Construction of a Square-Planar Molecular Box: Self-Assembly of Palladium(II) Complexes of 3,6,9,16,19,22-Hexaazatricyclo[22.2.2.211,14]triacon -11,13,24,26(1),27,29-hexaene through Hydrogen-Bonding Interactions
Weijiang He; Fang Liu; Chunying Duan; Zijian Guo; Shaozhen Zhou; Yongjiang Liu; Longgen Zhu; Inorganic Chemistry 40 (2001) 7065–7071; doi:10.1021/ic010101d

data_4320751
_publ_section_title
;
 Construction of a Square-Planar Molecular Box: Self-Assembly of
 Palladium(II) Complexes of
 3,6,9,16,19,22-Hexaazatricyclo[22.2.2.211,14]triacon
 -11,13,24,26(1),27,29-hexaene through Hydrogen-Bonding Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7065
_journal_page_last               7071
_journal_paper_doi               10.1021/ic010101d
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C52 H88 N16 O26 Pd4'
_chemical_formula_weight         1778.98
_chemical_name_systematic
;
  ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.30(3)
_cell_angle_beta                 90.63(3)
_cell_angle_gamma                104.05(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6960(19)
_cell_length_b                   13.320(3)
_cell_length_c                   14.605(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1826.2(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31071
_diffrn_reflns_theta_full        27.82
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    1.054
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8529
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0831P)^2^+0.7454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                5859
_reflns_number_total             8529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010101d_3.cif
_cod_data_source_block           pd1
_cod_original_cell_volume        1826.2(6)
_cod_database_code               4320751