Arsolyl-Supported Intermetallic Dative Bonding
Kirk, Ryan M.; Hill, Anthony; Chemical Science  (2022) –; doi:10.1039/D2SC01200F

data_1566911
_publ_section_title
;
 Arsolyl-Supported Intermetallic Dative Bonding
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01200F
_journal_year                    2022
_chemical_formula_moiety         'C18 H12 As Co O2'
_chemical_formula_sum            'C18 H12 As Co O2'
_chemical_formula_weight         394.13
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-26 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.23470(10)
_cell_length_b                   17.27710(10)
_cell_length_c                   7.83560(10)
_cell_measurement_reflns_used    11011
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6750
_cell_measurement_theta_min      4.6800
_cell_volume                     1520.91(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_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      150.01(10)
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -43.00 -18.00   1.00    5.00    --   16.00 134.00 115.30   25
  2  \w    -45.00 -20.00   1.00    5.00    --   24.00 150.00 -44.84   25
  3  \w    -97.00 -52.00   1.00    5.00    --  -36.95 -38.00-180.00   45
  4  \w    -68.00 -20.00   1.00    5.00    --  -36.95 -38.00 -30.00   48
  5  \w    -46.00  12.00   1.00    5.00    --  -36.95  57.00   0.00   58
  6  \w   -104.00 -73.00   1.00    5.00    --  -36.95 -38.00 -30.00   31
  7  \w    -49.00 -19.00   1.00    5.00    --  -36.95 -38.00-180.00   30
  8  \w     38.00  73.00   1.00    5.00    --   36.95 -99.00-180.00   35
  9  \w      6.00  71.00   1.00    5.00    --   36.95 -99.00  90.00   65
 10  \w      6.00  34.00   1.00    5.00    --   36.95 -99.00-180.00   28
 11  \w      5.00  30.00   1.00    5.00    --   36.95  87.00 145.01   25
 12  \w      3.00  28.00   1.00    5.00    --   36.95  90.00  43.98   25
 13  \w    -20.00  64.00   1.00    5.00    --   36.95 -77.00-180.00   84
 14  \w      6.00  38.00   1.00    5.00    --   36.95 -99.00  30.00   32
 15  \w     11.00  74.00   1.00    5.00    --   36.95 -99.00 -60.00   63
 16  \w     10.00  60.00   1.00    5.00    --   36.95 -99.00  60.00   50
 17  \w     10.00  35.00   1.00    5.00    --   40.00  82.00 -44.08   25
 18  \w     16.00  41.00   1.00    5.00    --   44.00  79.00  52.18   25
 19  \w     16.00  41.00   1.00    5.00    --   44.00  79.00-130.10   25
 20  \w     16.00  41.00   1.00    5.00    --   44.00  79.00 149.66   25
 21  \w     16.00  41.00   1.00    5.00    --   44.00  79.00   8.36   25
 22  \w     84.00 115.00   1.00    5.00    --   48.00  74.00 -96.83   31
 23  \w     28.00  55.00   1.00    5.00    --   48.00  74.00 -96.83   27
 24  \w     85.00 112.00   1.00    5.00    --   52.00  72.00  26.32   27
 25  \w     28.00  53.00   1.00    5.00    --   52.00  74.00-170.90   25
 26  \w     27.00  72.00   1.00    5.00    --   52.00  74.00 -26.88   45
 27  \w     29.00  67.00   1.00    5.00    --   52.00  72.00  26.32   38
 28  \w     29.00  54.00   1.00    5.00    --   52.00  72.00 122.36   25
 29  \w     92.00 117.00   1.00    5.00    --   52.00  72.00-137.72   25
 30  \w     65.00 119.00   1.00    5.00    --   52.00  74.00  83.78   54
 31  \w     27.00  53.00   1.00    5.00    --   52.00  74.00  83.78   26
 32  \w     93.00 119.00   1.00    5.00    --   52.00  72.00 122.36   26
 33  \w     92.00 118.00   1.00    5.00    --   52.00  74.00-170.90   26
 34  \w     28.00  77.00   1.00    5.00    --   52.00  72.00-137.72   49
 35  \w     82.00 108.00   1.00    5.00    --   52.00  74.00 -26.88   26
 36  \w     32.00  70.00   1.00    5.00    --   56.00  72.00 -81.01   38
 37  \w     97.00 123.00   1.00    5.00    --   56.00  72.00 -81.01   26
 38  \w     82.00 122.00   1.00    5.00    --   56.00  74.00 149.86   40
 39  \w     31.00  78.00   1.00    5.00    --   56.00  74.00 149.86   47
 40  \w     55.00  87.00   1.00   18.00    --   80.00  73.00  25.68   32
 41  \w    113.00 146.00   1.00   18.00    --   80.00  73.00  25.68   33
 42  \w     94.00 128.00   1.00   18.00    --  111.00  50.00 150.00   34
 43  \w     94.00 134.00   1.00   18.00    --  111.00  50.00-120.00   40
 44  \w    141.00 167.00   1.00   18.00    --  111.00  38.00 -30.00   26
 45  \w     92.00 118.00   1.00   18.00    --  111.00  38.00 -30.00   26
 46  \w     94.00 124.00   1.00   18.00    --  111.00  50.00 -30.00   30
 47  \w     94.00 157.00   1.00   18.00    --  111.00  50.00  60.00   63
 48  \w     91.00 170.00   1.00   18.00    --  111.00  64.00  90.00   79
 49  \w     45.00 103.00   1.00   18.00    --  111.00 -92.00  60.00   58
 50  \w     93.00 120.00   1.00   18.00    --  111.00  64.00   0.00   27
 51  \w     79.00 127.00   1.00   18.00    --  111.00 -50.00 -60.00   48
