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

data_7718628
_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         'C22 H32 Fe2 Li2 N6 O8'
_chemical_formula_sum            'C22 H32 Fe2 Li2 N6 O8'
_chemical_formula_weight         634.11
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-21
_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                116.394(14)
_cell_angle_beta                 108.038(12)
_cell_angle_gamma                97.046(13)
_cell_formula_units_Z            1
_cell_length_a                   9.6531(15)
_cell_length_b                   9.7961(15)
_cell_length_c                   10.6609(13)
_cell_measurement_reflns_used    2517
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.6200
_cell_measurement_theta_min      3.9980
_cell_volume                     817.6(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.807
_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     -5.00  28.00   1.00  110.00    --  -11.14 -99.00 -90.00   33
  2  \w    -10.00  81.00   1.00  110.00    --   11.46  57.00-180.00   91
  3  \w    -10.00  84.00   1.00  110.00    --   11.46  37.00 -30.00   94
  4  \w    -61.00  40.00   1.00  110.00    --   11.46 -57.00  30.00  101
;
_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      -0.0093156000
_diffrn_orient_matrix_UB_12      -0.0571976000
_diffrn_orient_matrix_UB_13      -0.0747438000
_diffrn_orient_matrix_UB_21      0.0569783000
_diffrn_orient_matrix_UB_22      -0.0284026000
_diffrn_orient_matrix_UB_23      0.0321520000
_diffrn_orient_matrix_UB_31      -0.0570272000
_diffrn_orient_matrix_UB_32      -0.0559437000
_diffrn_orient_matrix_UB_33      -0.0031099000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8226
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.813
_diffrn_reflns_theta_min         3.466
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78419
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         8226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1144P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5222
_reflns_number_total             8226
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 6.7489\% 
around [-0.30 -0.45 0.84] (reciprocal) or [-0.18 -0.26 0.95] (direct)
;
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_326_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_original_cell_volume        817.6(2)
_cod_database_code               7718628
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Fe N Li N'
_chemical_oxdiff_usercomment     'THF evap'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.787
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70212
 0.29788
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              75486
_shelx_hkl_checksum              58958
_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.758
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2