#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:25:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179376 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/73/4327396.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_4327396
loop_
_publ_author_name
'Nancy L. S. Yue'
'Dana J. Eisler'
'Michael C. Jennings'
'Richard J. Puddephatt'
_publ_section_title
;
 Macrocyclic and Lantern Complexes of Palladium(II) with
 Bis(amidopyridine) Ligands: Synthesis, Structure, and Host-Guest
 Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7671
_journal_page_last               7681
_journal_paper_doi               10.1021/ic048893+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C92 H92 Cl16 N16 O16 Pd2'
_chemical_formula_weight         2457.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.8814(2)
_cell_length_b                   19.8814(2)
_cell_length_c                   15.8966(2)
_cell_measurement_temperature    200(2)
_cell_volume                     6283.45(12)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'phi/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  0.074
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81158
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.8584
_exptl_absorpt_correction_T_min  0.7808
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         7219
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1742P)²+7.3235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2414
_refine_ls_wR_factor_ref         0.2668
_reflns_number_gt                5355
_reflns_number_total             7219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488932Bsi20040811_112932_6.cif
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4327396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
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 0.2500 0.2500 1.14079(4) 0.0412(2) Uani 1 4 d S . .
Pd2 Pd 0.2500 0.2500 0.54622(3) 0.0338(2) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.35276(13) 0.0469(5) Uani 1 4 d S . .
O2 O 0.2500 0.2500 0.7402(5) 0.067(2) Uani 1 4 d S . .
O3 O 0.2500 0.2500 0.9518(4) 0.0591(19) Uani 1 4 d S . .
Cl4 Cl 0.1075(5) 0.2963(4) 0.8392(8) 0.058(2) Uani 0.25 1 d P A 1
Cl5 Cl 0.1424(5) 0.1550(5) 0.8438(6) 0.069(2) Uani 0.25 1 d P B 2
O5 O 0.1729(8) 0.1246(6) 0.8386(6) 0.057(3) Uani 0.50 1 d P C 3
C1 C 0.0801(2) -0.0099(2) 0.8413(3) 0.0436(10) Uani 1 1 d . . .
H1A H 0.0782 0.0378 0.8426 0.052 Uiso 1 1 calc R . .
C2 C 0.0840(2) -0.0463(2) 0.9152(3) 0.0472(10) Uani 1 1 d . . .
C3 C 0.0866(3) -0.1165(2) 0.9124(3) 0.0558(12) Uani 1 1 d . . .
H3A H 0.0880 -0.1411 0.9636 0.067 Uiso 1 1 calc R . .
C4 C 0.0871(3) -0.1506(3) 0.8370(3) 0.0607(14) Uani 1 1 d . D .
C5 C 0.0821(3) -0.1137(2) 0.7632(3) 0.0543(12) Uani 1 1 d . . .
H5A H 0.0810 -0.1364 0.7107 0.065 Uiso 1 1 calc R . .
C6 C 0.0788(2) -0.0440(2) 0.7653(3) 0.0466(10) Uani 1 1 d . . .
C7 C 0.0921(5) -0.2277(3) 0.8331(5) 0.088(2) Uani 1 1 d . . .
