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

data_7718637
_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         'C13 H18 Fe N O4 P'
_chemical_formula_sum            'C13 H18 Fe N O4 P'
_chemical_formula_weight         339.10
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-24
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.8819(5)
_cell_length_b                   10.0111(3)
_cell_length_c                   16.0053(4)
_cell_measurement_reflns_used    5114
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.4290
_cell_measurement_theta_min      4.2400
_cell_volume                     3345.92(15)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.975
_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   -104.00 -72.00   0.50    1.00    --  -46.45 173.00-164.00   64
  2  \w    106.00 174.00   0.50   10.00    --  107.75  21.00 -34.00  136
  3  \w    110.00 166.00   0.50   10.00    --  107.75 110.00 149.00  112
  4  \w     67.00 147.00   0.50   10.00    --  107.75-173.00-175.00  160
  5  \w     -6.00  29.00   0.50    1.00    --  -46.45  19.00  60.00   70
  6  \w     -7.00  28.00   0.50    1.00    --  -46.45  19.00 -30.00   70
  7  \w     -1.00  25.00   0.50    1.00    --  -46.45  19.00-150.00   52
  8  \w    -20.00  22.00   0.50    1.00    --  -46.45  38.00-180.00   84
  9  \w     87.00 119.00   0.50    1.00    --   46.45 173.00-164.00   64
 10  \w     37.00  63.00   0.50   10.00    --  107.75 -45.00  30.00   52
 11  \w     32.00  57.00   0.50   10.00    --  107.75 -30.00-150.00   50
 12  \w     32.00  58.00   0.50   10.00    --  107.75 -30.00  30.00   52
 13  \w     36.00  61.00   0.50   10.00    --  107.75 -45.00 150.00   50
 14  \w     37.00  62.00   0.50   10.00    --  107.75 -45.00-120.00   50
 15  \w     75.00 101.00   0.50   10.00    --  107.75 -95.00   0.00   52
 16  \w     36.00  68.00   0.50   10.00    --  107.75 -45.00 120.00   64
 17  \w     34.00  59.00   0.50   10.00    --  107.75 -30.00  90.00   50
 18  \w     63.00  88.00   0.50   10.00    --  107.75 -61.00   0.00   50
 19  \w     33.00  58.00   0.50   10.00    --  107.75 -30.00   0.00   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      -0.0093009000
_diffrn_orient_matrix_UB_12      -0.0308805000
_diffrn_orient_matrix_UB_13      0.0935169000
_diffrn_orient_matrix_UB_21      -0.0173722000
_diffrn_orient_matrix_UB_22      0.1473305000
_diffrn_orient_matrix_UB_23      0.0160759000
_diffrn_orient_matrix_UB_31      -0.0710660000
_diffrn_orient_matrix_UB_32      -0.0321206000
_diffrn_orient_matrix_UB_33      -0.0162324000
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.129
_diffrn_reflns_theta_min         4.234
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.237
_exptl_absorpt_correction_T_max  0.38250
_exptl_absorpt_correction_T_min  0.30759
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.115
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0837P)^2^+0.5220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2781
_reflns_number_total             3503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_344_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718637
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C13H18Fe1O4N1P1 '
_chemical_oxdiff_usercomment     'pentane evap at -30 '
_shelx_estimated_absorpt_t_max   0.451
_shelx_estimated_absorpt_t_min   0.270
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              27115
_shelx_hkl_checksum              30852
_ins_header
;
TITL RMK_344_scale in Pbcn 
REM Pbcn (#60, found as Pbna in cab setting)
CELL 1.54184  20.881942  10.011102  16.005318  90.0000  90.0000  90.0000
ZERR    8.00   0.000491   0.000261   0.000351   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y+1/2, z+1/2 
SYMM -x, y,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H N O P Fe
UNIT 104.00 144.00 8.00 32.00 8.00 8.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=300.0; aver:225.0
TEMP -48
SIZE 0.11 0.21 0.21
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 2.928
_oxdiff_exptl_absorpt_empirical_full_min 0.451