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

data_1566917
_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         'C12 H21 As Co O4 P'
_chemical_formula_sum            'C12 H21 As Co O4 P'
_chemical_formula_weight         394.11
_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             2021-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-24 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.19800(10)
_cell_length_b                   14.8986(2)
_cell_length_c                   26.2475(3)
_cell_measurement_reflns_used    21894
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6290
_cell_measurement_theta_min      4.4970
_cell_volume                     3181.45(7)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.989
_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    -52.00 -22.00   1.00    1.50    --  -36.95  19.00 150.00   30
  2  \w    -13.00  27.00   1.00    1.50    --  -36.95  57.00 -60.00   40
  3  \w    -63.00 -27.00   1.00    1.50    --  -36.95  19.00  60.00   36
  4  \w     -7.00  32.00   1.00    1.50    --  -36.95  19.00 150.00   39
  5  \w    -13.00  33.00   1.00    1.50    --  -36.95  19.00  60.00   46
  6  \w    -58.00 -20.00   1.00    1.50    --  -36.95 -38.00  60.00   38
  7  \w     37.00  79.00   1.00    1.50    --   36.95-125.00-120.00   42
  8  \w     46.00  84.00   1.00    1.50    --   36.95  19.00  90.00   38
  9  \w     24.00  53.00   1.00    1.50    --   36.95  19.00 -30.00   29
 10  \w      6.00  31.00   1.00    1.50    --   36.95 -99.00 -90.00   25
 11  \w      8.00  40.00   1.00    1.50    --   36.95  19.00  90.00   32
 12  \w     20.00  52.00   1.00    1.50    --   36.95  57.00  30.00   32
 13  \w     74.00 106.00   1.00    1.50    --   36.95  19.00-150.00   32
 14  \w     23.00  58.00   1.00    1.50    --   36.95  57.00-150.00   35
 15  \w     20.00 104.00   1.00    1.50    --   36.95  57.00  90.00   84
 16  \w     30.00  89.00   1.00    1.50    --   36.95-125.00  90.00   59
 17  \w     51.00  76.00   1.00    1.50    --   36.95 -99.00  90.00   25
 18  \w     19.00  59.00   1.00    1.50    --   36.95 -77.00 -90.00   40
 19  \w    -29.00  -3.00   1.00    1.50    --   36.95 -57.00  60.00   26
 20  \w      7.00  34.00   1.00    1.50    --   36.95 -99.00 -60.00   27
 21  \w     71.00  98.00   1.00    1.50    --   36.95  19.00 -30.00   27
 22  \w     49.00  74.00   1.00    1.50    --   36.95 -99.00 -90.00   25
 23  \w     66.00 103.00   1.00    1.50    --   36.95  57.00-150.00   37
 24  \w     32.00  79.00   1.00    1.50    --   36.95-125.00 -90.00   47
 25  \w      7.00  32.00   1.00    1.50    --   36.95 -99.00  90.00   25
 26  \w     18.00  44.00   1.00    1.50    --   36.95 -57.00  60.00   26
 27  \w     41.00  67.00   1.00    1.50    --   36.95  19.00-150.00   26
 28  \w     93.00 119.00   1.00   10.00    --  111.00 -64.00   0.00   26
 29  \w     48.00  78.00   1.00   10.00    --  111.00 -64.00   0.00   30
 30  \w     62.00 102.00   1.00   10.00    --  111.00 -92.00 -90.00   40
 31  \w     83.00 109.00   1.00   10.00    --  111.00-111.00  90.00   26
 32  \w     99.00 143.00   1.00   10.00    --  111.00  38.00  30.00   44
 33  \w     89.00 151.00   1.00   10.00    --  111.00  25.00  90.00   62
 34  \w     58.00  84.00   1.00   10.00    --  111.00 -77.00  60.00   26
 35  \w     56.00  96.00   1.00   10.00    --  111.00 -92.00 -60.00   40
 36  \w     67.00 106.00   1.00   10.00    --  111.00 -92.00-120.00   39
 37  \w     43.00  89.00   1.00   10.00    --  111.00 -50.00   0.00   46
 38  \w    109.00 137.00   1.00   10.00    --  111.00 -77.00 -30.00   28
 39  \w    101.00 127.00   1.00   10.00    --  111.00 -25.00-180.00   26
 40  \w     42.00 131.00   1.00   10.00    --  111.00 -25.00  90.00   89
 41  \w     62.00  89.00   1.00   10.00    --  111.00 -82.00-151.09   27
 42  \w     56.00  90.00   1.00   10.00    --  111.00 -25.00-180.00   34
 43  \w     84.00 109.00   1.00   10.00    --  111.00-111.00-120.00   25
 44  \w     68.00 106.00   1.00   10.00    --  111.00-111.00-180.00   38
 45  \w     96.00 125.00   1.00   10.00    --  111.00 -38.00-120.00   29
 46  \w     55.00  84.00   1.00   10.00    --  111.00 -77.00 -30.00   29
 47  \w     42.00  88.00   1.00   10.00    --  111.00 -38.00-120.00   46
 48  \w    113.00 138.00   1.00   10.00    --  111.00 -77.00 -60.00   25
 49  \w     59.00 127.00   1.00   10.00    --  111.00 -50.00  60.00   68
 50  \w     45.00 103.00   1.00   10.00    --  111.00 -50.00 150.00   58
