#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:52:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179310 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/07/4320749.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320749
loop_
_publ_author_name
'Weijiang He'
'Fang Liu'
'Chunying Duan'
'Zijian Guo'
'Shaozhen Zhou'
'Yongjiang Liu'
'Longgen Zhu'
_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       '2θ/ω 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/[σ²(Fo²)+(0.1116P)²+3.6485P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.10053(4) -0.37757(9) -0.50604(5) 0.0410(3) Uani 1 1 d . . .
Pd2 Pd 0.39810(4) -0.51712(9) -0.57576(5) 0.0448(3) Uani 1 1 d . . .
Cl1 Cl 0.08389(14) -0.4993(3) -0.38509(17) 0.0577(8) Uani 1 1 d . . .
Cl2 Cl 0.42523(14) -0.6460(4) -0.45592(18) 0.0635(8) Uani 1 1 d . . .
C1 C 0.1377(7) -0.0787(12) -0.5145(7) 0.068(4) Uani 1 1 d . . .
H1B H 0.1811 -0.0857 -0.5246 0.081 Uiso 1 1 calc R . .
H1A H 0.1293 0.0192 -0.4969 0.081 Uiso 1 1 calc R . .
C2 C 0.0977(7) -0.1153(13) -0.5942(7) 0.070(4) Uani 1 1 d . . .
H2B H 0.0543 -0.1017 -0.5857 0.084 Uiso 1 1 calc R . .
H2A H 0.1088 -0.0542 -0.6394 0.084 Uiso 1 1 calc R . .
C3 C 0.0682(6) -0.3370(12) -0.6758(7) 0.056(3) Uani 1 1 d . . .
H3B H 0.0763 -0.3006 -0.7301 0.067 Uiso 1 1 calc R . .
H3A H 0.0258 -0.3156 -0.6650 0.067 Uiso 1 1 calc R . .
C4 C 0.0805(6) -0.4995(12) -0.6702(7) 0.053(3) Uani 1 1 d . . .
H4B H 0.0527 -0.5517 -0.7086 0.064 Uiso 1 1 calc R . .
H4A H 0.1225 -0.5209 -0.6829 0.064 Uiso 1 1 calc R . .
C5 C 0.0862(5) -0.6944(11) -0.5652(7) 0.048(3) Uani 1 1 d . . .
H5B H 0.0612 -0.7562 -0.6021 0.058 Uiso 1 1 calc R . .
H5A H 0.0765 -0.7174 -0.5092 0.058 Uiso 1 1 calc R . .
C6 C 0.1523(5) -0.7269(11) -0.5748(7) 0.047(3) Uani 1 1 d . . .
C7 C 0.1692(6) -0.7911(12) -0.6476(7) 0.056(3) Uani 1 1 d . . .
H7 H 0.1391 -0.8112 -0.6891 0.067 Uiso 1 1 calc R . .
C8 C 0.2299(6) -0.8257(12) -0.6592(7) 0.056(3) Uani 1 1 d . . .
H8 H 0.2400 -0.8711 -0.7077 0.067 Uiso 1 1 calc R . .
C9 C 0.2768(6) -0.7924(11) -0.5980(7) 0.055(3) Uani 1 1 d . . .
C10 C 0.2592(5) -0.7314(12) -0.5250(7) 0.054(3) Uani 1 1 d . . .
H10 H 0.2891 -0.7120 -0.4830 0.065 Uiso 1 1 calc R . .
C11 C 0.1980(6) -0.6987(11) -0.5134(7) 0.051(3) Uani 1 1 d . . .
H11 H 0.1875 -0.6574 -0.4640 0.061 Uiso 1 1 calc R . .
C12 C 0.3424(6) -0.8246(12) -0.6129(8) 0.060(3) Uani 1 1 d . . .
H12B H 0.3437 -0.9041 -0.6517 0.072 Uiso 1 1 calc R . .