C8 C 0.1482(9) -0.2516(10) 0.9095(12) 0.102(5) Uiso 0.50 1 d P D 1
H8A H 0.1271 -0.2471 0.9649 0.154 Uiso 0.50 1 calc PR D 1
H8B H 0.1882 -0.2229 0.9067 0.154 Uiso 0.50 1 calc PR D 1
H8C H 0.1613 -0.2986 0.9005 0.154 Uiso 0.50 1 calc PR D 1
C9 C 0.0297(17) -0.2587(17) 0.870(2) 0.186(13) Uiso 0.50 1 d P D 1
H9A H 0.0160 -0.2331 0.9200 0.279 Uiso 0.50 1 calc PR D 1
H9B H 0.0391 -0.3053 0.8863 0.279 Uiso 0.50 1 calc PR D 1
H9C H -0.0065 -0.2578 0.8284 0.279 Uiso 0.50 1 calc PR D 1
C10 C 0.1287(11) -0.2532(10) 0.7552(12) 0.101(6) Uiso 0.50 1 d P D 1
H10A H 0.0963 -0.2739 0.7167 0.152 Uiso 0.50 1 calc PR D 1
H10B H 0.1625 -0.2866 0.7718 0.152 Uiso 0.50 1 calc PR D 1
H10C H 0.1510 -0.2154 0.7269 0.152 Uiso 0.50 1 calc PR D 1
C8 C 0.1067(9) -0.2620(8) 0.9111(11) 0.091(4) Uiso 0.50 1 d P D 2
H8D H 0.0724 -0.2504 0.9530 0.137 Uiso 0.50 1 calc PR D 2
H8E H 0.1510 -0.2481 0.9317 0.137 Uiso 0.50 1 calc PR D 2
H8F H 0.1064 -0.3107 0.9017 0.137 Uiso 0.50 1 calc PR D 2
C9 C 0.0255(7) -0.2582(7) 0.8002(9) 0.075(3) Uiso 0.50 1 d P D 2
H9D H -0.0109 -0.2481 0.8399 0.112 Uiso 0.50 1 calc PR D 2
H9E H 0.0304 -0.3071 0.7947 0.112 Uiso 0.50 1 calc PR D 2
H9F H 0.0147 -0.2388 0.7452 0.112 Uiso 0.50 1 calc PR D 2
C10 C 0.1544(9) -0.2444(9) 0.7677(12) 0.088(5) Uiso 0.50 1 d P D 2
H10D H 0.1943 -0.2187 0.7843 0.132 Uiso 0.50 1 calc PR D 2
H10E H 0.1413 -0.2318 0.7104 0.132 Uiso 0.50 1 calc PR D 2
H10F H 0.1647 -0.2926 0.7696 0.132 Uiso 0.50 1 calc PR D 2
N11 N 0.1791(2) 0.1772(2) 1.1428(2) 0.0441(8) Uani 1 1 d . . .
C12 C 0.1662(2) 0.1388(2) 1.0758(3) 0.0444(9) Uani 1 1 d . . .
H12A H 0.1898 0.1475 1.0250 0.053 Uiso 1 1 calc R . .
C13 C 0.1195(2) 0.0865(3) 1.0775(3) 0.0482(10) Uani 1 1 d . . .
C14 C 0.0854(3) 0.0741(3) 1.1509(3) 0.0621(15) Uani 1 1 d . . .
H14A H 0.0530 0.0391 1.1540 0.075 Uiso 1 1 calc R . .
C15 C 0.0993(3) 0.1137(3) 1.2202(3) 0.0666(15) Uani 1 1 d . . .
H15A H 0.0765 0.1057 1.2718 0.080 Uiso 1 1 calc R . .
C16 C 0.1458(3) 0.1643(3) 1.2149(3) 0.0601(13) Uani 1 1 d . . .
H16A H 0.1548 0.1910 1.2632 0.072 Uiso 1 1 calc R . .
N17 N 0.1111(2) 0.0488(2) 1.0037(3) 0.0545(10) Uani 1 1 d . . .
H17A H 0.1242 0.0673 0.9561 0.065 Uiso 1 1 calc R . .
C18 C 0.0843(3) -0.0142(3) 0.9999(3) 0.0515(11) Uani 1 1 d . . .
O19 O 0.0635(2) -0.0430(2) 1.0610(2) 0.0729(12) Uani 1 1 d . . .
N21 N 0.17008(18) 0.18592(18) 0.5463(2) 0.0382(8) Uani 1 1 d . . .
C22 C 0.1608(2) 0.1426(2) 0.6102(3) 0.0395(9) Uani 1 1 d . . .
H22A H 0.1914 0.1435 0.6561 0.047 Uiso 1 1 calc R . .
C23 C 0.1084(2) 0.0967(2) 0.6118(3) 0.0440(9) Uani 1 1 d . . .
C24 C 0.0631(2) 0.0962(3) 0.5446(3) 0.0539(12) Uani 1 1 d . . .
H24A H 0.0263 0.0658 0.5438 0.065 Uiso 1 1 calc R . .
C25 C 0.0734(3) 0.1413(3) 0.4788(3) 0.0574(12) Uani 1 1 d . . .
H25A H 0.0435 0.1417 0.4321 0.069 Uiso 1 1 calc R . .
C26 C 0.1267(2) 0.1852(3) 0.4815(3) 0.0499(11) Uani 1 1 d . . .
H26A H 0.1330 0.2158 0.4363 0.060 Uiso 1 1 calc R . .
