Structural and Magnetic Effects of meso-Substitution in Alkyl-Substituted Metalloporphyrinate π-Cation Radicals: Characterization of [Fe(TalkylP.)(Cl)]SbCl6 (alkyl = ethyl andn-propyl)
Ming Li; Teresa J. Neal; Graeme R. A. Wyllie; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 49 (2010) 8078–8085; doi:10.1021/ic101099z

data_4316430
_publ_section_title
;
 Structural and Magnetic Effects of meso-Substitution in Alkyl-Substituted
 Metalloporphyrinate \p-Cation Radicals: Characterization of
 [Fe(TalkylP.)(Cl)]SbCl6 (alkyl = ethyl andn-propyl)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8078
_journal_page_last               8085
_journal_paper_doi               10.1021/ic101099z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C29 H30 Cl9 Fe N4 Sb'
_chemical_formula_weight         931.22
_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                76.90(3)
_cell_angle_beta                 87.32(3)
_cell_angle_gamma                71.77(3)
_cell_formula_units_Z            2
_cell_length_a                   9.768(2)
_cell_length_b                   13.585(3)
_cell_length_c                   14.508(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1780.4(8)
_computing_cell_refinement       Madnes
_computing_data_collection       Madnes
_computing_data_reduction        'madnes (Messerschmitt &Pflugraph,1987)'
_computing_molecular_graphics    'Ortep III (burnett, Johnson, 1996)'
_computing_publication_material  Shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Enraf-nonius Fast Area-Detector'
_diffrn_measurement_method       'Ellipsoid-mask Fitting'
_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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17182
_diffrn_reflns_theta_full        29.95
_diffrn_reflns_theta_max         28.7
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        'No measurable crystal decay'
_exptl_absorpt_coefficient_mu    1.870
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Dark-purple
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       Rhombohedron
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.46
_refine_diff_density_min         -1.71
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.0008(5)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+5.4668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                7801
_reflns_number_total             9071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101099z_si_002_1.cif
_cod_data_source_block           sd:fetetsbcl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1780.2(6)
_cod_database_code               4316430