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_7710908
_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 H13 Cl4 O2 P'
_chemical_formula_sum            'C24 H13 Cl4 O2 P'
_chemical_formula_weight         506.11
_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             2021-06-23
_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                89.651(7)
_cell_angle_beta                 85.511(7)
_cell_angle_gamma                84.269(7)
_cell_formula_units_Z            4
_cell_length_a                   9.3999(8)
_cell_length_b                   13.5076(13)
_cell_length_c                   17.3444(15)
_cell_measurement_reflns_used    2191
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.9480
_cell_measurement_theta_min      2.8030
_cell_volume                     2184.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     87.00 113.00   0.50    0.70    --   30.00  54.00 120.00   52
  2  \w      5.00  36.00   0.50    0.70    --   30.00  54.00-120.00   62
  3  \w    -63.00 119.00   0.50    0.70    --   30.00  54.00 -30.00  364
  4  \w    -69.00  19.00   0.50    0.70    --   30.00  54.00 120.00  176
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0744129000
_diffrn_orient_matrix_UB_12      0.0144998000
_diffrn_orient_matrix_UB_13      -0.0012703000
_diffrn_orient_matrix_UB_21      0.0018693000
_diffrn_orient_matrix_UB_22      -0.0216816000
_diffrn_orient_matrix_UB_23      -0.0372550000
_diffrn_orient_matrix_UB_31      -0.0156783000
_diffrn_orient_matrix_UB_32      -0.0458788000
_diffrn_orient_matrix_UB_33      0.0171222000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13004
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
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    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.457
_exptl_crystal_size_min          0.236
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.2090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5056
_reflns_number_total             8934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02145e2.cif
_cod_data_source_block           11
_cod_database_code               7710908
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOClP
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.751
_reflns_odcompleteness_completeness 99.91
_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:
 C33(H33), C36(H36), C29(H29), C2(H2), C26(H26), C38(H38), C27(H27), C28(H28),
 C5(H5), C42(H42), C34(H34), C35(H35), C3(H3), C12(H12), C4(H4), C24(H24),
 C41(H41), C9(H9), C40(H40), C39(H39), C22(H22), C11(H11), C23(H23), C10(H10),
 C20(H20), C21(H21)
;
_shelx_res_checksum              33706
_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 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.851