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

data_7713703
_publ_section_title
;
 Free and Coordinated Biarsolyls
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02070C
_journal_year                    2023
_chemical_formula_moiety         'C21 H17 As Cr Mo O8'
_chemical_formula_sum            'C21 H17 As Cr Mo O8'
_chemical_formula_weight         620.21
_chemical_properties_physical    Air-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2b0fc5
_audit_creation_date             2022-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-29 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                77.541(3)
_cell_angle_beta                 70.581(3)
_cell_angle_gamma                61.676(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0861(3)
_cell_length_b                   10.5319(4)
_cell_length_c                   13.2660(5)
_cell_measurement_reflns_used    6590
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.0550
_cell_measurement_theta_min      4.7690
_cell_volume                     1167.06(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 2018/3 (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 0.994
_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    -84.00 -13.00   1.00    1.00    --  -36.63 125.00 120.00   71
  2  \w    -52.00   2.00   1.00    1.00    --  -36.63  38.00 120.00   54
  3  \w   -107.00  -7.00   1.00    1.00    --  -36.63 -19.00 -60.00  100
  4  \w     74.00 102.00   1.00    1.00    --   36.63  57.00 -90.00   28
  5  \w     22.00  99.00   1.00    1.00    --   36.63  57.00 120.00   77
  6  \w    -18.00  54.00   1.00    1.00    --   36.63 -77.00-120.00   72
  7  \w     36.00  88.00   1.00    1.00    --   36.63-125.00  30.00   52
  8  \w     54.00  98.00   1.00    2.00    --  109.00 -95.00  90.00   44
  9  \w     63.00  93.00   1.00    2.00    --  109.00 -95.00 -90.00   30
 10  \w     40.00 129.00   1.00    2.00    --  109.00 -30.00-150.00   89
 11  \w    104.00 161.00   1.00    2.00    --  109.00 111.00 150.00   57
 12  \w    152.00 178.00   1.00    2.00    --  109.00 111.00  60.00   26
 13  \w     40.00 120.00   1.00    2.00    --  109.00 -30.00  90.00   80
 14  \w     56.00  81.00   1.00    2.00    --  109.00-111.00  60.00   25
 15  \w     76.00 109.00   1.00    2.00    --  109.00-111.00 150.00   33
 16  \w     40.00 129.00   1.00    2.00    --  109.00 -30.00   0.00   89
 17  \w     41.00  72.00   1.00    2.00    --  109.00-111.00-120.00   31
 18  \w     80.00 109.00   1.00    2.00    --  109.00-111.00-150.00   29
 19  \w     80.00 108.00   1.00    2.00    --  109.00-111.00  30.00   28
 20  \w     67.00 108.00   1.00    2.00    --  109.00-111.00 -30.00   41
 21  \w    114.00 153.00   1.00    2.00    --  109.00  61.00 150.00   39
 22  \w     84.00 149.00   1.00    2.00    --  109.00  15.00 -30.00   65
 23  \w    118.00 151.00   1.00    2.00    --  109.00 111.00 120.00   33
 24  \w     42.00  70.00   1.00    2.00    --  109.00 -77.00  30.00   28
 25  \w     93.00 119.00   1.00    2.00    --  109.00 -77.00  30.00   26
 26  \w    128.00 154.00   1.00    2.00    --  109.00 111.00  90.00   26
 27  \w    120.00 145.00   1.00    2.00    --  109.00 178.00  90.00   25
 28  \w     75.00 106.00   1.00    2.00    --  109.00-111.00 -90.00   31
 29  \w     50.00  94.00   1.00    2.00    --  109.00 -15.00 -60.00   44
 30  \w    112.00 145.00   1.00    2.00    --  109.00 -15.00 -60.00   33
 31  \w     44.00  69.00   1.00    2.00    --  109.00 -95.00 -30.00   25
 32  \w     68.00 125.00   1.00    2.00    --  109.00 -77.00-180.00   57
 33  \w    100.00 126.00   1.00    2.00    --  109.00 -61.00  60.00   26
 34  \w     81.00 118.00   1.00    2.00    --  109.00 -61.00 -90.00   37
 35  \w     64.00 100.00   1.00    2.00    --  109.00 -95.00  60.00   36
 36  \w     84.00 109.00   1.00    2.00    --  109.00-111.00-180.00   25
 37  \w     95.00 172.00   1.00    2.00    --  109.00  45.00-120.00   77
 38  \w     42.00  67.00   1.00    2.00    --  109.00-111.00 -60.00   25
 39  \w     65.00  91.00   1.00    2.00    --  109.00 -61.00  60.00   26
 40  \w    145.00 170.00   1.00    2.00    --  109.00 111.00-120.00   25
 41  \w    144.00 169.00   1.00    2.00    --  109.00 111.00   0.00   25
 42  \w    116.00 141.00   1.00    2.00    --  109.00 178.00 -90.00   25
 43  \w     43.00  68.00   1.00    2.00    --  109.00 -77.00 120.00   25
 44  \w     79.00 104.00   1.00    2.00    --  109.00  15.00 -60.00   25
 45  \w    138.00 164.00   1.00    2.00    --  109.00  15.00 -60.00   26
 46  \w    128.00 166.00   1.00    2.00    --  109.00  77.00-180.00   38
;
_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      -0.0204483000
_diffrn_orient_matrix_UB_12      0.1099934000
_diffrn_orient_matrix_UB_13      0.0705547000
_diffrn_orient_matrix_UB_21      -0.1062168000
_diffrn_orient_matrix_UB_22      0.1240675000
_diffrn_orient_matrix_UB_23      -0.0639842000
_diffrn_orient_matrix_UB_31      -0.1439852000
_diffrn_orient_matrix_UB_32      -0.0160295000
_diffrn_orient_matrix_UB_33      0.0785120000
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11692
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.294
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.200
_exptl_absorpt_correction_T_max  0.52082
_exptl_absorpt_correction_T_min  0.47990
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.765
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl2/n-heptane'
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.044
_exptl_crystal_size_rad          0.047
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0408P)^2^+0.2024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             4647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02070c2.cif
_cod_data_source_block           rmk_234_b_scale
_cod_database_code               7713703
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H24As1Mo1Mn1O5
_chemical_oxdiff_usercomment     'hot hexane recryst'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C15(H15), C14(H14), C13(H13)
2.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C11(H11a,H11b,H11c), C10(H10a,H10b,H10c), C9(H9a,H9b,H9c)
;
_shelx_res_checksum              18120
_ins_header
;
TITL RMK_234_B_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.086103  10.531855  13.266042  77.5411  70.5810  61.6757
ZERR    2.00   0.000290   0.000370   0.000451   0.0029   0.0028   0.0033
LATT  1
SFAC C H O Mn As Mo
UNIT 48.00 48.00 10.00 2.00 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 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.785