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_7716528
_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         'C20 H17 As F6 Mo O3'
_chemical_formula_sum            'C20 H17 As F6 Mo O3'
_chemical_formula_weight         590.20
_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             2022-01-29
_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                90
_cell_angle_beta                 103.3860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.62420(10)
_cell_length_b                   17.9549(2)
_cell_length_c                   14.1123(2)
_cell_measurement_reflns_used    8558
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6210
_cell_measurement_theta_min      5.7960
_cell_volume                     2125.87(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 0.997
_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     39.00  97.00   1.00    1.00    --   36.95  57.00-120.00   58
  2  \w     55.00  89.00   1.00    1.00    --   36.95-125.00   0.00   34
  3  \w     18.00  67.00   1.00    1.00    --   36.95  38.00-180.00   49
  4  \w     53.00  91.00   1.00    1.00    --   36.95  57.00  90.00   38
  5  \w     -7.00  57.00   1.00    1.00    --   36.95 -77.00 150.00   64
  6  \w     49.00  80.00   1.00    1.00    --   36.95-125.00  90.00   31
  7  \w     32.00 105.00   1.00    1.00    --   36.95  38.00  90.00   73
  8  \w     30.00  77.00   1.00    1.00    --   36.95  38.00-150.00   47
  9  \w    103.00 177.00   1.00    4.00    --  111.00  77.00-150.00   74
 10  \w     73.00 109.00   1.00    4.00    --  111.00-111.00 -30.00   36
 11  \w    145.00 177.00   1.00    4.00    --  111.00  77.00-180.00   32
 12  \w     61.00  88.00   1.00    4.00    --  111.00-111.00-150.00   27
 13  \w    142.00 168.00   1.00    4.00    --  111.00  38.00 120.00   26
 14  \w     95.00 131.00   1.00    4.00    --  111.00  50.00  90.00   36
 15  \w    103.00 177.00   1.00    4.00    --  111.00  77.00 -90.00   74
 16  \w     50.00 109.00   1.00    4.00    --  111.00-111.00  60.00   59
 17  \w     74.00  99.00   1.00    4.00    --  111.00  12.00  30.00   25
 18  \w     74.00 100.00   1.00    4.00    --  111.00 -92.00-120.00   26
 19  \w     81.00 108.00   1.00    4.00    --  111.00-111.00  30.00   27
 20  \w    143.00 171.00   1.00    4.00    --  111.00  12.00  30.00   28
 21  \w     43.00  68.00   1.00    4.00    --  111.00-111.00  30.00   25
 22  \w     61.00 129.00   1.00    4.00    --  111.00 -38.00  90.00   68
 23  \w     63.00 109.00   1.00    4.00    --  111.00-111.00 -90.00   46
 24  \w     84.00 133.00   1.00    4.00    --  111.00 -77.00  90.00   49
 25  \w     84.00 109.00   1.00    4.00    --  111.00-111.00 150.00   25
 26  \w    122.00 175.00   1.00    4.00    --  111.00  50.00 -30.00   53
 27  \w    105.00 146.00   1.00    4.00    --  111.00  64.00-120.00   41
 28  \w    134.00 159.00   1.00    4.00    --  111.00 111.00-120.00   25
 29  \w     96.00 129.00   1.00    4.00    --  111.00 178.00  60.00   33
 30  \w    103.00 128.00   1.00    4.00    --  111.00 178.00 -90.00   25
 31  \w     80.00 109.00   1.00    4.00    --  111.00-111.00   0.00   29
 32  \w     42.00  69.00   1.00    4.00    --  111.00 -92.00-120.00   27
 33  \w     64.00 124.00   1.00    4.00    --  111.00 -64.00 -90.00   60
;
_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      -0.0905806000
_diffrn_orient_matrix_UB_12      -0.0608838000
_diffrn_orient_matrix_UB_13      -0.0676549000
_diffrn_orient_matrix_UB_21      -0.0931891000
_diffrn_orient_matrix_UB_22      0.0603749000
_diffrn_orient_matrix_UB_23      -0.0674471000
_diffrn_orient_matrix_UB_31      0.1298390000
_diffrn_orient_matrix_UB_32      0.0009274000
_diffrn_orient_matrix_UB_33      -0.0588911000
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13901
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.748
_diffrn_reflns_theta_min         4.053
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.451
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.333
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0833P)^2^+0.7784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4044
_reflns_number_total             4288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_233_a_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716528
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H17As1O3Mo1F6
_chemical_oxdiff_usercomment     'Et2O evap at -30 '
_reflns_odcompleteness_completeness 98.60
_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:
 C18(H18), C19(H19), C17(H17), C16(H16), C20(H20)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C12(H12a,H12b,H12c), C14(H14a,H14b,
 H14c)
;
_shelx_res_checksum              49126
_shelx_hkl_checksum              97077
_ins_header
;
TITL RMK_233_A_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   8.624161  17.954878  14.112303  90.0000 103.3861  90.0000
ZERR    4.00   0.000111   0.000237   0.000179   0.0000   0.0013   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O F As Mo
UNIT 80.00 68.00 12.00 24.00 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 1.613
_oxdiff_exptl_absorpt_empirical_full_min 0.709