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

data_1566914
_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           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.2220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.83040(10)
_cell_length_b                   14.2969(2)
_cell_length_c                   11.8460(2)
_cell_measurement_reflns_used    4896
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6700
_cell_measurement_theta_min      5.8850
_cell_volume                     1491.47(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 (Sheldrick, 2015)'
_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 0.996
_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     42.00  68.00   1.00    1.00    --   36.95  57.00-120.00   26
  2  \w     21.00  52.00   1.00    1.00    --   36.95  57.00 -30.00   31
  3  \w      7.00  76.00   1.00    1.00    --   36.95 -99.00-150.00   69
  4  \w     71.00  98.00   1.00    1.00    --   36.95  57.00-120.00   27
  5  \w     11.00  36.00   1.00    1.00    --   36.95 -99.00 150.00   25
  6  \w    -31.00  53.00   1.00    1.00    --   36.95 -38.00  60.00   84
  7  \w     25.00  65.00   1.00    1.00    --   36.95 -99.00  30.00   40
  8  \w     28.00  54.00   1.00    1.00    --   36.95-125.00 120.00   26
  9  \w     57.00 104.00   1.00    1.00    --   36.95  57.00 -30.00   47
 10  \w     71.00  97.00   1.00    2.00    --  111.00-111.00  90.00   26
 11  \w    141.00 171.00   1.00    2.00    --  111.00  38.00-150.00   30
 12  \w     92.00 119.00   1.00    2.00    --  111.00  38.00-150.00   27
 13  \w    102.00 134.00   1.00    2.00    --  111.00  50.00 -90.00   32
 14  \w     48.00 104.00   1.00    2.00    --  111.00 -77.00  90.00   56
 15  \w     41.00  67.00   1.00    2.00    --  111.00-111.00  90.00   26
 16  \w     41.00 126.00   1.00    2.00    --  111.00 -25.00 -90.00   85
 17  \w     70.00 100.00   1.00    2.00    --  111.00-111.00 -90.00   30
 18  \w     77.00 103.00   1.00    2.00    --  111.00 -92.00 -90.00   26
 19  \w     87.00 130.00   1.00    2.00    --  111.00 -38.00-180.00   43
 20  \w     72.00 106.00   1.00    2.00    --  111.00 -92.00 -30.00   34
 21  \w    108.00 134.00   1.00    2.00    --  111.00 -77.00  90.00   26
 22  \w     66.00  99.00   1.00    2.00    --  111.00 178.00 -60.00   33
 23  \w     58.00  91.00   1.00    2.00    --  111.00 -92.00  30.00   33
 24  \w     62.00 106.00   1.00    2.00    --  111.00 178.00-120.00   44
 25  \w     72.00 104.00   1.00    2.00    --  111.00 -64.00-150.00   32
 26  \w    113.00 140.00   1.00    2.00    --  111.00  77.00 120.00   27
 27  \w     42.00  82.00   1.00    2.00    --  111.00 -38.00-180.00   40
 28  \w    146.00 175.00   1.00    2.00    --  111.00  50.00 -90.00   29
 29  \w     46.00  78.00   1.00    2.00    --  111.00 -64.00  30.00   32
 30  \w     62.00 104.00   1.00    2.00    --  111.00 -92.00-180.00   42
 31  \w     69.00  95.00   1.00    2.00    --  111.00 -92.00  90.00   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      -0.0307309000
_diffrn_orient_matrix_UB_12      0.0961159000
_diffrn_orient_matrix_UB_13      -0.0557787000
_diffrn_orient_matrix_UB_21      -0.0098931000
_diffrn_orient_matrix_UB_22      -0.0464312000
_diffrn_orient_matrix_UB_23      -0.1176740000
_diffrn_orient_matrix_UB_31      -0.1719707000
_diffrn_orient_matrix_UB_32      -0.0145386000
_diffrn_orient_matrix_UB_33      0.0069252000
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8025
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.767
_diffrn_reflns_theta_min         4.856
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    32.581
_exptl_absorpt_correction_T_max  0.17197
_exptl_absorpt_correction_T_min  0.07271
_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    2.536
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.046
_exptl_crystal_size_rad          0.061
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0711P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2842
_reflns_number_total             3000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_290_c_yellow_scale
_cod_database_code               1566914
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H24As2Cl4Co2Hg2O4
_chemical_oxdiff_usercomment     'acetone-d6 at -20 '
_shelx_estimated_absorpt_t_max   0.316
_shelx_estimated_absorpt_t_min   0.021
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C7(H7A,H7B,H7C), C0AA(H0AA,H0AB,H0AC), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_ins_header
;
TITL RMK_290_C_yellow_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   8.830438  14.296879  11.845976  90.0000  94.2216  90.0000
ZERR    2.00   0.000106   0.000201   0.000171   0.0000   0.0012   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O Cl Co As Hg
UNIT 40.00 48.00 8.00 8.00 4.00 4.00 4.00
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 2.739
_oxdiff_exptl_absorpt_empirical_full_min 0.625