Characterization of the mixed axial ligand complex (4-cyanopyridine)(imidazole)(tetramesitylporphinato)iron(iii) perchlorate. Stabilization by synergic bonding
Judith A. Serth-Guzzo; Ilona Turowska-Tyrk; Martin K. Safo; F. Ann Walker; Peter G. Debrunner; W. Robert Scheidt; Journal of Porphyrins and Phthalocyanines 20 (2016) 254–264; doi:10.1142/S1088424616500206

data_1548449
_publ_section_title
;
 Characterization of the mixed axial ligand complex
 (4-cyanopyridine)(imidazole)(tetramesitylporphinato)iron(iii)
 perchlorate. Stabilization by synergic bonding
;
_journal_name_full               'Journal of Porphyrins and Phthalocyanines'
_journal_page_first              254
_journal_page_last               264
_journal_paper_doi               10.1142/S1088424616500206
_journal_volume                  20
_journal_year                    2016
_chemical_formula_sum            'C68.08 H67 Cl2.12 Fe N8 O4'
_chemical_formula_weight         1192.35
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.256(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4318(12)
_cell_length_b                   20.696(2)
_cell_length_c                   19.970(5)
_cell_measurement_reflns_used    202
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.6
_cell_volume                     6294.9(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      127(2)
_diffrn_measured_fraction_theta_full .984
_diffrn_measured_fraction_theta_max .896
_diffrn_measurement_device       '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  0.1251
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31189
_diffrn_reflns_theta_full        28.800
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  .951
_exptl_absorpt_correction_T_min  .926
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block-like
_exptl_crystal_F_000             2502
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         16220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.202
_refine_ls_R_factor_all          0.1685
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.310
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+11.9827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2609
_refine_ls_wR_factor_ref         0.2095
_reflns_number_gt                8397
_reflns_number_total             16241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NIHMS809767.cif
_cod_data_source_block           Fe
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C68.08 H67.0 Cl2.12 Fe N8 O4'
_cod_database_code               1548449