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

data_7718636
_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         'C15 H11 N O5 W'
_chemical_formula_sum            'C15 H11 N O5 W'
_chemical_formula_weight         469.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-20
_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                 103.5200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.21210(10)
_cell_length_b                   15.24780(10)
_cell_length_c                   11.81920(10)
_cell_measurement_reflns_used    10261
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      77.8870
_cell_measurement_theta_min      2.8860
_cell_volume                     1614.17(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      149.99(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 0.984
_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    -29.00  26.00   0.50    0.50    --  -46.45  60.00  88.00  110
  2  \w   -115.00 -39.00   0.50    0.50    --  -46.45 -60.00 -51.00  152
  3  \w     50.00  75.00   0.50    0.50    --   46.45  60.00  88.00   50
  4  \w     24.00  62.00   0.50    0.50    --   46.45 -60.00 -51.00   76
  5  \w    102.00 176.00   0.50    0.50    --  107.75  60.00  88.00  148
  6  \w     44.00  75.00   0.50    0.50    --  107.75 -60.00 -51.00   62
  7  \w     -8.00  22.00   0.50    0.50    --  -46.45  19.00  90.00   60
  8  \w      3.00  30.00   0.50    0.50    --  -46.45  19.00-120.00   54
  9  \w     -8.00  29.00   0.50    0.50    --  -46.45  19.00-150.00   74
 10  \w    -22.00   5.00   0.50    0.50    --  -46.45  38.00-120.00   54
 11  \w     37.00  72.00   0.50    0.50    --  107.75 -45.00-180.00   70
 12  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00 -60.00   50
 13  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00 150.00   50
 14  \w     35.00  60.00   0.50    0.50    --  107.75 -77.00-120.00   50
 15  \w     32.00  59.00   0.50    0.50    --  107.75 -30.00 -30.00   54
 16  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 17  \w     32.00  58.00   0.50    0.50    --  107.75 -30.00-180.00   52
 18  \w     41.00  66.00   0.50    0.50    --  107.75 -45.00   0.00   50
 19  \w     39.00  67.00   0.50    0.50    --  107.75 -45.00 150.00   56
 20  \w     37.00  86.00   0.50    0.50    --  107.75 -95.00 -60.00   98
 21  \w     40.00  77.00   0.50    0.50    --  107.75 -61.00   0.00   74
 22  \w    142.00 167.00   0.50    0.50    --  107.75  45.00-180.00   50
 23  \w     61.00  87.00   0.50    0.50    --  107.75 -61.00  60.00   52
 24  \w     94.00 119.00   0.50    0.50    --  107.75  45.00-180.00   50
 25  \w     34.00  59.00   0.50    0.50    --  107.75 -30.00   0.00   50
 26  \w     88.00 119.00   0.50    0.50    --  107.75 -77.00-120.00   62
 27  \w     34.00  59.00   0.50    0.50    --  107.75 -30.00 -90.00   50
 28  \w     60.00  85.00   0.50    0.50    --  107.75 -61.00-180.00   50
 29  \w     97.00 133.00   0.50    0.50    --  107.75  77.00   0.00   72
 30  \w     41.00  66.00   0.50    0.50    --  107.75 -45.00  90.00   50
 31  \w     46.00  73.00   0.50    0.50    --  107.75 -45.00-120.00   54
 32  \w     37.00  62.00   0.50    0.50    --  107.75 -45.00  30.00   50
 33  \w     44.00  71.00   0.50    0.50    --  107.75 -61.00  90.00   54
 34  \w     33.00  58.00   0.50    0.50    --  107.75 -30.00 120.00   50
;
_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      -0.0351524000
_diffrn_orient_matrix_UB_12      0.0675944000
_diffrn_orient_matrix_UB_13      0.0867329000
_diffrn_orient_matrix_UB_21      -0.1478449000
_diffrn_orient_matrix_UB_22      0.0227789000
_diffrn_orient_matrix_UB_23      -0.0866371000
_diffrn_orient_matrix_UB_31      -0.0805436000
_diffrn_orient_matrix_UB_32      -0.0715773000
_diffrn_orient_matrix_UB_33      0.0542252000
_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  0.0218
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.142
_diffrn_reflns_theta_min         4.819
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.468
_exptl_absorpt_correction_T_max  0.27269
_exptl_absorpt_correction_T_min  0.17688
_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 colourless'
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/hexane'
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.098
_exptl_crystal_size_rad          0.092
_refine_diff_density_max         0.461
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0322P)^2^+0.8492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3286
_reflns_number_total             3408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_365_a_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718636
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H11N1O5W1
_chemical_oxdiff_usercomment     'Et2O/hexane at 0 deg'
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.140
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11)
1.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              8178
_shelx_hkl_checksum              26316
_ins_header
;
TITL RMK_365_A_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.212120  15.247762  11.819159  90.0000 103.5198  90.0000
ZERR    4.00   0.000084   0.000138   0.000105   0.0000   0.0010   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O W
UNIT 60.00 44.00 4.00 20.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.10 0.20 0.24
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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.755