Triptycene Tripods for the Formation of Highly Uniform and Densely Packed Self-Assembled Monolayers with Controlled Molecular Orientation.
Ishiwari, Fumitaka; Nascimbeni, Giulia; Sauter, Eric; Tago, Hiromu; Shoji, Yoshiaki; Fujii, Shintaro; Kiguchi, Manabu; Tada, Tomofumi; Zharnikov, Michael; Zojer, Egbert; Fukushima, Takanori; Journal of the American Chemical Society 141 (2019) 5995–6005; doi:10.1021/jacs.9b00950

data_4128428
_publ_section_title
;
 Triptycene Tripods for the Formation of Highly Uniform and Densely Packed
 Self-Assembled Monolayers with Controlled Molecular Orientation.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5995
_journal_page_last               6005
_journal_paper_doi               10.1021/jacs.9b00950
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C23 H20 S3'
_chemical_formula_weight         392.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.9240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7750(12)
_cell_length_b                   8.5272(6)
_cell_length_c                   14.2714(11)
_cell_measurement_reflns_used    7936
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.820
_cell_measurement_theta_min      2.630
_cell_volume                     1885.0(2)
_computing_cell_refinement       'APEX3 v2015.9 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service V4.2.9 '
_computing_data_reduction        'SAINT V8.35A (Bruker AXS'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS Inc., 2004)'
_computing_publication_material
'Generate Report V2014.1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11880
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.315
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0363P)^2^+1.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3084
_reflns_number_total             3323
_reflns_threshold_expression     'I > 2\s'
_cod_data_source_file            ja9b00950_si_002.cif
_cod_data_source_block           TripCH2SH_by_0ma_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128428
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              66719
_shelx_hkl_checksum              66165