9-Oxo-4,5-diazoniafluorene sulfate
Rillema, D. Paul; Kirgan, Robert; Moore, Curtis; Acta Crystallographica Section E 63 (2007) o3740–o3740; doi:10.1107/S1600536807038457

data_2215092
_publ_section_title
;
 9-Oxo-4,5-diazoniafluorene sulfate
;
_journal_coeditor_code           FL2152
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3740
_journal_page_last               o3740
_journal_paper_doi               10.1107/S1600536807038457
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C11 H8 N2 O1 2+, S O4 2-'
_chemical_formula_moiety         'C11 H8 N2 O1 2+, S O4 2-'
_chemical_formula_sum            'C11 H8 N2 O5 S'
_chemical_formula_weight         280.25
_chemical_name_systematic
;
9-Oxo-4,5-diazoniafluorene sulfate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   11.9016(12)
_cell_length_b                   11.9344(12)
_cell_length_c                   7.8351(7)
_cell_measurement_reflns_used    2024
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      3.11
_cell_volume                     1112.89(19)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2006)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area-detector'
_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  0.1338
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9704
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.9560
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.409
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0556P)^2^+0.4328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                794
_reflns_number_total             1140
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2152.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P2ac2n
_cod_database_code               2215092
_cod_database_fobs_code          2215092