Effect of the Sixth Axial Ligand in CS-Ligated Iron(II)octaethylporphyrinates: Structural and Mössbauer Studies
Changsheng Cao; S. Dahal; Mayou Shang; Alicia M. Beatty; Wendy Hibbs; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 42 (2003) 5202–5210; doi:10.1021/ic030043r

data_4314009
_publ_section_title
;
 Effect of the Sixth Axial Ligand in CS-Ligated
 Iron(II)octaethylporphyrinates: Structural and M\"ossbauer Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5202
_journal_page_last               5210
_journal_paper_doi               10.1021/ic030043r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C41 H50 Fe N6 S'
_chemical_formula_sum            'C41 H50 Fe N6 S'
_chemical_formula_weight         714.78
_chemical_name_systematic
;

Fe(1)(OEP)(CS)(1-MeIm)

;
_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                 100.453(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5906(5)
_cell_length_b                   16.704(4)
_cell_length_c                   23.1417(6)
_cell_measurement_reflns_used    244
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3645.8(9)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL-v5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.1008
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22290
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.8119
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;

Walker, N. & Stuart D. (1983) Acta Cryst. A39, 158-166.

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+4.8633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1902
_reflns_number_gt                6057
_reflns_number_total             7882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030043r_1.cif
_cod_data_source_block           fecs
_cod_original_cell_volume        3645.9(8)
_cod_database_code               4314009