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

data_1566916
_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
'0.25(C52 H48 As4 Au3 Co4 F10 O8), 0.5(Au C12 F10), 0.25(C20 H24 As2 Au Co2 O4), 0.25(C32 H24 As2 Au2 Co2 F10 O4)'
_chemical_formula_sum            'C32 H24 As2 Au2 Co2 F10 O4'
_chemical_formula_weight         1324.14
_chemical_properties_physical    Air-sensitive
_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             2021-12-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-24 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                100.2830(10)
_cell_angle_beta                 104.7800(10)
_cell_angle_gamma                91.0780(10)
_cell_formula_units_Z            8
_cell_length_a                   15.12080(10)
_cell_length_b                   21.7675(2)
_cell_length_c                   23.8537(2)
_cell_measurement_reflns_used    74244
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.0070
_cell_measurement_theta_min      3.8480
_cell_volume                     7452.43(11)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  32.00   1.00    2.00    --  -36.64  38.00-120.00   87
  2  \w    -85.00  -7.00   1.00    2.00    --  -36.64 -19.00  30.00   78
  3  \w    -56.00  27.00   1.00    2.00    --  -36.64  38.00 120.00   83
  4  \w    -46.00  27.00   1.00    2.00    --  -36.64  38.00  30.00   73
  5  \w     18.00 104.00   1.00    2.00    --   36.64  38.00-120.00   86
  6  \w      3.00  29.00   1.00    2.00    --   36.64  90.00 -47.63   26
  7  \w    -20.00  35.00   1.00    2.00    --   36.64 -77.00 -60.00   55
  8  \w    -19.00  26.00   1.00    2.00    --   36.64 -77.00 150.00   45
  9  \w      4.00  30.00   1.00    2.00    --   36.64  89.00 113.26   26
 10  \w     43.00  89.00   1.00    2.00    --   36.64-125.00 150.00   46
 11  \w     18.00  92.00   1.00    2.00    --   36.64  38.00 -30.00   74
 12  \w      4.00  30.00   1.00    2.00    --   36.64  89.00-111.76   26
 13  \w      5.00  30.00   1.00    2.00    --   36.64  85.00 -69.85   25
 14  \w     19.00  90.00   1.00    2.00    --   36.64  38.00  30.00   71
 15  \w     11.00  40.00   1.00    2.00    --   36.64  77.00-120.57   29
 16  \w     15.00  42.00   1.00    2.00    --   36.64  78.00  28.60   27
 17  \w      9.00  42.00   1.00    2.00    --   36.64  80.00 170.34   33
 18  \w     22.00  89.00   1.00    2.00    --   36.64  57.00  90.00   67
 19  \w     50.00  77.00   1.00    2.00    --   36.64-125.00  30.00   27
 20  \w     35.00  60.00   1.00    2.00    --   36.64 -77.00 150.00   25
 21  \w     22.00  87.00   1.00    2.00    --   36.64  72.00 146.31   65
 22  \w     21.00  76.00   1.00    2.00    --   36.64 -99.00 -90.00   55
 23  \w      4.00  30.00   1.00    2.00    --   36.64  89.00  74.87   26
 24  \w     14.00  45.00   1.00    2.00    --   36.64  70.00 -17.95   31
 25  \w    136.00 162.00   1.00   12.00    --  109.00  30.00  90.00   26
 26  \w     42.00  93.00   1.00   12.00    --  109.00-111.00  60.00   51
 27  \w    149.00 174.00   1.00   12.00    --  109.00  61.00 -60.00   25
 28  \w     89.00 122.00   1.00   12.00    --  109.00  30.00  90.00   33
 29  \w     91.00 117.00   1.00   12.00    --  109.00  61.00-150.00   26
 30  \w    139.00 176.00   1.00   12.00    --  109.00  61.00-150.00   37
 31  \w     82.00 122.00   1.00   12.00    --  109.00 -49.00-151.05   40
 32  \w     91.00 117.00   1.00   12.00    --  109.00  61.00 -60.00   26
 33  \w     44.00 107.00   1.00   12.00    --  109.00-111.00  30.00   63
 34  \w    136.00 166.00   1.00   12.00    --  109.00  30.00 120.00   30
 35  \w     88.00 116.00   1.00   12.00    --  109.00  30.00 120.00   28
 36  \w     92.00 125.00   1.00   12.00    --  109.00  45.00  30.00   33
 37  \w     56.00  94.00   1.00   12.00    --  109.00-111.00 120.00   38
