Assembly of High-Spin [Fe<sub>3</sub>] Clusters by Ligand-Based Multielectron Reduction.
Toniolo, Davide; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Journal of the American Chemical Society 142 (2020) 7301–7305; doi:10.1021/jacs.0c01664

data_4134636
_publ_section_title
;
 Assembly of High-Spin [Fe<sub>3</sub>] Clusters by Ligand-Based
 Multielectron Reduction.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7301
_journal_page_last               7305
_journal_paper_doi               10.1021/jacs.0c01664
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C176 H196 Fe6 N12 Na12 O26'
_chemical_formula_sum            'C176 H196 Fe6 N12 Na12 O26'
_chemical_formula_weight         3506.44
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 105.404(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4845(3)
_cell_length_b                   33.0195(12)
_cell_length_c                   22.9829(7)
_cell_measurement_reflns_used    17529
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.5880
_cell_measurement_theta_min      3.3280
_cell_volume                     9865.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury 4.0.0 (CCDC, 2018)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_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   -120.00  47.00   1.00    7.50    --  -40.91   0.00 -60.00  167
  2  \w    -62.00  15.00   1.00    7.50    --  -40.91  38.00 150.00   77
  3  \w     26.00  80.00   1.00    7.50    --   40.91-125.00  60.00   54
  4  \w     28.00  97.00   1.00    7.50    --   40.91-125.00-120.00   69
  5  \w      6.00  54.00   1.00    7.50    --   40.91 -99.00 -60.00   48
  6  \w     70.00  97.00   1.00   30.00    --  111.85 -94.00 150.00   27
  7  \w     99.00 146.00   1.00   30.00    --  111.85 125.00 150.00   47
  8  \w     38.00 140.00   1.00   30.00    --  111.85 -30.00  30.00  102
  9  \w     61.00 122.00   1.00   30.00    --  111.85-125.00   0.00   61
 10  \w     55.00 141.00   1.00   30.00    --  111.85 -77.00  60.00   86
 11  \w     96.00 175.00   1.00   30.00    --  111.85 125.00 120.00   79
 12  \w    100.00 140.00   1.00   30.00    --  111.85 125.00  90.00   40
 13  \w     39.00  99.00   1.00   30.00    --  111.85 -94.00  60.00   60
 14  \w     93.00 151.00   1.00   30.00    --  111.85  30.00 -60.00   58
 15  \w     67.00 104.00   1.00   30.00    --  111.85 -94.00-150.00   37
 16  \w     39.00  79.00   1.00   30.00    --  111.85 -30.00-180.00   40
 17  \w     86.00 178.00   1.00   30.00    --  111.85  45.00-150.00   92
 18  \w     40.00 138.00   1.00   30.00    --  111.85 -61.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_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  0.0584
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69497
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.077
_diffrn_reflns_theta_min         2.676
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.209
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       prism
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.572
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.164
_refine_diff_density_max         2.379
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         20221
_refine_ls_number_restraints     1812
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1400P)^2^+33.5565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2570
_refine_ls_wR_factor_ref         0.2640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17161
_reflns_number_total             20221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01664_si_003.cif
_cod_data_source_block           dt200
_cod_depositor_comments
'Adding full bibliography for 4134635--4134636.cif.'
_cod_original_cell_volume        9865.5(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4134636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.197
_shelx_estimated_absorpt_t_max   0.545
_shelx_res_checksum              28408
_shelx_hkl_checksum              63816
_shelx_fab_checksum              25066