Subphthalocyanines Axially Substituted with a Tetracyanobuta-1,3-diene-Aniline Moiety: Synthesis, Structure, and Physicochemical Properties.
Winterfeld, Kim A.; Lavarda, Giulia; Guilleme, Julia; Sekita, Michael; Guldi, Dirk M.; Torres, Tomás; Bottari, Giovanni; Journal of the American Chemical Society 139 (2017) 5520–5529; doi:10.1021/jacs.7b01460

data_4125913
_publ_section_title
;
 Subphthalocyanines Axially Substituted with a
 Tetracyanobuta-1,3-diene-Aniline Moiety: Synthesis, Structure, and
 Physicochemical Properties.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5520
_journal_page_last               5529
_journal_paper_doi               10.1021/jacs.7b01460
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C40.5 H10.5 B Cl1.5 F12 N11'
_chemical_formula_weight         943.08
_chemical_name_common            TCNE-05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 117.894(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4663(7)
_cell_length_b                   17.0450(6)
_cell_length_c                   16.9234(7)
_cell_measurement_reflns_used    2673
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      18.1459
_cell_measurement_theta_min      2.3655
_cell_volume                     4198.0(3)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1643
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63993
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'intense pink'
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.406
_refine_ls_extinction_coef       0.0127(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         7693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.2400
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2840
_refine_ls_wR_factor_ref         0.3700
_reflns_number_gt                3067
_reflns_number_total             7693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b01460_si_005.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 4125913.cif.'
_cod_original_formula_sum        'C40.50 H10.50 B Cl1.50 F12 N11'
_cod_database_code               4125913