N27 N 0.1031(2) 0.0548(2) 0.6813(3) 0.0482(9) Uani 1 1 d . . .
H27A H 0.1195 0.0699 0.7291 0.058 Uiso 1 1 calc R . .
C28 C 0.0748(2) -0.0078(2) 0.6825(3) 0.0495(11) Uani 1 1 d . . .
O29 O 0.0491(2) -0.03317(19) 0.6206(3) 0.0685(11) Uani 1 1 d . . .
C30 C 0.0263(7) -0.1935(7) 1.2259(8) 0.137(9) Uani 0.50 1 d PD E 1
H30A H -0.0157 -0.1875 1.1920 0.164 Uiso 0.50 1 calc PR E 1
Cl31 Cl 0.0063(4) -0.2303(3) 1.3190(4) 0.1312(19) Uani 0.50 1 d PD E 1
Cl32 Cl 0.0570(3) -0.1141(3) 1.2548(4) 0.1185(16) Uani 0.50 1 d PD E 1
Cl33 Cl 0.0838(6) -0.2414(6) 1.1677(7) 0.166(5) Uani 0.50 1 d PD E 1
C40 C 0.1412(6) -0.0546(6) 0.4596(10) 0.092(9) Uani 0.30 1 d PD F 2
H40A H 0.1096 -0.0394 0.5047 0.111 Uiso 0.30 1 calc PR F 2
Cl41 Cl 0.1006(4) -0.0535(8) 0.3619(6) 0.163(5) Uani 0.30 1 d PD F 2
Cl42 Cl 0.1563(6) -0.1408(4) 0.4693(6) 0.137(3) Uani 0.30 1 d PD F 2
Cl43 Cl 0.2158(5) -0.0136(6) 0.4688(7) 0.122(4) Uani 0.30 1 d PD F 2
C50 C 0.0160(10) -0.188(2) 1.1450(10) 0.110(17) Uani 0.20 1 d PD G 3
H50A H 0.0317 -0.1407 1.1343 0.132 Uiso 0.20 1 calc PR G 3
Cl51 Cl -0.0215(10) -0.1873(14) 1.2434(10) 0.195(10) Uani 0.20 1 d PD G 3
Cl52 Cl 0.0871(8) -0.2375(10) 1.1452(10) 0.080(4) Uani 0.20 1 d PD G 3
Cl53 Cl -0.0365(7) -0.2086(7) 1.0620(7) 0.115(4) Uani 0.20 1 d PD G 3
Cl61 Cl 0.0317(5) -0.1395(6) 1.1823(12) 0.145(5) Uani 0.25 1 d P H 4
O62 O 0.2207(6) -0.0432(8) 0.5721(12) 0.151(7) Uani 0.50 1 d P I 4
O63 O 0.1845(8) -0.0024(11) 0.4217(12) 0.158(7) Uani 0.50 1 d P J 4
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
N11 Pd1 N11 178.2(2) 2 .
N11 Pd1 N11 89.986(4) 2 4
N11 Pd1 N11 89.986(4) . 4
N11 Pd1 N11 89.986(4) 2 3
N11 Pd1 N11 89.986(4) . 3
N11 Pd1 N11 178.2(2) 4 3
N21 Pd2 N21 90.000(1) 4 2
N21 Pd2 N21 90.000(1) 4 .
N21 Pd2 N21 179.9(2) 2 .
N21 Pd2 N21 179.95(18) 4 3
N21 Pd2 N21 90.000(1) 2 3
N21 Pd2 N21 90.0 . 3
C2 C1 C6 119.1(4) . .
C1 C2 C3 119.9(4) . .
C1 C2 C18 123.0(4) . .
C3 C2 C18 117.1(4) . .
C4 C3 C2 121.3(5) . .
C3 C4 C5 118.4(5) . .
C3 C4 C7 121.8(5) . .
C5 C4 C7 119.8(5) . .
C6 C5 C4 120.8(5) . .
C1 C6 C5 120.5(5) . .
C1 C6 C28 122.0(4) . .
C5 C6 C28 117.5(4) . .
C8 C7 C9 68.6(15) . .
C8 C7 C10 116.5(12) . .
C9 C7 C10 125.2(17) . .
C8 C7 C4 116.6(9) . .
C9 C7 C4 109.8(15) . .
C10 C7 C4 113.3(9) . .
