Octasubstituted Metal-Free Phthalocyanine as Core of Phosphorus Dendrimers: A Probe for the Properties of the Internal Structure
Julien Leclaire; Rodolphe Dagiral; Suzanne Fery-Forgues; Yannick Coppel; Bruno Donnadieu; Anne-Marie Caminade; Jean-Pierre Majoral; Journal of the American Chemical Society 127 (2005) 15762–15770; doi:10.1021/ja054797b

data_4112056
_publ_contact_author             'Dr A. M. Caminade'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination du CNRS
205 route de Narbonne
31077 Toulouse cedex 4
France
;
_publ_contact_author_email       ' caminade@lcc-toulouse.fr '
_publ_contact_author_fax         '(33) 5 61 55 30 03'
_publ_section_title
;
 Octasubstituted Metal-Free Phthalocyanine as Core of Phosphorus
 Dendrimers: A Probe for the Properties of the Internal Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15762
_journal_page_last               15770
_journal_paper_doi               10.1021/ja054797b
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C24 H16 N2 O4.5'
_chemical_formula_weight         404.39
_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                83.553(18)
_cell_angle_beta                 79.032(17)
_cell_angle_gamma                80.968(16)
_cell_formula_units_Z            2
_cell_length_a                   7.9113(10)
_cell_length_b                   10.7582(16)
_cell_length_c                   13.113(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      1.85
_cell_volume                     1078.2(3)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7878
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1125P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                1792
_reflns_number_total             2919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054797bsi20050718_092823.cif
_cod_data_source_block           C24H16N2O4.50
_cod_original_cell_volume        1078.1(3)
_cod_original_sg_symbol_H-M      ' P -1'
_cod_original_formula_sum        'C24 H16 N2 O4.50'
_cod_database_code               4112056