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

data_7716436
_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         'C16 H17 As O3 W'
_chemical_formula_sum            'C16 H17 As O3 W'
_chemical_formula_weight         516.06
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 106.6740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.66960(10)
_cell_length_b                   28.8296(3)
_cell_length_c                   7.74520(10)
_cell_measurement_reflns_used    19371
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9400
_cell_measurement_theta_min      6.0150
_cell_volume                     1640.54(4)
_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_temperature      150.00(10)
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -82.00 -44.00   1.00    2.00    --  -36.63 125.00  60.00   38
  2  \w    -21.00  63.00   1.00    2.00    --   36.63 -77.00 150.00   84
  3  \w     22.00  54.00   1.00    2.00    --   36.63  57.00 -90.00   32
  4  \w     12.00  41.00   1.00    2.00    --   36.63  78.00-150.41   29
  5  \w     20.00  93.00   1.00    2.00    --   36.63  57.00-180.00   73
  6  \w     58.00 103.00   1.00    2.00    --   36.63  64.00   2.48   45
  7  \w     21.00  56.00   1.00    2.00    --   36.63  57.00  30.00   35
  8  \w     22.00  70.00   1.00    2.00    --   36.63  38.00  30.00   48
  9  \w    -30.00  52.00   1.00    2.00    --   36.63 -57.00-150.00   82
 10  \w    -19.00   9.00   1.00    2.00    --   36.63 -57.00 -60.00   28
 11  \w    -21.00  17.00   1.00    2.00    --   36.63 -77.00   0.00   38
 12  \w     18.00  43.00   1.00    2.00    --   36.63  64.00   2.48   25
 13  \w     33.00  85.00   1.00    2.00    --   36.63  19.00 -90.00   52
 14  \w      5.00  30.00   1.00    2.00    --   36.63  86.00 157.26   25
 15  \w      8.00  42.00   1.00    2.00    --   36.63  80.00  92.11   34
 16  \w     18.00 106.00   1.00    2.00    --   36.63  38.00 120.00   88
 17  \w     14.00 103.00   1.00    2.00    --   36.63  73.00 -76.74   89
 18  \w      4.00  29.00   1.00    2.00    --   36.63  88.00 -29.01   25
 19  \w     23.00  56.00   1.00    2.00    --   36.63 -77.00   0.00   33
 20  \w     30.00  76.00   1.00    2.00    --   36.63 -99.00 -60.00   46
 21  \w    -31.00  38.00   1.00    2.00    --   36.63 -38.00  60.00   69
 22  \w     94.00 132.00   1.00   10.00    --  109.00  45.00 120.00   38
 23  \w     87.00 113.00   1.00   10.00    --  109.00  68.00 145.00   26
 24  \w     91.00 171.00   1.00   10.00    --  109.00  61.00  30.00   80
 25  \w     92.00 130.00   1.00   10.00    --  109.00  45.00 -30.00   38
 26  \w    140.00 175.00   1.00   10.00    --  109.00  61.00 -90.00   35
 27  \w     93.00 133.00   1.00   10.00    --  109.00  45.00-120.00   40
 28  \w     89.00 114.00   1.00   10.00    --  109.00  30.00  90.00   25
 29  \w     46.00  72.00   1.00   10.00    --  109.00 -95.00   0.00   26
 30  \w     41.00  72.00   1.00   10.00    --  109.00 -95.00-180.00   31
 31  \w     50.00  99.00   1.00   10.00    --  109.00 -61.00-180.00   49
 32  \w     91.00 121.00   1.00   10.00    --  109.00  61.00 -90.00   30
 33  \w     93.00 119.00   1.00   10.00    --  109.00  45.00-150.00   26
 34  \w     45.00 109.00   1.00   10.00    --  109.00-111.00 -30.00   64
 35  \w     91.00 119.00   1.00   10.00    --  109.00  61.00-180.00   28
 36  \w     93.00 130.00   1.00   10.00    --  109.00  45.00-180.00   37
 37  \w    133.00 173.00   1.00   10.00    --  109.00  61.00  60.00   40
 38  \w     92.00 118.00   1.00   10.00    --  109.00  45.00  90.00   26
 39  \w    126.00 175.00   1.00   10.00    --  109.00  61.00  90.00   49
 40  \w     91.00 117.00   1.00   10.00    --  109.00  61.00  90.00   26
 41  \w     91.00 117.00   1.00   10.00    --  109.00  61.00  60.00   26
 42  \w     92.00 130.00   1.00   10.00    --  109.00  45.00  60.00   38
 43  \w     92.00 129.00   1.00   10.00    --  109.00  45.00  30.00   37
 44  \w     93.00 132.00   1.00   10.00    --  109.00  45.00 -90.00   39
 45  \w     40.00  68.00   1.00   10.00    --  109.00 -30.00 120.00   28
