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_2013292
_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            'phthalocyanine germanium'
_chemical_name_systematic
;
 dichloro(phthalocyaninato(2-))germanium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.124(2)
_cell_length_b                   14.810(3)
_cell_length_c                   10.233(2)
_cell_measurement_reflns_used    2102
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3.41
_cell_volume                     1367.6(5)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12868
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
face-indexed, SHELXTL (Sheldrick, 1990)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      1.59
_exptl_crystal_density_method    'floatation in CHCl3/CHBr3'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0407P)^2^+0.2270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                2102
_reflns_number_total             3561
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg1161.cif
_cod_data_source_block           IIb
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013292
_cod_database_fobs_code          2013292