Axial Functionalization of Sterically Hindered Titanium Phthalocyanines
Elisabeth Seikel; Benjamin Oelkers; Jörg Sundermeyer; Inorganic Chemistry 51 (2012) 2709–2717; doi:10.1021/ic202749v

data_4328471
_publ_section_title
;
 Axial Functionalization of Sterically Hindered Titanium Phthalocyanines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2709
_journal_page_last               2717
_journal_paper_doi               10.1021/ic202749v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '3(C64 H74 N8), C5 H12, 6(C7 H8)'
_chemical_formula_sum            'C239 H282 N24'
_chemical_formula_weight         3490.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   32.4964(18)
_cell_length_b                   32.4964(18)
_cell_length_c                   16.3282(10)
_cell_measurement_reflns_used    3768
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.53
_cell_measurement_theta_min      1.25
_cell_volume                     14932.7(15)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.2931
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18941
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.0492
_exptl_absorpt_correction_T_min  0.9724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       plate
_exptl_crystal_F_000             5652
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7016
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.3209
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1782
_reflns_number_gt                1547
_reflns_number_total             7016
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202749v_si_005.cif
_cod_data_source_block           es-pc-h2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4328471