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

data_7718638
_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 N O5 P W'
_chemical_formula_sum            'C14 H18 N O5 P W'
_chemical_formula_weight         495.11
_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             2024-04-12
_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                   22.1015(3)
_cell_length_b                   13.5912(2)
_cell_length_c                   5.92670(10)
_cell_measurement_reflns_used    14426
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      77.5270
_cell_measurement_theta_min      3.9560
_cell_volume                     1780.30(5)
_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      150.01(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 0.995
_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     -2.00  24.00   0.50    0.50    --  -46.45  19.00-180.00   52
  2  \w     -1.00  25.00   0.50    0.50    --  -46.45  19.00   0.00   52
  3  \w    -43.00   1.00   0.50    0.50    --  -46.45  57.00 -60.00   88
  4  \w    -19.00  22.00   0.50    0.50    --  -46.45  38.00 150.00   82
  5  \w   -119.00  24.00   0.50    0.50    --  -46.45   0.00 -30.00  286
  6  \w     39.00  93.00   0.50    0.50    --   46.45-125.00  60.00  108
  7  \w     49.00  78.00   0.50    0.50    --   46.45-125.00-150.00   58
  8  \w    117.00 176.00   0.50    2.00    --  107.75  15.00 -60.00  118
  9  \w     33.00  59.00   0.50    2.00    --  107.75 -30.00 120.00   52
 10  \w     94.00 125.00   0.50    2.00    --  107.75-141.00-179.35   62
 11  \w     36.00  91.00   0.50    2.00    --  107.75 -95.00  30.00  110
 12  \w     48.00  73.00   0.50    2.00    --  107.75 -61.00 120.00   50
 13  \w     32.00  59.00   0.50    2.00    --  107.75 -30.00  30.00   54
 14  \w    104.00 175.00   0.50    2.00    --  107.75  30.00   0.00  142
 15  \w     32.00  57.00   0.50    2.00    --  107.75 -30.00 -60.00   50
 16  \w     49.00 110.00   0.50    2.00    --  107.75-125.00   0.00  122
 17  \w     35.00  92.00   0.50    2.00    --  107.75 -61.00-150.00  114
 18  \w     79.00 108.00   0.50    2.00    --  107.75-107.00-126.09   58
 19  \w     84.00 109.00   0.50    2.00    --  107.75-111.00-172.38   50
 20  \w     39.00  68.00   0.50    2.00    --  107.75 -45.00  60.00   58
 21  \w    140.00 178.00   0.50    2.00    --  107.75 125.00 -60.00   76
 22  \w     39.00  65.00   0.50    2.00    --  107.75 -45.00-150.00   52
 23  \w     37.00  65.00   0.50    2.00    --  107.75-107.00-126.09   56
 24  \w     37.00  70.00   0.50    2.00    --  107.75 -95.00 150.00   66
 25  \w     79.00 104.00   0.50    2.00    --  107.75 -95.00 150.00   50
 26  \w    104.00 159.00   0.50    2.00    --  107.75  30.00-150.00  110
 27  \w     95.00 146.00   0.50    2.00    --  107.75 125.00  90.00  102
 28  \w     53.00  90.00   0.50    2.00    --  107.75 -95.00  90.00   74
 29  \w     53.00 103.00   0.50    2.00    --  107.75 -95.00-150.00  100
 30  \w     45.00  75.00   0.50    2.00    --  107.75 -61.00 -30.00   60
 31  \w     59.00 104.00   0.50    2.00    --  107.75 -95.00 -90.00   90
 32  \w     95.00 131.00   0.50    2.00    --  107.75  45.00  60.00   72
 33  \w     37.00  73.00   0.50    2.00    --  107.75 -45.00-120.00   72
 34  \w    103.00 129.00   0.50    2.00    --  107.75 125.00 -60.00   52
 35  \w     45.00  72.00   0.50    2.00    --  107.75 -45.00 -30.00   54
 36  \w     83.00 108.00   0.50    2.00    --  107.75-110.00  81.01   50
 37  \w     78.00 104.00   0.50    2.00    --  107.75 -95.00   0.00   52
 38  \w     42.00  68.00   0.50    2.00    --  107.75-111.00-172.38   52
 39  \w     42.00  83.00   0.50    2.00    --  107.75-141.00-179.35   82
 40  \w     96.00 175.00   0.50    2.00    --  107.75  15.00 -90.00  158
 41  \w     42.00  67.00   0.50    2.00    --  107.75 -45.00 -90.00   50
 42  \w     35.00 106.00   0.50    2.00    --  107.75 -95.00  60.00  142
 43  \w     69.00 108.00   0.50    2.00    --  107.75-104.00 -17.11   78
;
_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      0.0540484000
_diffrn_orient_matrix_UB_12      0.0715095000
_diffrn_orient_matrix_UB_13      0.0081543000
_diffrn_orient_matrix_UB_21      -0.0438485000
_diffrn_orient_matrix_UB_22      0.0878884000
_diffrn_orient_matrix_UB_23      -0.0143791000
_diffrn_orient_matrix_UB_31      -0.0041498000
_diffrn_orient_matrix_UB_32      0.0026227000
_diffrn_orient_matrix_UB_33      0.2593790000
_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  0.0851
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            21172
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.082
_diffrn_reflns_theta_min         4.000
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.064
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0694P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1831
_reflns_number_total             1978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_353_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718638
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H18W1N1P1O5
_chemical_oxdiff_usercomment     'pentane evap'
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.132
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              71166
_shelx_hkl_checksum              83073
_ins_header
;
TITL RMK_353_scale in Pnma 
REM Pnma (#62, found as Pcmn in -cba setting)
CELL 1.54184  22.101511  13.591167   5.926654  90.0000  90.0000  90.0000
ZERR    4.00   0.000255   0.000167   0.000052   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 P 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 0.02 0.10 0.26
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 2.101
_oxdiff_exptl_absorpt_empirical_full_min 0.511