 38  \w     78.00 104.00   1.00   12.00    --  109.00 -95.00-150.00   26
 39  \w     41.00  67.00   1.00   12.00    --  109.00 -49.00-151.05   26
 40  \w     42.00  68.00   1.00   12.00    --  109.00 -95.00-150.00   26
 41  \w     92.00 133.00   1.00   12.00    --  109.00  45.00 150.00   41
 42  \w    124.00 150.00   1.00   12.00    --  109.00  30.00   0.00   26
 43  \w     92.00 137.00   1.00   12.00    --  109.00  45.00-120.00   45
 44  \w    133.00 175.00   1.00   12.00    --  109.00  61.00-120.00   42
 45  \w     92.00 118.00   1.00   12.00    --  109.00  45.00 -60.00   26
 46  \w    138.00 172.00   1.00   12.00    --  109.00  45.00 -60.00   34
 47  \w     92.00 136.00   1.00   12.00    --  109.00  45.00 -90.00   44
 48  \w    109.00 163.00   1.00   12.00    --  109.00 111.00 -30.00   54
 49  \w     92.00 124.00   1.00   12.00    --  109.00  45.00  90.00   32
 50  \w     92.00 144.00   1.00   12.00    --  109.00  45.00-150.00   52
 51  \w    131.00 173.00   1.00   12.00    --  109.00  61.00-180.00   42
 52  \w     92.00 134.00   1.00   12.00    --  109.00  45.00 120.00   42
 53  \w     92.00 118.00   1.00   12.00    --  109.00  45.00 -30.00   26
 54  \w     92.00 124.00   1.00   12.00    --  109.00  45.00  60.00   32
 55  \w    142.00 177.00   1.00   12.00    --  109.00  45.00  60.00   35
 56  \w     92.00 127.00   1.00   12.00    --  109.00  45.00   0.00   35
 57  \w     92.00 126.00   1.00   12.00    --  109.00  45.00-180.00   34
 58  \w    135.00 176.00   1.00   12.00    --  109.00  45.00-180.00   41
 59  \w     40.00 109.00   1.00   12.00    --  109.00-111.00-150.00   69
 60  \w     91.00 117.00   1.00   12.00    --  109.00  61.00-120.00   26
 61  \w     91.00 117.00   1.00   12.00    --  109.00  61.00-180.00   26
 62  \w     91.00 117.00   1.00   12.00    --  109.00  61.00  90.00   26
 63  \w    131.00 176.00   1.00   12.00    --  109.00  30.00 -30.00   45
 64  \w    140.00 165.00   1.00   12.00    --  109.00  61.00 -30.00   25
 65  \w    131.00 171.00   1.00   12.00    --  109.00  61.00  30.00   40
 66  \w     98.00 135.00   1.00   12.00    --  109.00 -82.00-128.87   37
 67  \w     91.00 117.00   1.00   12.00    --  109.00  61.00 -30.00   26
 68  \w     88.00 118.00   1.00   12.00    --  109.00  30.00  30.00   30
 69  \w     91.00 120.00   1.00   12.00    --  109.00  61.00  30.00   29
 70  \w     88.00 149.00   1.00   12.00    --  109.00  30.00-120.00   61
 71  \w    131.00 161.00   1.00   12.00    --  109.00  30.00 -90.00   30
 72  \w     42.00  94.00   1.00   12.00    --  109.00 -95.00 120.00   52
 73  \w     88.00 115.00   1.00   12.00    --  109.00  30.00 -90.00   27
 74  \w    132.00 176.00   1.00   12.00    --  109.00  61.00   0.00   44
 75  \w     88.00 120.00   1.00   12.00    --  109.00  30.00 150.00   32
 76  \w    147.00 173.00   1.00   12.00    --  109.00  30.00  30.00   26
 77  \w     88.00 151.00   1.00   12.00    --  109.00  30.00-180.00   63
 78  \w     90.00 117.00   1.00   12.00    --  109.00  30.00 -30.00   27
 79  \w    151.00 176.00   1.00   12.00    --  109.00  61.00  60.00   25
 80  \w     90.00 123.00   1.00   12.00    --  109.00  30.00  60.00   33
 81  \w    139.00 165.00   1.00   12.00    --  109.00  30.00  60.00   26
 82  \w     43.00  75.00   1.00   12.00    --  109.00-111.00   0.00   32
 83  \w     84.00 109.00   1.00   12.00    --  109.00-111.00   0.00   25
 84  \w     89.00 116.00   1.00   12.00    --  109.00  30.00 -60.00   27
 85  \w     91.00 117.00   1.00   12.00    --  109.00  61.00  60.00   26
 86  \w     89.00 118.00   1.00   12.00    --  109.00  30.00   0.00   29
 87  \w     91.00 117.00   1.00   12.00    --  109.00  61.00   0.00   26
 88  \w     41.00  90.00   1.00   12.00    --  109.00 -45.00 -30.00   49
 89  \w    101.00 126.00   1.00   12.00    --  109.00 -45.00 -30.00   25
 90  \w     40.00 109.00   1.00   12.00    --  109.00-111.00-180.00   69
