Alkali-Controlled C-H Cleavage or N-C Bond Formation by N2-Derived Iron Nitrides and Imides.
MacLeod, K. Cory; Menges, Fabian S.; McWilliams, Sean F.; Craig, Stephanie M.; Mercado, Brandon Q.; Johnson, Mark A.; Holland, Patrick L.; Journal of the American Chemical Society 138 (2016) 11185–11191; doi:10.1021/jacs.6b04984

data_4125204
_publ_section_title
;
 Alkali-Controlled C-H Cleavage or N-C Bond Formation by N2-Derived Iron
 Nitrides and Imides.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11185
_journal_page_last               11191
_journal_paper_doi               10.1021/jacs.6b04984
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C66 H81 Fe3 N8, C18 H35 K N2 O6, 3(C7 H8)'
_chemical_formula_sum            'C105 H141 Fe3 K N10 O6'
_chemical_formula_weight         1845.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                89.068(6)
_cell_angle_beta                 71.963(5)
_cell_angle_gamma                81.667(6)
_cell_formula_units_Z            2
_cell_length_a                   13.9066(4)
_cell_length_b                   18.4465(5)
_cell_length_c                   20.5506(14)
_cell_measurement_reflns_used    32068
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      2.3
_cell_volume                     4957.5(4)
_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
; 
 'Rigaku MicroMax-007HF, Rigaku Saturn 944+ CCD' 
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
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_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.5579
_diffrn_reflns_av_unetI/netI     0.5582
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            115732
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        65.090
_diffrn_reflns_theta_max         65.090
_diffrn_reflns_theta_min         2.262
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    4.296
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.680
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         16644
_refine_ls_number_restraints     1209
_refine_ls_restrained_S_all      0.673
_refine_ls_R_factor_all          0.3108
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3569
_reflns_number_total             16644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04984_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4125204--4125208.cif.'
_cod_database_code               4125204
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              18071
_shelx_hkl_checksum              43803