Fe-TPP Coordination Network with Metalloporphyrinic Neutral Radicals and Face-to-Face and Edge-to-Face π-π Stacking
Arkaitz Fidalgo-Marijuan; Gotzone Barandika; Begoña Bazán; Miren Karmele Urtiaga; Luis Lezama; María Isabel Arriortua; Inorganic Chemistry 52 (2013) 8074–8081; doi:10.1021/ic4007372

data_4335471
_publ_contact_author
;
   Dra. Gotzone Barandika
   Facultad de Farmacia
   Dpto. de Quimica Inorganica 
   Universidad del Pais Vasco
   Paseo de la Universidad, 7
   01006 Vitoria-Gasteiz
   Spain
;
_publ_contact_author_email       gotzone.barandika@ehu.es
_publ_contact_author_fax         +34(945)013014
_publ_contact_author_phone       +34(945)013080
_publ_section_title
;
 Fe-TPP Coordination Network with Metalloporphyrinic Neutral Radicals and
 Face-to-Face and Edge-to-Face \p-\p Stacking
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8074
_journal_page_last               8081
_journal_paper_doi               10.1021/ic4007372
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C54 H36 Fe N6'
_chemical_formula_sum            'C54 H36 Fe N6'
_chemical_formula_weight         824.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
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_symmetry_space_group_name_Hall  '-C 2yc'
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_cell_angle_alpha                90
_cell_angle_beta                 97.354(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6833(8)
_cell_length_b                   11.0827(4)
_cell_length_c                   17.6206(6)
_cell_measurement_reflns_used    4635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9408
_cell_measurement_theta_min      2.6194
_cell_measurement_wavelength     0.71073
_cell_volume                     4199.6(3)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
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_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia,1997)'
_computing_publication_material  'WinGX publication routines (Farrugia,1999)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0000012703
_diffrn_orient_matrix_UB_12      0.0639897676
_diffrn_orient_matrix_UB_13      0.0003329821
_diffrn_orient_matrix_UB_21      -0.0099829239
_diffrn_orient_matrix_UB_22      0.0004442047
_diffrn_orient_matrix_UB_23      -0.0399479378
_diffrn_orient_matrix_UB_31      -0.0314560491
_diffrn_orient_matrix_UB_32      -0.000225341
_diffrn_orient_matrix_UB_33      0.0072241137
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
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_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10334
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.896
_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_density_diffrn    1.304
_exptl_crystal_density_meas      1.309(5)
_exptl_crystal_density_method    Flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.3403
_exptl_crystal_size_mid          0.0774
_exptl_crystal_size_min          0.0718
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00015(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.91
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.91
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                2856
_reflns_number_total             3907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4007372_si_002.cif
_cod_data_source_block           af247
_cod_database_code               4335471