Three-Coordinate Terminal Imidoiron(III) Complexes: Structure, Spectroscopy, and Mechanism of Formation
Ryan E. Cowley; Nathan J. DeYonker; Nathan A. Eckert; Thomas R. Cundari; Serena DeBeer; Eckhard Bill; Xavier Ottenwaelder; Christine Flaschenriem; Patrick L. Holland; Inorganic Chemistry 49 (2010) 6172–6187; doi:10.1021/ic100846b

data_4315983
_publ_section_title
;
 Three-Coordinate Terminal Imidoiron(III) Complexes: Structure,
 Spectroscopy, and Mechanism of Formation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6172
_journal_page_last               6187
_journal_paper_doi               10.1021/ic100846b
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C80 H121 Fe2 N7, 2(C5 H12)'
_chemical_formula_sum            'C90 H145 Fe2 N7'
_chemical_formula_weight         1436.83
_chemical_name_common            holrc23
_chemical_name_systematic
; 
 ? 
;
_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                94.791(4)
_cell_angle_beta                 102.722(4)
_cell_angle_gamma                93.567(4)
_cell_formula_units_Z            2
_cell_length_a                   13.282(3)
_cell_length_b                   15.629(3)
_cell_length_c                   21.057(4)
_cell_measurement_reflns_used    8140
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.24
_cell_volume                     4234.3(15)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1404
_diffrn_reflns_av_sigmaI/netI    0.1526
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44611
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.311
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         14949
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2449
_reflns_number_gt                8511
_reflns_number_total             14949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100846b_si_001_3.cif
_cod_data_source_block           holrc23
_cod_original_cell_volume        4234.4(15)
_cod_database_code               4315983