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_4028102
_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            'C44 H52 N2 O2 Si2'
_chemical_formula_weight         697.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.320(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.000(5)
_cell_length_b                   7.9673(11)
_cell_length_c                   34.764(4)
_cell_measurement_reflns_used    2147
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.98
_cell_measurement_theta_min      2.37
_cell_volume                     8139(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19411
_diffrn_reflns_theta_full        19.39
_diffrn_reflns_theta_max         19.39
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.9625
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       needle
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         6973
_refine_ls_number_restraints     1521
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0836P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                3826
_reflns_number_total             6973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400092r_si_007.cif
_cod_data_source_block           mas8
_cod_original_cell_volume        8139.2(19)
_cod_database_code               4028102