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

data_7718631
_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 Cr N O5 P'
_chemical_formula_sum            'C14 H18 Cr N O5 P'
_chemical_formula_weight         363.26
_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                   21.7679(3)
_cell_length_b                   13.5735(2)
_cell_length_c                   5.92480(10)
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.6700
_cell_measurement_theta_min      3.8220
_cell_volume                     1750.58(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      150.00(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 0.980
_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    -15.00  10.00   0.50    0.50    --  -46.45  32.00-117.00   50
  2  \w     30.00  56.00   0.50    0.50    --   46.45-119.00-132.00   52
  3  \w    103.00 129.00   0.50    0.50    --  107.75  92.00  58.00   52
  4  \w    152.00 178.00   0.50    0.50    --  107.75  92.00  58.00   52
  5  \w     35.00  61.00   0.50    0.50    --  107.75 -32.00  83.00   52
  6  \w     73.00 154.00   0.50    0.50    --  107.75 156.00 107.00  162
  7  \w   -102.00 -52.00   0.50    0.50    --  -46.45 -32.00  83.00  100
  8  \w    -21.00  26.00   0.50    0.50    --  -46.45  38.00   0.00   94
  9  \w    -12.00  24.00   0.50    0.50    --  -46.45  38.00  30.00   72
 10  \w     32.00  58.00   0.50    0.50    --  107.75 -30.00  60.00   52
 11  \w     32.00  59.00   0.50    0.50    --  107.75 -30.00  30.00   54
 12  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00 150.00   50
 13  \w     32.00  57.00   0.50    0.50    --  107.75 -30.00 -30.00   50
 14  \w     59.00 122.00   0.50    0.50    --  107.75 -77.00-150.00  126
 15  \w     52.00  92.00   0.50    0.50    --  107.75 -61.00-150.00   80
 16  \w     34.00  59.00   0.50    0.50    --  107.75 -30.00  90.00   50
 17  \w     42.00  70.00   0.50    0.50    --  107.75 -45.00 120.00   56
;
_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      -0.0651665000
_diffrn_orient_matrix_UB_12      -0.1014308000
_diffrn_orient_matrix_UB_13      -0.0009113000
_diffrn_orient_matrix_UB_21      -0.0029111000
_diffrn_orient_matrix_UB_22      0.0304750000
_diffrn_orient_matrix_UB_23      -0.1126339000
_diffrn_orient_matrix_UB_31      0.0274580000
_diffrn_orient_matrix_UB_32      -0.2374236000
_diffrn_orient_matrix_UB_33      -0.0140688000
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7056
_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         77.884
_diffrn_reflns_theta_min         4.062
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.431
_exptl_absorpt_correction_T_max  0.35752
_exptl_absorpt_correction_T_min  0.27915
_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    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.139
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0732P)^2^+0.1698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1847
_reflns_number_total             1919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_361_a_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718631
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H18N1P1O5Cr1
_chemical_oxdiff_usercomment     'benzene evap'
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.126
_olex2_refinement_description
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              11915
_shelx_hkl_checksum              14426
_ins_header
;
TITL RMK_361_A_scale in Pna2(1) 
REM Pna2(1) (#33, found as Pc2(1)n in cab setting)
CELL 1.54184  21.767924   5.924773  13.573534  90.0000  90.0000  90.0000
ZERR    4.00   0.000313   0.000087   0.000215   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 Cr
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 0.12 0.24 0.55
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 2.037
_oxdiff_exptl_absorpt_empirical_full_min 0.575