Synthesis and properties of arylvinylidene-bridged triphenylamines.
Hammer, Natalie; Shubina, Tatyana E.; Gisselbrecht, Jean-Paul; Hampel, Frank; Kivala, Milan; The Journal of organic chemistry 80 (2015) 2418–2424; doi:10.1021/jo502605e

data_4030572
_publ_section_title
;
 Synthesis and properties of arylvinylidene-bridged triphenylamines.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2418
_journal_page_last               2424
_journal_paper_doi               10.1021/jo502605e
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C93 H93 N S3 Si3, 2(C4 H8 O2)'
_chemical_formula_sum            'C101 H109 N O4 S3 Si3'
_chemical_formula_weight         1581.34
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-28
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9240(4)
_cell_length_b                   37.2892(7)
_cell_length_c                   10.7444(2)
_cell_measurement_reflns_used    8234
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      61.5560
_cell_measurement_theta_min      4.7120
_cell_volume                     8783.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.9903
_diffrn_measured_fraction_theta_max 0.9903
_diffrn_measurement_details
;
  1 omega  -56.00   30.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   45.0000  -60.0000 86

  2 omega   64.00  109.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  -77.0000   90.0000 45

  3 omega   95.00  127.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  125.0000  -30.0000 32

  4 omega   45.00  110.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168 -125.0000  -30.0000 65

  5 omega  101.00  150.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  125.0000 -120.0000 49

  6 omega    9.00   36.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  -77.0000   90.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0293449000
_diffrn_orient_matrix_UB_12      0.0375567000
_diffrn_orient_matrix_UB_13      -0.0008325000
_diffrn_orient_matrix_UB_21      -0.0084774000
_diffrn_orient_matrix_UB_22      0.0026030000
_diffrn_orient_matrix_UB_23      0.1420185000
_diffrn_orient_matrix_UB_31      0.0633113000
_diffrn_orient_matrix_UB_32      -0.0169966000
_diffrn_orient_matrix_UB_33      0.0196388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16074
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         4.20
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69562
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_recrystallization_method 'crystallized from DCM/Hexane/EtOAc'
_exptl_crystal_size_max          0.2015
_exptl_crystal_size_mid          0.1145
_exptl_crystal_size_min          0.0494
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0834P)^2^+9.8238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                5471
_reflns_number_total             6379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502605e_si_002.cif
_cod_data_source_block           nag12
_cod_depositor_comments
'Adding full bibliography for 4030570--4030572.cif.'
_cod_original_cell_volume        8783.8(3)
_cod_database_code               4030572
_chemical_oxdiff_formula         'C87 H97 N S3 Si3'
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86