Synthesis and acid‒base properties of a proton-bridged biaryl compound based on pyridylazulene
Ninomiya, Kazuki; Harada, Yumi; Kanetou, Tomoaki; Suenaga, Yuma; Murafuji, Toshihiro; Tsunashima, Ryo; New J. Chem. 39 (2015) 9079–; doi:10.1039/C5NJ01651G

data_7055110
_publ_section_title
;
 Synthesis and acid--base properties of a proton-bridged biaryl compound
 based on pyridylazulene
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              9079
_journal_paper_doi               10.1039/C5NJ01651G
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C100.5 H71.5 B3 F12 N6 O1.83'
_chemical_formula_weight         1652.83
_chemical_name_common            AzPy2HBF4
_chemical_name_systematic        AzPy2H_BF4
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-12 deposited with the CCDC.
2015-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                70.956(18)
_cell_angle_beta                 76.30(2)
_cell_angle_gamma                87.68(2)
_cell_formula_units_Z            2
_cell_length_a                   13.677(7)
_cell_length_b                   16.455(8)
_cell_length_c                   19.539(8)
_cell_measurement_reflns_used    14536
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.0307
_cell_measurement_theta_min      1.5333
_cell_volume                     4035(3)
_computing_data_collection       CrystalClear
_computing_molecular_graphics    PAYMOL
_computing_publication_material  YADOKARIGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.7275
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
scan:
    Number of images: 720
               Slice: -70.0000 - 110.0000
         Image width: 0.2500
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.3767
              2theta: 20.5760
scan:
    Number of images: 720
               Slice: -70.0000 - 110.0000
         Image width: 0.2500
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.3767
              2theta: 20.5760
scan:
    Number of images: 720
               Slice: -70.0000 - 110.0000
         Image width: 0.2500
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.3767
              2theta: 20.5760

;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Mercury (2x2 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.1407
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40023
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         17603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.314
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.1034
_refine_ls_shift/su_max          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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.3137
_reflns_number_gt                7211
_reflns_number_total             17603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01651g2.cif
_cod_data_source_block           crystalclear
_cod_depositor_comments          'Adding full bibliography for 7055110.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C100.50 H71.50 B3 F12 N6 O1.83'
_cod_database_code               7055110