Aluminum Chloride Activation of Chloro-Boronsubphthalocyanine: a Rapid and Flexible Method for Axial Functionalization with an Expanded Set of Nucleophiles
Graham E. Morse; Timothy P. Bender; Inorganic Chemistry 51 (2012) 6460–6467; doi:10.1021/ic2016935

data_4329408
_publ_contact_author_address
;
Department of Chemical Engineering & Applied Chemistry
University of Toronto
200 College Street, Rm. 225
Toronto, Ontario, Canada.   M5S 3E5
;
_publ_contact_author_email       tim.bender@utoronto.ca
_publ_contact_author_fax         1-416-978-8605
_publ_contact_author_name        'Timothy P Bender'
_publ_contact_author_phone       1-416-978-6140
_publ_section_title
;
 Aluminum Chloride Activation of Chloro-Boronsubphthalocyanine: a Rapid
 and Flexible Method for Axial Functionalization with an Expanded Set of
 Nucleophiles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6460
_journal_page_last               6467
_journal_paper_doi               10.1021/ic2016935
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C31 H19 B N6 S'
_chemical_formula_sum            'C31 H19 B N6 S'
_chemical_formula_weight         518.39
_chemical_name_common            4-Methylthiophenoxy-boronsubphthalocyanine
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.582(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3506(4)
_cell_length_b                   22.6651(9)
_cell_length_c                   10.7047(3)
_cell_measurement_reflns_used    14105
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2450.99(15)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14105
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0889P)^2^+0.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                3425
_reflns_number_total             5356
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2016935_si_002.cif
_cod_data_source_block           Compound3_k1185
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329408