Molecular Design of Anionic Phthalocyanines with π‒π Stacking Columnar Arrangement. Crystal Structures, Optical, and Magnetic Properties of Salts with the Iron(I) Hexadecachlorophthalocyanine Anions
Konarev, Dmitri V.; Zorina, Leokadiya V.; Ishikawa, Manabu; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; Crystal Growth & Design 13 (2013) 4930–; doi:10.1021/cg401118s

data_4508479
_publ_section_title
;
 Molecular Design of Anionic Phthalocyanines with \p--\p Stacking Columnar
 Arrangement. Crystal Structures, Optical, and Magnetic Properties of
 Salts with the Iron(I) Hexadecachlorophthalocyanine Anions
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4930
_journal_paper_doi               10.1021/cg401118s
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety
'3(C32 Cl16 Fe N8), 2(C36 H30 N P2), 4(C6 H4 Cl2)'
_chemical_formula_sum            'C192 H76 Cl56 Fe3 N26 P4'
_chemical_formula_weight         5023.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                109.829(2)
_cell_angle_beta                 91.093(2)
_cell_angle_gamma                96.175(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7389(18)
_cell_length_b                   19.612(3)
_cell_length_c                   23.441(4)
_cell_measurement_reflns_used    7400
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     4609.1(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'WinGX (L.J. Farrugia, 1999)'
_computing_publication_material  'WinGX (L.J. Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.1776
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22520
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         16612
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1997
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                7135
_reflns_number_total             16612
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg401118s_si_001.cif
_cod_data_source_block           (FePc)3(PPN)2(C6H4Cl2)4-150k
_cod_original_cell_volume        4609.2(13)
_cod_database_code               4508479