A Dimeric Hydride-Bridged Complex with Geometrically Distinct Iron Centers Giving Rise to an <i>S</i> = 3 Ground State.
Hickey, Anne K.; Greer, Samuel M.; Valdez-Moreira, Juan A; Lutz, Sean A.; Pink, Maren; DeGayner, Jordan A.; Harris, T. David; Hill, Stephen; Telser, Joshua; Smith, Jeremy M.; Journal of the American Chemical Society 141 (2019) 11970–11975; doi:10.1021/jacs.9b04389

data_4128545
_publ_section_title
;
 A Dimeric Hydride-Bridged Complex with Geometrically Distinct Iron
 Centers Giving Rise to an <i>S</i> = 3 Ground State.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11970
_journal_page_last               11975
_journal_paper_doi               10.1021/jacs.9b04389
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C52 H66 B2 Fe2 N8'
_chemical_formula_weight         936.45
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.7024(18)
_cell_angle_beta                 89.0943(18)
_cell_angle_gamma                68.2116(17)
_cell_formula_units_Z            2
_cell_length_a                   10.8558(4)
_cell_length_b                   13.0976(5)
_cell_length_c                   19.9752(7)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.52
_cell_volume                     2503.64(17)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXTL (Bruker, 2012)'
_computing_structure_solution    'SHELXTL (Bruker, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
'0.50 degree frames measured for 30 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38636
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.9577
_exptl_absorpt_correction_T_min  0.8500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2014'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         11455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.2311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                8126
_reflns_number_total             11455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b04389_si_002.cif
_cod_data_source_block           15075
_cod_original_cell_volume        2503.64(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4128545