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_4510791
_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
'(C32 Cl16 Fe N8), 2(C19 H18 P), (C6 H4 Cl2) (Br)'
_chemical_formula_sum            'C76 H40 Br Cl18 Fe N8 P2'
_chemical_formula_weight         1900.96
_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                79.53(1)
_cell_angle_beta                 76.34(1)
_cell_angle_gamma                84.04(1)
_cell_formula_units_Z            2
_cell_length_a                   10.765(1)
_cell_length_b                   17.305(2)
_cell_length_c                   20.621(2)
_cell_measurement_reflns_used    1349
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      2.40
_cell_volume                     3663.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    sir2004
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker SMART ApexII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.2465
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21665
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1898
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         16371
_refine_ls_number_restraints     977
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.2454
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.2318
_reflns_number_gt                5754
_reflns_number_total             16371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401118s_si_004.cif
_cod_data_source_block           (Ph3MeP)2[Fe(Cl16Pc)](Br)PhCl2
_cod_database_code               4510791