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_1555425
_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            'C39 H46 N2 Si2'
_chemical_formula_weight         598.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9869(11)
_cell_length_b                   12.5966(11)
_cell_length_c                   19.4789(18)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.65
_cell_volume                     3431.9(5)
_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 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23143
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.414
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.8485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 2607 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.2764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                6076
_reflns_number_total             6479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b02860_si_002.cif
_cod_data_source_block           phnsime3
_cod_database_code               1555425
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              17197
_shelx_hkl_checksum              96582