Free and Coordinated Biarsolyls
Hill, Anthony; Kirk, Ryan M.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02070C

data_7713702
_publ_section_title
;
 Free and Coordinated Biarsolyls
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02070C
_journal_year                    2023
_chemical_formula_moiety         'C16 H12 As'
_chemical_formula_sum            'C16 H12 As'
_chemical_formula_weight         279.18
_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             2023-01-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 140.098(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2484(13)
_cell_length_b                   7.16710(10)
_cell_length_c                   12.0812(7)
_cell_measurement_reflns_used    6577
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6100
_cell_measurement_theta_min      6.4790
_cell_volume                     1180.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 1.000
_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    -40.00 -13.00   1.00    2.00    --  -36.95  38.00   0.00   27
  2  \w    -72.00 -44.00   1.00    2.00    --  -36.95 -19.00-180.00   28
  3  \w     -2.00  24.00   1.00    2.00    --  -36.95  38.00   0.00   26
  4  \w   -105.00 -78.00   1.00    2.00    --  -36.95 -19.00-180.00   27
  5  \w    -28.00  36.00   1.00    2.00    --   36.95 -57.00  90.00   64
  6  \w    -28.00  54.00   1.00    2.00    --   36.95 -57.00 -60.00   82
  7  \w     21.00 101.00   1.00    2.00    --   36.95  57.00 -90.00   80
  8  \w     30.00  56.00   1.00    2.00    --   36.95-125.00 -90.00   26
  9  \w    -33.00  62.00   1.00    2.00    --   36.95 -19.00 120.00   95
 10  \w     18.00  74.00   1.00    2.00    --   36.95 -99.00-180.00   56
 11  \w     37.00  89.00   1.00    2.00    --   36.95-125.00  90.00   52
 12  \w     10.00  54.00   1.00    2.00    --   36.95 -38.00 -30.00   44
 13  \w     45.00  77.00   1.00    2.00    --   36.95-125.00 -30.00   32
 14  \w     49.00  90.00   1.00    3.00    --  111.00 -92.00 -90.00   41
 15  \w     44.00 128.00   1.00    3.00    --  111.00 -50.00 -90.00   84
 16  \w     42.00  88.00   1.00    3.00    --  111.00 -92.00 120.00   46
 17  \w    103.00 130.00   1.00    3.00    --  111.00 -64.00  90.00   27
 18  \w    100.00 136.00   1.00    3.00    --  111.00  25.00  90.00   36
 19  \w    143.00 170.00   1.00    3.00    --  111.00  25.00  60.00   27
 20  \w     95.00 132.00   1.00    3.00    --  111.00  50.00   0.00   37
 21  \w    104.00 130.00   1.00    3.00    --  111.00 -25.00  60.00   26
 22  \w     94.00 120.00   1.00    3.00    --  111.00 178.00  60.00   26
 23  \w     93.00 124.00   1.00    3.00    --  111.00  38.00 150.00   31
 24  \w    143.00 177.00   1.00    3.00    --  111.00  25.00  90.00   34
 25  \w     86.00 135.00   1.00    3.00    --  111.00  25.00  60.00   49
 26  \w     67.00 109.00   1.00    3.00    --  111.00-111.00  30.00   42
 27  \w     43.00 120.00   1.00    3.00    --  111.00 -25.00-180.00   77
 28  \w    134.00 162.00   1.00    3.00    --  111.00  50.00 -30.00   28
 29  \w     70.00  99.00   1.00    3.00    --  111.00 -64.00 -30.00   29
 30  \w     65.00  90.00   1.00    3.00    --  111.00 -50.00-150.00   25
 31  \w    108.00 134.00   1.00    3.00    --  111.00  25.00 120.00   26
 32  \w     60.00 109.00   1.00    3.00    --  111.00-111.00 120.00   49
 33  \w     84.00 109.00   1.00    3.00    --  111.00-111.00-120.00   25
 34  \w     81.00 108.00   1.00    3.00    --  111.00-111.00 -30.00   27
 35  \w     76.00 101.00   1.00    3.00    --  111.00 -92.00-180.00   25
 36  \w     45.00  99.00   1.00    3.00    --  111.00 -64.00 120.00   54
 37  \w     42.00  68.00   1.00    3.00    --  111.00-111.00-120.00   26
 38  \w    147.00 177.00   1.00    3.00    --  111.00  25.00 120.00   30
 39  \w    106.00 176.00   1.00    3.00    --  111.00  77.00 -60.00   70
 40  \w     58.00 102.00   1.00    3.00    --  111.00 -50.00   0.00   44
 41  \w     49.00 106.00   1.00    3.00    --  111.00 -92.00 -60.00   57
 42  \w     77.00 106.00   1.00    3.00    --  111.00-111.00-180.00   29
 43  \w    138.00 177.00   1.00    3.00    --  111.00  50.00   0.00   39
 44  \w    106.00 131.00   1.00    3.00    --  111.00 178.00  90.00   25
 45  \w     51.00  77.00   1.00    3.00    --  111.00 -50.00-180.00   26
 46  \w     52.00  78.00   1.00    3.00    --  111.00 -50.00 120.00   26
 47  \w     57.00 106.00   1.00    3.00    --  111.00-111.00 -90.00   49
 48  \w     84.00 110.00   1.00    3.00    --  111.00 -38.00  30.00   26
 49  \w     55.00 127.00   1.00    3.00    --  111.00 -32.00 -18.17   72
;
_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      0.0728561000
_diffrn_orient_matrix_UB_12      0.0155039000
_diffrn_orient_matrix_UB_13      -0.0354976000
_diffrn_orient_matrix_UB_21      -0.1638220000
_diffrn_orient_matrix_UB_22      0.1050607000
_diffrn_orient_matrix_UB_23      -0.0922671000
_diffrn_orient_matrix_UB_31      0.0858506000
_diffrn_orient_matrix_UB_32      0.1868512000
_diffrn_orient_matrix_UB_33      0.0547386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11177
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.649
_diffrn_reflns_theta_min         6.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.639
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CDCl3'
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0348P)^2^+0.3989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2251
_reflns_number_total             2383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02070c2.cif
_cod_data_source_block           rmk_105_b_scale1
_cod_original_cell_volume        1180.2(2)
_cod_database_code               7713702
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H12As1Cl1
_chemical_oxdiff_usercomment     'slow evap of CDCl3 at Rt overnight '
_reflns_odcompleteness_completeness 99.96
_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:
 C2(H2), C3(H3), C6(H6), C12(H12), C10(H10), C16(H16), C15(H15), C9(H9),
 C7(H7), C14(H14), C8(H8), C13(H13)
;
_shelx_res_checksum              93976
_ins_header
;
TITL RMK_105_B_scale1 in P2(1)/a 
REM P2(1)/a (#14 in standard setting)
CELL 1.54184  12.081160   7.167101  21.248350  90.0000 140.0984  90.0000
ZERR    4.00   0.000720   0.000126   0.001297   0.0000   0.0122   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z 
SFAC C H Cl As
UNIT 64.00 48.00 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 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.876