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

data_7713700
_publ_section_title
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 Free and Coordinated Biarsolyls
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02070C
_journal_year                    2023
_chemical_formula_moiety         'C25 H18 As Co3 Mo O11'
_chemical_formula_sum            'C25 H18 As Co3 Mo O11'
_chemical_formula_weight         842.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2f0plr
_audit_creation_date             2023-01-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-08 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.5150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.0109(4)
_cell_length_b                   11.14800(10)
_cell_length_c                   17.8024(2)
_cell_measurement_reflns_used    9326
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6050
_cell_measurement_theta_min      4.2270
_cell_volume                     5855.98(12)
_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 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 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    -12.00  29.00   1.00    5.00    --  -36.95  57.00 150.00   41
  2  \w    -12.00  13.00   1.00    5.00    --   36.95 -77.00-180.00   25
  3  \w    -16.00  61.00   1.00    5.00    --   36.95 -77.00  90.00   77
  4  \w     15.00  41.00   1.00    5.00    --   36.95-107.00-100.00   26
  5  \w      2.00  53.00   1.00    5.00    --   36.95 -57.00-150.00   51
  6  \w      6.00  55.00   1.00    5.00    --   36.95 -77.00 150.00   49
  7  \w      9.00  34.00   1.00    5.00    --   36.95 -99.00   0.00   25
  8  \w     45.00  76.00   1.00    5.00    --   36.95 -99.00   0.00   31
  9  \w     49.00  77.00   1.00    5.00    --   36.95-107.00-100.00   28
 10  \w     32.00  59.00   1.00    5.00    --   36.95-125.00  60.00   27
 11  \w     24.00  58.00   1.00    5.00    --   36.95 -77.00-180.00   34
 12  \w     56.00 100.00   1.00    5.00    --   36.95  57.00 -60.00   44
 13  \w    147.00 178.00   1.00   25.00    --  111.00  50.00 -90.00   31
 14  \w    101.00 126.00   1.00   25.00    --  111.00 -42.00 118.00   25
 15  \w     94.00 144.00   1.00   25.00    --  111.00  50.00 -90.00   50
 16  \w     97.00 123.00   1.00   25.00    --  111.00 -77.00 -60.00   26
 17  \w    104.00 163.00   1.00   25.00    --  111.00  77.00   0.00   59
 18  \w    132.00 167.00   1.00   25.00    --  111.00  25.00 -30.00   35
 19  \w     67.00  95.00   1.00   25.00    --  111.00-111.00 -60.00   28
 20  \w     44.00 120.00   1.00   25.00    --  111.00 -50.00 -30.00   76
 21  \w     44.00 100.00   1.00   25.00    --  111.00 -50.00 120.00   56
 22  \w     94.00 142.00   1.00   25.00    --  111.00  25.00-150.00   48
 23  \w    113.00 142.00   1.00   25.00    --  111.00  77.00 -30.00   29
 24  \w     76.00 112.00   1.00   25.00    --  111.00 178.00  30.00   36
 25  \w     65.00  91.00   1.00   25.00    --  111.00 -77.00 -90.00   26
 26  \w    127.00 159.00   1.00   25.00    --  111.00 111.00 -90.00   32
 27  \w     46.00 106.00   1.00   25.00    --  111.00-111.00 120.00   60
 28  \w     44.00  69.00   1.00   25.00    --  111.00 -92.00-180.00   25
 29  \w     51.00  86.00   1.00   25.00    --  111.00 -92.00  60.00   35
 30  \w     62.00  88.00   1.00   25.00    --  111.00-111.00  30.00   26
 31  \w     45.00  71.00   1.00   25.00    --  111.00 -38.00  60.00   26
 32  \w     94.00 162.00   1.00   25.00    --  111.00  25.00-120.00   68
 33  \w     94.00 119.00   1.00   25.00    --  111.00  25.00 -30.00   25
 34  \w     51.00  90.00   1.00   25.00    --  111.00 -45.00 -68.64   39
;
_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      0.0310805000
_diffrn_orient_matrix_UB_12      0.0703325000
_diffrn_orient_matrix_UB_13      -0.0443137000
_diffrn_orient_matrix_UB_21      -0.0400258000
_diffrn_orient_matrix_UB_22      0.0176989000
_diffrn_orient_matrix_UB_23      -0.0667455000
_diffrn_orient_matrix_UB_31      -0.0125161000
_diffrn_orient_matrix_UB_32      0.1176399000
_diffrn_orient_matrix_UB_33      0.0364689000
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17415
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.828
_diffrn_reflns_theta_min         4.239
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.264
_exptl_absorpt_correction_T_max  0.17627
_exptl_absorpt_correction_T_min  0.07636
_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    1.910
_exptl_crystal_description       prism
_exptl_crystal_F_000             3296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.115
_exptl_crystal_size_rad          0.107
_refine_diff_density_max         0.504
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0548P)^2^+6.1070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5676
_reflns_number_total             5839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02070c2.cif
_cod_data_source_block           rmk_247_a_scale
_cod_database_code               7713700
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H18As1Mo1O11Co3
_chemical_oxdiff_usercomment     'DCM/hexane evap -20 '
_reflns_odcompleteness_completeness 97.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Ternary CH refined with riding coordinates:
 C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C21(H21), C25(H25), C24(H24), C22(H22)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              83266
_ins_header
;
TITL RMK_247_A_scale in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  30.010917  11.147985  17.802448  90.0000 100.5149  90.0000
ZERR    8.00   0.000364   0.000125   0.000229   0.0000   0.0012   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H O Co As Mo
UNIT 200.00 144.00 88.00 24.00 8.00 8.00
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 1.610
_oxdiff_exptl_absorpt_empirical_full_min 0.585