 52  \w    111.00 136.00   1.00   18.00    --  111.00 -25.00 -30.00   25
 53  \w    123.00 155.00   1.00   18.00    --  111.00  64.00   0.00   32
 54  \w     80.00 106.00   1.00   18.00    --  111.00 -25.00 -30.00   26
 55  \w     46.00  75.00   1.00   18.00    --  111.00 -25.00 -30.00   29
 56  \w     86.00 160.00   1.00   18.00    --  111.00  25.00-120.00   74
 57  \w     81.00 107.00   1.00   18.00    --  111.00-123.00 176.00   26
 58  \w     94.00 153.00   1.00   18.00    --  111.00  50.00 -90.00   59
 59  \w    135.00 161.00   1.00   18.00    --  111.00  38.00 150.00   26
 60  \w    137.00 163.00   1.00   18.00    --  111.00  50.00-180.00   26
 61  \w     92.00 118.00   1.00   18.00    --  111.00  38.00 150.00   26
 62  \w     91.00 123.00   1.00   18.00    --  111.00  64.00  30.00   32
 63  \w     95.00 120.00   1.00   18.00    --  111.00  50.00-180.00   25
 64  \w    144.00 177.00   1.00   18.00    --  111.00  50.00 -60.00   33
 65  \w    108.00 156.00   1.00   18.00    --  111.00 111.00 -90.00   48
 66  \w     94.00 130.00   1.00   18.00    --  111.00  50.00 -60.00   36
 67  \w     67.00 121.00   1.00   18.00    --  111.00 -64.00  60.00   54
 68  \w     91.00 176.00   1.00   18.00    --  111.00  64.00-120.00   85
 69  \w     94.00 133.00   1.00   18.00    --  111.00  50.00   0.00   39
 70  \w    137.00 177.00   1.00   18.00    --  111.00  50.00 120.00   40
 71  \w     70.00 109.00   1.00   18.00    --  111.00-111.00-150.00   39
 72  \w     92.00 124.00   1.00   18.00    --  111.00  64.00 -30.00   32
 73  \w     94.00 138.00   1.00   18.00    --  111.00  50.00  90.00   44
 74  \w     42.00  68.00   1.00   18.00    --  111.00-111.00-150.00   26
 75  \w     94.00 120.00   1.00   18.00    --  111.00  50.00 120.00   26
 76  \w     88.00 113.00   1.00   18.00    --  111.00 -50.00  60.00   25
 77  \w     91.00 125.00   1.00   18.00    --  111.00  64.00-150.00   34
 78  \w     44.00  95.00   1.00   18.00    --  111.00 -92.00   0.00   51
 79  \w     44.00  85.00   1.00   18.00    --  111.00 -50.00  60.00   41
 80  \w    140.00 166.00   1.00   18.00    --  111.00  50.00  30.00   26
 81  \w    148.00 175.00   1.00   18.00    --  111.00  64.00 -30.00   27
 82  \w     91.00 117.00   1.00   18.00    --  111.00  64.00  60.00   26
 83  \w     96.00 122.00   1.00   18.00    --  111.00  50.00  30.00   26
 84  \w     74.00 109.00   1.00   18.00    --  111.00-111.00  60.00   35
 85  \w     90.00 131.00   1.00   18.00    --  111.00 178.00  90.00   41
 86  \w     87.00 129.00   1.00   18.00    --  111.00-150.00  14.00   42
 87  \w     92.00 117.00   1.00   18.00    --  111.00  64.00 -90.00   25
 88  \w     46.00  96.00   1.00   18.00    --  111.00 -50.00   0.00   50
 89  \w     91.00 117.00   1.00   18.00    --  111.00  64.00-180.00   26
 90  \w     50.00 130.00   1.00   18.00    --  111.00 -38.00-180.00   80
 91  \w     86.00 113.00   1.00   18.00    --  111.00  25.00 -60.00   27
 92  \w     45.00 133.00   1.00   18.00    --  111.00 -25.00 150.00   88
 93  \w     96.00 136.00   1.00   18.00    --  111.00  38.00 -60.00   40
 94  \w     97.00 129.00   1.00   18.00    --  111.00  38.00  60.00   32
 95  \w     82.00 107.00   1.00   18.00    --  111.00-111.00   0.00   25
 96  \w    125.00 173.00   1.00   18.00    --  111.00  64.00 150.00   48
 97  \w     71.00 123.00   1.00   18.00    --  111.00 -81.00-179.65   52
 98  \w     42.00  77.00   1.00   18.00    --  111.00-111.00   0.00   35
 99  \w     47.00 124.00   1.00   18.00    --  111.00 -64.00-180.00   77
100  \w     91.00 117.00   1.00   18.00    --  111.00  64.00 150.00   26
101  \w     97.00 124.00   1.00   18.00    --  111.00  50.00-150.00   27
102  \w     87.00 114.00   1.00   18.00    --  111.00  25.00 120.00   27
;
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            27398
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.954
_diffrn_reflns_theta_min         4.695
_exptl_absorpt_coefficient_mu    11.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       needle
_exptl_crystal_F_000             784
_exptl_crystal_recrystallization_method 'Benzene/hexane at -20'
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1259 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0385P)^2^+3.8902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2974
_reflns_number_total             3057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_129_b_scale
_cod_database_code               1566911
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C5)
3.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C18(H18), C9(H9), C17(H17), C11(H11), C12(H12), C16(H16),
 C14(H14), C15(H15)
;
_shelx_res_checksum              48010
_shelx_hkl_checksum              71895
_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
;