Heterocyclic arsinocarbynes via tandem transmetallation.
Frogley, Benjamin J.; Hill, Anthony F.; Kirk, Ryan M.; Chemical communications (Cambridge, England) 57 (2021) 8770–8773; doi:10.1039/d1cc03015a

data_7128785
_publ_section_title
;
 Heterocyclic arsinocarbynes via tandem transmetallation.
;
_journal_issue                   70
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8770
_journal_page_last               8773
_journal_paper_doi               10.1039/d1cc03015a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C30 H31 As B N7 O2 W'
_chemical_formula_sum            'C30 H31 As B N7 O2 W'
_chemical_formula_weight         791.20
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-11 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                98.025(3)
_cell_angle_beta                 95.841(2)
_cell_angle_gamma                115.100(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5457(3)
_cell_length_b                   10.9949(3)
_cell_length_c                   14.6439(4)
_cell_measurement_reflns_used    12616
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6480
_cell_measurement_theta_min      5.9760
_cell_volume                     1497.81(8)
_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 (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 0.995
_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    -41.00 -12.00   1.00    1.00    --  -36.95 125.00   0.00   29
  2  \w   -103.00 -49.00   1.00    1.00    --  -36.95 -38.00  60.00   54
  3  \w     27.00  76.00   1.00    1.00    --   36.95 -99.00  30.00   49
  4  \w     13.00  62.00   1.00    1.00    --   36.95 -99.00 150.00   49
  5  \w      8.00  35.00   1.00    1.00    --   36.95 -77.00 150.00   27
  6  \w    -31.00  55.00   1.00    1.00    --   36.95 -38.00 -90.00   86
  7  \w      4.00  34.00   1.00    1.00    --   36.95   0.00-120.00   30
  8  \w     32.00  65.00   1.00    1.00    --   36.95  57.00 120.00   33
  9  \w     10.00  38.00   1.00    1.00    --   36.95 -99.00-120.00   28
 10  \w     35.00  60.00   1.00    1.00    --   36.95-125.00  90.00   25
 11  \w      7.00  34.00   1.00    1.00    --   36.95 -99.00 -60.00   27
 12  \w     31.00 106.00   1.00    1.00    --   36.95  19.00  60.00   75
 13  \w    -11.00  27.00   1.00    1.00    --   36.95 -77.00-120.00   38
 14  \w    -28.00  31.00   1.00    1.00    --   36.95 -57.00-120.00   59
 15  \w    -20.00   5.00   1.00    1.00    --   36.95 -77.00 150.00   25
 16  \w     66.00  91.00   1.00    1.00    --   36.95   0.00-120.00   25
 17  \w     45.00  89.00   1.00    1.00    --   36.95-125.00   0.00   44
 18  \w     49.00  90.00   1.00    1.00    --   36.95-125.00 -90.00   41
 19  \w    132.00 177.00   1.00    1.50    --  111.00  50.00   0.00   45
 20  \w     74.00 109.00   1.00    1.50    --  111.00-111.00  30.00   35
 21  \w     62.00  88.00   1.00    1.50    --  111.00 -92.00 120.00   26
 22  \w    109.00 178.00   1.00    1.50    --  111.00  77.00 -60.00   69
 23  \w     96.00 177.00   1.00    1.50    --  111.00  50.00 -90.00   81
 24  \w     47.00  77.00   1.00    1.50    --  111.00 -77.00 -60.00   30
 25  \w     41.00 109.00   1.00    1.50    --  111.00-111.00-180.00   68
 26  \w     81.00 106.00   1.00    1.50    --  111.00 -92.00 -60.00   25
 27  \w     49.00  75.00   1.00    1.50    --  111.00-111.00 150.00   26
 28  \w     52.00  78.00   1.00    1.50    --  111.00 -50.00-180.00   26
 29  \w     61.00 109.00   1.00    1.50    --  111.00-111.00 120.00   48
 30  \w     50.00  77.00   1.00    1.50    --  111.00 -50.00 150.00   27
 31  \w    108.00 140.00   1.00    1.50    --  111.00  25.00  90.00   32
 32  \w     89.00 130.00   1.00    1.50    --  111.00 -25.00-180.00   41
 33  \w    121.00 166.00   1.00    1.50    --  111.00  38.00  60.00   45
 34  \w    143.00 168.00   1.00    1.50    --  111.00  50.00-180.00   25
