Effect of the Ruffled Porphyrin Ring on Electronic Structures: Structure and Characterization of [Fe(TalkylP)(OClO3)] and [Fe(TPrP)(THF)2]ClO4 (alkyl = Ethyl, Et and n-Propyl, Pr)
Ming Li; Allen G. Oliver; Teresa J. Neal; Charles E. Schulz; W. Robert Scheidt; Journal of Porphyrins and Phthalocyanines 17 (2013) 118–124; doi:10.1142/S1088424612501362

data_1548715
_publ_section_title
;
 Effect of the Ruffled Porphyrin Ring on Electronic Structures: Structure
 and Characterization of [Fe(TalkylP)(OClO3)] and [Fe(TPrP)(THF)2]ClO4
 (alkyl = Ethyl, Et and n-Propyl, Pr)
;
_journal_name_full               'Journal of Porphyrins and Phthalocyanines'
_journal_page_first              118
_journal_page_last               124
_journal_paper_doi               10.1142/S1088424612501362
_journal_volume                  17
_journal_year                    2013
_chemical_formula_moiety         'C44 H60 Fe N4 O3, Cl O4'
_chemical_formula_sum            'C44 H60 Cl Fe N4 O7'
_chemical_formula_weight         848.26
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.085(2)
_cell_length_b                   18.8929(5)
_cell_length_c                   9.4840(4)
_cell_measurement_reflns_used    253
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      2.6
_cell_volume                     4136.4(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 9.23
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_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  0.1068
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            29047
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_correction_T_min  0.7934
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   REFDELF
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.227
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.69(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7497
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1394P)^2^+6.3833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2320
_reflns_number_gt                6149
_reflns_number_total             7497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NIHMS432021-supplement-cif3.cif
_cod_data_source_block           fetprpthfclo4
_cod_database_code               1548715