<i>N</i>-Alkyl substituted triazenide-bridged homoleptic iron(II) dimers with an exceptionally short Fe-Fe bond.
Soussi, Khaled; Jeanneau, Erwann; Maldivi, Pascale; Clémancey, Martin; Latour, Jean-Marc; Khrouz, Lhoussain; Lorentz, Chantal; Daniele, Stéphane; Mishra, Shashank; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1439–1444; doi:10.1039/d3dt03132b

data_7714797
_publ_section_title
;
 <i>N</i>-Alkyl substituted triazenide-bridged homoleptic iron(II) dimers
 with an exceptionally short Fe-Fe bond.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1439
_journal_page_last               1444
_journal_paper_doi               10.1039/d3dt03132b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H56 Fe2 N12'
_chemical_formula_sum            'C24 H56 Fe2 N12'
_chemical_formula_weight         624.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-28 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1992(15)
_cell_length_b                   12.3984(18)
_cell_length_c                   21.399(3)
_cell_measurement_reflns_used    5344
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.1000
_cell_measurement_theta_min      3.7350
_cell_volume                     3236.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_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     -4.00  54.00   1.00   30.41    --   12.39 -99.00 -30.00   58
  2  \w    -20.00  21.00   1.00   30.41    --   12.39  77.00-120.00   41
  3  \w    -29.00  73.00   1.00   30.41    --   12.39  19.00 -30.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035667000
_diffrn_orient_matrix_UB_12      0.0245147000
_diffrn_orient_matrix_UB_13      -0.0298919000
_diffrn_orient_matrix_UB_21      -0.0018193000
_diffrn_orient_matrix_UB_22      -0.0516414000
_diffrn_orient_matrix_UB_23      -0.0142575000
_diffrn_orient_matrix_UB_31      -0.0579235000
_diffrn_orient_matrix_UB_32      0.0035712000
_diffrn_orient_matrix_UB_33      -0.0013398000
_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     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4014
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.549
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.163
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+7.8410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3190
_reflns_number_total             4014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03132b2.cif
_cod_data_source_block           kso_7_00_2_autored
_cod_depositor_comments
'Adding full bibliography for 7714797--7714798.cif.'
_cod_original_cell_volume        3236.6(7)
_cod_database_code               7714797
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H56 Fe2 N12'
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.760(3)
 0.240(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              4717
_shelx_hkl_checksum              468
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id KSO_7_00_2
_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 2.480
_oxdiff_exptl_absorpt_empirical_full_min 0.827