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

data_7718635
_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         'C24 H32 Li2 N6 O10 W2'
_chemical_formula_sum            'C24 H32 Li2 N6 O10 W2'
_chemical_formula_weight         946.13
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2024-05-14
_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                112.5180(10)
_cell_angle_beta                 111.564(2)
_cell_angle_gamma                93.9840(10)
_cell_formula_units_Z            1
_cell_length_a                   8.71120(10)
_cell_length_b                   10.7852(2)
_cell_length_c                   11.3689(2)
_cell_measurement_reflns_used    10165
_cell_measurement_temperature    149(4)
_cell_measurement_theta_max      77.7900
_cell_measurement_theta_min      4.5540
_cell_volume                     889.73(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(4)
_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 0.980
_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     16.00  58.00   0.50    0.50    --   46.45 -34.00  54.00   84
  2  \w    -28.00   9.00   0.50    0.50    --   46.45 -34.00  54.00   74
  3  \w     33.00 120.00   0.50    0.50    --   46.45  34.00-147.00  174
  4  \w     32.00  61.00   0.50    0.50    --  107.75 -34.00  54.00   58
  5  \w    142.00 168.00   0.50    0.50    --  107.75  34.00-147.00   52
  6  \w     95.00 133.00   0.50    0.50    --  107.75  34.00-147.00   76
  7  \w     -6.00  21.00   0.50    0.50    --  -46.45  34.00-147.00   54
  8  \w    -58.00 -33.00   0.50    0.50    --  -46.45 -38.00 150.00   50
  9  \w    -86.00 -18.00   0.50    0.50    --  -46.45 125.00 -90.00  136
 10  \w   -121.00 -33.00   0.50    0.50    --  -46.45 -34.00  54.00  176
 11  \w   -120.00 -68.00   0.50    0.50    --  -46.45 -38.00 150.00  104
 12  \w     59.00  86.00   0.50    0.50    --   46.45-125.00 -60.00   54
 13  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00-150.00   50
 14  \w     81.00 106.00   0.50    0.50    --  107.75 -95.00-180.00   50
 15  \w     99.00 128.00   0.50    0.50    --  107.75 125.00  90.00   58
 16  \w     44.00  70.00   0.50    0.50    --  107.75 -45.00-180.00   52
 17  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 18  \w     67.00 111.00   0.50    0.50    --  107.75-125.00 150.00   88
 19  \w     51.00  87.00   0.50    0.50    --  107.75 -61.00-120.00   72
 20  \w     64.00 105.00   0.50    0.50    --  107.75 -95.00 -90.00   82
 21  \w     32.00  59.00   0.50    0.50    --  107.75 -30.00-120.00   54
 22  \w     36.00  76.00   0.50    0.50    --  107.75 -95.00-180.00   80
 23  \w     87.00 117.00   0.50    0.50    --  107.75 -77.00-180.00   60
 24  \w     34.00  79.00   0.50    0.50    --  107.75 -77.00-180.00   90
 25  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00 -30.00   50
 26  \w     36.00  70.00   0.50    0.50    --  107.75 -95.00 -30.00   68
 27  \w     78.00 104.00   0.50    0.50    --  107.75 -95.00 -30.00   52
 28  \w     39.00  73.00   0.50    0.50    --  107.75 -45.00  30.00   68
 29  \w    102.00 139.00   0.50    0.50    --  107.75  30.00 -90.00   74
 30  \w    146.00 171.00   0.50    0.50    --  107.75  30.00 -90.00   50
 31  \w     95.00 138.00   0.50    0.50    --  107.75 125.00 150.00   86
 32  \w    145.00 171.00   0.50    0.50    --  107.75 125.00 150.00   52
 33  \w     39.00  70.00   0.50    0.50    --  107.75 -61.00 120.00   62
 34  \w     52.00 103.00   0.50    0.50    --  107.75 -95.00  60.00  102
 35  \w     78.00 104.00   0.50    0.50    --  107.75 -95.00  30.00   52
