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_7716526
_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         'C29 H22.998 As'
_chemical_formula_sum            'C29 H23 As'
_chemical_formula_weight         446.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-01 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.5014(2)
_cell_length_b                   26.5014(2)
_cell_length_c                   12.16700(10)
_cell_measurement_reflns_used    6296
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.3400
_cell_measurement_theta_min      5.1920
_cell_volume                     8545.18(12)
_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 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 0.998
_diffrn_measured_fraction_theta_max 0.984
_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     44.00  69.00   1.00    5.00    --   36.95 -99.00-120.00   25
  2  \w     31.00  85.00   1.00    5.00    --   36.95-125.00  60.00   54
  3  \w    -32.00  48.00   1.00    5.00    --   36.95 -38.00-180.00   80
  4  \w     41.00  69.00   1.00   25.00    --  111.00-111.00 150.00   28
  5  \w    140.00 174.00   1.00   25.00    --  111.00  38.00  60.00   34
  6  \w     45.00  70.00   1.00   25.00    --  111.00 -64.00-120.00   25
  7  \w    144.00 172.00   1.00   25.00    --  111.00 111.00-150.00   28
  8  \w    106.00 131.00   1.00   25.00    --  111.00 111.00-150.00   25
  9  \w     98.00 131.00   1.00   25.00    --  111.00 -64.00-120.00   33
 10  \w     93.00 133.00   1.00   25.00    --  111.00  38.00  60.00   40
 11  \w     55.00  90.00   1.00   25.00    --  111.00 -92.00-150.00   35
 12  \w     45.00  78.00   1.00   25.00    --  111.00 -92.00-180.00   33
 13  \w     46.00  72.00   1.00   25.00    --  111.00 -77.00 -60.00   26
 14  \w     90.00 121.00   1.00   25.00    --  111.00 -77.00 -60.00   31
 15  \w    131.00 177.00   1.00   25.00    --  111.00  77.00 -60.00   46
 16  \w    139.00 172.00   1.00   25.00    --  111.00  77.00 -90.00   33
;
_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      0.0530373000
_diffrn_orient_matrix_UB_12      -0.0066150000
_diffrn_orient_matrix_UB_13      0.0497497000
_diffrn_orient_matrix_UB_21      -0.0106024000
_diffrn_orient_matrix_UB_22      0.0433386000
_diffrn_orient_matrix_UB_23      0.0811535000
_diffrn_orient_matrix_UB_31      -0.0212619000
_diffrn_orient_matrix_UB_32      -0.0381732000
_diffrn_orient_matrix_UB_33      0.0835479000
_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  0.0137
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11604
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.569
_diffrn_reflns_theta_min         3.998
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.388
_exptl_crystal_description       prism
_exptl_crystal_F_000             3680
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/n-hexane'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0372P)^2^+19.0023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4103
_reflns_number_total             4256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_211_c_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_original_cell_volume        8545.18(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7716526
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H23As
_chemical_oxdiff_usercomment     'DCM/MeOH at -20'
_reflns_odcompleteness_completeness 97.34
_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. Restrained distances
 As1-C5 \\sim As1'-C5
 with sigma of 0.02
 As1-C1 \\sim As1'-C1'
 with sigma of 0.02
 C1-H1A \\sim C1'-H1A
 with sigma of 0.02
 As1-C2 \\sim As1'-C2
 with sigma of 0.02
 C1-H1B \\sim C1'-H1B
 with sigma of 0.02
 C1-H1C \\sim C1'-H1C
 with sigma of 0.02
 As1-H1A \\sim As1'-H1A
 with sigma of 0.04
 As1-H1B \\sim As1'-H1B
 with sigma of 0.04
 As1-H1C \\sim As1'-H1C
 with sigma of 0.04
 C5-C1 \\sim C5-C1'
 with sigma of 0.04
 C1-C2 \\sim C1'-C2
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1') = Uanis(C1)
4. Others
 Sof(As1')=Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=1-FVAR(1)
 Sof(As1)=Sof(C1)=FVAR(1)
 Fixed Sof: H1A(0.88921) H1B(0.88921) H1C(0.88921)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C25(H25), C23(H23), C29(H29), C19(H19), C15(H15), C17(H17), C9(H9),
 C27(H27), C26(H26), C14(H14), C16(H16), C11(H11), C10(H10), C13(H13), C22(H22),
  C8(H8), C20(H20), C28(H28), C21(H21)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1'(H1'A,H1'B,H1'C)
;
_shelx_res_checksum              29482
_shelx_hkl_checksum              18031
_ins_header
;
TITL RMK_211_C_scale in I4(1)/a 
REM I4(1)/a (#88 in standard setting)
CELL 1.54184  26.501388  26.501388  12.166972  90.0000  90.0000  90.0000
ZERR   16.00   0.000199   0.000199   0.000134   0.0000   0.0000   0.0000
LATT  2
SYMM -x+1/2,-y, z+1/2 
SYMM -y+3/4, x+1/4, z+1/4 
SYMM  y+3/4,-x+3/4, z+3/4 
SFAC C H As
UNIT 464.00 368.00 16.00
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 1.060
_oxdiff_exptl_absorpt_empirical_full_min 0.943