<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_7714798
_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         'C32 H72 Fe2 N12'
_chemical_formula_sum            'C32 H72 Fe2 N12'
_chemical_formula_weight         736.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 120.907(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.115(2)
_cell_length_b                   11.7866(8)
_cell_length_c                   21.137(2)
_cell_measurement_reflns_used    11941
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.2500
_cell_measurement_theta_min      3.5430
_cell_volume                     4086.0(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      100.00(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 0.937
_diffrn_measurement_details
;
  1 omega  -46.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5328   80.0000  -34.5480 96

  2 omega -102.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5328 -178.0000  120.0000 67

  3 omega  -88.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5328  -37.0000  150.0000 103

  4 omega  -62.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  -57.0000   60.0000 104

  5 omega   57.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  178.0000 -120.0000 45

  6 omega  -17.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3922   57.0000   90.0000 103

  7 omega  -41.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5328   57.0000 -120.0000 103

  8 omega  -88.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5328  -37.0000  -90.0000 103

  9 omega   24.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3922 -133.0000  -59.9794 51

 10 omega   -4.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  -99.0000  150.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0400903000
_diffrn_orient_matrix_UB_12      -0.0095117000
_diffrn_orient_matrix_UB_13      -0.0072328000
_diffrn_orient_matrix_UB_21      0.0117929000
_diffrn_orient_matrix_UB_22      -0.0546772000
_diffrn_orient_matrix_UB_23      0.0161220000
_diffrn_orient_matrix_UB_31      0.0111060000
_diffrn_orient_matrix_UB_32      0.0232866000
_diffrn_orient_matrix_UB_33      0.0348672000
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42383
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.607
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.766
_exptl_crystal_size_mid          0.449
_exptl_crystal_size_min          0.3438
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         5396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0727P)^2^+10.5838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4413
_reflns_number_total             5396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03132b2.cif
_cod_data_source_block           kso-a-009
_cod_depositor_comments
'Adding full bibliography for 7714797--7714798.cif.'
_cod_database_code               7714798
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H72 Fe2 N12'
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.599
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              14808
_shelx_hkl_checksum              73772
_olex2_date_sample_data_collection 2014-09-24
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id KSO-A-009
_olex2_submission_special_instructions 'No special instructions were received'