Interaction of Azobenzene and Benzalaniline with Strong Amido Bases.
Kornev, Alexander N.; Sushev, Vyacheslav V.; Zolotareva, Natalia V.; Baranov, Evgenii V.; Fukin, Georgy K.; Abakumov, Gleb A.; Organic letters 17 (2015) 6154–6157; doi:10.1021/acs.orglett.5b02860

data_1555423
_publ_section_title
;
 Interaction of Azobenzene and Benzalaniline with Strong Amido Bases.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6154
_journal_page_last               6157
_journal_paper_doi               10.1021/acs.orglett.5b02860
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C28 H32 N2 Si2'
_chemical_formula_weight         452.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.9280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4866(4)
_cell_length_b                   18.1483(8)
_cell_length_c                   16.7017(8)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.04
_cell_measurement_theta_min      2.56
_cell_volume                     2547.8(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25397
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.423
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.9152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       stick
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.8390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4515
_reflns_number_total             4995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b02860_si_002.cif
_cod_data_source_block           sinnm
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1555423
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              92562
_shelx_hkl_checksum              65173