Structural and Spectroscopic Characterization of an Electrophilic Iron Nitrido Complex
Jeremiah J. Scepaniak; Meita D. Fulton; Ranko P. Bontchev; Eileen N. Duesler; Martin L. Kirk; Jeremy M. Smith; Journal of the American Chemical Society 130 (2008) 10515–10517; doi:10.1021/ja8027372

data_4108179
_publ_section_title
;
 Structural and Spectroscopic Characterization of an Electrophilic Iron
 Nitrido Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10515
_journal_page_last               10517
_journal_paper_doi               10.1021/ja8027372
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C180 H212 B4 Fe4 N28 P4'
_chemical_formula_weight         3158.28
_chemical_name_systematic
;
 Triphenylphosphamidophenyltris(1-mesitylimidazol-2-ylidene)boratoiron(II).
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.653(4)
_cell_angle_beta                 97.227(4)
_cell_angle_gamma                91.830(4)
_cell_formula_units_Z            1
_cell_length_a                   14.2125(10)
_cell_length_b                   14.4329(10)
_cell_length_c                   20.4911(14)
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      56.50
_cell_measurement_theta_min      4.77
_cell_volume                     4165.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  diffractometer
_diffrn_measurement_method       diffractometer
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98193
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  224
_exptl_absorpt_correction_T_min  223
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.0083(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         13091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+1.5159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                11405
_reflns_number_total             13091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8027372-file003.cif
_cod_data_source_block           b
_cod_database_code               4108179