 51  \w     68.00  93.00   1.00   10.00    --  111.00 -25.00 120.00   25
 52  \w    129.00 177.00   1.00   10.00    --  111.00  25.00 120.00   48
 53  \w    125.00 176.00   1.00   10.00    --  111.00  64.00 150.00   51
 54  \w     90.00 127.00   1.00   10.00    --  111.00 -77.00  60.00   37
 55  \w     65.00 109.00   1.00   10.00    --  111.00-111.00  30.00   44
 56  \w     44.00  89.00   1.00   10.00    --  111.00 -50.00-150.00   45
 57  \w     59.00 138.00   1.00   10.00    --  111.00 -12.00 150.00   79
 58  \w     47.00  73.00   1.00   10.00    --  111.00 -50.00 -30.00   26
 59  \w     58.00 109.00   1.00   10.00    --  111.00-111.00 120.00   51
 60  \w    104.00 132.00   1.00   10.00    --  111.00  77.00-150.00   28
 61  \w    139.00 165.00   1.00   10.00    --  111.00 111.00-180.00   26
 62  \w    125.00 176.00   1.00   10.00    --  111.00  25.00-150.00   51
 63  \w    102.00 127.00   1.00   10.00    --  111.00 178.00-120.00   25
 64  \w     74.00 100.00   1.00   10.00    --  111.00 -92.00-180.00   26
 65  \w     66.00  91.00   1.00   10.00    --  111.00 178.00-120.00   25
 66  \w    107.00 132.00   1.00   10.00    --  111.00 -77.00  90.00   25
 67  \w     43.00  71.00   1.00   10.00    --  111.00 -38.00  90.00   28
 68  \w     71.00  98.00   1.00   10.00    --  111.00 -77.00  90.00   27
 69  \w     70.00 102.00   1.00   10.00    --  111.00-111.00  60.00   32
 70  \w     69.00  94.00   1.00   10.00    --  111.00 -92.00-150.00   25
 71  \w     84.00 109.00   1.00   10.00    --  111.00-111.00   0.00   25
 72  \w    118.00 143.00   1.00   10.00    --  111.00 111.00 120.00   25
 73  \w    153.00 178.00   1.00   10.00    --  111.00  25.00   0.00   25
 74  \w    123.00 149.00   1.00   10.00    --  111.00  77.00  90.00   26
 75  \w     97.00 123.00   1.00   10.00    --  111.00  25.00   0.00   26
 76  \w     43.00  70.00   1.00   10.00    --  111.00-111.00   0.00   27
 77  \w    103.00 130.00   1.00   10.00    --  111.00  25.00  30.00   27
 78  \w     68.00 134.00   1.00   10.00    --  111.00 -25.00   0.00   66
 79  \w    101.00 127.00   1.00   10.00    --  111.00 -82.00-151.09   26
 80  \w     57.00  83.00   1.00   10.00    --  111.00 -77.00 -60.00   26
 81  \w     74.00  99.00   1.00   10.00    --  111.00 -70.00   5.41   25
 82  \w     74.00  99.00   1.00   10.00    --  111.00 -77.00 150.00   25
 83  \w     83.00 108.00   1.00   10.00    --  111.00 -80.00 -66.60   25
;
_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      -0.0119695000
_diffrn_orient_matrix_UB_12      0.1025870000
_diffrn_orient_matrix_UB_13      0.0057186000
_diffrn_orient_matrix_UB_21      -0.0504881000
_diffrn_orient_matrix_UB_22      0.0087940000
_diffrn_orient_matrix_UB_23      -0.0583051000
_diffrn_orient_matrix_UB_31      -0.1821177000
_diffrn_orient_matrix_UB_32      -0.0091962000
_diffrn_orient_matrix_UB_33      0.0082194000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42721
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.369
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.788
_exptl_absorpt_correction_T_max  0.37651
_exptl_absorpt_correction_T_min  0.29678
_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    1.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Tetramethylsilane'
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.075
_exptl_crystal_size_rad          0.072
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+6.1181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6086
_reflns_number_total             6425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_213_a_scale
_cod_database_code               1566917
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H42As2Co2O8P2
_chemical_oxdiff_usercomment     'pentane at -30'
_reflns_odcompleteness_completeness 99.97
_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:
 C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C2B(H2BA,H2BB,H2BC), C4B(H4BA,H4BB,H4BC), C3(H3A,H3B,H3C),
  C12B(H12D,H12E,H12F), C3B(H3BA,H3BB,H3BC), C2(H2A,H2B,H2C), C9B(H9BA,H9BB,
 H9BC), C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F)
;
_ins_header
;
TITL RMK_213_A_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   8.197976  14.898604  26.247506  90.0000  97.0714  90.0000
ZERR    4.00   0.000093   0.000205   0.000339   0.0000   0.0011   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O P Co As
UNIT 96.00 168.00 32.00 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 2.651
_oxdiff_exptl_absorpt_empirical_full_min 0.615