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_7716522
_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         'C17 H20 As Mo O3, C F3 O3 S'
_chemical_formula_sum            'C18 H20 As F3 Mo O6 S'
_chemical_formula_weight         592.26
_chemical_properties_physical    Air-sensitive,Moisture-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_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.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                98.816(2)
_cell_angle_beta                 95.151(2)
_cell_angle_gamma                93.888(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2247(2)
_cell_length_b                   8.7800(3)
_cell_length_c                   15.8527(5)
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3410
_cell_measurement_theta_min      5.1080
_cell_volume                     1122.80(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.982
_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    -32.00  56.00   1.00    3.93    --   37.17 -38.00-180.00   88
  2  \w     53.00 102.00   1.00    3.93    --   37.17  57.00  90.00   49
  3  \w     32.00  91.00   1.00    3.93    --   37.17-125.00-120.00   59
  4  \w     14.00  51.00   1.00    3.93    --   37.17 -57.00  90.00   37
  5  \w    -19.00  33.00   1.00    3.93    --   37.17 -77.00 -90.00   52
  6  \w    -20.00  61.00   1.00    3.93    --   37.17 -77.00  30.00   81
  7  \w     17.00  74.00   1.00    3.93    --   37.17 -99.00 -30.00   57
  8  \w     11.00 101.00   1.00    3.93    --   37.17  19.00  30.00   90
  9  \w     43.00 123.00   1.00   15.74    --  111.00 -50.00 -90.00   80
 10  \w     67.00 106.00   1.00   15.74    --  111.00 -92.00 150.00   39
 11  \w    105.00 132.00   1.00   15.74    --  111.00 -77.00-180.00   27
 12  \w     42.00 103.00   1.00   15.74    --  111.00-111.00 -60.00   61
 13  \w     95.00 171.00   1.00   15.74    --  111.00  50.00 120.00   76
 14  \w    119.00 172.00   1.00   15.74    --  111.00  77.00  60.00   53
 15  \w     60.00 105.00   1.00   15.74    --  111.00-111.00 -90.00   45
 16  \w     41.00 109.00   1.00   15.74    --  111.00-111.00 120.00   68
 17  \w     74.00 108.00   1.00   15.74    --  111.00-111.00 -30.00   34
 18  \w    152.00 178.00   1.00   15.74    --  111.00 111.00-180.00   26
 19  \w     49.00 126.00   1.00   15.74    --  111.00 -38.00 -30.00   77
 20  \w    107.00 136.00   1.00   15.74    --  111.00 111.00-180.00   29
 21  \w     42.00 109.00   1.00   15.74    --  111.00-111.00  30.00   67
 22  \w     63.00 115.00   1.00   15.74    --  111.00 -50.00  60.00   52
 23  \w     44.00 130.00   1.00   15.74    --  111.00 -38.00 120.00   86
 24  \w    115.00 176.00   1.00   15.74    --  111.00  77.00 -90.00   61
 25  \w     55.00  92.00   1.00   15.74    --  111.00 -77.00-180.00   37
 26  \w     56.00 178.00   1.00   15.74    --  111.00   0.00  60.00  122
;
_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      -0.1686559000
_diffrn_orient_matrix_UB_12      -0.0549185000
_diffrn_orient_matrix_UB_13      -0.0496648000
_diffrn_orient_matrix_UB_21      0.0841861000
_diffrn_orient_matrix_UB_22      -0.0922883000
_diffrn_orient_matrix_UB_23      -0.0720012000
_diffrn_orient_matrix_UB_31      -0.0091014000
_diffrn_orient_matrix_UB_32      -0.1421702000
_diffrn_orient_matrix_UB_33      0.0460560000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8310
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.635
_diffrn_reflns_theta_min         5.115
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.804
_exptl_absorpt_correction_T_max  0.59151
_exptl_absorpt_correction_T_min  0.55803
_exptl_absorpt_correction_type   analytical
_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    1.752
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.046
_exptl_crystal_size_rad          0.051
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0480P)^2^+0.1934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3954
_reflns_number_total             4447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_219_e_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716522
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         S1F3Mo1As1O6C18H20
_reflns_odcompleteness_completeness 96.82
_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:
 C17(H17), C13(H13), C14(H14), C16(H16), C15(H15)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              67264
_shelx_hkl_checksum              28943
_ins_header
;
TITL RMK_219_E_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.224652   8.780038  15.852747  98.8163  95.1513  93.8883
ZERR    2.00   0.000244   0.000255   0.000478   0.0025   0.0024   0.0024
LATT  1
SFAC C H O F S As Mo
UNIT 36.00 40.00 12.00 6.00 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 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.812