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_1543442
_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 H82 Fe3 N8, 0.5(C6 H14)'
_chemical_formula_sum            'C69 H89 Fe3 N8'
_chemical_formula_weight         1198.03
_chemical_name_common            007-14177
_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-2014/7
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.547(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.7232(18)
_cell_length_b                   12.6083(4)
_cell_length_c                   38.521(4)
_cell_measurement_reflns_used    61855
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      2.3
_cell_volume                     12481.0(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-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.2679
_diffrn_reflns_av_unetI/netI     0.1112
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            191159
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        62.390
_diffrn_reflns_theta_max         62.390
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    5.874
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         9856
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.2180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5894
_reflns_number_total             9856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00423g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1543441--1543447.cif.'
_cod_original_cell_volume        12481.1(16)
_cod_database_code               1543442
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.386
_shelx_estimated_absorpt_t_max   0.758
_shelx_res_checksum              99840