Alkynylated Diazadioxaacenes: Syntheses and Properties
Manuel Schaffroth; Benjamin D. Lindner; Vladislav Vasilenko; Frank Rominger; U. H. F. Bunz; Journal of Organic Chemistry 78 (2013) 3142–3150; doi:10.1021/jo400092r

data_4028101
_publ_section_title
;
 Alkynylated Diazadioxaacenes: Syntheses and Properties
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3142
_journal_page_last               3150
_journal_paper_doi               10.1021/jo400092r
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C40 H50 N2 O2 Si2'
_chemical_formula_weight         647.00
_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
_cell_angle_alpha                87.374(4)
_cell_angle_beta                 81.836(4)
_cell_angle_gamma                78.822(4)
_cell_formula_units_Z            4
_cell_length_a                   8.4932(12)
_cell_length_b                   17.857(3)
_cell_length_c                   25.874(4)
_cell_measurement_reflns_used    6046
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      2.39
_cell_volume                     3810.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27205
_diffrn_reflns_theta_full        24.04
_diffrn_reflns_theta_max         24.04
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9949
_exptl_absorpt_correction_T_min  0.8905
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       needle-plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         11672
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.1054
_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^)+(0.0492P)^2^+12.1016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2381
_refine_ls_wR_factor_ref         0.2597
_reflns_number_gt                7864
_reflns_number_total             11672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400092r_si_006.cif
_cod_data_source_block           mas5
_cod_original_cell_volume        3810.0(9)
_cod_database_code               4028101