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_4030571
_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         'C78 H69 N O6 S3'
_chemical_formula_sum            'C78 H69 N O6 S3'
_chemical_formula_weight         1212.52
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-03
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  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            8
_cell_length_a                   30.7925(9)
_cell_length_b                   16.2373(6)
_cell_length_c                   34.0415(16)
_cell_measurement_reflns_used    7839
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      54.2220
_cell_measurement_theta_min      4.1760
_cell_volume                     17020.3(11)
_computing_cell_refinement
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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)
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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)
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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)
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_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
;
SHELXL, 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(1)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.9851
_diffrn_measured_fraction_theta_max 0.9683
_diffrn_measurement_details
;
  1 omega  -87.00  -34.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -150.0000 53

  2 omega   26.00  117.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       70.2455 -125.0000   30.0000 91

  3 omega  100.00  143.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       70.2455  109.0000  -11.0000 43

  4 omega   45.00  137.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       70.2455   57.0000  -60.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0320247000
_diffrn_orient_matrix_UB_12      -0.0446687000
_diffrn_orient_matrix_UB_13      -0.0274411000
_diffrn_orient_matrix_UB_21      0.0082038000
_diffrn_orient_matrix_UB_22      0.0813136000
_diffrn_orient_matrix_UB_23      -0.0222592000
_diffrn_orient_matrix_UB_31      0.0374976000
_diffrn_orient_matrix_UB_32      0.0206928000
_diffrn_orient_matrix_UB_33      0.0282017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28109
_diffrn_reflns_theta_full        55.79
_diffrn_reflns_theta_max         55.79
_diffrn_reflns_theta_min         3.87
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51362
_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            'clear brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5120
_exptl_crystal_recrystallization_method 'crystallized from DCM/Hexane'
_exptl_crystal_size_max          0.3045
_exptl_crystal_size_mid          0.0781
_exptl_crystal_size_min          0.0602
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10689
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0966
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2928
_refine_ls_wR_factor_ref         0.3178
_reflns_number_gt                7056
_reflns_number_total             10689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502605e_si_003.cif
_cod_data_source_block           nag09
_cod_depositor_comments
'Adding full bibliography for 4030570--4030572.cif.'
_cod_database_code               4030571
_chemical_oxdiff_formula         'C78 H69 N O3 S3'
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     54.18