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_4320749
_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            'C24 H40 Cl2 N8 O7 Pd2'
_chemical_formula_weight         836.34
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 93.580(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.744(3)
_cell_length_b                   9.2435(15)
_cell_length_c                   16.259(2)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.24
_cell_measurement_theta_min      6.41
_cell_volume                     3261.5(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w 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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7211
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        28.83
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.5539
_exptl_absorpt_correction_T_min  0.5073
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.114
_refine_diff_density_min         -2.770
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5721
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1116P)^2^+3.6485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.2042
_reflns_number_gt                3521
_reflns_number_total             5721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010101d_1.cif
_cod_data_source_block           62a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320749