Stepwise N–H bond formation from N2-derived iron nitride, imide and amide intermediates to ammonia
MacLeod, K. Cory; McWilliams, Sean F.; Mercado, Brandon Q.; Holland, Patrick L.; Chem. Sci. 7 (2016) 5736–; doi:10.1039/C6SC00423G

data_1543445
_publ_section_title
;
 Stepwise N--H bond formation from N2-derived iron nitride, imide and
 amide intermediates to ammonia
;
_journal_issue                   9
_journal_name_full               'Chem. Sci.'
_journal_page_first              5736
_journal_paper_doi               10.1039/C6SC00423G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C44 H56 Fe2 N4 O2, C4 H10 O'
_chemical_formula_sum            'C48 H66 Fe2 N4 O3'
_chemical_formula_weight         858.75
_chemical_name_common            holkg01
_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
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                77.782(1)
_cell_angle_beta                 84.648(1)
_cell_angle_gamma                82.055(1)
_cell_formula_units_Z            2
_cell_length_a                   12.7872(8)
_cell_length_b                   12.8768(8)
_cell_length_c                   14.4731(9)
_cell_measurement_reflns_used    4060
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.23
_cell_volume                     2301.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1025
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46337
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.9481
_exptl_absorpt_correction_T_min  0.8551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         11415
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0479P)^2^+0.4219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                6795
_reflns_number_total             11415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc00423g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1543441--1543447.cif.'
_cod_database_code               1543445