Pnictogen-functionalised isocyanide ligands.
Kirk, Ryan M.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8881–8887; doi:10.1039/d5dt00992h

data_7718633
_publ_section_title
;
 Pnictogen-functionalised isocyanide ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8881
_journal_page_last               8887
_journal_paper_doi               10.1039/d5dt00992h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C14 H18 As N O5 W'
_chemical_formula_sum            'C14 H18 As N O5 W'
_chemical_formula_weight         539.06
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2713(2)
_cell_length_b                   13.80740(10)
_cell_length_c                   5.94700(10)
_cell_measurement_reflns_used    6068
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.6180
_cell_measurement_theta_min      3.1200
_cell_volume                     1828.75(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -32.00  -6.00   0.50    0.50    --  -46.45 103.00  17.00   52
  2  \w    106.00 150.00   0.50    0.50    --  107.75 100.00 -76.00   88
  3  \w     33.00  58.00   0.50    0.50    --  107.75 -33.00  15.00   50
  4  \w     96.00 145.00   0.50    0.50    --  107.75  33.00 174.00   98
  5  \w    149.00 176.00   0.50    0.50    --  107.75  33.00 174.00   54
  6  \w     36.00  75.00   0.50    0.50    --  107.75-103.00 -84.00   78
  7  \w     -5.00  20.00   0.50    0.50    --  -46.45  19.00-150.00   50
  8  \w     -8.00  28.00   0.50    0.50    --  -46.45  19.00 -30.00   72
  9  \w     -9.00  21.00   0.50    0.50    --  -46.45  33.00 174.00   60
 10  \w     -8.00  28.00   0.50    0.50    --  -46.45  19.00 -90.00   72
 11  \w    -22.00  13.00   0.50    0.50    --  -46.45  38.00 120.00   70
 12  \w     32.00  58.00   0.50    0.50    --  107.75 -30.00 150.00   52
 13  \w     40.00  68.00   0.50    0.50    --  107.75 -45.00 -90.00   56
 14  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00   0.00   50
 15  \w     63.00 109.00   0.50    0.50    --  107.75-125.00 -90.00   92
 16  \w     36.00  66.00   0.50    0.50    --  107.75 -45.00 150.00   60
 17  \w     38.00  73.00   0.50    0.50    --  107.75 -61.00   0.00   70
 18  \w     52.00  89.00   0.50    0.50    --  107.75 -61.00-120.00   74
 19  \w     38.00  70.00   0.50    0.50    --  107.75 -45.00 -60.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0552730000
_diffrn_orient_matrix_UB_12      0.0669274000
_diffrn_orient_matrix_UB_13      -0.0094628000
_diffrn_orient_matrix_UB_21      0.0369060000
_diffrn_orient_matrix_UB_22      0.0820897000
_diffrn_orient_matrix_UB_23      0.1078358000
_diffrn_orient_matrix_UB_31      0.0192387000
_diffrn_orient_matrix_UB_32      0.0349952000
_diffrn_orient_matrix_UB_33      -0.2353476000
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7592
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.051
_diffrn_reflns_theta_min         3.970
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.901
_exptl_absorpt_correction_T_max  0.34913
_exptl_absorpt_correction_T_min  0.26864
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.958
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.066
_refine_diff_density_max         2.699
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+7.8339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1955
_reflns_number_total             2010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_360_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718633
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H18As1W1N1O5
_chemical_oxdiff_usercomment     'benzene evap'
_shelx_estimated_absorpt_t_max   0.543
_shelx_estimated_absorpt_t_min   0.091
_olex2_refinement_description
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              27001
_shelx_hkl_checksum              39810
_ins_header
;
TITL RMK_360_scale in Pnma 
REM Pnma (#62, found as Pcmn in -cba setting)
CELL 1.54184  22.271304  13.807379   5.946994  90.0000  90.0000  90.0000
ZERR    4.00   0.000215   0.000130   0.000062   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z+1/2 
SFAC C H N O As W
UNIT 56.00 72.00 4.00 20.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.05 0.23 0.33
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 2.703
_oxdiff_exptl_absorpt_empirical_full_min 0.669