Unusual Dinitrogen Binding and Electron Storage in Dinuclear Iron Complexes.
Sorsche, Dieter; Miehlich, Matthias E.; Searles, Keith; Gouget, Guillaume; Zolnhofer, Eva M.; Fortier, Skye; Chen, Chun-Hsing; Gau, Michael; Carroll, Patrick J.; Murray, Christopher B.; Caulton, Kenneth G.; Khusniyarov, Marat M.; Meyer, Karsten; Mindiola, Daniel J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01488

data_4134774
_publ_section_title
;
 Unusual Dinitrogen Binding and Electron Storage in Dinuclear Iron
 Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01488
_journal_year                    2020
_chemical_formula_moiety         'C58 H82 Fe2 K2 N8, 0.5(C5 H12)'
_chemical_formula_sum            'C60.5 H88 Fe2 K2 N8'
_chemical_formula_weight         1117.28
_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     direct
_audit_creation_date             2019-12-30
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5799)
;
_cell_angle_alpha                103.576(4)
_cell_angle_beta                 103.321(4)
_cell_angle_gamma                93.031(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0380(6)
_cell_length_b                   14.8077(8)
_cell_length_c                   19.1696(11)
_cell_measurement_reflns_used    8885
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.46
_cell_volume                     2944.7(3)
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1432
_diffrn_reflns_av_unetI/netI     0.1604
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47842
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         1.908
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         13073
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.0937
_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^)+(0.1023P)^2^+24.3383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2901
_reflns_number_gt                6773
_reflns_number_total             13073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01488_si_003.cif
_cod_data_source_block           9016
_cod_original_formula_sum        'C60.50 H88 Fe2 K2 N8'
_cod_database_code               4134774
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.865