Bis{[phthalocyaninato(2‒)]arsenic(III)} tetradecaiodotetraarsenic(III)
Janczak, Jan; Kubiak, Ryszard; Acta Crystallographica Section C 59 (2003) m70–m72; doi:10.1107/S0108270102020759

data_2013156
_publ_section_title
;
 Bis{[phthalocyaninato(2--)]arsenic(III)}
 tetradecaiodotetraarsenic(III)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m70
_journal_page_last               m72
_journal_paper_doi               10.1107/S0108270102020759
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[As (C32 H16 N8)]2 [As4 I14]'
_chemical_formula_moiety         '2C32 H16 As N8 + , As4 I14 2-'
_chemical_formula_sum            'C64 H32 As6 I14 N16'
_chemical_formula_weight         3251.18
_chemical_melting_point          decomposition
_chemical_name_common
;
Arsenic phthalocyanine--arsenic iodide'
;
_chemical_name_systematic
;
Bis{[phthalocyaninato(2-)]arsenic(III)} tetradecaiodotetraarsenic(III)
;
_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
_cell_angle_alpha                82.32(3)
_cell_angle_beta                 71.63(3)
_cell_angle_gamma                83.05(3)
_cell_formula_units_Z            1
_cell_length_a                   12.081(2)
_cell_length_b                   12.600(2)
_cell_length_c                   13.950(3)
_cell_measurement_reflns_used    6210
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      3.27
_cell_volume                     1990.2(7)
_computing_cell_refinement       'KM-4 CCD Software'
_computing_data_collection       'KM-4 CCD Software (Kuma Diffraction, 1999)'
_computing_data_reduction        'KM-4 CCD Software'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type
'Kuma KM-4 with two-dimensional CCD area-detector'
_diffrn_measurement_method       \w
_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  0.016
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15578
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    7.970
_exptl_absorpt_correction_T_max  0.402
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'face-indexed (SHELXTL; Sheldrick, 1990)'
_exptl_crystal_colour            black-violet
_exptl_crystal_density_diffrn    2.713
_exptl_crystal_density_meas      2.71
_exptl_crystal_density_method    'flotation in what'
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.65
_refine_ls_extinction_coef       0.00059(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_gt           0.027
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.053
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                6210
_reflns_number_total             8037
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1232.cif
_cod_data_source_block           I
_cod_database_code               2013156
_cod_database_fobs_code          2013156