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

data_1566910
_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         'C30 H20 As Co O2'
_chemical_formula_sum            'C30 H20 As Co O2'
_chemical_formula_weight         546.31
_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
_audit_creation_date             2021-05-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-24 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                76.116(4)
_cell_angle_beta                 84.418(4)
_cell_angle_gamma                78.076(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0514(4)
_cell_length_b                   10.5907(5)
_cell_length_c                   12.8357(6)
_cell_measurement_reflns_used    6567
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6920
_cell_measurement_theta_min      5.9740
_cell_volume                     1167.24(10)
_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 (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 0.994
_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    -62.00 -35.00   1.00    1.00    --  -36.95 125.00-150.00   27
  2  \w     49.00  87.00   1.00    1.00    --   36.95-125.00 -90.00   38
  3  \w    -16.00  54.00   1.00    1.00    --   36.95 -57.00   0.00   70
  4  \w     19.00 105.00   1.00    1.00    --   36.95  38.00-180.00   86
  5  \w     46.00  72.00   1.00    1.00    --   36.95  57.00  30.00   26
  6  \w    -18.00  64.00   1.00    1.00    --   36.95 -77.00 -30.00   82
  7  \w     24.00  94.00   1.00    1.00    --   36.95  38.00-120.00   70
  8  \w     50.00  86.00   1.00    1.00    --   36.95-125.00 150.00   36
  9  \w     28.00  55.00   1.00    1.00    --   36.95  57.00 -60.00   27
 10  \w     43.00 103.00   1.00    1.00    --   36.95  57.00  90.00   60
 11  \w    -14.00  58.00   1.00    1.00    --   36.95 -77.00-120.00   72
 12  \w     58.00  92.00   1.00    1.00    --   36.95  57.00 -60.00   34
 13  \w     23.00  50.00   1.00    1.00    --   36.95 -57.00  90.00   27
 14  \w     56.00 103.00   1.00    3.00    --  111.00 -92.00   0.00   47
 15  \w     42.00 130.00   1.00    3.00    --  111.00 -38.00 150.00   88
 16  \w    125.00 152.00   1.00    3.00    --  111.00  77.00 -30.00   27
 17  \w     95.00 121.00   1.00    3.00    --  111.00 -64.00  60.00   26
 18  \w    101.00 137.00   1.00    3.00    --  111.00  50.00 -90.00   36
 19  \w     43.00  68.00   1.00    3.00    --  111.00 -92.00 -90.00   25
 20  \w     43.00 124.00   1.00    3.00    --  111.00 -50.00 -60.00   81
 21  \w    106.00 141.00   1.00    3.00    --  111.00  77.00-150.00   35
 22  \w     42.00 109.00   1.00    3.00    --  111.00-111.00 -30.00   67
 23  \w     90.00 128.00   1.00    3.00    --  111.00 -50.00 -30.00   38
 24  \w    106.00 153.00   1.00    3.00    --  111.00 111.00  90.00   47
 25  \w     64.00 157.00   1.00    3.00    --  111.00 -12.00   0.00   93
 26  \w     41.00  77.00   1.00    3.00    --  111.00-111.00-150.00   36
 27  \w     81.00 107.00   1.00    3.00    --  111.00-111.00 150.00   26
 28  \w     41.00  75.00   1.00    3.00    --  111.00-111.00 150.00   34
 29  \w     41.00  70.00   1.00    3.00    --  111.00 -25.00   0.00   29
 30  \w     81.00 106.00   1.00    3.00    --  111.00 -25.00   0.00   25
 31  \w    112.00 137.00   1.00    3.00    --  111.00 -77.00-150.00   25
 32  \w     94.00 123.00   1.00    3.00    --  111.00 -38.00  30.00   29
 33  \w    148.00 174.00   1.00    3.00    --  111.00  25.00  60.00   26
 34  \w     83.00 109.00   1.00    3.00    --  111.00-111.00-120.00   26
 35  \w     95.00 123.00   1.00    3.00    --  111.00  25.00  60.00   28
 36  \w     61.00  89.00   1.00    3.00    --  111.00 -77.00-150.00   28
 37  \w     96.00 122.00   1.00    3.00    --  111.00 -50.00   0.00   26
 38  \w     72.00  98.00   1.00    3.00    --  111.00 -64.00 -60.00   26
 39  \w     43.00 102.00   1.00    3.00    --  111.00 -92.00  90.00   59
 40  \w    103.00 158.00   1.00    3.00    --  111.00  77.00 -90.00   55
 41  \w     63.00  94.00   1.00    3.00    --  111.00 178.00 -60.00   31
 42  \w    100.00 126.00   1.00    3.00    --  111.00 -77.00 120.00   26
 43  \w     73.00 101.00   1.00    3.00    --  111.00 -92.00 -60.00   28
 44  \w     77.00 108.00   1.00    3.00    --  111.00-111.00  60.00   31
 45  \w     52.00  77.00   1.00    3.00    --  111.00-111.00-120.00   25
 46  \w     69.00 117.00   1.00    3.00    --  111.00  12.00-120.00   48
 47  \w     83.00 109.00   1.00    3.00    --  111.00-111.00  90.00   26
 48  \w    102.00 141.00   1.00    3.00    --  111.00  50.00   0.00   39
 49  \w     94.00 126.00   1.00    3.00    --  111.00 -64.00-180.00   32
 50  \w     42.00  67.00   1.00    3.00    --  111.00 -25.00 -60.00   25
 51  \w     60.00 109.00   1.00    3.00    --  111.00-114.00-156.31   49
;
_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      0.0114144000
_diffrn_orient_matrix_UB_12      -0.1513553000
_diffrn_orient_matrix_UB_13      0.0326203000
_diffrn_orient_matrix_UB_21      0.1670429000
_diffrn_orient_matrix_UB_22      -0.0195159000
_diffrn_orient_matrix_UB_23      -0.0409399000
_diffrn_orient_matrix_UB_31      0.0479941000
_diffrn_orient_matrix_UB_32      -0.0011339000
_diffrn_orient_matrix_UB_33      0.1121780000
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.772
_diffrn_reflns_theta_min         3.552
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.541
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/n-hexane'
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0616P)^2^+0.2670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4506
_reflns_number_total             4691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_124_scale1
_cod_database_code               1566910
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H20 As1 Co1 O2'
_chemical_oxdiff_usercomment     'benzene/hexane at -20'
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.212
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C18(H18), C30(H30), C12(H12), C27(H27), C24(H24), C9(H9), C8(H8),
 C20(H20), C21(H21), C29(H29), C14(H14), C28(H28), C22(H22), C15(H15), C10(H10),
  C26(H26), C17(H17), C23(H23), C16(H16)
;
_ins_header
;
TITL RMK_124_scale1 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.051355  10.590676  12.835658  76.1159  84.4183  78.0764
ZERR    2.00   0.000409   0.000501   0.000571   0.0039   0.0037   0.0039
LATT  1
SFAC C H O Co As
UNIT 60.00 40.00 4.00 2.00 2.00
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 1.484
_oxdiff_exptl_absorpt_empirical_full_min 0.706