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_7716525
_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         'C16 H20 As I Mo O2'
_chemical_formula_sum            'C16 H20 As I Mo O2'
_chemical_formula_weight         542.08
_chemical_properties_physical    Air-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                104.867(3)
_cell_angle_beta                 104.316(3)
_cell_angle_gamma                91.742(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8572(3)
_cell_length_b                   13.9206(4)
_cell_length_c                   16.0715(5)
_cell_measurement_reflns_used    7113
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1350
_cell_measurement_theta_min      5.1620
_cell_volume                     1846.43(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.964
_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    -86.00 -32.00   1.00    1.00    --  -36.18 125.00   0.00   54
  2  \w     -9.00  41.00   1.00    1.00    --   36.18 -38.00 120.00   50
  3  \w    -27.00  40.00   1.00    1.00    --   36.18 -57.00 -60.00   67
  4  \w     23.00 105.00   1.00    1.00    --   36.18  38.00  60.00   82
  5  \w     43.00  90.00   1.00    1.00    --   36.18-125.00-120.00   47
  6  \w    -22.00  44.00   1.00    1.00    --   36.18 -57.00  90.00   66
  7  \w     18.00 103.00   1.00    1.00    --   36.18  38.00 -90.00   85
  8  \w     42.00 126.00   1.00    1.00    --  109.99 -45.00  60.00   84
  9  \w     42.00 123.00   1.00    1.00    --  109.99 -45.00 -30.00   81
 10  \w     43.00 105.00   1.00    1.00    --  109.99 -61.00-120.00   62
 11  \w     42.00 106.00   1.00    1.00    --  109.99 -95.00   0.00   64
 12  \w     77.00 174.00   1.00    1.00    --  109.99  15.00 -30.00   97
 13  \w     40.00 109.00   1.00    1.00    --  109.99-111.00 -90.00   69
 14  \w     62.00 106.00   1.00    1.00    --  109.99 -95.00 150.00   44
 15  \w     58.00 131.00   1.00    1.00    --  109.99 -30.00-120.00   73
 16  \w     97.00 149.00   1.00    1.00    --  109.99  45.00  90.00   52
 17  \w    106.00 171.00   1.00    1.00    --  109.99 111.00 -30.00   65
 18  \w     98.00 176.00   1.00    1.00    --  109.99  61.00  30.00   78
 19  \w     46.00 109.00   1.00    1.00    --  109.99-111.00 120.00   63
;
_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      0.1513110000
_diffrn_orient_matrix_UB_12      -0.0338095000
_diffrn_orient_matrix_UB_13      -0.0243162000
_diffrn_orient_matrix_UB_21      -0.0888000000
_diffrn_orient_matrix_UB_22      -0.0310496000
_diffrn_orient_matrix_UB_23      -0.0996945000
_diffrn_orient_matrix_UB_31      0.0420646000
_diffrn_orient_matrix_UB_32      0.1055289000
_diffrn_orient_matrix_UB_33      -0.0065461000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11500
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.367
_diffrn_reflns_theta_min         3.781
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.938
_exptl_absorpt_correction_T_max  0.50578
_exptl_absorpt_correction_T_min  0.46185
_exptl_absorpt_correction_type   sphere
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.142
_exptl_crystal_size_rad          0.101
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.4711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6786
_reflns_number_total             7149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_219_c_red_a_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716525
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mo1As1O3I1C16H20
_reflns_odcompleteness_completeness 95.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.08
_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:
 C12B(H12B), C14A(H14A), C16B(H16B), C15B(H15B), C13A(H13A), C15A(H15A),
 C16A(H16A), C12A(H12A), C13B(H13B), C14B(H14B)
2.b Idealised Me refined as rotating group:
 C7B(H7BA,H7BB,H7BC), C10A(H10D,H10E,H10F), C8B(H8BA,H8BB,H8BC), C7A(H7AA,H7AB,
 H7AC), C11A(H11D,H11E,H11F), C8A(H8AA,H8AB,H8AC), C11B(H11A,H11B,H11C),
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C10B(H10A,H10B,H10C)
;
_shelx_res_checksum              60567
_shelx_hkl_checksum              16048
_ins_header
;
TITL RMK_219_C_red_a_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.857208  13.920570  16.071542 104.8674 104.3165  91.7418
ZERR    5.00   0.000296   0.000398   0.000527   0.0027   0.0029   0.0025
LATT  1
SFAC C H O As Mo I
UNIT 80.00 100.00 15.00 5.00 5.00 5.00
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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.713