Crystallographic and spectroscopic studies on persistent triarylpropargyl cations.
Shimajiri, Takuya; Tsue, Taiga; Koakutsu, Shumpei; Ishigaki, Yusuke; Suzuki, Takanori; Chemical communications (Cambridge, England) 60 (2024) 7152–7155; doi:10.1039/d4cc01786b

data_7133112
_publ_section_title
;
 Crystallographic and spectroscopic studies on persistent triarylpropargyl
 cations.
;
_journal_issue                   56
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7152
_journal_page_last               7155
_journal_paper_doi               10.1039/d4cc01786b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C24 H19 O, B F4'
_chemical_formula_sum            'C24 H19 B F4 O'
_chemical_formula_weight         410.20
_chemical_name_systematic        ts240206-tsue2-150K_auto
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-06 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.309(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8567(3)
_cell_length_b                   19.3806(9)
_cell_length_c                   14.5799(6)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    150
_cell_measurement_theta_max      75.1350
_cell_measurement_theta_min      3.7400
_cell_volume                     1934.25(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -89.00  -2.00   0.50    9.09    --  -42.78 111.00-162.00  174
  2  \w      3.00  89.00   0.50    9.09    --   42.78-111.00 104.00  172
  3  \w   -177.00 -81.00   0.50   15.27    -- -106.00-111.00 104.00  192
  4  \w   -108.00 -30.00   0.50   15.27    -- -106.00 111.00-162.00  156
  5  \w     82.00 178.00   0.50   15.27    --  112.36 111.00-162.00  192
  6  \w     38.00 108.00   0.50   15.27    --  112.36-111.00 104.00  140
  7  \w    -43.00  34.00   0.50    9.09    --  -42.78  38.00 -30.00  154
  8  \w   -117.00 -14.00   0.50    9.09    --  -42.78 -77.00  30.00  206
  9  \w    -37.00  26.00   0.50    9.09    --   42.78 -19.00-150.00  126
 10  \w    -71.00 -32.00   0.50   15.27    -- -106.00  61.00  30.00   78
 11  \w   -105.00 -32.00   0.50   15.27    -- -106.00  77.00-180.00  146
 12  \w    -71.00 -32.00   0.50   15.27    -- -106.00  61.00 -30.00   78
 13  \w   -177.00 -82.00   0.50   15.27    -- -106.00 -30.00 120.00  190
 14  \w     39.00  71.00   0.50   15.27    --  112.36 -61.00-120.00   64
 15  \w     39.00  71.00   0.50   15.27    --  112.36 -61.00  60.00   64
 16  \w     39.00  71.00   0.50   15.27    --  112.36 -61.00 120.00   64
 17  \w     39.00  71.00   0.50   15.27    --  112.36 -61.00 150.00   64
 18  \w     90.00 178.00   0.50   15.27    --  112.36  61.00-150.00  176
 19  \w     90.00 178.00   0.50   15.27    --  112.36  45.00 -60.00  176
 20  \w     39.00 105.00   0.50   15.27    --  112.36 -95.00 120.00  132
 21  \w     39.00  71.00   0.50   15.27    --  112.36 -61.00 -60.00   64
 22  \w     39.00  71.00   0.50   15.27    --  112.36 -61.00   0.00   64
 23  \w   -117.00 -14.00   0.50    9.09    --  -42.78 -77.00 -60.00  206
 24  \w   -117.00 -18.00   0.50    9.09    --  -42.78 -77.00 120.00  198
 25  \w   -117.00 -14.00   0.50    9.09    --  -42.78 -77.00-150.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0920156000
_diffrn_orient_matrix_UB_12      0.0681753000
_diffrn_orient_matrix_UB_13      -0.0353719000
_diffrn_orient_matrix_UB_21      -0.1942821000
_diffrn_orient_matrix_UB_22      -0.0377716000
_diffrn_orient_matrix_UB_23      -0.0237461000
_diffrn_orient_matrix_UB_31      -0.0667385000
_diffrn_orient_matrix_UB_32      0.0156873000
_diffrn_orient_matrix_UB_33      0.0968588000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16551
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.416
_diffrn_reflns_theta_min         3.798
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method
'obtained by recrystallization from CH2Cl2/THF'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0873
_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^)+(0.1334P)^2^+1.7974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3128
_reflns_number_total             3923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01786b2.cif
_cod_data_source_block           ts240206-tsue2-150k_auto
_cod_depositor_comments
'Adding full bibliography for 7133110--7133114.cif.'
_cod_original_cell_volume        1934.24(14)
_cod_database_code               7133112
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C24 H19 O B F4'
_chemical_oxdiff_usercomment     150K
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C19(H19), C8(H8), C14(H14), C15(H15), C22(H22), C00O(H00O),
 C20(H20), C21(H21)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              28861
_shelx_hkl_checksum              91661
_olex2_submission_original_sample_id ts240206-tsue2-150K_auto
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.415
_oxdiff_exptl_absorpt_empirical_full_min 0.484