Crystal Structure of a Six-coordinated [5,10,15,20-Tetrakis(2,4,6-trimethylphenyl)porphyrinato-<i>k</i><sup>4</sup><i>N</i>]iron(III) Complex with Two 3,5-Dimethylpyridine <i>N</i>-Oxides
IDE, Yuki; HOSODA, Haruka; ISHIMAE, Hiroki; MORI, Shigeki; IKEUE, Takahisa; X-ray Structure Analysis Online 33 (2017) 49–; doi:10.2116/xraystruct.33.49

data_1551578
_publ_section_title
;
 Crystal Structure of a Six-coordinated
 [5,10,15,20-Tetrakis(2,4,6-trimethylphenyl)porphyrinato-&lt;i&gt;k&lt;/i&gt;&lt;sup&gt;4&lt;/sup&gt;&lt;i&gt;N&lt;/i&gt;]iron(III)
 Complex with Two 3,5-Dimethylpyridine &lt;i&gt;N&lt;/i&gt;-Oxides
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              49
_journal_paper_doi               10.2116/xraystruct.33.49
_journal_volume                  33
_journal_year                    2017
_chemical_formula_moiety         'C70 H70 Fe N6 O2, Cl O4, 2(C H Cl3)'
_chemical_formula_sum            'C72 H72 Cl7 Fe N6 O6'
_chemical_formula_weight         1421.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2016/6
_cell_angle_alpha                84.596(2)
_cell_angle_beta                 63.769(3)
_cell_angle_gamma                84.162(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2889(4)
_cell_length_b                   15.8587(4)
_cell_length_c                   16.2403(5)
_cell_measurement_reflns_used    23180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.91
_cell_measurement_theta_min      1.88
_cell_volume                     3508.49(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.4'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59918
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.853
_diffrn_source                   'Varimax 50 kV 24 mA Rotating anode'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         16923
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+4.0012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11522
_reflns_number_total             16923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            33_49_1.txt
_cod_data_source_block           shelxl
_cod_database_code               1551578
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              67554
_shelx_hkl_checksum              15429