Probing the Delicate Balance between Pauli Repulsion and London Dispersion with Triphenylmethyl Derivatives.
Rösel, Sören; Becker, Jonathan; Allen, Wesley D.; Schreiner, Peter R.; Journal of the American Chemical Society 140 (2018) 14421–14432; doi:10.1021/jacs.8b09145

data_4133249
_publ_section_title
;
 Probing the Delicate Balance between Pauli Repulsion and London
 Dispersion with Triphenylmethyl Derivatives.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14421
_journal_page_last               14432
_journal_paper_doi               10.1021/jacs.8b09145
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration nd
_chemical_formula_sum            'C37 H52'
_chemical_formula_weight         496.78
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.2294(11)
_cell_length_b                   23.2294(11)
_cell_length_c                   10.0567(5)
_cell_measurement_reflns_used    9663
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.10
_cell_measurement_theta_min      3.81
_cell_volume                     4699.6(4)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            82852
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.469
_diffrn_reflns_theta_min         2.196
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7541
_exptl_absorpt_correction_T_min  0.4657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.725
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
; 
 Flack x determined using 3069 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.5(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         11262
_refine_ls_number_restraints     4058
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+2.9746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2210
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.750
_reflns_Friedel_fraction_max     0.752
_reflns_number_gt                9376
_reflns_number_total             11262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            D18011.cif
_cod_data_source_block           D18011
_cod_original_cell_volume        4699.6(5)
_cod_database_code               4133249
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              99613
_shelx_hkl_checksum              55699