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_4125207
_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 H82 Fe3 N8, C20 H40 K O8'
_chemical_formula_sum            'C86 H122 Fe3 K N8 O8'
_chemical_formula_weight         1602.56
_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
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                88.986(2)
_cell_angle_beta                 84.849(2)
_cell_angle_gamma                85.023(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5997(10)
_cell_length_b                   18.2403(13)
_cell_length_c                   20.2851(14)
_cell_measurement_reflns_used    988
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      2.4
_cell_volume                     4992.5(6)
_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 0.984
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.2217
_diffrn_reflns_av_unetI/netI     0.0939
_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            170343
_diffrn_reflns_point_group_measured_fraction_full 0.984
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_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         2.432
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1710
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         17354
_refine_ls_number_restraints     1061
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1941
_refine_ls_R_factor_gt           0.0980
_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^)+(0.0967P)^2^+13.2518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2278
_refine_ls_wR_factor_ref         0.2863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8230
_reflns_number_total             17354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04984_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4125204--4125208.cif.'
_cod_database_code               4125207
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.921
_shelx_res_checksum              12317
_shelx_hkl_checksum              53233
_shelx_fab_checksum              50285