Synthesis and Crystallographic Characterization of Low-Dimensional and Porous Coordination Compounds Capable of Supramolecular Aromatic Interaction Using the 4,4'-Azobis(pyridine) Ligand
Shin-ichiro Noro; Susumu Kitagawa; Takayoshi Nakamura; Tatsuo Wada; Inorganic Chemistry 44 (2005) 3960–3971; doi:10.1021/ic048371u

data_4308884
_publ_section_title
;
Synthesis and Crystallographic Characterization of Low-Dimensional and
Porous Coordination Compounds Capable of Supramolecular Aromatic
Interaction Using the 4,4'-Azobis(pyridine) Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3960
_journal_page_last               3971
_journal_paper_doi               10.1021/ic048371u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C70 H68 F24 N28 Ni2 O6 P4'
_chemical_formula_weight         2094.75
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                105.17(1)
_cell_angle_beta                 90.06(2)
_cell_angle_gamma                83.11(1)
_cell_formula_units_Z            1
_cell_length_a                   11.635(4)
_cell_length_b                   17.631(7)
_cell_length_c                   10.580(4)
_cell_measurement_reflns_used    15761
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2078.5(13)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  'teXsan Ver. 2.0'
_computing_structure_solution    DirectMethod
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9912
_diffrn_measured_fraction_theta_max 0.9912
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20410
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064.00
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.041
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9437
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.0034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2154
_reflns_number_gt                6712
_reflns_number_total             20410
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic048371usi20050228_095810.cif
_cod_data_source_block           {[Ni2(azpy)6(H2O)5](PF6)4(
_cod_original_cell_volume        2078(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C70 H68 F24 N28 O6 Ni2 P4 '
_cod_database_code               4308884