer, Gerd; Acta Crystallographica Section E 69 (2013) o1027–; doi:10.1107/S1600536813014463

data_2238223
_publ_section_title
;
 Theobrominium perchlorate dibenzo-18-crown-6 3.25-hydrate
;
_journal_coeditor_code           NC2312
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1027
_journal_paper_doi               10.1107/S1600536813014463
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'C7 H9 N4 O2 +, Cl O4 -, C20 H24 O6, 3.23H2 O'
_chemical_formula_moiety
'C7 H9 N4 O2 +, Cl O4 -, C20 H24 O6, 3.23(H2 O)'
_chemical_formula_sum            'C27 H40 Cl N4 O15.25'
_chemical_formula_weight         699.58
_chemical_name_common
;
Theobrominium perchlorate dibenzo-18-crown-6 3.25-hydrate
;
_chemical_name_systematic
;
3,7-Dimethyl-2,6-dioxo-1<i>H</i>-purin-9-ium perchlorate dibenzo-18-crown-6
3.25-hydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9292(3)
_cell_length_b                   15.2505(5)
_cell_length_c                   18.1222(5)
_cell_measurement_reflns_used    51177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      0.80
_cell_volume                     3296.90(16)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe & Cie IPDS II'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51074
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.9969
_exptl_absorpt_correction_T_min  0.9908
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pentagonal prism'
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.329
_refine_ls_abs_structure_details 'Flack (1983), 3092 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(10)
_refine_ls_extinction_coef       0.0142(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+0.3494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                5299
_reflns_number_total             7018
_reflns_threshold_expression     I>4sigma(I)
_cod_data_source_file            nc2312.cif
_cod_data_source_block           I
_cod_database_code               2238223
_cod_database_fobs_code          2238223
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-21
;