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

data_1566915
_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         'C16 H33 As Co O4 P Si2'
_chemical_formula_sum            'C16 H33 As Co O4 P Si2'
_chemical_formula_weight         510.42
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-15
_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                 90.3000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.93850(10)
_cell_length_b                   19.9045(2)
_cell_length_c                   15.36370(10)
_cell_measurement_reflns_used    17302
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6610
_cell_measurement_theta_min      5.7250
_cell_volume                     2427.61(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 (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 0.999
_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     57.00  88.00   1.00    3.00    --   36.95  38.00  30.00   31
  2  \w     15.00  65.00   1.00    3.00    --   36.95 -99.00  60.00   50
  3  \w     21.00  66.00   1.00    3.00    --   36.95  38.00 -60.00   45
  4  \w      3.00  29.00   1.00    3.00    --   36.95 -57.00 150.00   26
  5  \w     20.00  46.00   1.00    3.00    --   36.95  38.00  30.00   26
  6  \w     53.00  98.00   1.00    3.00    --   36.95  57.00 120.00   45
  7  \w     81.00 106.00   1.00    3.00    --   36.95  38.00 -60.00   25
  8  \w     46.00 101.00   1.00    3.00    --   36.95  19.00-120.00   55
  9  \w      4.00 106.00   1.00    3.00    --   36.95   0.00  60.00  102
 10  \w    -17.00  16.00   1.00    3.00    --   36.95 -77.00 -60.00   33
 11  \w     28.00  89.00   1.00    3.00    --   36.95-125.00-150.00   61
 12  \w    -32.00  -6.00   1.00    3.00    --   36.95   0.00  60.00   26
 13  \w     24.00  53.00   1.00    3.00    --   36.95  57.00-180.00   29
 14  \w     22.00  50.00   1.00    3.00    --   36.95 -57.00  60.00   28
 15  \w     19.00  47.00   1.00    3.00    --   36.95  38.00   0.00   28
 16  \w    -14.00  13.00   1.00    3.00    --   36.95 -77.00 -90.00   27
 17  \w     21.00  46.00   1.00    3.00    --   36.95  57.00 120.00   25
 18  \w    -26.00  12.00   1.00    3.00    --   36.95 -57.00  60.00   38
 19  \w     40.00  92.00   1.00    3.00    --   36.95-128.00 -20.00   52
 20  \w    -22.00  48.00   1.00    3.00    --   36.95 -57.00-150.00   70
 21  \w      4.00  29.00   1.00    3.00    --   36.95  89.00 132.18   25
 22  \w     24.00  50.00   1.00    3.00    --   36.95 -77.00 -60.00   26
 23  \w     24.00  50.00   1.00    3.00    --   36.95 -77.00 -90.00   26
 24  \w      6.00  31.00   1.00    3.00    --   36.95  86.00  83.14   25
 25  \w      5.00  30.00   1.00    3.00    --   36.95  87.00-109.70   25
 26  \w      4.00  29.00   1.00    3.00    --   36.95  89.00  13.89   25
 27  \w     19.00  64.00   1.00    3.00    --   36.95  65.00-147.79   45
 28  \w      6.00  31.00   1.00    3.00    --   36.95  87.00 -67.26   25
 29  \w    -14.00  49.00   1.00    3.00    --   36.95 -57.00 -30.00   63
 30  \w      8.00  43.00   1.00    3.00    --   36.95  19.00-120.00   35
 31  \w     82.00 107.00   1.00    3.00    --   36.95  19.00  60.00   25
 32  \w     14.00  58.00   1.00    3.00    --   36.95  19.00  60.00   44
 33  \w     38.00  98.00   1.00    3.00    --   36.95  38.00  90.00   60
 34  \w     16.00  55.00   1.00    3.00    --   36.95  70.00  44.31   39
 35  \w     91.00 117.00   1.00   15.00    --  111.00  64.00 -60.00   26
 36  \w     53.00  79.00   1.00   15.00    --  111.00 -77.00 -90.00   26
 37  \w    139.00 173.00   1.00   15.00    --  111.00  64.00  30.00   34
