Characterization of an Fe≡N-NH2 Intermediate Relevant to Catalytic N2 Reduction to NH3.
Anderson, John S.; Cutsail, 3rd, George E; Rittle, Jonathan; Connor, Bridget A.; Gunderson, William A.; Zhang, Limei; Hoffman, Brian M.; Peters, Jonas C.; Journal of the American Chemical Society 137 (2015) 7803–7809; doi:10.1021/jacs.5b03432

data_4123912
_publ_section_title
;
 Characterization of an Fe\\tb N-NH2 Intermediate Relevant to Catalytic N2
 Reduction to NH3.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7803
_journal_page_last               7809
_journal_paper_doi               10.1021/jacs.5b03432
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C78 H81 B2 F24 Fe N P3'
_chemical_formula_weight         1658.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                98.092(2)
_cell_angle_beta                 109.786(2)
_cell_angle_gamma                91.271(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2869(9)
_cell_length_b                   14.7963(9)
_cell_length_c                   19.1431(11)
_cell_measurement_temperature    100(2)
_cell_volume                     3759.3(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V7.68A (Bruker-AXS, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f 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  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            101295
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2001)'
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1706
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         14778
_refine_ls_number_restraints     960
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+2.8731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                9299
_reflns_number_total             14778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b03432_si_002.cif
_cod_data_source_block           bac001
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4123912