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_7710901
_publ_section_title
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 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         'C27 H21 As Cl4 O5'
_chemical_formula_sum            'C27 H21 As Cl4 O5'
_chemical_formula_weight         642.15
_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             2021-04-23
_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                92.495(3)
_cell_angle_beta                 97.124(3)
_cell_angle_gamma                99.593(3)
_cell_formula_units_Z            4
_cell_length_a                   10.0471(3)
_cell_length_b                   12.8490(5)
_cell_length_c                   21.2792(7)
_cell_measurement_reflns_used    6286
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      31.5940
_cell_measurement_theta_min      2.6780
_cell_volume                     2681.93(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (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      93.15
_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    -73.00  33.00   0.10    2.50    --   30.00  54.00  90.00 1060
  2  \w     81.00 107.00   0.10    2.50    --   30.00  54.00  90.00  260
  3  \w    -72.00  33.00   0.10    2.50    --   30.00  54.00 -30.00 1050
  4  \w    -74.00  33.00   0.10    2.50    --   30.00  54.00-150.00 1070
;
_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      0.0174617000
_diffrn_orient_matrix_UB_12      -0.0372340000
_diffrn_orient_matrix_UB_13      0.0218576000
_diffrn_orient_matrix_UB_21      -0.0361260000
_diffrn_orient_matrix_UB_22      -0.0418870000
_diffrn_orient_matrix_UB_23      -0.0215077000
_diffrn_orient_matrix_UB_31      0.0600757000
_diffrn_orient_matrix_UB_32      -0.0026564000
_diffrn_orient_matrix_UB_33      -0.0138920000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16672
_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         2.597
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.703
_exptl_absorpt_correction_T_max  0.100
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (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    1.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.687
_exptl_crystal_size_mid          0.393
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0843P)^2^+1.1228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9083
_reflns_number_total             10965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02145e2.cif
_cod_data_source_block           3
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H42 As2 Cl8 O10'
_cod_original_formula_weight         1284.31
_cod_original_formula_moiety         '2(C27 H21 As Cl4 O5)'
_cod_original_formula_units_Z            2
_cod_database_code               7710901
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOClAs
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.387
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C15(H15), C50(H50), C25(H25), C46(H46), C8(H8), C16(H16), C26(H26), C38(H38),
 C53(H53), C12(H12), C42(H42), C52(H52), C9(H9), C22(H22), C19(H19), C43(H43),
 C18(H18), C39(H39), C45(H45), C36(H36), C49(H49), C35(H35), C23(H23), C11(H11)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C), C27(H27A,H27B,
 H27C), C40(H40A,H40B,H40C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              55543
_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 3.015
_oxdiff_exptl_absorpt_empirical_full_min 0.401