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_1543443
_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         'C66 H83 Fe3 N8, C5 H12'
_chemical_formula_sum            'C71 H95 Fe3 N8'
_chemical_formula_weight         1228.09
_chemical_name_common            spider-14106
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.725(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.1506(18)
_cell_length_b                   12.4838(2)
_cell_length_c                   39.818(4)
_cell_measurement_reflns_used    70753
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     12997.9(16)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            111246
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5240
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.649
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         14885
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+29.2875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11500
_reflns_number_total             14885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00423g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1543441--1543447.cif.'
_cod_database_code               1543443
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.871
_shelxl_version_number           2014-3
_shelx_res_checksum              13152