Crystal structures of 3,3'-bis(hydroxydimethylsilanyl)azobenzene and 4,4'-bis(hydroxydimethylsilane)azobenzene
Strüben, Jan; Hoffmann, Jonas; Presa-Soto, David; Näther, Christian; Staubitz, Anne; Acta Crystallographica Section E 72 (2016) 1590–1594; doi:10.1107/S2056989016016297

data_2241889
_publ_section_title
;
 Crystal structures of 3,3'-bis(hydroxydimethylsilanyl)azobenzene and
 4,4'-bis(hydroxydimethylsilane)azobenzene
;
_journal_coeditor_code           WM5327
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1590
_journal_page_last               1594
_journal_paper_doi               10.1107/S2056989016016297
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C16 H22 N2 O2 Si2'
_chemical_formula_moiety         'C16 H22 N2 O2 Si2'
_chemical_formula_sum            'C16 H22 N2 O2 Si2'
_chemical_formula_weight         330.53
_chemical_name_systematic
;
(<i>E</i>)-[Diazene-1,2-diylbis(4,1-phenylene)]bis(dimethylsilanol)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.013(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8705(4)
_cell_length_b                   10.0016(3)
_cell_length_c                   20.5323(5)
_cell_measurement_reflns_used    30514
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.61
_cell_volume                     3642.36(16)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30514
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.611
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0466P)^2^+1.1330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                6720
_reflns_number_total             7877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5327sup1.cif
_cod_data_source_block           II
_cod_database_code               2241889
_cod_database_fobs_code          2241889
_shelx_hkl_checksum              4547
_shelx_res_checksum              52041
_shelxl_version_number           2.014