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_4329409
_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 H20 B N7,  0.05(H2 O)'
_chemical_formula_sum            'C31 H20.1 B N7 O0.05'
_chemical_formula_weight         502.25
_chemical_name_common            N-Phenyl-N-methyl-amino-boronsubphthalocyanine
_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                72.9030(14)
_cell_angle_beta                 81.8810(12)
_cell_angle_gamma                75.8510(13)
_cell_formula_units_Z            4
_cell_length_a                   11.5120(3)
_cell_length_b                   11.7673(3)
_cell_length_c                   19.3022(5)
_cell_measurement_reflns_used    42414
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.7
_cell_volume                     2416.61(11)
_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(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42414
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.906
_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    1.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         11050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0851P)^2^+0.0931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                6666
_reflns_number_total             11050
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2016935_si_003.cif
_cod_data_source_block           Compound5_k1182
_cod_original_formula_sum        'C31 H20.10 B N7 O0.05'
_cod_database_code               4329409