Homo- and Heterobismetal Complexes of 5-Hydroxy-10,15,25,30-tetrakis(pentafluorophenyl)-Substituted [26]Hexaphyrin(1.1.1.1.1.1)
Taro Koide; Gengo Kashiwazaki; Ko Furukawa; Atsuhiro Osuka; Inorganic Chemistry 48 (2009) 4595–4597; doi:10.1021/ic900084p

data_4302196
_publ_section_title
;
Homo- and Heterobismetal Complexes of
5-Hydroxy-10,15,25,30-tetrakis(pentafluorophenyl)-Substituted
[26]Hexaphyrin(1.1.1.1.1.1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4595
_journal_page_last               4597
_journal_paper_doi               10.1021/ic900084p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C54 H13 Cl F20 N6 O Zn2, 3(C Cl3)'
_chemical_formula_sum            'C57 H13 Cl10 F20 N6 O Zn2'
_chemical_formula_weight         1662.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.946(2)
_cell_length_b                   11.5872(14)
_cell_length_c                   26.101(3)
_cell_measurement_temperature    90(2)
_cell_volume                     5828.0(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34380
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.948
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         13123
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0807
_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 w=1/[\s^2^(Fo^2^)+(0.1270P)^2^+26.1601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2428
_reflns_number_gt                10275
_reflns_number_total             13123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900084p_si_001_2.cif
_cod_data_source_block           zn2
_cod_original_cell_volume        5828.0(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4302196