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_4126615
_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         'C93 H97 Fe N5 Si, 2(C4 H10 O2)'
_chemical_formula_sum            'C101 H117 Fe N5 O2 Si'
_chemical_formula_weight         1516.93
_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   mixed
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 105.8930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.5236(9)
_cell_length_b                   14.0703(5)
_cell_length_c                   23.6909(8)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.157
_cell_measurement_theta_min      2.395
_cell_volume                     8503.4(5)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.959
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62433
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.437
_diffrn_reflns_theta_min         0.798
_diffrn_source                   'fine-focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.23
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.663
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         22596
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1000P)^2^+0.6799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16193
_reflns_number_total             22596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06919_si_006.cif
_cod_data_source_block           1351SF_0mSa_a
_cod_database_code               4126615
_shelxl_version_number           2014/6
_shelx_res_checksum              61392
_shelx_hkl_checksum              65633