The geometry and structural properties of the 4,8,12-trioxa-4,8,12,12c-tetrahydrodibenzo[cd,mn]pyrene system in the cationic state. Structures of a planar organic cation with various monovalent and divalent anions
Krebs, Frederik C.; Laursen, Bo W.; Johannsen, Ib; Faldt, André; Bechgaard, Klaus; Jacobsen, Claus S.; Thorup, Niels; Boubekeur, Kamal; Acta Crystallographica, Section B: Structural Science 55 (1999) 410–423; doi:10.1107/S0108768198016140

data_2003085
_publ_section_title
;
 The geometry and structural properties of the
 4,8,12-trioxa-4,8,12,12c-tetrahydrodibenzo[cd,mn]pyrene system
 in the cationic state. Structures of a planar organic cation with
 various monovalent and divalent anions
;
_journal_coden_ASTM              ASBSDK
_journal_issue                   3
_journal_name_full
;
 Acta Crystallographica, Section B: Structural Science
;
_journal_page_first              410
_journal_page_last               423
_journal_paper_doi               10.1107/S0108768198016140
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         '2(C19 H9 O3), O6 S2'
_chemical_formula_sum            'C38 H18 O12 S2'
_chemical_formula_weight         730.64
_chemical_name_systematic
;
 Bis(4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium)
dithionate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.91(3)
_cell_angle_beta                 102.37(3)
_cell_angle_gamma                108.61(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6300(17)
_cell_length_b                   8.9680(18)
_cell_length_c                   9.876(2)
_cell_measurement_temperature    120(2)
_cell_volume                     689.8(3)
_computing_cell_refinement       'SAINT Siemens'
_computing_data_collection       'SMART Siemens'
_computing_data_reduction        'SAINT Siemens'
_computing_molecular_graphics    'SHELXTL (Sheldrick)'
_computing_publication_material  'XCIF (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega scan, frame data integration'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5953
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.1004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                2452
_reflns_number_total             2779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            os0007.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.1004P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.1004P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2019-10-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C19 H9 O6 S'
_cod_original_formula_weight         365.32
_cod_original_formula_moiety         'C19 H9 O3,O3 S'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        689.8(2)
_cod_database_code               2003085