Tuning rotational barriers through substituent modification in catechol-diyl molecular gyrotops.
Kishii, Hyu; Inagaki, Yusuke; Ohara, Kazuaki; Yamaguchi, Kentaro; Setaka, Wataru; Organic & biomolecular chemistry 23 (2025) 10100–10105; doi:10.1039/d5ob01474c

data_7160790
_publ_section_title
;
 Tuning rotational barriers through substituent modification in
 catechol-diyl molecular gyrotops.
;
_journal_issue                   44
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              10100
_journal_page_last               10105
_journal_paper_doi               10.1039/d5ob01474c
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C50 H92 O2 Si2'
_chemical_formula_sum            'C50 H92 O2 Si2'
_chemical_formula_weight         781.41
_chemical_melting_point          429.1(10)
_chemical_name_common            C14Ph(OMe)2cage
_chemical_name_systematic        C14Ph(OMe)2cage
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-09-12 deposited with the CCDC.	2025-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                114.7100(10)
_cell_angle_beta                 90.6160(10)
_cell_angle_gamma                104.5210(10)
_cell_formula_units_Z            4
_cell_length_a                   11.9574(3)
_cell_length_b                   20.9583(6)
_cell_length_c                   23.0968(6)
_cell_measurement_reflns_used    9054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.5113
_cell_measurement_theta_min      3.8520
_cell_volume                     5046.1(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Sir-2019 (IUCr, 2019)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72665
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.360
_diffrn_reflns_theta_min         2.124
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: a mixture of tetrahydrofuran and methanol'
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         20488
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+3.3671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17606
_reflns_number_total             20488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01474c2.cif
_cod_data_source_block           C14Ph(OMe)2cage
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '155-157 oC' was changed to
'429.1(10)' -- it was converted from degrees Celsius (C) to kelvins
(K), the average value was taken and precision was estimated.

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7160788--7160790.cif.
;
_cod_database_code               7160790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              92555