H12A H 0.3634 -0.8558 -0.5615 0.072 Uiso 1 1 calc R . .
C13 C 0.3472(6) -0.6441(13) -0.7257(7) 0.065(3) Uani 1 1 d . . .
H13B H 0.3041 -0.6230 -0.7194 0.078 Uiso 1 1 calc R . .
H13A H 0.3499 -0.7175 -0.7679 0.078 Uiso 1 1 calc R . .
C14 C 0.3811(7) -0.5063(12) -0.7504(7) 0.068(4) Uani 1 1 d . . .
H14B H 0.4239 -0.5267 -0.7595 0.082 Uiso 1 1 calc R . .
H14A H 0.3616 -0.4642 -0.8001 0.082 Uiso 1 1 calc R . .
C15 C 0.4136(5) -0.2740(13) -0.6812(7) 0.059(3) Uani 1 1 d . . .
H15B H 0.3963 -0.2085 -0.7231 0.071 Uiso 1 1 calc R . .
H15A H 0.4556 -0.2970 -0.6934 0.071 Uiso 1 1 calc R . .
C16 C 0.4121(6) -0.2056(13) -0.5958(7) 0.060(3) Uani 1 1 d . . .
H16B H 0.4410 -0.1259 -0.5907 0.072 Uiso 1 1 calc R . .
H16A H 0.3712 -0.1684 -0.5877 0.072 Uiso 1 1 calc R . .
C17 C 0.4181(5) -0.2660(13) -0.4488(7) 0.059(3) Uani 1 1 d . . .
H17B H 0.4410 -0.1769 -0.4389 0.071 Uiso 1 1 calc R . .
H17A H 0.4347 -0.3372 -0.4096 0.071 Uiso 1 1 calc R . .
C18 C 0.3524(5) -0.2393(13) -0.4328(6) 0.050(3) Uani 1 1 d . . .
C19 C 0.3328(5) -0.1067(14) -0.4100(7) 0.058(3) Uani 1 1 d . . .
H19 H 0.3608 -0.0305 -0.4067 0.069 Uiso 1 1 calc R . .
C20 C 0.2723(5) -0.0812(12) -0.3914(6) 0.051(3) Uani 1 1 d . . .
H20 H 0.2601 0.0109 -0.3763 0.062 Uiso 1 1 calc R . .
C21 C 0.2305(5) -0.1941(12) -0.3954(6) 0.048(3) Uani 1 1 d . . .
C22 C 0.2500(5) -0.3316(13) -0.4178(7) 0.053(3) Uani 1 1 d . . .
H22 H 0.2226 -0.4088 -0.4197 0.064 Uiso 1 1 calc R . .
C23 C 0.3102(5) -0.3526(12) -0.4369(7) 0.054(3) Uani 1 1 d . . .
H23 H 0.3229 -0.4440 -0.4529 0.064 Uiso 1 1 calc R . .
C24 C 0.1646(5) -0.1723(13) -0.3762(7) 0.053(3) Uani 1 1 d . . .
H24B H 0.1537 -0.2439 -0.3360 0.063 Uiso 1 1 calc R . .
H24A H 0.1603 -0.0774 -0.3517 0.063 Uiso 1 1 calc R . .
N1 N 0.1220(4) -0.1840(10) -0.4495(6) 0.057(2) Uani 1 1 d . . .
H1N H 0.0854 -0.1516 -0.4323 0.068 Uiso 1 1 calc R . .
N2 N 0.1111(4) -0.2714(10) -0.6119(5) 0.053(2) Uani 1 1 d . . .
H2N H 0.1506 -0.2808 -0.6267 0.064 Uiso 1 1 calc R . .
N3 N 0.0697(4) -0.5413(9) -0.5826(5) 0.046(2) Uani 1 1 d . . .
H3N H 0.0280 -0.5389 -0.5803 0.055 Uiso 1 1 calc R . .
N4 N 0.3768(4) -0.6969(9) -0.6462(5) 0.050(2) Uani 1 1 d . . .
