Electrophilic As-functionalisation of σ-arsolido complexes.
Kirk, Ryan M.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11959–11969; doi:10.1039/d4dt01371a

data_7716524
_publ_section_title
;
 Electrophilic As-functionalisation of &#x3c3;-arsolido complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11959
_journal_page_last               11969
_journal_paper_doi               10.1039/d4dt01371a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H24 As Mo O3 Si, C F3 O3 S'
_chemical_formula_sum            'C19 H24 As F3 Mo O6 S Si'
_chemical_formula_weight         636.39
_chemical_properties_physical    Moisture-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_creation_date             2022-01-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-30 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.920(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9991(3)
_cell_length_b                   23.3532(3)
_cell_length_c                   7.29480(10)
_cell_measurement_reflns_used    5795
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.4980
_cell_measurement_theta_min      5.9730
_cell_volume                     2509.95(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.981
_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    -27.00  -1.00   1.00    1.00    --   36.95 -57.00  30.00   26
  2  \w     31.00  75.00   1.00    1.00    --   36.95 -99.00-120.00   44
  3  \w      1.00  54.00   1.00    1.00    --   36.95 -57.00  30.00   53
  4  \w    -30.00  54.00   1.00    1.00    --   36.95 -57.00 -60.00   84
  5  \w     20.00 105.00   1.00    1.00    --   36.95  38.00-180.00   85
  6  \w    100.00 177.00   1.00    3.30    --  111.00  50.00 120.00   77
  7  \w    114.00 177.00   1.00    3.30    --  111.00  77.00  60.00   63
  8  \w     74.00 131.00   1.00    3.30    --  111.00 -64.00-120.00   57
  9  \w     43.00 118.00   1.00    3.30    --  111.00 -38.00 -30.00   75
 10  \w     43.00 126.00   1.00    3.30    --  111.00 -50.00  60.00   83
 11  \w    119.00 177.00   1.00    3.30    --  111.00 111.00   0.00   58
 12  \w     51.00 106.00   1.00    3.30    --  111.00 -92.00  30.00   55
 13  \w    110.00 178.00   1.00    3.30    --  111.00  38.00 150.00   68
;
_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      -0.1018680000
_diffrn_orient_matrix_UB_12      -0.0001760000
_diffrn_orient_matrix_UB_13      -0.0708387000
_diffrn_orient_matrix_UB_21      -0.0112215000
_diffrn_orient_matrix_UB_22      0.0582545000
_diffrn_orient_matrix_UB_23      -0.1094414000
_diffrn_orient_matrix_UB_31      -0.0206302000
_diffrn_orient_matrix_UB_32      -0.0309689000
_diffrn_orient_matrix_UB_33      -0.2057850000
_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  0.0207
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9888
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.656
_diffrn_reflns_theta_min         4.832
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.470
_exptl_absorpt_correction_T_max  0.54879
_exptl_absorpt_correction_T_min  0.51041
_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    1.684
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.087
_exptl_crystal_size_rad          0.065
_refine_diff_density_max         1.504
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0607P)^2^+4.6537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4570
_reflns_number_total             4964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_223_c_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_original_cell_volume        2509.95(9)
_cod_database_code               7716524
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H24As1F3Mo1O6S1
_reflns_odcompleteness_completeness 96.76
_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 Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C16(H16), C17(H17), C18(H18), C4(H4)
2.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c),
 C13(H13a,H13b,H13c), C11(H11a,H11b,H11c)
;
_shelx_res_checksum              10174
_shelx_hkl_checksum              37445
_ins_header
;
TITL RMK_223_C_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  16.999093  23.353169   7.294825  90.0000 119.9198  90.0000
ZERR    4.00   0.000331   0.000316   0.000145   0.0000   0.0026   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O F S As Mo
UNIT 76.00 96.00 24.00 12.00 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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.745