Dibenzoarsacrowns: an experimental and computational study on the coordination behaviors.
Sumida, Akifumi; Kobayashi, Ryosuke; Yumura, Takashi; Imoto, Hiroaki; Naka, Kensuke; Chemical communications (Cambridge, England) 57 (2021) 2013–2016; doi:10.1039/d0cc07191a

data_7127704
_publ_section_title
;
 Dibenzoarsacrowns: an experimental and computational study on the
 coordination behaviors.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2013
_journal_page_last               2016
_journal_paper_doi               10.1039/d0cc07191a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '4(C20 H19 As O2), C H2 Cl2'
_chemical_formula_sum            'C81 H78 As4 Cl2 O8'
_chemical_formula_weight         1550.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-01 deposited with the CCDC.	2020-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.278(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.1368(10)
_cell_length_b                   7.4077(3)
_cell_length_c                   21.7648(8)
_cell_measurement_reflns_used    6109
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      32.8960
_cell_measurement_theta_min      3.4040
_cell_volume                     3569.0(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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_area_resol_mean 6.83
_diffrn_detector_type            'Rigaku Mercury area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.876
_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  67.00   0.10    5.00    --   30.00  54.00  90.00 1400
  2  \w    -31.00  45.00   0.10    5.00    --   30.00  54.00   0.00  760
;
_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_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            9755
_diffrn_reflns_point_group_measured_fraction_full 0.727
_diffrn_reflns_point_group_measured_fraction_max 0.587
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.684
_diffrn_reflns_theta_min         2.618
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91712
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       needle
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.590
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7687
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0599P)^2^+42.2537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.255
_reflns_Friedel_fraction_full    0.418
_reflns_Friedel_fraction_max     0.255
_reflns_number_gt                7474
_reflns_number_total             7687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07191a2.cif
_cod_data_source_block           bis(o-anisyl)phenylarsine
_cod_depositor_comments
'Adding full bibliography for 7127700--7127710.cif.'
_cod_database_code               7127704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.310
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H41A(0.5) H41B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C17(H17), C37(H37), C25(H25), C12(H12), C36(H36), C10(H10), C2(H2),
 C32(H32), C29(H29), C16(H16), C23(H23), C11(H11), C9(H9), C24(H24), C20(H20),
 C18(H18), C3(H3), C38(H38), C5(H5), C30(H30), C31(H31), C4(H4), C39(H39),
 C19(H19), C40(H40)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              58326
_shelx_hkl_checksum              98006
_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
;