 91  \w     89.00 116.00   1.00   12.00    --  109.00  30.00-150.00   27
 92  \w     40.00 109.00   1.00   12.00    --  109.00-111.00  90.00   69
 93  \w    124.00 175.00   1.00   12.00    --  109.00  61.00 -90.00   51
 94  \w     43.00 109.00   1.00   12.00    --  109.00-111.00 -60.00   66
 95  \w    142.00 172.00   1.00   12.00    --  109.00  61.00 120.00   30
 96  \w    143.00 168.00   1.00   12.00    --  109.00  61.00 150.00   25
 97  \w     91.00 117.00   1.00   12.00    --  109.00  61.00 120.00   26
 98  \w    127.00 174.00   1.00   12.00    --  109.00  61.00  90.00   47
 99  \w     91.00 117.00   1.00   12.00    --  109.00  61.00 150.00   26
100  \w     42.00  68.00   1.00   12.00    --  109.00 -77.00 120.00   26
101  \w     93.00 128.00   1.00   12.00    --  109.00 -77.00 120.00   35
102  \w     91.00 118.00   1.00   12.00    --  109.00  61.00 -90.00   27
103  \w     43.00  85.00   1.00   12.00    --  109.00 -82.00-128.87   42
;
_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      0.0316064000
_diffrn_orient_matrix_UB_12      0.0004953000
_diffrn_orient_matrix_UB_13      -0.0564259000
_diffrn_orient_matrix_UB_21      0.0998875000
_diffrn_orient_matrix_UB_22      -0.0045962000
_diffrn_orient_matrix_UB_23      0.0346808000
_diffrn_orient_matrix_UB_31      -0.0133227000
_diffrn_orient_matrix_UB_32      -0.0719458000
_diffrn_orient_matrix_UB_33      -0.0155304000
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            149532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.147
_diffrn_reflns_theta_min         3.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.075
_exptl_absorpt_correction_T_max  0.20750
_exptl_absorpt_correction_T_min  0.10891
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_description       needle
_exptl_crystal_F_000             4928
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/diethyl ether'
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.068
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1905
_refine_ls_number_reflns         29642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+3.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26210
_reflns_number_total             29642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_209_d_scale
_cod_database_code               1566916
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H24 As2 Au2 Co2 F10 O4'
_chemical_oxdiff_usercomment     'DCM/SiMe4 at -20 '
_reflns_odcompleteness_completeness 97.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.83
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C20B(H20J,H20K,H20L), C20A(H20G,H20H,H20I), C20C(H20A,H20B,H20C), C17B(H17J,
 H17K,H17L), C10C(H10A,H10B,H10C), C11C(H11A,H11B,H11C), C9B(H9BA,H9BB,H9BC),
 C17C(H17A,H17B,H17C), C19C(H19A,H19B,H19C), C20D(H20D,H20E,H20F), C17A(H17G,
 H17H,H17I), C18C(H18A,H18B,H18C), C12B(H12J,H12K,H12L), C17D(H17D,H17E,H17F),
 C18A(H18G,H18H,H18I), C19B(H19J,H19K,H19L), C18B(H18J,H18K,H18L), C11A(H11G,
 H11H,H11I), C9A(H9AA,H9AB,H9AC), C10A(H10G,H10H,H10I), C12C(H12A,H12B,H12C),
 C12A(H12G,H12H,H12I), C19A(H19G,H19H,H19I), C9C(H9CA,H9CB,H9CC), C12D(H12D,
 H12E,H12F), C9D(H9DA,H9DB,H9DC), C19D(H19D,H19E,H19F), C18D(H18D,H18E,H18F),
 C10B(H10J,H10K,H10L), C11B(H11J,H11K,H11L), C10D(H10D,H10E,H10F), C11D(H11D,
 H11E,H11F)
;
_shelx_res_checksum              57546
_shelx_hkl_checksum              21225
_ins_header
;
TITL RMK_209_D_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  15.120766  21.767457  23.853686 100.2834 104.7802  91.0781
ZERR    8.00   0.000108   0.000176   0.000174   0.0006   0.0006   0.0006
LATT  1
SFAC C H O F Co As Au
UNIT 256.00 192.00 32.00 80.00 16.00 16.00 16.00
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 5.472
_oxdiff_exptl_absorpt_empirical_full_min 0.649