Synthesis and Structural Characterization of Integrally Oxidized, Metal-Free Phthalocyanine Compounds: [H2(pc)][IBr2] and [H2(pc)]2[IBr2]Br.C10H7Br
Anna S. Gardberg; Syaulan Yang; Brian M. Hoffman; James A. Ibers; Inorganic Chemistry 41 (2002) 1778–1781; doi:10.1021/ic010994+

data_4327506
_publ_section_title
;
 Synthesis and Structural Characterization of Integrally Oxidized,
 Metal-Free Phthalocyanine Compounds: [H2(pc)][IBr2] and
 [H2(pc)]2[IBr2]Br.C10H7Br
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1778
_journal_page_last               1781
_journal_paper_doi               10.1021/ic010994+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H18 Br2 I N8'
_chemical_formula_weight         801.26
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_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                 113.975(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0272(9)
_cell_length_b                   21.258(2)
_cell_length_c                   18.143(2)
_cell_measurement_temperature    153(2)
_cell_volume                     2828.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33975
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    3.997
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_F_000             1556
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0469
_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
  [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l]
  where P = 1.00000Fo^2^ + 0.00000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                3998
_reflns_number_total             6992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109942B_1.cif
_cod_data_source_block           H2pcIBr2
_cod_original_cell_volume        2828.8(5)
_cod_database_code               4327506