 36  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00 -90.00   50
 37  \w     45.00  71.00   0.50    0.50    --  107.75-100.00 163.50   52
 38  \w     94.00 175.00   0.50    0.50    --  107.75  30.00 150.00  162
 39  \w     34.00  59.00   0.50    0.50    --  107.75 -30.00  60.00   50
 40  \w     32.00  58.00   0.50    0.50    --  107.75 -30.00   0.00   52
 41  \w     79.00 107.00   0.50    0.50    --  107.75-100.00 163.50   56
 42  \w     36.00  65.00   0.50    0.50    --  107.75 -95.00  30.00   58
 43  \w     97.00 140.00   0.50    0.50    --  107.75  45.00 -30.00   86
 44  \w    145.00 176.00   0.50    0.50    --  107.75  45.00 -30.00   62
 45  \w     69.00  95.00   0.50    0.50    --  107.75 -95.00  90.00   52
 46  \w     44.00 106.00   0.50    0.50    --  107.75 -95.00-120.00  124
 47  \w     41.00  66.00   0.50    0.50    --  107.75-125.00 -60.00   50
 48  \w    138.00 173.00   0.50    0.50    --  107.75 125.00  90.00   70
;
_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      0.1585761000
_diffrn_orient_matrix_UB_12      0.0478289000
_diffrn_orient_matrix_UB_13      0.1404839000
_diffrn_orient_matrix_UB_21      0.1086665000
_diffrn_orient_matrix_UB_22      -0.0506438000
_diffrn_orient_matrix_UB_23      -0.0811456000
_diffrn_orient_matrix_UB_31      0.0388459000
_diffrn_orient_matrix_UB_32      0.1434600000
_diffrn_orient_matrix_UB_33      0.0039522000
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.051
_diffrn_reflns_theta_min         4.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.236
_exptl_absorpt_correction_T_max  0.27716
_exptl_absorpt_correction_T_min  0.18262
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         1.214
_refine_diff_density_min         -2.720
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0570P)^2^+2.5208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3677
_reflns_number_total             3729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_325_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718635
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H32Li2N6O10W2
_chemical_oxdiff_usercomment     'THF evap at -30 '
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.079
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C11 \\sim N3-C11'
 with sigma of 0.02
 N3-C12 \\sim N3-C12'
 with sigma of 0.02
 N3-C10 \\sim N3-C10'
 with sigma of 0.02
 C9-C10 \\sim C9-C10'
 with sigma of 0.02
3. Others
 Sof(H9bc)=Sof(H9bd)=Sof(C10')=Sof(H10c)=Sof(H10d)=Sof(C11')=Sof(H11d)=
 Sof(H11e)=Sof(H11f)=Sof(C12')=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(1)
 Sof(H9aa)=Sof(H9ab)=Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(H11c)=Sof(C12)=Sof(H12a)=
 Sof(H12b)=Sof(H12c)=Sof(C10)=Sof(H10a)=Sof(H10b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9aa,H9ab), C9(H9bc,H9bd), C10(H10a,H10b), C10'(H10c,H10d)
4.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C8(H8a,H8b,H8c),
 C11'(H11d,H11e,H11f), C12'(H12d,H12e,H12f)
;
_shelx_res_checksum              76056
_shelx_hkl_checksum              68220
_ins_header
;
TITL RMK_325_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.711187  10.785237  11.368916 112.5179 111.5643  93.9840
ZERR    1.00   0.000149   0.000160   0.000179   0.0014   0.0015   0.0013
LATT  1
SFAC C H Li N O W
UNIT 24.00 32.00 2.00 6.00 10.00 2.00
REM  CrysAlisPro recorded range (K): Min=146.2; max=150.0; aver:148.1
TEMP -125
SIZE 0.11 0.19 0.42
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 5.489
_oxdiff_exptl_absorpt_empirical_full_min 0.484