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

data_7713704
_publ_section_title
;
 Free and Coordinated Biarsolyls
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02070C
_journal_year                    2023
_chemical_formula_moiety         'C24 H24 As Mn Mo O5'
_chemical_formula_sum            'C24 H24 As Mn Mo O5'
_chemical_formula_weight         618.23
_chemical_properties_physical    Air-sensitive
_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_block_doi                 10.5517/ccdc.csd.cc2b0fb4
_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                90
_cell_angle_beta                 96.5650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9876(2)
_cell_length_b                   9.27920(10)
_cell_length_c                   17.3004(2)
_cell_measurement_reflns_used    8539
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6320
_cell_measurement_theta_min      5.1360
_cell_volume                     2390.24(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 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 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    -48.00  -8.00   1.00    1.00    --  -36.95 125.00 -90.00   40
  2  \w     50.00  89.00   1.00    1.00    --   36.95-125.00-180.00   39
  3  \w     34.00  77.00   1.00    1.00    --   36.95-125.00  90.00   43
  4  \w     32.00  69.00   1.00    1.00    --   36.95-125.00-150.00   37
  5  \w    -27.00  35.00   1.00    1.00    --   36.95 -38.00-150.00   62
  6  \w    -17.00   9.00   1.00    1.00    --   36.95 -57.00 -30.00   26
  7  \w     22.00 103.00   1.00    1.00    --   36.95  57.00  30.00   81
  8  \w     34.00  90.00   1.00    1.00    --   36.95-125.00 -60.00   56
  9  \w    139.00 174.00   1.00    7.00    --  111.00  50.00-150.00   35
 10  \w    117.00 176.00   1.00    7.00    --  111.00  64.00   0.00   59
 11  \w    102.00 127.00   1.00    7.00    --  111.00 -50.00-180.00   25
 12  \w     58.00  95.00   1.00    7.00    --  111.00 -92.00  30.00   37
 13  \w     43.00  69.00   1.00    7.00    --  111.00-111.00 -30.00   26
 14  \w    122.00 148.00   1.00    7.00    --  111.00  50.00 120.00   26
 15  \w    101.00 137.00   1.00    7.00    --  111.00  12.00 120.00   36
 16  \w    150.00 176.00   1.00    7.00    --  111.00 111.00-150.00   26
 17  \w    106.00 136.00   1.00    7.00    --  111.00  50.00 -90.00   30
 18  \w    106.00 132.00   1.00    7.00    --  111.00 111.00-150.00   26
 19  \w     44.00  96.00   1.00    7.00    --  111.00 -50.00-180.00   52
 20  \w     47.00 113.00   1.00    7.00    --  111.00 -50.00 -30.00   66
 21  \w     79.00 118.00   1.00    7.00    --  111.00 -52.00-147.00   39
 22  \w     41.00 122.00   1.00    7.00    --  111.00 -25.00 -90.00   81
 23  \w    103.00 161.00   1.00    7.00    --  111.00  77.00  90.00   58
 24  \w     53.00 109.00   1.00    7.00    --  111.00-111.00-180.00   56
 25  \w     67.00  93.00   1.00    7.00    --  111.00-111.00-120.00   26
 26  \w     54.00 102.00   1.00    7.00    --  111.00-111.00 -60.00   48
 27  \w    105.00 130.00   1.00    7.00    --  111.00 -38.00   0.00   25
 28  \w     51.00  77.00   1.00    7.00    --  111.00 -38.00   0.00   26
 29  \w     97.00 157.00   1.00    7.00    --  111.00  50.00 -30.00   60
 30  \w     53.00  86.00   1.00    7.00    --  111.00 -50.00  60.00   33
 31  \w     65.00  91.00   1.00    7.00    --  111.00  12.00 120.00   26
;
_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      -0.0873207000
_diffrn_orient_matrix_UB_12      0.0266351000
_diffrn_orient_matrix_UB_13      -0.0542623000
_diffrn_orient_matrix_UB_21      0.0334120000
_diffrn_orient_matrix_UB_22      -0.1012875000
_diffrn_orient_matrix_UB_23      -0.0610825000
_diffrn_orient_matrix_UB_31      -0.0442202000
_diffrn_orient_matrix_UB_32      -0.1289450000
_diffrn_orient_matrix_UB_33      0.0368523000
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14799
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.802
_diffrn_reflns_theta_min         5.147
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.406
_exptl_absorpt_correction_T_max  0.54283
_exptl_absorpt_correction_T_min  0.50377
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.047
_exptl_crystal_size_rad          0.045
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0279P)^2^+1.3665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4507
_reflns_number_total             4827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02070c2.cif
_cod_data_source_block           rmk_234_a_scale
_cod_database_code               7713704
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H24As1Mn1Mo1O5
_chemical_oxdiff_usercomment     'hexane at -20 '
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C19(H19), C21(H21), C20(H20), C12(H12), C13(H13), C15(H15),
 C14(H14), C16(H16)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C24(H24a,H24b,
 H24c), C9(H9a,H9b,H9c)
;
_shelx_res_checksum              50070
_ins_header
;
TITL RMK_234_A_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  14.987576   9.279193  17.300397  90.0000  96.5651  90.0000
ZERR    4.00   0.000189   0.000120   0.000248   0.0000   0.0012   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H O Mn As Mo
UNIT 96.00 96.00 20.00 4.00 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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.789