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_4126611
_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         'C86 H92 Cl Fe N3 O, C4 H10 O'
_chemical_formula_sum            'C90 H102 Cl Fe N3 O2'
_chemical_formula_weight         1349.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.5410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2688(6)
_cell_length_b                   26.1296(13)
_cell_length_c                   23.6139(11)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.197
_cell_volume                     8116.3(7)
_computing_cell_refinement       APEX2
_computing_data_collection       APEX2
_computing_data_reduction        APEX2
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    APEX2
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            95216
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.314
_diffrn_reflns_theta_min         1.168
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.057
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.7152
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         20175
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0598
_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^)+(0.1000P)^2^+0.7192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14483
_reflns_number_total             20175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06919_si_007.cif
_cod_data_source_block           930sf01_0ms_a_sqd
_cod_database_code               4126611
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              42300
_shelx_hkl_checksum              34023