H4N H 0.4138 -0.7333 -0.6593 0.060 Uiso 1 1 calc R . .
N5 N 0.3759(5) -0.4079(10) -0.6786(5) 0.053(2) Uani 1 1 d . . .
H5N H 0.3357 -0.3810 -0.6774 0.064 Uiso 1 1 calc R . .
N6 N 0.4287(4) -0.3174(10) -0.5333(5) 0.049(2) Uani 1 1 d . . .
H6N H 0.4705 -0.3237 -0.5338 0.059 Uiso 1 1 calc R . .
N7 N 0.5000 0.8658(18) -0.2500 0.077(4) Uani 1 2 d SU . .
O71 O 0.5000 0.7347(16) -0.2500 0.095(4) Uani 1 2 d SU . .
O72 O 0.4675(5) 0.9256(13) -0.2040(8) 0.123(4) Uani 1 1 d U . .
N8 N 0.2350(6) 0.2450(16) -0.2360(9) 0.097(4) Uani 1 1 d U . .
O81 O 0.1875(5) 0.1766(13) -0.2556(7) 0.108(4) Uani 1 1 d U . .
O82 O 0.2409(5) 0.3104(13) -0.1715(6) 0.096(3) Uani 1 1 d U . .
O83 O 0.2763(6) 0.2498(18) -0.2833(9) 0.149(5) Uani 1 1 d U . .
N9 N 0.0000 -0.107(3) -0.2500 0.111(5) Uani 1 2 d SU . .
O91 O 0.0000 0.020(2) -0.2500 0.129(6) Uani 1 2 d SU . .
O92 O -0.0287(7) -0.1705(17) -0.2001(10) 0.149(5) Uani 1 1 d U . .
O1W O 0.0712(7) 0.1181(15) -0.3812(9) 0.157(6) Uani 1 1 d . . .
H1WB H 0.0499 0.1953 -0.3839 0.188 Uiso 1 1 d R . .
H1WA H 0.0487 0.0546 -0.3602 0.188 Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N3 83.7(3) . . ?
N2 Pd1 N1 85.6(4) . . ?
N3 Pd1 N1 167.0(4) . . ?
N2 Pd1 Cl1 177.6(3) . . ?
N3 Pd1 Cl1 95.4(2) . . ?
N1 Pd1 Cl1 94.9(3) . . ?
N5 Pd2 N4 84.7(3) . . ?
N5 Pd2 N6 83.3(4) . . ?
N4 Pd2 N6 164.9(3) . . ?
N5 Pd2 Cl2 179.3(3) . . ?
N4 Pd2 Cl2 95.1(3) . . ?
N6 Pd2 Cl2 96.8(3) . . ?
N1 C1 C2 107.9(10) . . ?
N2 C2 C1 105.4(10) . . ?
N2 C3 C4 105.1(9) . . ?
N3 C4 C3 105.8(9) . . ?
N3 C5 C6 113.4(8) . . ?
C11 C6 C7 118.4(10) . . ?
C11 C6 C5 122.7(10) . . ?
C7 C6 C5 119.0(10) . . ?
C8 C7 C6 121.3(11) . . ?
C7 C8 C9 120.4(11) . . ?
C10 C9 C8 117.7(11) . . ?
C10 C9 C12 122.4(12) . . ?
C8 C9 C12 119.8(10) . . ?
C9 C10 C11 121.4(11) . . ?
C6 C11 C10 120.7(10) . . ?
C9 C12 N4 113.6(9) . . ?
N4 C13 C14 108.1(10) . . ?
N5 C14 C13 103.8(9) . . ?
N5 C15 C16 106.0(8) . . ?
N6 C16 C15 108.5(9) . . ?
N6 C17 C18 114.9(9) . . ?
C19 C18 C23 118.4(10) . . ?
C19 C18 C17 121.2(11) . . ?
