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_4134635
_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_absolute_configuration rmad
_chemical_formula_moiety         'C105 H87 Fe3 N15 Na6 O6, 2(C5 H5 N)'
_chemical_formula_sum            'C115 H97 Fe3 N17 Na6 O6'
_chemical_formula_weight         2118.58
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 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                112.076(2)
_cell_angle_beta                 111.146(2)
_cell_angle_gamma                92.244(2)
_cell_formula_units_Z            1
_cell_length_a                   13.3029(3)
_cell_length_b                   14.1443(3)
_cell_length_c                   15.9246(4)
_cell_measurement_reflns_used    16005
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      32.2000
_cell_measurement_theta_min      3.0230
_cell_volume                     2536.25(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Mercury 4.1.3 (CCDC, 2019)'
_computing_publication_material  'CIFTab (Sheldrick, 2016)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.911
_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  92.00   1.00   52.50    --   19.83  38.00 -30.00   97
  2  \w     -7.00  90.00   1.00   52.50    --   19.83  57.00-180.00   97
  3  \w    -42.00  52.00   1.00   52.50    --   19.83 -77.00  30.00   94
  4  \w     -8.00  93.00   1.00   52.50    --   19.83  57.00  60.00  101
  5  \w    -15.00  61.00   1.00   52.50    --   19.83 -99.00 150.00   76
  6  \w    -52.00  48.00   1.00   52.50    --   19.83 -57.00 -90.00  100
  7  \w    -42.00  13.00   1.00   52.50    --  -19.91 -77.00-180.00   55
  8  \w    -24.00  35.00   1.00   52.50    --  -19.91  38.00-150.00   59
  9  \w    -75.00 -26.00   1.00   52.50    --  -19.91 123.00-179.77   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.915
_diffrn_reflns_theta_min         2.530
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            'clear dark red'
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       plate
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.012(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1402
_refine_ls_number_reflns         33321
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.843
_reflns_number_gt                24942
_reflns_number_total             33321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01664_si_002.cif
_cod_data_source_block           dt414-pybis
_cod_depositor_comments
'Adding full bibliography for 4134635--4134636.cif.'
_cod_original_cell_volume        2536.26(12)
_cod_database_code               4134635
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              35079
_shelx_hkl_checksum              96306