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_7716529
_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         'I, C10 H18 As'
_chemical_formula_sum            'C10 H18 As I'
_chemical_formula_weight         340.06
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 91.549(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9883(4)
_cell_length_b                   7.6338(3)
_cell_length_c                   21.1208(8)
_cell_measurement_reflns_used    8577
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      31.9870
_cell_measurement_theta_min      3.6540
_cell_volume                     1287.50(10)
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_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    -94.00 -22.00   1.00   60.00    --  -17.53 155.00   0.72   72
  2  \w    -93.00 -33.00   1.00   60.00    --  -17.53 153.00 -99.35   60
  3  \w    -22.00  97.00   1.00   60.00    --   17.84  19.00-120.00  119
  4  \w     -6.00  92.00   1.00   60.00    --   17.84  37.00 -30.00   98
  5  \w     -5.00  42.00   1.00   60.00    --   17.84  77.00 150.00   47
  6  \w    -36.00  50.00   1.00   60.00    --   17.84 -77.00 -90.00   86
  7  \w    -40.00  49.00   1.00   60.00    --   17.84 -77.00-180.00   89
  8  \w     -9.00  41.00   1.00   60.00    --   17.84  57.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0760374000
_diffrn_orient_matrix_UB_12      -0.0268874000
_diffrn_orient_matrix_UB_13      0.0151765000
_diffrn_orient_matrix_UB_21      0.0351987000
_diffrn_orient_matrix_UB_22      -0.0154629000
_diffrn_orient_matrix_UB_23      -0.0299617000
_diffrn_orient_matrix_UB_31      0.0295121000
_diffrn_orient_matrix_UB_32      0.0875851000
_diffrn_orient_matrix_UB_33      -0.0006259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.410
_diffrn_reflns_theta_min         3.240
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.995
_exptl_absorpt_correction_T_max  0.50085
_exptl_absorpt_correction_T_min  0.48902
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: C6D6'
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.056
_exptl_crystal_size_rad          0.065
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         4258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0178P)^2^+1.0580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3488
_reflns_number_total             4258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_219_c_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716529
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H18As1I1
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C2(H2a,H2b,H2c), C8(H8a,H8b,H8c), C1(H1a,H1b,H1c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c)
;
_shelx_res_checksum              37856
_shelx_hkl_checksum              90989
_ins_header
;
TITL RMK_219_C_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073   7.988313   7.633773  21.120777  90.0000  91.5493  90.0000
ZERR    6.00   0.000384   0.000288   0.000791   0.0000   0.0042   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H As I
UNIT 60.00 108.00 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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.890