Dehydroaromatization of Quinoxalines: One-Step Syntheses of Trinuclear 1,6,7,12,13,18-Hexaazatrinaphthylene Titanium Complexes
Ingmar M. Piglosiewicz; Ruediger Beckhaus; Wolfgang Saak; Detlev Haase; Journal of the American Chemical Society 127 (2005) 14190–14191; doi:10.1021/ja054740p

data_4112020
_publ_section_title
;
 Dehydroaromatization of Quinoxalines: One-Step Syntheses of Trinuclear
 1,6,7,12,13,18-Hexaazatrinaphthylene Titanium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14190
_journal_page_last               14191
_journal_paper_doi               10.1021/ja054740p
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C58 H50 N6 O Ti3'
_chemical_formula_weight         990.74
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_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            2
_cell_length_a                   18.5416(9)
_cell_length_b                   15.6225(10)
_cell_length_c                   7.8136(3)
_cell_measurement_temperature    193(2)
_cell_volume                     2263.3(2)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (Stoe, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.1332
_diffrn_reflns_av_sigmaI/netI    0.1507
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19505
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_correction_T_min  0.9047
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       needle
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.19(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.796
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4483
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0164P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                2510
_reflns_number_total             4483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054740psi20050901_034942.cif
_cod_data_source_block           IP35
_cod_database_code               4112020