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_7716527
_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         'C22 H23 As Mo O7'
_chemical_formula_sum            'C22 H23 As Mo O7'
_chemical_formula_weight         570.26
_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                80.769(3)
_cell_angle_beta                 87.205(3)
_cell_angle_gamma                81.552(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3557(3)
_cell_length_b                   8.5540(2)
_cell_length_c                   15.9822(6)
_cell_measurement_reflns_used    10561
_cell_measurement_temperature    149.98(15)
_cell_measurement_theta_max      31.9190
_cell_measurement_theta_min      4.2070
_cell_volume                     1114.92(6)
_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      149.98(15)
_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 0.885
_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    -50.00  42.00   1.00   12.63    --  -17.69  77.00 -30.00   92
  2  \w    -74.00  -6.00   1.00   12.63    --  -17.69 125.00  95.61   68
  3  \w    -10.00  91.00   1.00   12.63    --   18.00  57.00-120.00  101
  4  \w     -6.00  91.00   1.00   12.63    --   18.00  37.00  30.00   97
  5  \w    -41.00  51.00   1.00   12.63    --   18.00 -77.00-120.00   92
  6  \w    -42.00  51.00   1.00   12.63    --   18.00 -77.00  90.00   93
  7  \w     -9.00  90.00   1.00   12.63    --   18.00  57.00 120.00   99
  8  \w    -15.00  19.00   1.00   12.63    --   18.00  77.00   0.00   34
;
_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      0.0098754000
_diffrn_orient_matrix_UB_12      0.0131010000
_diffrn_orient_matrix_UB_13      -0.0447940000
_diffrn_orient_matrix_UB_21      -0.0683970000
_diffrn_orient_matrix_UB_22      -0.0385314000
_diffrn_orient_matrix_UB_23      -0.0035795000
_diffrn_orient_matrix_UB_31      -0.0509327000
_diffrn_orient_matrix_UB_32      0.0744611000
_diffrn_orient_matrix_UB_33      -0.0019224000
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23753
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.639
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
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    1.699
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.3554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5997
_reflns_number_total             7225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_225_e_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C22H23As1Mo1O7
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.475
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C19(H19), C18(H18), C20(H20), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C8(H8a,H8b,H8c), C15(H15a,H15b,H15c), C14(H14a,H14b,
 H14c), C16(H16a,H16b,H16c), C9(H9a,H9b,H9c)
;
_shelx_res_checksum              77780
_shelx_hkl_checksum              78144
_ins_header
;
TITL RMK_225_E_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073   8.355720   8.553967  15.982212  80.7685  87.2054  81.5525
ZERR    2.00   0.000265   0.000249   0.000585   0.0027   0.0028   0.0025
LATT  1
SFAC C H O As Mo
UNIT 44.00 46.00 14.00 2.00 2.00
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 1.474
_oxdiff_exptl_absorpt_empirical_full_min 0.884