A Terminal Iron(IV) Nitride Supported by a Super Bulky Guanidinate Ligand and Examination of Its Electronic Structure and Reactivity.
Maity, Arnab K.; Murillo, Jesse; Metta-Magaña, Alejandro J; Pinter, Balazs; Fortier, Skye; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b06919

data_4126614
_publ_section_title
;
 A Terminal Iron(IV) Nitride Supported by a Super Bulky Guanidinate Ligand
 and Examination of Its Electronic Structure and Reactivity.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06919
_journal_year                    2017
_chemical_formula_moiety         'C96 H98 Fe N6'
_chemical_formula_sum            'C96 H98 Fe N6'
_chemical_formula_weight         1391.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.569(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0290(15)
_cell_length_b                   18.8827(16)
_cell_length_c                   22.8543(19)
_cell_measurement_reflns_used    6754
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.091
_cell_measurement_theta_min      2.26
_cell_volume                     7780.0(11)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.1072
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84233
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         1.129
_diffrn_source                   'fine-focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6476
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         17840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0601P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10005
_reflns_number_total             17840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06919_si_005.cif
_cod_data_source_block           1352SF_0mS_a
_cod_database_code               4126614
_shelxl_version_number           2014/6
_shelx_res_checksum              59814
_shelx_hkl_checksum              14050