Two isomorphous complexes: dichloro[phthalocyaninato(2‒)]tin(IV) and dichloro[phthalocyaninato(2‒)]germanium(IV)
Jan Janczak; Ryszard Kubiak; Acta Crystallographica Section C 59 (2003) m237–m240; doi:10.1107/S0108270103009417

data_2013291
_publ_section_title
;
 Two isomorphous complexes: dichloro[phthalocyaninato(2--)]tin(IV) and
 dichloro[phthalocyaninato(2--)]germanium(IV)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m237
_journal_page_last               m240
_journal_paper_doi               10.1107/S0108270103009417
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ge (C32 H16 N8) Cl2]'
_chemical_formula_moiety         'C32 H16 Cl2 Ge N8'
_chemical_formula_sum            'C32 H16 Cl2 Ge N8'
_chemical_formula_weight         656.02
_chemical_melting_point          sublimation
_chemical_name_common            'dichlorphthalocyanine germanium'
_chemical_name_systematic
;
 dichloro(phthalocyaninato(2-))germanium(IV)
;
_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                73.85(3)
_cell_angle_beta                 80.61(3)
_cell_angle_gamma                86.39(3)
_cell_formula_units_Z            1
_cell_length_a                   7.3650(10)
_cell_length_b                   8.704(2)
_cell_length_c                   10.966(2)
_cell_measurement_reflns_used    3082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.8
_cell_volume                     666.1(2)
_computing_cell_refinement       'KM-4 CCD software'
_computing_data_collection       'KM-4 CCD software (Kuma, 2000)'
_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, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'KUMA KM-4 CCD area-detector'
_diffrn_measurement_method       '\w scan'
_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  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5657
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
face-indexed, SHELXTL (Sheldrick, 1990)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      1.63
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.285
_refine_ls_extinction_coef       0.110(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0686P)^2^+0.2297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                1936
_reflns_number_total             3082
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg1161.cif
_cod_data_source_block           IIa
_cod_database_code               2013291
_cod_database_fobs_code          2013291