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_4134776
_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         'C66 H102 Fe K2 N6 O2, 2(C7 H8)'
_chemical_formula_sum            'C80 H118 Fe K2 N6 O2'
_chemical_formula_weight         1329.85
_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     dual
_audit_creation_date             2019-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                106.4811(14)
_cell_angle_beta                 107.3077(13)
_cell_angle_gamma                99.2665(14)
_cell_formula_units_Z            2
_cell_length_a                   14.1935(5)
_cell_length_b                   14.9296(5)
_cell_length_c                   20.5175(7)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.517
_cell_measurement_theta_min      2.909
_cell_volume                     3834.6(2)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2018.7-2'
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_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  0.1082
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            75367
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.562
_diffrn_reflns_theta_min         2.948
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         17574
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0881
_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^)+(0.0646P)^2^+13.7823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                11072
_reflns_number_total             17574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01488_si_007.cif
_cod_data_source_block           9520
_cod_database_code               4134776
_shelx_shelxl_version_number     2018/3