Spin-crossover between high-spin (S = 5/2) and low-spin (S = 1/2) states in six-coordinate iron(iii) porphyrin complexes having two pyridine-N oxide derivatives.
Ide, Yuki; Murai, Nami; Ishimae, Hiroki; Suzuki, Masaaki; Mori, Shigeki; Takahashi, Masashi; Nakamura, Mikio; Yoshino, Katsumi; Ikeue, Takahisa; Dalton transactions (Cambridge, England : 2003) 46 (2016) 242–249; doi:10.1039/c6dt03859j

data_7041268
_publ_section_title
;
 Spin-crossover between high-spin (S = 5/2) and low-spin (S = 1/2) states
 in six-coordinate iron(iii) porphyrin complexes having two pyridine-N
 oxide derivatives.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              242
_journal_page_last               249
_journal_paper_doi               10.1039/c6dt03859j
_journal_volume                  46
_journal_year                    2016
_chemical_formula_moiety
'C58 H28 F20 Fe N8 O2, 2.5(C7 H8), B F4, C H2 Cl2'
_chemical_formula_sum            'C76.5 H50 B Cl2 F24 Fe N8 O2'
_chemical_formula_weight         1706.80
_chemical_name_systematic        '[Fe(TPFPP)(4NMe2PyNO)2]BF4'
_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
_audit_update_record
;
2016-10-27 deposited with the CCDC.
2016-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.515(14)
_cell_angle_beta                 108.315(10)
_cell_angle_gamma                117.216(8)
_cell_formula_units_Z            2
_cell_length_a                   14.7563(16)
_cell_length_b                   15.299(2)
_cell_length_c                   18.938(2)
_cell_measurement_reflns_used    5983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.13
_cell_measurement_theta_min      2.15
_cell_volume                     3519.2(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1.1 (Rigaku, 2015)'
_computing_publication_material  'CrystalStructure 4.1.1'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0770
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'Varimax 50 kV 24 mA Rotating anode'
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1724
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         14590
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.0988
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10094
_reflns_number_total             14590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03859j3.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7041264--7041268.cif.'
_cod_original_cell_volume        3519.3(8)
_cod_original_formula_sum        'C76.50 H50 B Cl2 F24 Fe N8 O2'
_cod_database_code               7041268
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              60498