5,6-Dioxo-1,10-phenanthrolin-1-ium trifluoromethanesulfonate
Onuegbu, Jonathan; Butcher, Ray J.; Hosten, Charles; Udeochu, Uche Charles; Bakare, Oladapo; Acta Crystallographica Section E 64 (2008) o1543–; doi:10.1107/S1600536808016632

data_2219113
_publ_section_title
;
 5,6-Dioxo-1,10-phenanthrolin-1-ium trifluoromethanesulfonate
;
_journal_coeditor_code           NG2417
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1543
_journal_paper_doi               10.1107/S1600536808016632
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C12 H7 N2 O2 + , C F3 O3 S -'
_chemical_formula_moiety         'C12 H7 N2 O2 + , C F3 O3 S -'
_chemical_formula_sum            'C13 H7 F3 N2 O5 S'
_chemical_formula_weight         360.27
_chemical_name_systematic
;
5,6-Dioxo-1,10-phenanthrolin-1-ium trifluoromethanesulfonate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.393(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4896(2)
_cell_length_b                   16.3963(5)
_cell_length_c                   13.2430(3)
_cell_measurement_reflns_used    5857
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.4702
_cell_measurement_theta_min      4.7329
_cell_volume                     1404.99(7)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f and \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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13319
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         4.74
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm (Oxford Diffraction,
2007)]
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.376
_refine_ls_abs_structure_details 'Flack (1983), with 2713 Friedel pairs'
_refine_ls_abs_structure_Flack   0.40(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7960
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0394P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                5208
_reflns_number_total             7960
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2417.cif
_cod_data_source_block           I
_cod_database_code               2219113
_cod_database_fobs_code          2219113