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

data_7718640
_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         'C30 H33 Fe N O3 P2, C3 H7'
_chemical_formula_sum            'C33 H40 Fe N O3 P2'
_chemical_formula_weight         616.45
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-18
_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                 110.203(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9002(17)
_cell_length_b                   10.5291(9)
_cell_length_c                   18.4283(19)
_cell_measurement_reflns_used    9154
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.9680
_cell_measurement_theta_min      3.8630
_cell_volume                     3259.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.845
_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  31.00   1.00   10.00    --   -9.57 -99.00  90.00   46
  2  \w    -63.00  38.00   1.00   10.00    --    9.73 -57.00  60.00  101
  3  \w    -65.00  34.00   1.00   10.00    --    9.73 -37.00 -90.00   99
  4  \w    -23.00  12.00   1.00   10.00    --    9.73  77.00-120.00   35
  5  \w    -65.00  34.00   1.00   10.00    --    9.73 -37.00 150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0330661000
_diffrn_orient_matrix_UB_12      0.0415352000
_diffrn_orient_matrix_UB_13      -0.0079643000
_diffrn_orient_matrix_UB_21      0.0261129000
_diffrn_orient_matrix_UB_22      0.0510000000
_diffrn_orient_matrix_UB_23      0.0169059000
_diffrn_orient_matrix_UB_31      0.0029016000
_diffrn_orient_matrix_UB_32      0.0144855000
_diffrn_orient_matrix_UB_33      -0.0365138000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34437
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.614
_diffrn_reflns_theta_min         3.569
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.256
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_size_max          0.807
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0506P)^2^+3.6031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5590
_reflns_number_total             7761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_376_b_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718640
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C33H40Fe1N1P2O3
_chemical_oxdiff_usercomment     'DCM/hexane evap at -30 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C20(H20), C26(H26), C14(H14), C18(H18), C24(H24), C22(H22),
 C17(H17), C28(H28), C21(H21), C29(H29), C27(H27), C16(H16), C15(H15), C23(H23)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C12(H12A,H12B,H12C), C31(H31A,H31B,H31C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              38302
_shelx_hkl_checksum              38302
_ins_header
;
TITL RMK_376_B_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  17.900214  10.529076  18.428276  90.0000 110.2032  90.0000
ZERR    4.00   0.001739   0.000932   0.001894   0.0000   0.0115   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O P Fe
UNIT 132.00 160.00 4.00 12.00 8.00 4.00
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 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.905