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_7710904
_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         'C20 H9 As Cl4 O2 S2'
_chemical_formula_sum            'C20 H9 As Cl4 O2 S2'
_chemical_formula_weight         562.11
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-23
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                106.101(3)
_cell_angle_beta                 103.786(4)
_cell_angle_gamma                98.692(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8878(5)
_cell_length_b                   10.6388(4)
_cell_length_c                   12.0109(5)
_cell_measurement_reflns_used    4090
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      32.5380
_cell_measurement_theta_min      3.1910
_cell_volume                     1030.60(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 6.83
_diffrn_detector_type            'Rigaku Mercury area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -70.00  34.00   1.00    1.00    --   30.00  54.00 -30.00  104
  2  \w    -73.00 -48.00   1.00    1.00    --   30.00  54.00  90.00   25
  3  \w      8.00  34.00   1.00    1.00    --   30.00  54.00  90.00   26
  4  \w    -74.00 109.00   1.00    1.00    --   30.00  54.00-150.00  183
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0833101000
_diffrn_orient_matrix_UB_12      0.0050864000
_diffrn_orient_matrix_UB_13      0.0137534000
_diffrn_orient_matrix_UB_21      -0.0056470000
_diffrn_orient_matrix_UB_22      -0.0137193000
_diffrn_orient_matrix_UB_23      -0.0623034000
_diffrn_orient_matrix_UB_31      0.0129200000
_diffrn_orient_matrix_UB_32      0.0698374000
_diffrn_orient_matrix_UB_33      0.0082118000
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6186
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.386
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.811
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+0.1649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3834
_reflns_number_total             4195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02145e2.cif
_cod_data_source_block           8
_cod_database_code               7710904
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         As1O2S2C20Cl4H9
_shelx_estimated_absorpt_t_max   0.598
_shelx_estimated_absorpt_t_min   0.315
_diffrn_oxdiff_digest_frames
;
01b26f939902f9f2211962863dfa2f24e50033816a1
;
_diffrn_oxdiff_digest_hkl
;
01bd6063c8e58f59ec6f28c58d2ee83585b1a2
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C4(H4), C21(H21), C9(H9), C25(H25), C24(H24), C23(H23),
 C22(H22)
;
_shelx_res_checksum              50793
_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 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.828