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

data_1566912
_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         'C10 H12 As Cl2 Co Hg O2'
_chemical_formula_sum            'C10 H12 As Cl2 Co Hg O2'
_chemical_formula_weight         569.54
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-29
_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                90
_cell_angle_beta                 99.340(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1928(3)
_cell_length_b                   14.4745(3)
_cell_length_c                   14.7169(3)
_cell_measurement_reflns_used    5362
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.7590
_cell_measurement_theta_min      4.3660
_cell_volume                     2983.27(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 1.000
_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     51.00  76.00   1.00    1.00    --   36.95 -99.00  60.00   25
  2  \w      8.00  49.00   1.00    1.00    --   36.95 -99.00 -60.00   41
  3  \w     28.00  89.00   1.00    1.00    --   36.95-125.00-120.00   61
  4  \w     51.00  77.00   1.00    1.00    --   36.95-125.00-180.00   26
  5  \w     16.00  64.00   1.00    1.00    --   36.95 -77.00 -60.00   48
  6  \w     26.00  68.00   1.00    1.00    --   36.95  57.00  60.00   42
  7  \w    -14.00  12.00   1.00    1.00    --   36.95 -77.00 -60.00   26
  8  \w     59.00  97.00   1.00    1.00    --   36.95  57.00 -90.00   38
  9  \w     21.00  92.00   1.00    1.00    --   36.95  57.00 120.00   71
 10  \w     43.00 106.00   1.00    4.00    --  111.00 -92.00 120.00   63
 11  \w    113.00 139.00   1.00    4.00    --  111.00  25.00  90.00   26
 12  \w     91.00 162.00   1.00    4.00    --  111.00  64.00-180.00   71
 13  \w     47.00  78.00   1.00    4.00    --  111.00 -77.00 -30.00   31
 14  \w     42.00  85.00   1.00    4.00    --  111.00 -38.00-150.00   43
 15  \w     43.00 125.00   1.00    4.00    --  111.00 -50.00 -30.00   82
 16  \w     97.00 124.00   1.00    4.00    --  111.00  50.00   0.00   27
 17  \w     73.00 100.00   1.00    4.00    --  111.00 -92.00  30.00   27
 18  \w     89.00 114.00   1.00    4.00    --  111.00 -77.00-120.00   25
 19  \w     44.00  78.00   1.00    4.00    --  111.00 -77.00-120.00   34
 20  \w    106.00 158.00   1.00    4.00    --  111.00  77.00 150.00   52
 21  \w     59.00  89.00   1.00    4.00    --  111.00-111.00-120.00   30
 22  \w     72.00  98.00   1.00    4.00    --  111.00-111.00-150.00   26
 23  \w    140.00 177.00   1.00    4.00    --  111.00  55.00  73.00   37
 24  \w    112.00 178.00   1.00    4.00    --  111.00 111.00   0.00   66
 25  \w     87.00 119.00   1.00    4.00    --  111.00 -38.00-150.00   32
 26  \w     59.00  95.00   1.00    4.00    --  111.00 -92.00 -60.00   36
 27  \w     77.00 107.00   1.00    4.00    --  111.00-111.00 -60.00   30
 28  \w    106.00 133.00   1.00    4.00    --  111.00  77.00  60.00   27
 29  \w    106.00 131.00   1.00    4.00    --  111.00  38.00 150.00   25
 30  \w     99.00 150.00   1.00    4.00    --  111.00  38.00 120.00   51
;
_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      0.0457088000
_diffrn_orient_matrix_UB_12      0.0710111000
_diffrn_orient_matrix_UB_13      -0.0575346000
_diffrn_orient_matrix_UB_21      0.0899502000
_diffrn_orient_matrix_UB_22      0.0022842000
_diffrn_orient_matrix_UB_23      0.0742415000
_diffrn_orient_matrix_UB_31      0.0436097000
_diffrn_orient_matrix_UB_32      -0.0792930000
_diffrn_orient_matrix_UB_33      -0.0494204000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8233
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.861
_diffrn_reflns_theta_min         4.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    32.578
_exptl_absorpt_correction_T_max  0.10591
_exptl_absorpt_correction_T_min  0.02226
_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    2.536
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.118
_exptl_crystal_size_rad          0.099
_refine_diff_density_max         4.249
_refine_diff_density_min         -2.610
_refine_diff_density_rms         0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0660
_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^)+(0.1383P)^2^+5.1383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.1782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2887
_reflns_number_total             3020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_209_c_orange_scale
_cod_original_cell_volume        2983.26(11)
_cod_database_code               1566912
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H24As2Cl4Co2Hg2O4
_chemical_oxdiff_usercomment     'acetone-d6 at -20 '
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              22437
_shelx_hkl_checksum              21623
_ins_header
;
TITL RMK_209_C_orange_scale in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  14.192832  14.474476  14.716885  90.0000  99.3401  90.0000
ZERR    4.00   0.000298   0.000294   0.000292   0.0000   0.0019   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H O Cl Co As Hg
UNIT 80.00 96.00 16.00 16.00 8.00 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 3.396
_oxdiff_exptl_absorpt_empirical_full_min 0.481