 38  \w     44.00  70.00   1.00   15.00    --  111.00 -50.00-180.00   26
 39  \w     92.00 117.00   1.00   15.00    --  111.00  64.00  30.00   25
 40  \w     42.00 133.00   1.00   15.00    --  111.00 -25.00  90.00   91
 41  \w     95.00 121.00   1.00   15.00    --  111.00  50.00  30.00   26
 42  \w     42.00  88.00   1.00   15.00    --  111.00 -38.00-180.00   46
 43  \w     84.00 109.00   1.00   15.00    --  111.00-111.00  30.00   25
 44  \w     96.00 139.00   1.00   15.00    --  111.00  38.00-150.00   43
 45  \w     94.00 137.00   1.00   15.00    --  111.00  38.00  90.00   43
 46  \w     49.00  79.00   1.00   15.00    --  111.00 -64.00 150.00   30
 47  \w    103.00 137.00   1.00   15.00    --  111.00 -77.00  30.00   34
 48  \w     94.00 121.00   1.00   15.00    --  111.00  50.00-180.00   27
 49  \w     94.00 120.00   1.00   15.00    --  111.00  50.00 -30.00   26
 50  \w     44.00  71.00   1.00   15.00    --  111.00-111.00  30.00   27
 51  \w    141.00 167.00   1.00   15.00    --  111.00  64.00 -90.00   26
 52  \w     94.00 126.00   1.00   15.00    --  111.00  50.00-150.00   32
 53  \w     95.00 147.00   1.00   15.00    --  111.00  50.00 -90.00   52
 54  \w     94.00 133.00   1.00   15.00    --  111.00  50.00 150.00   39
 55  \w     95.00 126.00   1.00   15.00    --  111.00  38.00 120.00   31
 56  \w     95.00 127.00   1.00   15.00    --  111.00 -50.00-180.00   32
 57  \w     94.00 140.00   1.00   15.00    --  111.00  50.00-120.00   46
 58  \w     95.00 159.00   1.00   15.00    --  111.00  50.00   0.00   64
 59  \w     91.00 116.00   1.00   15.00    --  111.00  64.00 -90.00   25
 60  \w    118.00 144.00   1.00   15.00    --  111.00  64.00 120.00   26
 61  \w     92.00 118.00   1.00   15.00    --  111.00  64.00   0.00   26
 62  \w     91.00 117.00   1.00   15.00    --  111.00  64.00 120.00   26
 63  \w    141.00 167.00   1.00   15.00    --  111.00  50.00 120.00   26
 64  \w    139.00 173.00   1.00   15.00    --  111.00  38.00-180.00   34
 65  \w     93.00 118.00   1.00   15.00    --  111.00  38.00-180.00   25
 66  \w     94.00 126.00   1.00   15.00    --  111.00  50.00 120.00   32
 67  \w    145.00 178.00   1.00   15.00    --  111.00  50.00  60.00   33
 68  \w     86.00 131.00   1.00   15.00    --  111.00  25.00  60.00   45
 69  \w    137.00 163.00   1.00   15.00    --  111.00  25.00 -90.00   26
 70  \w     94.00 136.00   1.00   15.00    --  111.00  50.00  60.00   42
 71  \w     71.00 132.00   1.00   15.00    --  111.00 -32.00-138.15   61
 72  \w     94.00 172.00   1.00   15.00    --  111.00  50.00 -60.00   78
 73  \w     91.00 117.00   1.00   15.00    --  111.00  64.00 150.00   26
 74  \w     91.00 130.00   1.00   15.00    --  111.00  64.00  90.00   39
 75  \w    133.00 176.00   1.00   15.00    --  111.00  64.00-120.00   43
 76  \w     92.00 117.00   1.00   15.00    --  111.00  64.00-180.00   25
 77  \w    134.00 177.00   1.00   15.00    --  111.00  64.00 150.00   43
 78  \w     87.00 121.00   1.00   15.00    --  111.00  25.00 -90.00   34
 79  \w     94.00 119.00   1.00   15.00    --  111.00  38.00 -60.00   25
 80  \w     91.00 117.00   1.00   15.00    --  111.00  64.00-120.00   26
 81  \w    134.00 159.00   1.00   15.00    --  111.00  25.00  60.00   25
 82  \w     61.00 133.00   1.00   15.00    --  111.00 -25.00 -60.00   72
 83  \w     48.00  98.00   1.00   15.00    --  111.00 -92.00 -90.00   50
 84  \w    145.00 174.00   1.00   15.00    --  111.00  38.00 -30.00   29
 85  \w     92.00 118.00   1.00   15.00    --  111.00  38.00   0.00   26
 86  \w     97.00 148.00   1.00   15.00    --  111.00  38.00 150.00   51
