Two salts of the 6,6-difluoro-6<i>H</i>-dibenzo[<i>c</i>,<i>e</i>][1,2]oxaborinin-6-ide anion with different cations
Budanow, Alexandra; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 76 (2020) 1837–1840; doi:10.1107/S2056989020015066

data_2243678
_publ_section_title
;
 Two salts of the
 6,6-difluoro-6<i>H</i>-dibenzo[<i>c</i>,<i>e</i>][1,2]oxaborinin-6-ide
 anion with different cations
;
_journal_coeditor_code           HB7952
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1837
_journal_page_last               1840
_journal_paper_doi               10.1107/S2056989020015066
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '2C24 H20 P +, 2C12 H8 B F2 O -, 3C2 H3 N'
_chemical_formula_moiety
'2(C24 H20 P +), 2(C12 H8 B F2 O -), 3(C2 H3 N)'
_chemical_formula_sum            'C78 H65 B2 F4 N3 O2 P2'
_chemical_formula_weight         1235.89
_chemical_name_common
;
Bis(tetraphenylphosphonium) bis(9,9-difluoro-10-oxa-9-boraphenanthren-9-ide)
acetonitrile trisolvate
;
_chemical_name_systematic
;
Bis(tetraphenylphosphonium)
6,6-difluoro-6<i>H</i>-dibenzo[<i>c</i>,<i>e</i>][1,2]oxaborinin-6-ide
acetonitrile trisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                86.218(3)
_cell_angle_beta                 78.916(3)
_cell_angle_gamma                87.104(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3527(4)
_cell_length_b                   13.5958(5)
_cell_length_c                   23.4352(9)
_cell_measurement_reflns_used    61056
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.0
_cell_volume                     3227.6(2)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2001)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2001)
;
_computing_data_reduction
;
X-Area (Stoe & Cie, 2001)
;
_computing_molecular_graphics
;
XP   (Sheldrick, 2015b) and Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
publCif (Westrip, 2010)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47827
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.435
_diffrn_reflns_theta_min         2.006
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-Area; Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         11854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.4271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                10863
_reflns_number_total             11854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7952sup1.cif
_cod_data_source_block           III
_cod_database_code               2243678
_cod_database_fobs_code          2243678
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.963
_shelx_hkl_checksum              42882
_shelx_res_checksum              81696