Synthesis of bis(azafulvene)s by dehydration of hydroxymethylpyrrole derivatives.
Setsune, Jun-ichiro; Tanabe, Aya; Watanabe, Junko; Maeda, Satoshi; Organic & biomolecular chemistry 4 (2006) 2247–2252; doi:10.1039/b518340e

data_7151203
_publ_section_title
;
 Synthesis of bis(azafulvene)s by dehydration of hydroxymethylpyrrole
 derivatives.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2247
_journal_page_last               2252
_journal_paper_doi               10.1039/b518340e
_journal_volume                  4
_journal_year                    2006
_chemical_formula_sum            'C25 H22 N2'
_chemical_formula_weight         350.45
_chemical_name_common
6,6f-Diphenyl-2,2f-bis(azafulvenyl)-gem-dimethylmethane
_chemical_name_systematic
;
6,6f-Diphenyl-2,2f-bis(azafulvenyl)-gem-dimethylmethane
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            8
_cell_length_a                   17.135(3)
_cell_length_b                   38.228(8)
_cell_length_c                   6.1877(12)
_cell_measurement_reflns_used    632
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.226
_cell_measurement_theta_min      3.194
_cell_volume                     4053.2(14)
_computing_cell_refinement       'Bruker SAINT+ ver. 6.45'
_computing_data_collection       'Bruker SAINT+ ver. 6.45'
_computing_data_reduction        'Bruker SAINT+ ver. 6.45'
_computing_molecular_graphics    'Bruker XSHELL ver. 4.02'
_computing_publication_material  'Bruker SHELXTL ver. 6.14'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5681
_diffrn_reflns_theta_full        27.31
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS ver. 2.03 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.093
_refine_diff_density_min         -0.087
_refine_diff_density_rms         0.022
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0467P)^2^+0.4669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                1359
_reflns_number_total             2076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b518340e.txt
_cod_data_source_block           (9)
_cod_original_cell_volume        4053.1(14)
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7151203