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_4030570
_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
'0.75(C93 H99 N Si3), 0.25(C93 H98 N Si3), 0.25(C6 H14)'
_chemical_formula_sum            'C94.5 H102.25 N Si3'
_chemical_formula_weight         1336.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-25
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                93.1848(15)
_cell_angle_beta                 103.5237(16)
_cell_angle_gamma                107.6346(17)
_cell_formula_units_Z            8
_cell_length_a                   20.0898(4)
_cell_length_b                   29.1629(5)
_cell_length_c                   30.1260(6)
_cell_measurement_reflns_used    32377
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      75.6170
_cell_measurement_theta_min      3.2230
_cell_volume                     16201.4(6)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
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      173.0(1)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.9938
_diffrn_measured_fraction_theta_max 0.9938
_diffrn_measurement_details
;
  1 omega -111.00  -15.00   1.0000   29.3800
omega____ theta____ kappa____ phi______ frames
    -      -42.7322  -57.0000  150.0000 96

  2 omega  -66.00   30.00   1.0000   29.3800
omega____ theta____ kappa____ phi______ frames
    -      -42.7322   57.0000  -60.0000 96

  3 omega -124.00  -87.00   1.0000   29.3800
omega____ theta____ kappa____ phi______ frames
    -      -42.7322  -99.0000  -60.0000 37

  4 omega  -96.00   -2.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  125.0000    0.0000 94

  5 omega   38.00   99.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  120.0000 61

  6 omega   47.00   99.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 52

  7 omega   38.00  120.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 82

  8 omega   92.00  178.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 86

  9 omega   52.00   91.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 39

 10 omega   28.00  109.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 81

 11 omega  103.00  175.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -180.0000 72

 12 omega   42.00  109.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 67

 13 omega   35.00   88.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   60.0000 53

 14 omega   58.00  173.00   1.0000  117.5100
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000    0.0000 115
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0515449000
_diffrn_orient_matrix_UB_12      -0.0520357000
_diffrn_orient_matrix_UB_13      -0.0187120000
_diffrn_orient_matrix_UB_21      0.0550844000
_diffrn_orient_matrix_UB_22      -0.0205136000
_diffrn_orient_matrix_UB_23      0.0295286000
_diffrn_orient_matrix_UB_31      -0.0355755000
_diffrn_orient_matrix_UB_32      0.0009448000
_diffrn_orient_matrix_UB_33      0.0399880000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            80660
_diffrn_reflns_theta_full        58.95
_diffrn_reflns_theta_max         58.95
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.980
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5746
_exptl_crystal_recrystallization_method 'crystallized from DCM/Hexane'
_exptl_crystal_size_max          0.2186
_exptl_crystal_size_mid          0.1619
_exptl_crystal_size_min          0.1111
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3594
_refine_ls_number_reflns         46273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+14.0732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2083
_reflns_number_gt                37244
_reflns_number_total             46273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502605e_si_004.cif
_cod_data_source_block           nag03
_cod_depositor_comments
'Adding full bibliography for 4030570--4030572.cif.'
_cod_original_cell_volume        16201.5(5)
_cod_original_formula_sum        'C94.50 H102.25 N Si3'
_cod_database_code               4030570
_chemical_oxdiff_formula         'C93 H99 Ni Si3'
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86