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

data_7718629
_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         'C12 H5 N O5 W'
_chemical_formula_sum            'C12 H5 N O5 W'
_chemical_formula_weight         427.02
_chemical_properties_physical    Air-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             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.33250(10)
_cell_length_b                   13.4583(2)
_cell_length_c                   9.66530(10)
_cell_measurement_reflns_used    6395
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.5280
_cell_measurement_theta_min      4.3480
_cell_volume                     1320.61(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.981
_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    -75.00 -38.00   0.50    0.50    --  -46.45 101.00 -89.00   74
  2  \w    -35.00  18.00   0.50    0.50    --  -46.45 101.00 -89.00  106
  3  \w     62.00  88.00   0.50    0.50    --  107.75-101.00 166.00   52
  4  \w    112.00 170.00   0.50    0.50    --  107.75 101.00 -89.00  116
  5  \w     -7.00  19.00   0.50    0.50    --  -46.45  19.00-120.00   52
  6  \w    -21.00  17.00   0.50    0.50    --  -46.45  38.00  30.00   76
  7  \w     -3.00  28.00   0.50    0.50    --  -46.45  19.00 -90.00   62
  8  \w     -7.00  25.00   0.50    0.50    --  -46.45  19.00   0.00   64
  9  \w      5.00  56.00   0.50    0.50    --   46.45-101.00 166.00  102
 10  \w     35.00  87.00   0.50    0.50    --  107.75 -61.00-150.00  104
 11  \w     32.00  59.00   0.50    0.50    --  107.75 -30.00-180.00   54
 12  \w     39.00  73.00   0.50    0.50    --  107.75 -45.00 -90.00   68
 13  \w     47.00  73.00   0.50    0.50    --  107.75 -45.00 -30.00   52
 14  \w     36.00  66.00   0.50    0.50    --  107.75 -45.00  60.00   60
 15  \w     55.00  81.00   0.50    0.50    --  107.75 -95.00-150.00   52
 16  \w     46.00  72.00   0.50    0.50    --  107.75-125.00   0.00   52
 17  \w     33.00  58.00   0.50    0.50    --  107.75 -30.00-120.00   50
 18  \w     34.00 121.00   0.50    0.50    --  107.75 -77.00-180.00  174
 19  \w     33.00  58.00   0.50    0.50    --  107.75 -30.00 120.00   50
 20  \w     35.00  85.00   0.50    0.50    --  107.75 -61.00-120.00  100
 21  \w     33.00  58.00   0.50    0.50    --  107.75 -30.00  60.00   50
 22  \w     95.00 163.00   0.50    0.50    --  107.75 125.00 -30.00  136
 23  \w    113.00 139.00   0.50    0.50    --  107.75  45.00 150.00   52
 24  \w    152.00 177.00   0.50    0.50    --  107.75  45.00 150.00   50
 25  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00-150.00   50
 26  \w     94.00 148.00   0.50    0.50    --  107.75 125.00-180.00  108
 27  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 28  \w     74.00  99.00   0.50    0.50    --  107.75 -95.00-120.00   50
 29  \w     33.00  58.00   0.50    0.50    --  107.75 -30.00 150.00   50
 30  \w     40.00  67.00   0.50    0.50    --  107.75 -45.00 -60.00   54
;
_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      -0.0719130000
_diffrn_orient_matrix_UB_12      0.0850964000
_diffrn_orient_matrix_UB_13      -0.0896457000
_diffrn_orient_matrix_UB_21      0.0223450000
_diffrn_orient_matrix_UB_22      0.0682038000
_diffrn_orient_matrix_UB_23      0.1302833000
_diffrn_orient_matrix_UB_31      0.1317223000
_diffrn_orient_matrix_UB_32      0.0348274000
_diffrn_orient_matrix_UB_33      -0.0361964000
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9690
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.868
_diffrn_reflns_theta_min         4.355
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.379
_exptl_absorpt_correction_T_max  0.32130
_exptl_absorpt_correction_T_min  0.23454
_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            'translucent dark yellow'
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_description       needle
_exptl_crystal_F_000             792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/hexane'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          0.063
_refine_diff_density_max         2.774
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0597P)^2^+0.6654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2571
_reflns_number_total             2774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_365_b_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718629
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12H5W1O5N1 '
_chemical_oxdiff_usercomment     'Et2O/hexane at 0 deg'
_shelx_estimated_absorpt_t_max   0.440
_shelx_estimated_absorpt_t_min   0.167
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C8(H8), C9(H9), C11(H11)
;
_shelx_res_checksum              50616
_shelx_hkl_checksum              54237
_ins_header
;
TITL RMK_365_B_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  10.332470  13.458264   9.665321  90.0000 100.7130  90.0000
ZERR    4.00   0.000148   0.000209   0.000140   0.0000   0.0014   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O W
UNIT 48.00 20.00 4.00 20.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.06 0.13 0.17
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 2.287
_oxdiff_exptl_absorpt_empirical_full_min 0.696