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_4108178
_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_moiety         'C27 H38 B Fe N7, C2 H3 N'
_chemical_formula_sum            'C29 H41 B Fe N8'
_chemical_formula_weight         568.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.1318(6)
_cell_length_b                   18.1789(6)
_cell_length_c                   18.3767(6)
_cell_measurement_reflns_used    8356
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      2.51
_cell_volume                     6057.3(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            177688
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.23
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker,SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       prism
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         10471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+2.3605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                7557
_reflns_number_total             10471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8027372-file002.cif
_cod_data_source_block           js82
_cod_database_code               4108178