Heterogeneous catalytic properties of unprecedented μ-O-[FeTCPP]2 dimers (H2TCPP = meso-tetra(4-carboxyphenyl)porphyrin): an unusual superhyperfine EPR structure.
Fidalgo-Marijuan, Arkaitz; Barandika, Gotzone; Bazán, Begoña; Urtiaga, Miren Karmele; Larrea, Edurne S.; Iglesias, Marta; Lezama, Luis; Arriortua, María Isabel; Dalton transactions (Cambridge, England : 2003) 44 (2015) 213–222; doi:10.1039/c4dt02250e

data_7032838
_publ_section_title
;
 Heterogeneous catalytic properties of unprecedented \m-O-[FeTCPP]2 dimers
 (H2TCPP = meso-tetra(4-carboxyphenyl)porphyrin): an unusual
 superhyperfine EPR structure.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              213
_journal_page_last               222
_journal_paper_doi               10.1039/c4dt02250e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C96 H48 Fe2 N8 O17,16(C3 H7 N)'
_chemical_formula_sum            'C144 H168 Fe2 N24 O33'
_chemical_formula_weight         2874.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-09-17T14:27:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.418(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.3340(4)
_cell_length_b                   19.8329(2)
_cell_length_c                   16.0292(2)
_cell_measurement_reflns_used    17186
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.8985
_cell_measurement_theta_min      2.4985
_cell_measurement_wavelength     1.54184
_cell_volume                     12369.8(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
        SHELXL, G.M. Sheldrick, Acta Cryst.
        (2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.2012
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0242603
_diffrn_orient_matrix_UB_12      0.0582367
_diffrn_orient_matrix_UB_13      0.0327605
_diffrn_orient_matrix_UB_21      -0.0151063
_diffrn_orient_matrix_UB_22      0.0433373
_diffrn_orient_matrix_UB_23      -0.0762826
_diffrn_orient_matrix_UB_31      -0.0274029
_diffrn_orient_matrix_UB_32      0.0276596
_diffrn_orient_matrix_UB_33      0.0504576
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50744
_diffrn_reflns_theta_full        71.5
_diffrn_reflns_theta_max         71.5
_diffrn_reflns_theta_min         2.5
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.692
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.82718
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      1.575(5)
_exptl_crystal_density_method    Flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             6064
_exptl_crystal_size_max          0.2172
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.0542
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         12049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2025
_reflns_number_gt                8890
_reflns_number_total             12049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02250e2.cif
_cod_data_source_block           af574_cu
_cod_depositor_comments          'Adding full bibliography for 7032838.cif.'
_cod_database_code               7032838
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.592