2,2'-(Disulfanediyl)dibenzoic acid–2,9-dimethylphenanthroline–tetrahydrofuran (1/2/1)
Arman, Hadi D.; Kaulgud, Trupta; Tiekink, Edward R. T.; Acta Crystallographica Section E 66 (2010) o2602–; doi:10.1107/S1600536810037165

data_2228018
_publ_section_title
;
 2,2'-(Disulfanediyl)dibenzoic
 acid--2,9-dimethylphenanthroline--tetrahydrofuran (1/2/1)
;
_journal_coeditor_code           SU2213
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2602
_journal_paper_doi               10.1107/S1600536810037165
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C14 H10 O4 S2, 2C14 H12 N2, C4 H8 O'
_chemical_formula_moiety         'C14 H10 O4 S2, 2(C14 H12 N2), C4 H8 O'
_chemical_formula_sum            'C46 H42 N4 O5 S2'
_chemical_formula_weight         794.96
_chemical_name_systematic
;
2,2'-(Disulfanediyl)dibenzoic acid--2,9-dimethylphenanthroline--tetrahydrofuran
(1/2/1)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 109.637(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.011(4)
_cell_length_b                   8.516(3)
_cell_length_c                   17.403(5)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.3
_cell_volume                     1955.7(11)
_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
'ORTEP-3 (Farrugia, 1997) 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_sigmaI/netI    0.076
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13023
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.85
_refine_ls_abs_structure_details 'Flack (1983), 3550 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max_lt       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^)+(0.0751P)^2^+1.2802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.162
_refine_ls_wR_factor_ref         0.169
_reflns_number_gt                7988
_reflns_number_total             8637
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2213.cif
_cod_data_source_block           I
_cod_original_cell_volume        1955.7(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2228018
_cod_database_fobs_code          2228018