An anti-tetraamination of a 1,3-diene unit via cascade annulations of the azulenone scaffold with dicarbonyl azo-compounds
Ishigaki, Yuhei; Mahendar, Velisoju; Oguri, Hiroki; Oikawa, Hideaki; Chemical Communications 46 (2010) 3304–3305; doi:10.1039/b926676c

data_7105496
_publ_section_title
;
 An anti-tetraamination of a 1,3-diene unit via cascade annulations of
 the azulenone scaffold with dicarbonyl azo-compounds
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              3304
_journal_page_last               3305
_journal_paper_doi               10.1039/b926676c
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C33 H34 Br N5 O8'
_chemical_formula_weight         708.56
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.9510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0539(2)
_cell_length_b                   23.6403(4)
_cell_length_c                   12.1023(2)
_cell_measurement_temperature    223(2)
_cell_volume                     3261.72(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            57974
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    2.218
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_correction_T_min  0.7320
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0831P)^2^+5.8952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.2151
_reflns_number_gt                3807
_reflns_number_total             5962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926676c.txt
_cod_data_source_block           shelxl
_cod_original_cell_volume        3261.70(10)
_cod_database_code               7105496