Bis(2,9-dimethyl-1,10-phenanthrolin-1-ium) 2,5-dicarboxybenzene-1,4-dicarboxylate–2,9-dimethyl-1,10-phenanthroline–benzene-1,2,4,5-tetracarboxylic acid (1/2/1)
Arman, Hadi D.; Kaulgud, Trupta; Tiekink, Edward R. T.; Acta Crystallographica Section E 69 (2013) o1445–o1446; doi:10.1107/S1600536813022691

data_2238582
_publ_section_title
;
 Bis(2,9-dimethyl-1,10-phenanthrolin-1-ium)
 2,5-dicarboxybenzene-1,4-dicarboxylate--2,9-dimethyl-1,10-phenanthroline--benzene-1,2,4,5-tetracarboxylic
 acid (1/2/1)
;
_journal_coeditor_code           XU5731
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1445
_journal_page_last               o1446
_journal_paper_doi               10.1107/S1600536813022691
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'2C14 H13 N2 +, C10 H4 O8 2-, 2C14 H12 N2, C10 H6 O8'
_chemical_formula_moiety
;
2(C14 H13 N2 +), C10 H6 O8 2-, 2(C14 H12 N2), C10 H4 O8
;
_chemical_formula_sum            'C76 H60 N8 O16'
_chemical_formula_weight         1341.32
_chemical_name_systematic
;Bis(2,9-dimethyl-1,10-phenanthrolin-1-ium)
2,5-dicarboxybenzene-1,4-dicarboxylate--2,9-dimethyl-1,10-phenanthroline--benzene-1,2,4,5-tetracarboxylic acid (1/2/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.216(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.798(4)
_cell_length_b                   13.893(4)
_cell_length_c                   19.163(6)
_cell_measurement_reflns_used    12762
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.7
_cell_measurement_theta_min      2.0
_cell_volume                     3138.7(17)
_computing_cell_refinement
'CrystalClear (Molecular Structure Corporation & Rigaku, 2005)'
_computing_data_collection
'CrystalClear (Molecular Structure Corporation & Rigaku, 2005)'
_computing_data_reduction
'CrystalClear (Molecular Structure Corporation & Rigaku, 2005)'
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC12\K/SATURN724'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0812
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22006
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7181
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0555P)^2^+1.3348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                6007
_reflns_number_total             7181
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5731.cif
_cod_data_source_block           I
_cod_original_cell_volume        3138.8(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2238582
_cod_database_fobs_code          2238582