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_7151202
_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            'C30 H32 N2'
_chemical_formula_weight         420.58
_chemical_name_common
6,6f-diphenyl-3,3f,4,4f-tetraethyl-2,2f-bis(azafulvene)
_chemical_name_systematic
;
6,6f-diphenyl-3,3f,4,4f-tetraethyl-2,2f-bis(azafulvene)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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                   14.883(4)
_cell_length_b                   7.830(2)
_cell_length_c                   20.587(6)
_cell_measurement_reflns_used    915
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.009
_cell_measurement_theta_min      2.406
_cell_volume                     2399.1(11)
_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      294(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11904
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS ver. 2.03 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0550P)^2^+0.2086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                1472
_reflns_number_total             2409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b518340e.txt
_cod_data_source_block           (6a)
_cod_original_cell_volume        2399.0(11)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7151202