Unraveling the Electronic Structures of Low-Valent Naphthalene and Anthracene Iron Complexes: X-ray, Spectroscopic, and Density Functional Theory Studies
Eva-Maria Schnöckelborg; Marat M. Khusniyarov; Bas de Bruin; František Hartl; Thorsten Langer; Matthias Eul; Stephen Schulz; Rainer Pöttgen; Robert Wolf; Inorganic Chemistry 51 (2012) 6719–6730; doi:10.1021/ic300366m

data_4329484
_publ_section_title
;
 Unraveling the Electronic Structures of Low-Valent Naphthalene and
 Anthracene Iron Complexes: X-ray, Spectroscopic, and Density Functional
 Theory Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6719
_journal_page_last               6730
_journal_paper_doi               10.1021/ic300366m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C36 H49 Fe K O6'
_chemical_formula_weight         672.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 116.4140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.6401(14)
_cell_length_b                   17.6383(12)
_cell_length_c                   22.0480(16)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.74
_cell_measurement_theta_min      1.55
_cell_volume                     6840.5(8)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67584
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_correction_T_min  0.8298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =   0.854049

;
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         16254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0417P)^2^+2.4691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                13036
_reflns_number_total             16254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300366m_si_002_1.cif
_cod_data_source_block           p21c_fin
_cod_database_code               4329484