Design of Rotational Potential in Phenyltriptycene Molecular Rotor by Exploiting CH/π-Interaction between Tripticil Hydrogen and Phenyl
Inami, Hazuki; Inagaki, Yusuke; Setaka, Wataru; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB01179D

data_7158831
_publ_section_title
;
 Design of Rotational Potential in Phenyltriptycene Molecular Rotor by
 Exploiting CH/\p-Interaction between Tripticil Hydrogen and Phenyl
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB01179D
_journal_year                    2022
_chemical_compound_source        no
_chemical_formula_moiety         'C28 H19 Cl3 O2'
_chemical_formula_sum            'C28 H19 Cl3 O2'
_chemical_formula_weight         493.78
_chemical_melting_point          458.5(5)
_chemical_name_common            (OMe)2PhTripCl3
_chemical_name_systematic        PhenylTriptyceneDeriv.
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-30 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5816(4)
_cell_length_b                   9.3605(2)
_cell_length_c                   31.6875(8)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.45
_cell_measurement_theta_min      3.98
_cell_volume                     4621.67(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-2019 (IUCr)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            38013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.596
_diffrn_reflns_theta_min         2.789
_diffrn_source                   'shield tube'
_exptl_absorpt_coefficient_mu    3.784
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8907
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0673P)^2^+7.4745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8341
_reflns_number_total             8907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob01179d2.cif
_cod_data_source_block           (OMe)2PhTripCl3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '458-459 K' was changed to
'458.5(5)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7158831
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.335
_shelx_estimated_absorpt_t_max   0.566
_shelx_res_checksum              84235