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_7716523
_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         'C8 H5 I Mo O3'
_chemical_formula_sum            'C8 H5 I Mo O3'
_chemical_formula_weight         371.96
_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                 90.736(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4658(3)
_cell_length_b                   7.8509(2)
_cell_length_c                   12.0747(3)
_cell_measurement_reflns_used    2189
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1050
_cell_measurement_theta_min      5.5530
_cell_volume                     992.05(5)
_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 0.993
_diffrn_measured_fraction_theta_max 0.974
_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    -97.00 -22.00   1.00    1.00    --  -36.18 -57.00  60.00   75
  2  \w    -12.00  33.00   1.00    1.00    --  -36.18  38.00-120.00   45
  3  \w     19.00  81.00   1.00    1.00    --   36.18  57.00   0.00   62
  4  \w     27.00  90.00   1.00    1.00    --   36.18-125.00 -90.00   63
  5  \w    141.00 174.00   1.00    1.00    --  109.99 111.00 -30.00   33
  6  \w    103.00 162.00   1.00    1.00    --  109.99  77.00 -90.00   59
  7  \w    104.00 170.00   1.00    1.00    --  109.99  77.00 -60.00   66
  8  \w     92.00 131.00   1.00    1.00    --  109.99 -30.00 150.00   39
  9  \w     41.00  85.00   1.00    1.00    --  109.99 -95.00 150.00   44
 10  \w    106.00 137.00   1.00    1.00    --  109.99 111.00 -30.00   31
 11  \w    111.00 168.00   1.00    1.00    --  109.99  77.00-180.00   57
 12  \w     40.00  84.00   1.00    1.00    --  109.99 -30.00 150.00   44
 13  \w     48.00 101.00   1.00    1.00    --  109.99 -95.00  60.00   53
 14  \w     96.00 177.00   1.00    1.00    --  109.99  61.00-120.00   81
;
_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      0.0885041000
_diffrn_orient_matrix_UB_12      0.1116526000
_diffrn_orient_matrix_UB_13      0.0725172000
_diffrn_orient_matrix_UB_21      0.1008368000
_diffrn_orient_matrix_UB_22      -0.1428387000
_diffrn_orient_matrix_UB_23      0.0014631000
_diffrn_orient_matrix_UB_31      0.0604838000
_diffrn_orient_matrix_UB_32      0.0749780000
_diffrn_orient_matrix_UB_33      -0.1050453000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3425
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.224
_diffrn_reflns_theta_min         5.559
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    35.053
_exptl_absorpt_correction_T_max  0.61017
_exptl_absorpt_correction_T_min  0.57918
_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    2.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.074
_exptl_crystal_size_rad          0.070
_refine_diff_density_max         2.289
_refine_diff_density_min         -2.023
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0861P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1845
_reflns_number_total             1924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_219_c_red_b2_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716523
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoIC8H5
_shelx_estimated_absorpt_t_max   0.181
_shelx_estimated_absorpt_t_min   0.054
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C8(H8), C5(H5)
;
_shelx_res_checksum              86075
_shelx_hkl_checksum              9656
_ins_header
;
TITL RMK_219_C_red_b2_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.465832   7.850881  12.074665  90.0000  90.7358  90.0000
ZERR    6.00   0.000254   0.000186   0.000295   0.0000   0.0021   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H Mo I
UNIT 48.00 30.00 6.00 6.00
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 2.385
_oxdiff_exptl_absorpt_empirical_full_min 0.521