Generation, spectroscopic and chemical characterization of an octahedral iron (V) - nitrido species with a neutral ligand platform.
Sabenya, Gerard; Lazaro, Laura; Gamba, Ilaria; Martin-Diaconescu, Vlad; Andris, Erik; Weyhermüller, Thomas; Neese, Frank; Roithova, Jana; Bill, Eckhard; Lloret-Fillol, Julio; Costas, Miquel; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b00429

data_4126256
_publ_section_title
;
 Generation, spectroscopic and chemical characterization of an octahedral
 iron (V) - nitrido species with a neutral ligand platform.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b00429
_journal_year                    2017
_chemical_formula_moiety         'C19 H27 Fe N8, 2(F6 P)'
_chemical_formula_sum            'C19 H27 F12 Fe N8 P2'
_chemical_formula_weight         713.27
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.837(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.312(6)
_cell_length_b                   10.407(5)
_cell_length_c                   22.323(11)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.57
_cell_measurement_theta_min      2.16
_cell_volume                     2627(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.1316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.226
_diffrn_reflns_theta_min         1.801
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.493718
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       plate
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6081
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0977P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2971
_reflns_number_total             6081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00429_si_002.cif
_cod_data_source_block           fe3n3lsrecris
_cod_database_code               4126256
_shelxl_version_number           2013-3
_shelx_res_checksum              60038
_shelx_hkl_checksum              82724