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_7128786
_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         'C14 H10 As N'
_chemical_formula_sum            'C14 H10 As N'
_chemical_formula_weight         267.15
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-01 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.826(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6500(3)
_cell_length_b                   6.7526(2)
_cell_length_c                   14.8906(4)
_cell_measurement_reflns_used    1864
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.3100
_cell_measurement_theta_min      4.3760
_cell_volume                     1142.18(6)
_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 0.990
_diffrn_measured_fraction_theta_max 0.959
_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   -103.00 -21.00   1.00    2.00    --  -36.03 -57.00 120.00   82
  2  \w    -84.00 -44.00   1.00    2.00    --  -36.03 125.00-180.00   40
  3  \w   -107.00 -15.00   1.00    2.00    --  -36.03 -19.00-180.00   92
  4  \w     53.00 127.00   1.00    8.00    --  105.15 -30.00 -60.00   74
  5  \w     37.00 106.00   1.00    8.00    --  105.15 -95.00-180.00   69
  6  \w     84.00 127.00   1.00    8.00    --  105.15 -30.00  30.00   43
  7  \w    142.00 175.00   1.00    8.00    --  105.15  30.00 150.00   33
  8  \w     85.00 129.00   1.00    8.00    --  105.15  30.00 150.00   44
  9  \w     36.00  71.00   1.00    8.00    --  105.15 -30.00  30.00   35
 10  \w     38.00 127.00   1.00    8.00    --  105.15 -77.00  30.00   89
;
_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      -0.0174765000
_diffrn_orient_matrix_UB_12      -0.0058633000
_diffrn_orient_matrix_UB_13      -0.1056143000
_diffrn_orient_matrix_UB_21      -0.1340857000
_diffrn_orient_matrix_UB_22      -0.0141454000
_diffrn_orient_matrix_UB_23      -0.0097559000
_diffrn_orient_matrix_UB_31      -0.0089175000
_diffrn_orient_matrix_UB_32      0.2277547000
_diffrn_orient_matrix_UB_33      -0.0033904000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3192
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.720
_diffrn_reflns_theta_min         4.377
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82290
_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    1.554
_exptl_crystal_description       needle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0322P)^2^+0.0843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1881
_reflns_number_total             2108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03015a2.cif
_cod_data_source_block           Compound_X
_cod_depositor_comments
'Adding full bibliography for 7128785--7128788.cif.'
_cod_database_code               7128786
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C14 H10 As N'
_chemical_oxdiff_usercomment     c/h
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.418
_reflns_odcompleteness_completeness 99.09
_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:
 C10(H10), C4(H4), C7(H7), C6(H6), C13(H13), C5(H5), C11(H11), C12(H12)
2.b :
 C2(H2)
;
_shelx_res_checksum              91352
_ins_header
;
TITL BF145A_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  11.649974   6.752625  14.890593  90.0000 102.8265  90.0000
ZERR    4.00   0.000309   0.000151   0.000362   0.0000   0.0025   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N As
UNIT 56.00 40.00 4.00 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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.731