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_4108177
_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            'C27 H38 B Cl Fe N6'
_chemical_formula_weight         548.38
_chemical_name_systematic
;
 phenyltris-(1-tert-butyl-imidazol-2-ylidene)boratoiron(ii)chloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.371(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7017(5)
_cell_length_b                   17.8773(11)
_cell_length_c                   16.4921(9)
_cell_measurement_reflns_used    6576
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      61.06
_cell_measurement_theta_min      4.68
_cell_volume                     2857.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18958
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  224
_exptl_absorpt_correction_T_min  223
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.0134(10)
_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   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                2913
_reflns_number_total             3503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8027372-file001.cif
_cod_data_source_block           js063a
_cod_database_code               4108177