 87  \w     96.00 122.00   1.00   15.00    --  111.00 -77.00 -60.00   26
 88  \w     91.00 118.00   1.00   15.00    --  111.00  64.00  60.00   27
 89  \w     54.00  94.00   1.00   15.00    --  111.00 -77.00 -60.00   40
 90  \w    127.00 162.00   1.00   15.00    --  111.00  25.00 120.00   35
 91  \w     46.00  73.00   1.00   15.00    --  111.00-111.00-180.00   27
 92  \w     77.00 108.00   1.00   15.00    --  111.00-111.00-180.00   31
 93  \w     88.00 115.00   1.00   15.00    --  111.00  25.00-150.00   27
 94  \w     44.00  75.00   1.00   15.00    --  111.00 -77.00  30.00   31
 95  \w     86.00 112.00   1.00   15.00    --  111.00  25.00 -60.00   26
 96  \w     49.00 105.00   1.00   15.00    --  111.00 -92.00  90.00   56
 97  \w     93.00 119.00   1.00   15.00    --  111.00 -64.00 150.00   26
 98  \w     87.00 112.00   1.00   15.00    --  111.00  25.00 120.00   25
 99  \w     73.00 124.00   1.00   15.00    --  111.00 -77.00 150.00   51
100  \w     55.00 102.00   1.00   15.00    --  111.00-111.00  90.00   47
101  \w     68.00 110.00   1.00   15.00    --  111.00 -50.00  30.00   42
102  \w     96.00 138.00   1.00   15.00    --  111.00  38.00 -30.00   42
103  \w     92.00 117.00   1.00   15.00    --  111.00  64.00 -30.00   25
104  \w    142.00 167.00   1.00   15.00    --  111.00  50.00  90.00   25
105  \w     98.00 126.00   1.00   15.00    --  111.00 143.00-134.00   28
106  \w     94.00 121.00   1.00   15.00    --  111.00  50.00  90.00   27
107  \w    110.00 136.00   1.00   15.00    --  111.00 -77.00 -90.00   26
108  \w     91.00 175.00   1.00   15.00    --  111.00  64.00-150.00   84
109  \w     43.00 101.00   1.00   15.00    --  111.00 -92.00-150.00   58
110  \w     43.00  69.00   1.00   15.00    --  111.00 -32.00-138.15   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      -0.0156389000
_diffrn_orient_matrix_UB_12      -0.0736178000
_diffrn_orient_matrix_UB_13      -0.0298871000
_diffrn_orient_matrix_UB_21      0.0166338000
_diffrn_orient_matrix_UB_22      -0.0235415000
_diffrn_orient_matrix_UB_23      0.0951882000
_diffrn_orient_matrix_UB_31      -0.1927158000
_diffrn_orient_matrix_UB_32      0.0039527000
_diffrn_orient_matrix_UB_33      0.0101317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23360
_diffrn_reflns_point_group_measured_fraction_full 0.866
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.759
_diffrn_reflns_theta_min         4.443
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.764
_exptl_absorpt_correction_T_max  0.672
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetramethylsilane'
_exptl_crystal_size_max          0.554
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4232
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0395P)^2^+1.0157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.731
_reflns_Friedel_fraction_max     0.718
_reflns_number_gt                4167
_reflns_number_total             4232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_217_b_scale_2
_cod_database_code               1566915
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H33As1Co1O4P1Si2
_chemical_oxdiff_usercomment     'SiMe4 evap at -30 '
_reflns_odcompleteness_completeness 99.96
_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:
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C13(H13A,H13B,
 H13C), C9(H9A,H9B,H9C), C3(H3A,H3B,H3C), C17(H17A,H17B,H17C), C4(H4A,H4B,H4C),
 C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C)
;
_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 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.694