Tetrachlorocatecholates of triarylarsines as a novel class of Lewis acids
Chishiro, Akane; Akioka, Ippei; Sumida, Akifumi; Oka, Kouki; Tonai, Norimitsu; Yumura, Takashi; Imoto, Hiroaki; Naka, Kensuke; Dalton Transactions  (2022) –; doi:10.1039/D2DT02145E

data_7710902
_publ_section_title
;
 Tetrachlorocatecholates of triarylarsines as a novel class of Lewis acids
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02145E
_journal_year                    2022
_chemical_formula_moiety         'C24 H8 As Cl4 F5 O2'
_chemical_formula_sum            'C24 H8 As Cl4 F5 O2'
_chemical_formula_weight         640.02
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-22
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.110(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5696(11)
_cell_length_b                   16.0085(5)
_cell_length_c                   17.3520(11)
_cell_measurement_reflns_used    5111
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      31.1470
_cell_measurement_theta_min      2.7800
_cell_volume                     4591.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 6.83
_diffrn_detector_type            'Rigaku Mercury area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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     26.00  51.00   0.05   15.00    --   30.00  54.00 -30.00  500
  2  \w    -53.00 -24.00   0.05   15.00    --   30.00  54.00 -60.00  580
  3  \w    -22.00 108.00   0.05   15.00    --   30.00  54.00-150.00 2600
  4  \w     81.00 107.00   0.05   15.00    --   30.00  54.00-180.00  520
  5  \w    -49.00  27.00   0.05   15.00    --   30.00  54.00 -30.00 1520
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9396
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.744
_diffrn_reflns_theta_min         2.521
_exptl_absorpt_coefficient_mu    2.010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0721P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5076
_reflns_number_total             9396
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.7085\% 
around [1.00 0.00 0.01] (reciprocal) or [0.90 0.00 0.44] (direct)
;
_cod_data_source_file            d2dt02145e2.cif
_cod_data_source_block           6
_cod_database_code               7710902
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9413(8)
 0.0587(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C27(H27), C8(H8), C11(H11), C34(H34), C35(H35), C2(H2), C3(H3),
 C5(H5), C26(H26), C9(H9), C28(H28), C10(H10), C29(H29), C32(H32), C33(H33)
;
_shelx_res_checksum              2881
_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
;