7-(1,3-Dioxolan-2-ylmethyl)-1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1<i>H</i>-purin-9-ium tetrachloridoferrate(III)
Wang, Ping Ping; Gong, Jiang; Ni, Shi-Feng; Acta Crystallographica Section E 66 (2010) m1247–; doi:10.1107/S1600536810034720

data_2227695
_publ_section_title
;
 7-(1,3-Dioxolan-2-ylmethyl)-1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1<i>H</i>-purin-9-ium
 tetrachloridoferrate(III)
;
_journal_coeditor_code           JH2188
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1247
_journal_paper_doi               10.1107/S1600536810034720
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C11 H15 N4 O4) [Fe Cl4]'
_chemical_formula_moiety         'C11 H15 N4 O4 +, Cl4 Fe -'
_chemical_formula_sum            'C11 H15 Cl4 Fe N4 O4'
_chemical_formula_weight         464.92
_chemical_name_systematic
;
7-(1,3-Dioxolan-2-ylmethyl)-1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-
1<i>H</i>-purin-9-ium tetrachloridoferrate(III)
;
_space_group_IT_number           77
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4c'
_symmetry_space_group_name_H-M   'P 42'
_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            8
_cell_length_a                   20.2947(4)
_cell_length_b                   20.2947(4)
_cell_length_c                   9.0692(4)
_cell_measurement_reflns_used    8917
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2.2
_cell_volume                     3735.38(19)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX area-detector'
_diffrn_measurement_method       '\f and \w scan'
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19874
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880.0
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.313
_refine_ls_abs_structure_details 'Flack (1983), 2724 Friedel pairs'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0992
_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^)+(0.0665P)^2^+7.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                5589
_reflns_number_total             6253
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jh2188.cif
_cod_data_source_block           I
_cod_database_code               2227695
_cod_database_fobs_code          2227695