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

data_7718632
_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 Mo N O5 P'
_chemical_formula_sum            'C14 H18 Mo N O5 P'
_chemical_formula_weight         407.20
_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                   22.1456(2)
_cell_length_b                   13.6345(2)
_cell_length_c                   5.93730(10)
_cell_measurement_reflns_used    7205
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.7930
_cell_measurement_theta_min      3.2430
_cell_volume                     1792.73(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 0.986
_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     -9.00  19.00   0.50    0.50    --  -46.45  11.00-110.00   56
  2  \w    -75.00 -49.00   0.50    0.50    --  -46.45 129.00  94.00   52
  3  \w     97.00 123.00   0.50    0.50    --  107.75 129.00  94.00   52
  4  \w     90.00 167.00   0.50    0.50    --  107.75  11.00-110.00  154
  5  \w    132.00 170.00   0.50    0.50    --  107.75 118.00  11.00   76
  6  \w     -8.00  29.00   0.50    0.50    --  -46.45  19.00 -90.00   74
  7  \w     -7.00  18.00   0.50    0.50    --  -46.45  19.00 -60.00   50
  8  \w     -2.00  24.00   0.50    0.50    --  -46.45  19.00-150.00   52
  9  \w     -1.00  25.00   0.50    0.50    --  -46.45  19.00-180.00   52
 10  \w     41.00  86.00   0.50    0.50    --   46.45-118.00 -75.00   90
 11  \w     36.00 105.00   0.50    0.50    --  107.75 -95.00 -60.00  138
 12  \w     71.00  98.00   0.50    0.50    --  107.75 -95.00  30.00   54
 13  \w     33.00  58.00   0.50    0.50    --  107.75 -30.00  90.00   50
 14  \w     38.00  63.00   0.50    0.50    --  107.75 -95.00  30.00   50
 15  \w     41.00  73.00   0.50    0.50    --  107.75 -45.00 -90.00   64
 16  \w     44.00  72.00   0.50    0.50    --  107.75 -95.00   0.00   56
 17  \w     80.00 105.00   0.50    0.50    --  107.75 -95.00   0.00   50
 18  \w     35.00  72.00   0.50    0.50    --  107.75 -45.00-120.00   74
 19  \w     35.00  60.00   0.50    0.50    --  107.75 -45.00   0.00   50
 20  \w     34.00  59.00   0.50    0.50    --  107.75 -30.00  60.00   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      -0.0099566000
_diffrn_orient_matrix_UB_12      -0.2174981000
_diffrn_orient_matrix_UB_13      0.0594181000
_diffrn_orient_matrix_UB_21      0.0029028000
_diffrn_orient_matrix_UB_22      0.1365016000
_diffrn_orient_matrix_UB_23      0.0959953000
_diffrn_orient_matrix_UB_31      -0.0687920000
_diffrn_orient_matrix_UB_32      0.0371511000
_diffrn_orient_matrix_UB_33      -0.0045633000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7801
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.010
_diffrn_reflns_theta_min         3.992
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.016
_exptl_absorpt_correction_T_max  0.27732
_exptl_absorpt_correction_T_min  0.18279
_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_density_diffrn    1.509
_exptl_crystal_description       sphere
_exptl_crystal_F_000             824
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.17
_exptl_crystal_size_rad          0.174
_refine_diff_density_max         0.433
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0581P)^2^+1.0174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1954
_reflns_number_total             1971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_363_a_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718632
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H18N1O5P1Mo1
_chemical_oxdiff_usercomment     'benzene evap'
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.144
_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              93637
_shelx_hkl_checksum              46222
_ins_header
;
TITL RMK_363_A_scale in Pna2(1) 
REM Pna2(1) (#33, found as Pc2(1)n in cab setting)
CELL 1.54184  22.145605   5.937315  13.634531  90.0000  90.0000  90.0000
ZERR    4.00   0.000245   0.000077   0.000166   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM  x+1/2,-y+1/2, z 
SYMM -x+1/2, y+1/2, z+1/2 
SFAC C H N O P Mo
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 0.17 0.32 0.45
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 2.650
_oxdiff_exptl_absorpt_empirical_full_min 0.602