C23 C18 C17 120.3(10) . . ?
C18 C19 C20 122.1(11) . . ?
C21 C20 C19 119.4(11) . . ?
C20 C21 C22 119.3(10) . . ?
C20 C21 C24 121.5(10) . . ?
C22 C21 C24 119.2(10) . . ?
C23 C22 C21 119.7(11) . . ?
C22 C23 C18 121.0(10) . . ?
N1 C24 C21 112.5(9) . . ?
C24 N1 C1 111.5(9) . . ?
C24 N1 Pd1 122.9(7) . . ?
C1 N1 Pd1 107.9(7) . . ?
C3 N2 C2 114.0(9) . . ?
C3 N2 Pd1 107.5(7) . . ?
C2 N2 Pd1 105.7(7) . . ?
C5 N3 C4 112.0(8) . . ?
C5 N3 Pd1 121.6(7) . . ?
C4 N3 Pd1 108.7(6) . . ?
C13 N4 C12 111.7(9) . . ?
C13 N4 Pd2 106.8(7) . . ?
C12 N4 Pd2 122.0(7) . . ?
C15 N5 C14 114.6(8) . . ?
C15 N5 Pd2 110.0(7) . . ?
C14 N5 Pd2 108.9(7) . . ?
C16 N6 C17 111.5(9) . . ?
C16 N6 Pd2 109.6(7) . . ?
C17 N6 Pd2 122.0(7) . . ?
O72 N7 O72 125(2) 2_654 . ?
O72 N7 O71 117.5(10) 2_654 . ?
O72 N7 O71 117.5(10) . . ?
O82 N8 O83 119.0(14) . . ?
O82 N8 O81 121.4(13) . . ?
O83 N8 O81 119.5(14) . . ?
O91 N9 O92 119.1(14) . 2_554 ?
O91 N9 O92 119.1(13) . . ?
O92 N9 O92 122(3) 2_554 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N2 2.007(8) . ?
Pd1 N3 2.046(9) . ?
Pd1 N1 2.052(10) . ?
Pd1 Cl1 2.313(3) . ?
Pd2 N5 1.986(8) . ?
Pd2 N4 2.054(9) . ?
Pd2 N6 2.066(9) . ?
Pd2 Cl2 2.328(3) . ?
C1 N1 1.493(14) . ?
C1 C2 1.552(16) . ?
C2 N2 1.503(15) . ?
C3 N2 1.481(14) . ?
C3 C4 1.527(15) . ?
C4 N3 1.508(13) . ?
C5 N3 1.483(13) . ?
C5 C6 1.484(15) . ?
C6 C11 1.388(15) . ?
C6 C7 1.394(15) . ?
C7 C8 1.383(16) . ?
C8 C9 1.414(17) . ?
C9 C10 1.390(15) . ?
C9 C12 1.491(16) . ?
C10 C11 1.391(15) . ?
C12 N4 1.516(14) . ?
C13 N4 1.489(14) . ?
C13 C14 1.538(16) . ?
C14 N5 1.490(14) . ?
C15 N5 1.486(14) . ?
C15 C16 1.528(16) . ?
C16 N6 1.478(14) . ?
C17 N6 1.486(14) . ?
C17 C18 1.489(16) . ?
C18 C19 1.357(16) . ?
C18 C23 1.391(15) . ?
C19 C20 1.387(15) . ?
C20 C21 1.383(15) . ?
C21 C22 1.396(15) . ?
C21 C24 1.498(15) . ?
C22 C23 1.378(15) . ?
C24 N1 1.468(14) . ?
N7 O72 1.197(11) 2_654 ?
N7 O72 1.197(11) . ?
N7 O71 1.21(2) . ?
N8 O82 1.210(14) . ?
N8 O83 1.220(15) . ?
N8 O81 1.236(14) . ?
N9 O91 1.18(3) . ?
N9 O92 1.206(16) 2_554 ?
N9 O92 1.206(16) . ?
