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

data_4328470
_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         'C64 H72 N8 O Ti, 3(C6 H6)'
_chemical_formula_sum            'C82 H90 N8 O Ti'
_chemical_formula_weight         1251.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_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                 111.031(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2868(11)
_cell_length_b                   18.8506(11)
_cell_length_c                   14.4279(12)
_cell_measurement_reflns_used    3645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.43
_cell_measurement_theta_min      1.76
_cell_volume                     3373.0(5)
_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, 1997)'
_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 0.995
_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  0.0997
_diffrn_reflns_av_sigmaI/netI    0.1407
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11419
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.9681
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1685
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                1568
_reflns_number_total             3685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202749v_si_004.cif
_cod_data_source_block           es-174
_cod_original_cell_volume        3373.0(4)
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               4328470