σ-Arsolido complexes.
Kirk, Ryan M.; HIll, Anthony F; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11809–11829; doi:10.1039/d4dt01308e

data_7716438
_publ_section_title
;
 &#x3c3;-Arsolido complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11809
_journal_page_last               11829
_journal_paper_doi               10.1039/d4dt01308e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H25 As O3 W, C6 H6'
_chemical_formula_sum            'C42 H31 As O3 W'
_chemical_formula_weight         842.44
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-29 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.88750(10)
_cell_length_b                   15.38100(10)
_cell_length_c                   23.5386(2)
_cell_measurement_reflns_used    14026
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5830
_cell_measurement_theta_min      4.4380
_cell_volume                     6838.17(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -55.00  -9.00   1.00    2.00    --  -37.03 125.00 -90.00   46
  2  \w     15.00  49.00   1.00    2.00    --   37.03 -99.00-180.00   34
  3  \w      8.00  34.00   1.00    2.00    --   37.03  19.00 150.00   26
  4  \w     33.00  88.00   1.00    2.00    --   37.03  57.00  60.00   55
  5  \w     43.00  89.00   1.00    2.00    --   37.03-125.00   0.00   46
  6  \w     62.00 101.00   1.00    2.00    --   37.03  19.00 150.00   39
  7  \w     46.00  85.00   1.00    6.00    --  111.00 -38.00  90.00   39
  8  \w    105.00 166.00   1.00    6.00    --  111.00  50.00 -60.00   61
  9  \w     51.00  77.00   1.00    6.00    --  111.00 -92.00 -90.00   26
 10  \w     81.00 106.00   1.00    6.00    --  111.00 -92.00 120.00   25
 11  \w    133.00 159.00   1.00    6.00    --  111.00  38.00-180.00   26
 12  \w     46.00 130.00   1.00    6.00    --  111.00 -38.00 -90.00   84
 13  \w     95.00 124.00   1.00    6.00    --  111.00  38.00-180.00   29
 14  \w     73.00 111.00   1.00    6.00    --  111.00 178.00 -90.00   38
 15  \w    117.00 142.00   1.00    6.00    --  111.00  49.00  22.00   25
 16  \w    153.00 178.00   1.00    6.00    --  111.00 111.00-150.00   25
 17  \w     84.00 122.00   1.00    6.00    --  111.00 -64.00  30.00   38
 18  \w    116.00 141.00   1.00    6.00    --  111.00 111.00  90.00   25
 19  \w     41.00  94.00   1.00    6.00    --  111.00-111.00 120.00   53
 20  \w     43.00  68.00   1.00    6.00    --  111.00 -92.00 -30.00   25
 21  \w    124.00 150.00   1.00    6.00    --  111.00 111.00 -60.00   26
 22  \w     64.00 124.00   1.00    6.00    --  111.00 -38.00 120.00   60
 23  \w    136.00 162.00   1.00    6.00    --  111.00 111.00-180.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0312831000
_diffrn_orient_matrix_UB_12      0.0654022000
_diffrn_orient_matrix_UB_13      0.0427491000
_diffrn_orient_matrix_UB_21      -0.0382921000
_diffrn_orient_matrix_UB_22      0.0748259000
_diffrn_orient_matrix_UB_23      -0.0308371000
_diffrn_orient_matrix_UB_31      -0.0648475000
_diffrn_orient_matrix_UB_32      -0.0125600000
_diffrn_orient_matrix_UB_33      0.0388080000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27682
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.726
_diffrn_reflns_theta_min         3.756
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.639
_exptl_absorpt_correction_T_max  0.55396
_exptl_absorpt_correction_T_min  0.51606
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.637
_exptl_crystal_description       prism
_exptl_crystal_F_000             3312
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/n-hexane'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.043
_exptl_crystal_size_rad          0.059
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0338P)^2^+3.8325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6262
_reflns_number_total             6869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_187_a_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716438
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C42H31As1O3W1
_chemical_oxdiff_usercomment     'benzene/hexane '
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C25(H25), C32(H32), C27(H27), C9(H9), C15(H15), C13(H13), C30(H30),
 C31(H31), C33(H33), C10(H10), C41(H41), C28(H28), C19(H19), C29(H29), C17(H17),
  C16(H16), C12(H12), C35(H35), C42(H42), C40(H40), C21(H21), C11(H11),
 C18(H18), C37(H37), C34(H34), C24(H24), C38(H38), C23(H23), C39(H39), C22(H22)
;
_shelx_res_checksum              2206
_ins_header
;
TITL RMK_187_A_scale in Pbca 
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 1.54184  18.887485  15.380979  23.538642  90.0000  90.0000  90.0000
ZERR    8.00   0.000142   0.000129   0.000196   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H O As W
UNIT 336.00 248.00 24.00 8.00 8.00
TREF
HKLF 4
END
;
_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 1.618
_oxdiff_exptl_absorpt_empirical_full_min 0.790