 46  \w     96.00 122.00   1.00   10.00    --  109.00  61.00 120.00   26
 47  \w     88.00 144.00   1.00   10.00    --  109.00  30.00 150.00   56
 48  \w    128.00 176.00   1.00   10.00    --  109.00  45.00 -60.00   48
 49  \w     93.00 120.00   1.00   10.00    --  109.00  45.00 150.00   27
 50  \w    121.00 176.00   1.00   10.00    --  109.00  61.00 -30.00   55
 51  \w     91.00 117.00   1.00   10.00    --  109.00  61.00-120.00   26
 52  \w    143.00 174.00   1.00   10.00    --  109.00  61.00-120.00   31
 53  \w     92.00 118.00   1.00   10.00    --  109.00  45.00 -60.00   26
 54  \w     93.00 119.00   1.00   10.00    --  109.00  45.00   0.00   26
 55  \w    133.00 174.00   1.00   10.00    --  109.00  61.00-150.00   41
 56  \w     90.00 157.00   1.00   10.00    --  109.00  30.00  30.00   67
 57  \w     91.00 117.00   1.00   10.00    --  109.00  61.00-150.00   26
 58  \w    119.00 144.00   1.00   10.00    --  109.00  30.00  90.00   25
 59  \w    141.00 173.00   1.00   10.00    --  109.00  30.00   0.00   32
 60  \w     78.00 106.00   1.00   10.00    --  109.00 -95.00   0.00   28
 61  \w     57.00  93.00   1.00   10.00    --  109.00 -95.00 120.00   36
 62  \w     41.00  74.00   1.00   10.00    --  109.00-111.00 -60.00   33
 63  \w     92.00 119.00   1.00   10.00    --  109.00  61.00 -30.00   27
 64  \w     89.00 114.00   1.00   10.00    --  109.00  30.00   0.00   25
 65  \w    136.00 162.00   1.00   10.00    --  109.00  30.00-180.00   26
 66  \w     89.00 122.00   1.00   10.00    --  109.00  30.00-180.00   33
 67  \w    144.00 170.00   1.00   10.00    --  109.00  30.00 -90.00   26
 68  \w     92.00 133.00   1.00   10.00    --  109.00  30.00 -30.00   41
 69  \w     88.00 114.00   1.00   10.00    --  109.00  30.00 120.00   26
 70  \w    145.00 176.00   1.00   10.00    --  109.00  30.00 120.00   31
 71  \w     90.00 116.00   1.00   10.00    --  109.00  30.00-150.00   26
 72  \w    100.00 126.00   1.00   10.00    --  109.00  61.00   0.00   26
 73  \w     40.00  70.00   1.00   10.00    --  109.00-111.00-150.00   30
 74  \w     84.00 109.00   1.00   10.00    --  109.00-111.00-150.00   25
 75  \w     41.00  95.00   1.00   10.00    --  109.00-111.00   0.00   54
 76  \w     91.00 125.00   1.00   10.00    --  109.00  30.00-120.00   34
 77  \w    140.00 176.00   1.00   10.00    --  109.00  30.00-120.00   36
 78  \w    113.00 172.00   1.00   10.00    --  109.00 111.00 120.00   59
 79  \w     48.00 103.00   1.00   10.00    --  109.00 -95.00-150.00   55
 80  \w     89.00 128.00   1.00   10.00    --  109.00  30.00 -90.00   39
 81  \w     78.00 117.00   1.00   10.00    --  109.00 -30.00 120.00   39
 82  \w     39.00 107.00   1.00   10.00    --  109.00-111.00  90.00   68
 83  \w     43.00  68.00   1.00   10.00    --  109.00-111.00 120.00   25
 84  \w     80.00 105.00   1.00   10.00    --  109.00-111.00 120.00   25
 85  \w    105.00 173.00   1.00   10.00    --  109.00 111.00 150.00   68
 86  \w     78.00 106.00   1.00   10.00    --  109.00-111.00 -60.00   28
 87  \w    130.00 174.00   1.00   10.00    --  109.00  77.00-180.00   44
 88  \w     81.00 106.00   1.00   10.00    --  109.00 -95.00-180.00   25
 89  \w     92.00 119.00   1.00   10.00    --  109.00  61.00 -60.00   27
 90  \w     40.00  97.00   1.00   10.00    --  109.00 -95.00 150.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            28908
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.081
_diffrn_reflns_theta_min         6.023
_exptl_absorpt_coefficient_mu    15.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+3.4978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3277
_reflns_number_total             3293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_232_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716436
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.480
_shelx_estimated_absorpt_t_min   0.170
_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:
 C12(H12), C13(H13), C16(H16), C14(H14), C15(H15)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              1031
_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
;