 35  \w     98.00 134.00   1.00    1.50    --  111.00  50.00-180.00   36
 36  \w     42.00  70.00   1.00    1.50    --  111.00 -25.00-180.00   28
 37  \w     44.00  81.00   1.00    1.50    --  111.00 -50.00  30.00   37
 38  \w    117.00 143.00   1.00    1.50    --  111.00 -12.00-180.00   26
 39  \w     79.00 122.00   1.00    1.50    --  111.00 -50.00 -90.00   43
 40  \w    137.00 177.00   1.00    1.50    --  111.00  50.00 150.00   40
 41  \w     73.00  99.00   1.00    1.50    --  111.00 -77.00-180.00   26
 42  \w    113.00 138.00   1.00    1.50    --  111.00 -77.00-180.00   25
 43  \w     81.00 106.00   1.00    1.50    --  111.00 -92.00  90.00   25
 44  \w    104.00 146.00   1.00    1.50    --  111.00  12.00-120.00   42
 45  \w     73.00  98.00   1.00    1.50    --  111.00 -64.00   0.00   25
 46  \w     63.00 126.00   1.00    1.50    --  111.00 -38.00-120.00   63
 47  \w     83.00 109.00   1.00    1.50    --  111.00-111.00 -60.00   26
 48  \w     52.00  78.00   1.00    1.50    --  111.00-111.00 -60.00   26
 49  \w     44.00  70.00   1.00    1.50    --  111.00 -92.00  60.00   26
 50  \w     62.00 109.00   1.00    1.50    --  111.00-111.00-150.00   47
 51  \w     81.00 106.00   1.00    1.50    --  111.00-111.00-120.00   25
 52  \w     83.00 129.00   1.00    1.50    --  111.00 178.00 -30.00   46
 53  \w     77.00 106.00   1.00    1.50    --  111.00-111.00 -30.00   29
 54  \w     45.00 107.00   1.00    1.50    --  111.00-111.00  60.00   62
 55  \w     42.00  74.00   1.00    1.50    --  111.00-111.00-120.00   32
 56  \w    146.00 175.00   1.00    1.50    --  111.00  77.00 120.00   29
 57  \w     70.00 130.00   1.00    1.50    --  111.00 -64.00-180.00   60
 58  \w     43.00  68.00   1.00    1.50    --  111.00-111.00   0.00   25
 59  \w     92.00 117.00   1.00    1.50    --  111.00 -50.00-180.00   25
 60  \w     43.00  69.00   1.00    1.50    --  111.00 -50.00  60.00   26
 61  \w     53.00 133.00   1.00    1.50    --  111.00 -27.00 -24.25   80
 62  \w     61.00  93.00   1.00    1.50    --  111.00 -53.00  87.76   32
;
_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      0.1074598000
_diffrn_orient_matrix_UB_12      -0.0009328000
_diffrn_orient_matrix_UB_13      0.0791415000
_diffrn_orient_matrix_UB_21      -0.1162919000
_diffrn_orient_matrix_UB_22      -0.0444122000
_diffrn_orient_matrix_UB_23      0.0608820000
_diffrn_orient_matrix_UB_31      -0.0426507000
_diffrn_orient_matrix_UB_32      -0.1516413000
_diffrn_orient_matrix_UB_33      -0.0411495000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17489
_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         73.857
_diffrn_reflns_theta_min         4.535
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.337
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0364P)^2^+2.6647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5925
_reflns_number_total             6058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03015a2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7128785--7128788.cif.'
_cod_database_code               7128785
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H31 As B N7 O2 W'
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C23(H23), C14(H14), C18(H18), C11(H11), C5(H5), C8(H8), C13(H13),
 C12(H12), C7(H7A), C6(H6)
1.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C30(H30A,H30B,
 H30C), C25(H25A,H25B,H25C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              80103
_ins_header
;
TITL BF131A2_scale in P1 
REM P1 (#1 in standard setting)
CELL 1.54184  10.545661  10.994886  14.643908  98.0248  95.8410 115.1002
ZERR    2.00   0.000322   0.000345   0.000450   0.0026   0.0025   0.0030
LATT -1
SFAC C H B N O As W
UNIT 60.00 62.00 2.00 14.00 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 1.351
_oxdiff_exptl_absorpt_empirical_full_min 0.808