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

data_7713705
_publ_section_title
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 Free and Coordinated Biarsolyls
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02070C
_journal_year                    2023
_chemical_formula_moiety         'C22 H17 As Au F5 Mo O3'
_chemical_formula_sum            'C22 H17 As Au F5 Mo O3'
_chemical_formula_weight         792.18
_chemical_properties_physical    Air-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2b0ff7
_audit_creation_date             2022-01-29
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2022-01-29 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 136.531(4)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.8893(5)
_cell_length_b                   38.4002(3)
_cell_length_c                   14.8049(3)
_cell_measurement_reflns_used    14490
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5910
_cell_measurement_theta_min      5.3610
_cell_volume                     9343.4(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (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 2018/2 (Sheldrick, 2018)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.975
_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     58.00 104.00   1.00    5.00    --   36.95  19.00  90.00   46
  2  \w     27.00  88.00   1.00    5.00    --   36.95-125.00-150.00   61
  3  \w     22.00 102.00   1.00    5.00    --   36.95  57.00  30.00   80
  4  \w    -21.00  64.00   1.00    5.00    --   36.95 -77.00 -90.00   85
  5  \w     11.00  49.00   1.00    5.00    --   36.95  19.00  90.00   38
  6  \w    149.00 178.00   1.00   20.00    --  111.00  50.00 -90.00   29
  7  \w    113.00 139.00   1.00   20.00    --  111.00 -12.00  90.00   26
  8  \w     96.00 124.00   1.00   20.00    --  111.00  50.00 -90.00   28
  9  \w     43.00 108.00   1.00   20.00    --  111.00 -12.00  90.00   65
 10  \w     42.00 106.00   1.00   20.00    --  111.00 -92.00-150.00   64
 11  \w     42.00 101.00   1.00   20.00    --  111.00 -38.00  90.00   59
 12  \w     91.00 174.00   1.00   20.00    --  111.00  25.00  90.00   83
 13  \w     48.00 138.00   1.00   20.00    --  111.00 -77.00  30.00   90
 14  \w     46.00 130.00   1.00   20.00    --  111.00 -38.00-120.00   84
;
_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      0.0717091000
_diffrn_orient_matrix_UB_12      0.0088868000
_diffrn_orient_matrix_UB_13      0.1468858000
_diffrn_orient_matrix_UB_21      -0.0495040000
_diffrn_orient_matrix_UB_22      -0.0129344000
_diffrn_orient_matrix_UB_23      0.0238480000
_diffrn_orient_matrix_UB_31      0.0345361000
_diffrn_orient_matrix_UB_32      -0.0369097000
_diffrn_orient_matrix_UB_33      0.0269080000
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37213
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.754
_diffrn_reflns_theta_min         3.798
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.183
_exptl_absorpt_correction_T_max  0.42673
_exptl_absorpt_correction_T_min  0.36701
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (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    2.253
_exptl_crystal_description       prism
_exptl_crystal_F_000             5952
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/Et2O'
_exptl_crystal_size_max          0.077
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.058
_exptl_crystal_size_rad          0.038
_refine_diff_density_max         3.861
_refine_diff_density_min         -1.987
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         18440
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0272P)^2^+37.4309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15682
_reflns_number_total             18440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02070c2.cif
_cod_data_source_block           rmk_225_ca_scale
_cod_original_cell_volume        9343.4(6)
_cod_database_code               7713705
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C22H17As1Au1Mo1F5O3
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Uiso/Uaniso restraints and constraints
C15C \\sim C14C \\sim C13C \\sim C12C \\sim C16C: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C14C) = Uanis(C15C) = Uanis(C16C) = Uanis(C12C) = Uanis(C13C)
3. Rigid body (RIGU) restrains
 C15C, C14C, C13C, C12C, C16C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C14B(H14B), C15B(H15B), C12A(H12A), C13A(H13A), C13B(H13B),
 C15A(H15A), C12B(H12B), C16B(H16B), C16A(H16A), C12C(H12C), C16D(H16D),
 C12D(H12D), C15D(H15D), C13C(H13C), C13D(H13D), C14D(H14D), C16C(H16C),
 C15C(H15C), C14C(H14C)
4.b Idealised Me refined as rotating group:
 C9B(H9Ba,H9Bb,H9Bc), C8A(H8Aa,H8Ab,H8Ac), C11B(H11a,H11b,H11c), C9A(H9Aa,H9Ab,
 H9Ac), C11A(H11d,H11e,H11f), C11D(H11g,H11h,H11i), C10A(H10d,H10e,H10f),
 C10B(H10a,H10b,H10c), C11C(H11j,H11k,H11l), C8D(H8Da,H8Db,H8Dc), C10D(H10g,
 H10h,H10i), C8C(H8Ca,H8Cb,H8Cc), C9C(H9Ca,H9Cb,H9Cc), C9D(H9Da,H9Db,H9Dc),
 C10C(H10j,H10k,H10l)
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_ins_header
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TITL RMK_225_Ca_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  23.889263  38.400152  14.804860  90.0000 136.5307  90.0000
ZERR   16.00   0.000500   0.000283   0.000317   0.0000   0.0039   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O F As Mo Au
UNIT 352.00 272.00 48.00 80.00 16.00 16.00 16.00
TREF
HKLF 4
END
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_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.879