C8 C7 C9 106.0(10) . .
C9 C7 C9 42.8(13) . .
C10 C7 C9 90.3(11) . .
C4 C7 C9 110.4(8) . .
C8 C7 C10 107.2(11) . .
C9 C7 C10 141.5(16) . .
C10 C7 C10 20.4(10) . .
C4 C7 C10 106.0(8) . .
C9 C7 C10 110.6(10) . .
C8 C7 C8 29.7(8) . .
C9 C7 C8 98.3(15) . .
C10 C7 C8 100.0(11) . .
C4 C7 C8 106.8(8) . .
C9 C7 C8 133.3(9) . .
C10 C7 C8 84.4(11) . .
C12 N11 C16 118.4(4) . .
C12 N11 Pd1 122.0(3) . .
C16 N11 Pd1 119.5(3) . .
N11 C12 C13 122.5(4) . .
C14 C13 C12 118.7(5) . .
C14 C13 N17 123.8(5) . .
C12 C13 N17 117.5(4) . .
C13 C14 C15 118.5(5) . .
C16 C15 C14 120.3(5) . .
N11 C16 C15 121.5(5) . .
C18 N17 C13 125.1(4) . .
O19 C18 N17 122.6(5) . .
O19 C18 C2 121.7(5) . .
N17 C18 C2 115.8(4) . .
C26 N21 C22 118.9(4) . .
C26 N21 Pd2 120.5(3) . .
C22 N21 Pd2 120.5(3) . .
N21 C22 C23 122.6(4) . .
C22 C23 N27 117.9(4) . .
C22 C23 C24 118.4(4) . .
N27 C23 C24 123.7(4) . .
C25 C24 C23 118.4(4) . .
C26 C25 C24 119.9(5) . .
N21 C26 C25 121.8(4) . .
C28 N27 C23 126.2(4) . .
O29 C28 N27 122.6(5) . .
O29 C28 C6 122.1(4) . .
N27 C28 C6 115.3(4) . .
Cl31 C30 Cl33 112.3(9) . .
Cl31 C30 Cl32 104.0(7) . .
Cl33 C30 Cl32 113.6(8) . .
Cl43 C40 Cl42 108.2(9) . .
Cl43 C40 Cl41 118.2(10) . .
Cl42 C40 Cl41 99.7(9) . .
Cl52 C50 Cl51 110.7(16) . .
Cl52 C50 Cl53 110.9(14) . .
Cl51 C50 Cl53 115.4(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N11 2.021(4) 2
Pd1 N11 2.021(4) .
Pd1 N11 2.021(4) 4
Pd1 N11 2.021(4) 3
Pd2 N21 2.037(3) 4
Pd2 N21 2.037(3) 2
Pd2 N21 2.037(3) .
Pd2 N21 2.037(3) 3
C1 C2 1.381(6) .
C1 C6 1.387(6) .
C2 C3 1.397(7) .
C2 C18 1.491(7) .
C3 C4 1.377(7) .
C4 C5 1.387(7) .
C4 C7 1.538(8) .
C5 C6 1.387(6) .
C6 C28 1.502(7) .
C7 C8 1.446(17) .
C7 C9 1.51(3) .
C7 C10 1.52(2) .
C7 C9 1.549(16) .
C7 C10 1.65(2) .
C7 C8 1.72(2) .
N11 C12 1.334(6) .
N11 C16 1.349(6) .
C12 C13 1.395(7) .
C13 C14 1.371(7) .
C13 N17 1.403(6) .
C14 C15 1.382(7) .
C15 C16 1.369(7) .
N17 C18 1.363(6) .
C18 O19 1.200(6) .
N21 C26 1.344(6) .
N21 C22 1.345(5) .
C22 C23 1.385(6) .
C23 N27 1.388(6) .
C23 C24 1.398(6) .
C24 C25 1.392(7) .
C25 C26 1.374(7) .
N27 C28 1.365(6) .
C28 O29 1.219(6) .
C30 Cl31 1.699(12) .
C30 Cl33 1.752(12) .
C30 Cl32 1.754(12) .
C40 Cl43 1.698(12) .
C40 Cl42 1.748(12) .
C40 Cl41 1.752(13) .
C50 Cl52 1.726(15) .
C50 Cl51 1.732(15) .
C50 Cl53 1.733(16) .
