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_7128788
_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 H21 As'
_chemical_formula_sum            'C30 H21 As'
_chemical_formula_weight         456.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.4510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0571(2)
_cell_length_b                   6.08720(10)
_cell_length_c                   20.2253(2)
_cell_measurement_reflns_used    8305
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.5580
_cell_measurement_theta_min      4.6550
_cell_volume                     2198.34(5)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -66.00 -39.00   1.00    2.00    --  -37.08 115.00 -17.00   27
  2  \w   -103.00 -43.00   1.00    2.00    --  -37.08 -57.00-120.00   60
  3  \w     46.00  83.00   1.00    2.00    --   37.08-125.00   0.00   37
  4  \w     21.00 101.00   1.00    2.00    --   37.08  38.00-120.00   80
  5  \w    -16.00  42.00   1.00    2.00    --   37.08 -77.00 150.00   58
  6  \w     11.00  61.00   1.00    2.00    --   37.08 -99.00  60.00   50
  7  \w    -27.00  54.00   1.00    2.00    --   37.08 -57.00  90.00   81
  8  \w     97.00 147.00   1.00    6.00    --  111.00  38.00 -60.00   50
  9  \w     56.00  91.00   1.00    6.00    --  111.00 -92.00-120.00   35
 10  \w    108.00 134.00   1.00    6.00    --  111.00 111.00  30.00   26
 11  \w     66.00 119.00   1.00    6.00    --  111.00 -57.00-167.44   53
 12  \w     55.00  81.00   1.00    6.00    --  111.00 -92.00   0.00   26
 13  \w     42.00  76.00   1.00    6.00    --  111.00 -25.00  60.00   34
 14  \w    111.00 136.00   1.00    6.00    --  111.00 -25.00  60.00   25
 15  \w     45.00  92.00   1.00    6.00    --  111.00 -92.00  60.00   47
 16  \w     60.00  93.00   1.00    6.00    --  111.00 -92.00 120.00   33
 17  \w     64.00 102.00   1.00    6.00    --  111.00 -92.00 -60.00   38
 18  \w    142.00 178.00   1.00    6.00    --  111.00  77.00-180.00   36
 19  \w    146.00 172.00   1.00    6.00    --  111.00  38.00 -30.00   26
 20  \w     43.00 111.00   1.00    6.00    --  111.00 -38.00 120.00   68
 21  \w     61.00  86.00   1.00    6.00    --  111.00 -92.00 -30.00   25
 22  \w    103.00 165.00   1.00    6.00    --  111.00  77.00-120.00   62
 23  \w     99.00 133.00   1.00    6.00    --  111.00  38.00 -30.00   34
 24  \w     61.00 105.00   1.00    6.00    --  111.00 -92.00-150.00   44
 25  \w    136.00 162.00   1.00    6.00    --  111.00  64.00-150.00   26
 26  \w     73.00  98.00   1.00    6.00    --  111.00 -42.00-167.12   25
 27  \w     95.00 121.00   1.00    6.00    --  111.00 -77.00-150.00   26
 28  \w     75.00 172.00   1.00    6.00    --  111.00  12.00-150.00   97
 29  \w     79.00 105.00   1.00    6.00    --  111.00 -50.00-120.00   26
 30  \w     54.00 106.00   1.00    6.00    --  111.00 -50.00  90.00   52
;
_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      0.0579550000
_diffrn_orient_matrix_UB_12      -0.0091047000
_diffrn_orient_matrix_UB_13      -0.0372330000
_diffrn_orient_matrix_UB_21      0.0633001000
_diffrn_orient_matrix_UB_22      0.0421245000
_diffrn_orient_matrix_UB_23      0.0710052000
_diffrn_orient_matrix_UB_31      0.0085718000
_diffrn_orient_matrix_UB_32      -0.2494968000
_diffrn_orient_matrix_UB_33      0.0134391000
_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     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13330
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.738
_diffrn_reflns_theta_min         4.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67384
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+1.8345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4153
_reflns_number_total             4440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03015a2.cif
_cod_data_source_block           rmk_164_scale
_cod_depositor_comments
'Adding full bibliography for 7128785--7128788.cif.'
_cod_database_code               7128788
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H21As1
_chemical_oxdiff_usercomment     DCM/MeOH
_reflns_odcompleteness_completeness 98.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H00A), C18(H00B), C26(H00C), C14(H00D), C20(H00E), C12(H00F), C16(H00G),
 C21(H00H), C17(H00I), C15(H00K), C30(H00L), C10(H00M), C9(H00N), C8(H00O),
 C11(H00P), C27(H00Q), C28(H00R), C22(H00S), C29(H00T), C23(H00U)
2.b :
 C2(H00V)
;
_ins_header
;
TITL RMK_164_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  19.057070   6.087223  20.225266  90.0000 110.4510  90.0000
ZERR    4.00   0.000238   0.000054   0.000243   0.0000   0.0014   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H As
UNIT 120.00 84.00 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 1.639
_oxdiff_exptl_absorpt_empirical_full_min 0.554