An unusual two-dimensional hydrogen-bonding network in bis(2,9-dimethyl-1,10-phenanthrolin-1-ium) peroxodisulfate dihydrate
Harvey, Miguel Angel; Baggio, Sergio; Garland, María Teresa; Baggio, Ricardo; Acta Crystallographica Section C 64 (2008) o489–o492; doi:10.1107/S0108270108024360

data_2016747
_publ_section_title
;
 An unusual two-dimensional hydrogen-bonding network in
 bis(2,9-dimethyl-1,10-phenanthrolin-1-ium) peroxodisulfate dihydrate
;
_journal_coeditor_code           BM3054
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o489
_journal_page_last               o492
_journal_paper_doi               10.1107/S0108270108024360
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '2C14 H13 N2 +, S2 O8 2-, 2H2 O'
_chemical_formula_moiety         '2(C14 H13 N2 +), O8 S2 2-, 2H2 O'
_chemical_formula_sum            'C28 H30 N4 O10 S2'
_chemical_formula_weight         646.68
_chemical_name_systematic
;
bis(2,9-dimethyl-1,10-phenanthrolin-1-ium) peroxodisulfate dihydrate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5644(19)
_cell_length_b                   13.228(3)
_cell_length_c                   11.201(2)
_cell_measurement_reflns_used    7236
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      3.12
_cell_volume                     1414.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_av_sigmaI/netI    0.017
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11488
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0754P)^2^+0.4898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.119
_refine_ls_wR_factor_ref         0.126
_reflns_number_gt                2625
_reflns_number_total             3039
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm3054.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016747
_cod_database_fobs_code          2016747