Crystal Structure of a Six-coordinated (2,3,7,8,12,13,17,18-Octaethylporphyrinato)iron(III) Complex with Two 4-Methylpyridine <i>N</i>-Oxides
IDE, Yuki; YAMADA, Yuya; MORI, Shigeki; IKEUE, Takahisa; X-ray Structure Analysis Online 33 (2017) 25–; doi:10.2116/xraystruct.33.25

data_1551575
_publ_section_title
;
 Crystal Structure of a Six-coordinated
 (2,3,7,8,12,13,17,18-Octaethylporphyrinato)iron(III) Complex with Two
 4-Methylpyridine &lt;i&gt;N&lt;/i&gt;-Oxides
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              25
_journal_paper_doi               10.2116/xraystruct.33.25
_journal_volume                  33
_journal_year                    2017
_chemical_formula_moiety         'C48 H58 Fe N6 O2, B F4'
_chemical_formula_sum            'C48 H58 B F4 Fe N6 O2'
_chemical_formula_weight         893.66
_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-2014/7
_cell_angle_alpha                90.870(2)
_cell_angle_beta                 92.579(2)
_cell_angle_gamma                93.419(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9064(2)
_cell_length_b                   13.7091(4)
_cell_length_c                   20.7535(6)
_cell_measurement_reflns_used    17271
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.18
_cell_measurement_theta_min      2.00
_cell_volume                     2242.83(11)
_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 4.2.1 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 1.000
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38256
_diffrn_reflns_point_group_measured_fraction_full 1.000
_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         1.769
_diffrn_source                   'Varimax 50 kV 24 mA Rotating anode'
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.835
_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    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         10829
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0400P)^2^+1.6202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8089
_reflns_number_total             10829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            33_25_2.txt
_cod_data_source_block           shelxl
_cod_database_code               1551575
_publcif_datablock.id            {4134f2b8-ffda-4b33-9725-03a9fe51f047}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              26809
_shelx_hkl_checksum              74088
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes y