Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'

#------------------ SUBMISSION DETAILS --------------------------------------#

# Name and address of author for correspondence

# Name and address of author for correspondence

_journal_coden_Cambridge         0222

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2006-11-16
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

_publ_contact_author_name        'Bernhard Lippert'
_publ_contact_author_address     
;
Anorganische Chemie
Universitat Dortmund
Otto-Hahn-Str. 6
44227 Dortmund
Germany
;
_publ_contact_author_email       bernhard.lippert@uni-dortmund.de
_publ_contact_author_fax         '+49 231 755 3797'
_publ_contact_author_phone       '+49 231 755 3840'

_publ_requested_category         metalorganic

_publ_section_title              
;
Pd2Ag triangle supported by two ?3-amidopyridine
ligands
;

loop_
_publ_author_name
_publ_author_address
'Weizheng Shen.'
;
Anorganische Chemie
Universitat Dortmund
Otto-Hahn-Str. 6
44227 Dortmund
Germany
;
B.Costisella
;
Anorganische Chemie
Universitaet Dortmund
Otto-Hahn-Str. 6
44227 Dortmund
Germany
;
B.Lippert
;
Anorganische Chemie
Universitat Dortmund
Otto-Hahn-Str. 6
44227 Dortmund
Germany
;

_publ_section_references         
;

Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565.

Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838.

Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure
refinement. University of Gottingen, Germany.

Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution.
University of Gottingen, Germany.

;
_publ_section_acknowledgements   
;
?
;

#END

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2006-11-16 at 13:12:07
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.2
# Request file : c:\wingx\wingx\files\cifdoc.dat
# CIF files read : 2739

data_2739
_database_code_depnum_ccdc_archive 'CCDC 622555'

_audit_creation_date             2006-11-16T13:12:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C22 H42 Ag2 N12 O12 Pd2'
_chemical_formula_sum            'C22 H42 Ag2 N12 O12 Pd2'
_chemical_formula_weight         1095.22

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.948(3)
_cell_length_b                   11.140(2)
_cell_length_c                   18.296(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.73(3)
_cell_angle_gamma                90
_cell_volume                     3414.2(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5490
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       cubes
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_exptl_absorpt_coefficient_mu    2.243
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8068
_exptl_absorpt_correction_T_max  0.8068

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       Profile-fitled
_diffrn_standards_number         N/A
_diffrn_reflns_number            5490
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.2
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_reflns_number_total             2998
_reflns_number_gt                1660
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    nonref
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2998
_refine_ls_number_parameters     226
_refine_ls_number_restraints     24
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.2267
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0
_refine_diff_density_max         3.226
_refine_diff_density_min         -1.207

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

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 0 '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 0.006 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Pd1 Pd 0.05714(4) 0.26619(7) 0.19077(4) 0.0238(2) Uani 1 d . . .
Ag1 Ag 0 0.50545(10) 0.25 0.0358(3) Uani 1 d S . .
Ag2 Ag -0.01962(11) 0.83757(15) 0.26210(10) 0.0439(7) Uani 0.5 d P . .
N1A N 0.0927(4) 0.4611(9) 0.3411(4) 0.030(2) Uani 1 d . . .
N2A N 0.0625(4) 0.2539(7) 0.3045(4) 0.020(2) Uani 1 d . . .
H1 H 0.0793 0.1769 0.319 0.024 Uiso 1 calc R . .
N1B N 0.0474(5) 0.2498(8) 0.0757(4) 0.036(2) Uani 1 d . . .
N4B N 0.1789(5) 0.2815(8) 0.1877(4) 0.031(2) Uani 1 d . . .
N1N N -0.1063(7) 0.6982(10) 0.3562(6) 0.066(3) Uani 1 d U . .
N2N N 0.1169(5) 0.9396(8) 0.3716(4) 0.034(2) Uani 1 d . . .
C2A C 0.1109(6) 0.3368(9) 0.3498(5) 0.027(3) Uani 1 d . . .
C3A C 0.1769(6) 0.2985(10) 0.4010(5) 0.034(3) Uani 1 d . . .
H4 H 0.1899 0.2157 0.4066 0.041 Uiso 1 calc R . .
C4A C 0.2215(6) 0.3827(11) 0.4421(5) 0.040(3) Uani 1 d . . .
H10 H 0.268 0.3607 0.4752 0.048 Uiso 1 calc R . .
C5A C 0.1972(6) 0.5028(8) 0.4345(5) 0.023(3) Uani 1 d . . .
H3 H 0.2247 0.5616 0.4663 0.027 Uiso 1 calc R . .
C6A C 0.1366(6) 0.5362(9) 0.3838(5) 0.031(3) Uani 1 d . . .
H2 H 0.1247 0.6194 0.3786 0.038 Uiso 1 calc R . .
C2B C 0.1289(7) 0.2135(11) 0.0634(5) 0.046(4) Uani 1 d . . .
H5 H 0.1335 0.2214 0.0103 0.055 Uiso 1 calc R . .
H6 H 0.1385 0.1285 0.0778 0.055 Uiso 1 calc R . .
C3B C 0.1900(6) 0.2921(11) 0.1087(5) 0.039(3) Uani 1 d . . .
H14 H 0.2445 0.2661 0.1026 0.047 Uiso 1 calc R . .
H15 H 0.1829 0.3766 0.0923 0.047 Uiso 1 calc R . .
C5B C 0.2198(7) 0.1730(11) 0.2201(5) 0.045(4) Uani 1 d . . .
H19 H 0.2772 0.1802 0.2191 0.068 Uiso 1 calc R . .
H20 H 0.199 0.1025 0.1915 0.068 Uiso 1 calc R . .
H21 H 0.2103 0.1642 0.2714 0.068 Uiso 1 calc R . .
C6B C 0.2170(6) 0.3863(12) 0.2266(5) 0.043(3) Uani 1 d . . .
H16 H 0.274 0.3866 0.2227 0.065 Uiso 1 calc R . .
H17 H 0.2102 0.3828 0.2788 0.065 Uiso 1 calc R . .
H18 H 0.1922 0.4597 0.2042 0.065 Uiso 1 calc R . .
C7B C 0.0218(7) 0.3610(10) 0.0349(5) 0.038(3) Uani 1 d . . .
H11 H 0.0185 0.3465 -0.0183 0.057 Uiso 1 calc R . .
H12 H 0.0607 0.4248 0.0499 0.057 Uiso 1 calc R . .
H13 H -0.0306 0.3853 0.046 0.057 Uiso 1 calc R . .
C8B C -0.0064(7) 0.1523(11) 0.0464(6) 0.049(4) Uani 1 d . . .
H7 H -0.0092 0.1483 -0.0074 0.074 Uiso 1 calc R . .
H8 H -0.0598 0.1674 0.0587 0.074 Uiso 1 calc R . .
H9 H 0.0139 0.0759 0.0683 0.074 Uiso 1 calc R . .
O11 O -0.1368(10) 0.6339(15) 0.3902(8) 0.159(5) Uani 1 d U . .
O12 O -0.1137(7) 0.8135(11) 0.3634(6) 0.099(4) Uani 1 d U . .
O13 O -0.0762(6) 0.6803(10) 0.3006(6) 0.087(3) Uani 1 d U . .
O21 O 0.0810(4) 0.9943(6) 0.3139(4) 0.0387(19) Uiso 1 d . . .
O22 O 0.1603(5) 0.9888(6) 0.4186(4) 0.052(2) Uani 1 d . . .
O23 O 0.1021(5) 0.8286(6) 0.3735(4) 0.046(2) Uani 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0217(4) 0.0254(4) 0.0238(3) 0.0000(3) 0.0021(3) 0.0019(4)
Ag1 0.0368(7) 0.0218(6) 0.0441(6) 0 -0.0092(6) 0
Ag2 0.0479(16) 0.0378(9) 0.0416(12) -0.0037(8) -0.0078(10) 0.0046(8)
N1A 0.009(4) 0.068(6) 0.011(3) -0.002(4) -0.003(3) -0.004(4)
N2A 0.019(4) 0.014(4) 0.027(4) 0.000(3) 0.006(3) 0.004(4)
N1B 0.022(5) 0.054(6) 0.033(4) 0.000(4) 0.004(4) 0.006(5)
N4B 0.026(5) 0.044(5) 0.025(4) -0.006(4) 0.004(4) 0.004(4)
N1N 0.058(6) 0.071(6) 0.063(5) 0.027(5) -0.010(5) -0.024(5)
N2N 0.024(5) 0.046(6) 0.038(4) 0.002(4) 0.018(4) 0.010(4)
C2A 0.023(6) 0.035(6) 0.027(5) 0.006(4) 0.016(4) 0.013(5)
C3A 0.041(7) 0.033(6) 0.027(5) -0.002(5) -0.001(5) 0.004(5)
C4A 0.028(6) 0.059(8) 0.029(5) 0.002(6) -0.010(5) -0.005(6)
C5A 0.035(6) 0.011(5) 0.022(5) -0.001(4) 0.004(4) -0.002(5)
C6A 0.043(7) 0.020(5) 0.034(5) -0.007(5) 0.015(5) 0.000(5)
C2B 0.051(8) 0.062(8) 0.020(5) 0.000(5) -0.005(5) 0.005(7)
C3B 0.021(6) 0.058(8) 0.034(6) 0.004(5) -0.012(5) 0.008(6)
C5B 0.031(7) 0.071(9) 0.031(6) -0.005(6) -0.004(5) 0.012(6)
C6B 0.026(6) 0.073(9) 0.033(6) 0.001(6) 0.011(5) -0.011(6)
C7B 0.039(7) 0.045(7) 0.028(5) 0.005(5) 0.001(5) 0.005(6)
C8B 0.044(8) 0.052(8) 0.050(7) -0.018(6) 0.002(6) -0.006(6)
O11 0.156(8) 0.162(8) 0.149(7) 0.024(6) -0.004(6) -0.022(6)
O12 0.089(6) 0.112(6) 0.095(6) -0.016(5) 0.010(5) 0.015(5)
O13 0.069(6) 0.079(6) 0.112(6) -0.032(5) 0.012(5) 0.004(5)
O22 0.044(5) 0.030(4) 0.078(5) -0.024(4) -0.002(4) -0.011(4)
O23 0.060(6) 0.021(4) 0.058(5) 0.001(4) 0.006(4) -0.002(4)

#------------------ MOLECULAR GEOMETRY --------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N2A 2.048(7) 2 ?
Pd1 N2A 2.074(7) . ?
Pd1 N4B 2.080(8) . ?
Pd1 N1B 2.094(8) . ?
Pd1 Ag1 3.0878(13) . ?
Pd1 Pd1 3.1181(17) 2 ?
Ag1 N1A 2.168(7) 2 ?
Ag1 N1A 2.168(7) . ?
Ag1 O13 2.585(11) 2 ?
Ag1 O13 2.585(10) . ?
Ag1 Pd1 3.0878(13) 2 ?
Ag2 Ag2 0.853(4) 2 ?
Ag2 O13 2.165(11) . ?
Ag2 O21 2.372(7) 2 ?
Ag2 O21 2.523(7) . ?
N1A C6A 1.299(12) . ?
N1A C2A 1.421(13) . ?
N2A C2A 1.415(12) . ?
N2A Pd1 2.048(7) 2 ?
N2A H1 0.93 . ?
N1B C8B 1.467(14) . ?
N1B C7B 1.477(13) . ?
N1B C2B 1.489(15) . ?
N4B C6B 1.466(14) . ?
N4B C5B 1.472(14) . ?
N4B C3B 1.489(12) . ?
N1N O11 1.126(18) . ?
N1N O13 1.220(14) . ?
N1N O12 1.299(15) . ?
N2N O22 1.178(10) . ?
N2N O23 1.263(11) . ?
N2N O21 1.289(10) . ?
C2A C3A 1.413(13) . ?
C3A C4A 1.358(15) . ?
C3A H4 0.95 . ?
C4A C5A 1.399(15) . ?
C4A H10 0.95 . ?
C5A C6A 1.329(13) . ?
C5A H3 0.95 . ?
C6A H2 0.95 . ?
C2B C3B 1.506(15) . ?
C2B H5 0.99 . ?
C2B H6 0.99 . ?
C3B H14 0.99 . ?
C3B H15 0.99 . ?
C5B H19 0.98 . ?
C5B H20 0.98 . ?
C5B H21 0.98 . ?
C6B H16 0.98 . ?
C6B H17 0.98 . ?
C6B H18 0.98 . ?
C7B H11 0.98 . ?
C7B H12 0.98 . ?
C7B H13 0.98 . ?
C8B H7 0.98 . ?
C8B H8 0.98 . ?
C8B H9 0.98 . ?
O21 Ag2 2.372(7) 2 ?

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
N2A Pd1 N2A 81.2(3) 2 . ?
N2A Pd1 N4B 178.8(3) 2 . ?
N2A Pd1 N4B 98.0(3) . . ?
N2A Pd1 N1B 96.2(3) 2 . ?
N2A Pd1 N1B 171.0(3) . . ?
N4B Pd1 N1B 84.7(3) . . ?
N2A Pd1 Ag1 71.2(2) 2 . ?
N2A Pd1 Ag1 70.9(2) . . ?
N4B Pd1 Ag1 107.7(2) . . ?
N1B Pd1 Ag1 116.5(2) . . ?
N2A Pd1 Pd1 41.17(19) 2 2 ?
N2A Pd1 Pd1 40.5(2) . 2 ?
N4B Pd1 Pd1 137.9(2) . 2 ?
N1B Pd1 Pd1 137.4(2) . 2 ?
Ag1 Pd1 Pd1 59.674(19) . 2 ?
N1A Ag1 N1A 153.6(5) 2 . ?
N1A Ag1 O13 103.9(3) 2 2 ?
N1A Ag1 O13 96.0(3) . 2 ?
N1A Ag1 O13 96.0(3) 2 . ?
N1A Ag1 O13 103.9(3) . . ?
O13 Ag1 O13 82.2(5) 2 . ?
N1A Ag1 Pd1 76.3(2) 2 . ?
N1A Ag1 Pd1 81.0(2) . . ?
O13 Ag1 Pd1 108.9(3) 2 . ?
O13 Ag1 Pd1 167.6(2) . . ?
N1A Ag1 Pd1 81.0(2) 2 2 ?
N1A Ag1 Pd1 76.3(2) . 2 ?
O13 Ag1 Pd1 167.6(2) 2 2 ?
O13 Ag1 Pd1 108.9(3) . 2 ?
Pd1 Ag1 Pd1 60.65(4) . 2 ?
Ag2 Ag2 O13 126.0(3) 2 . ?
Ag2 Ag2 O21 90.2(2) 2 2 ?
O13 Ag2 O21 127.6(3) . 2 ?
Ag2 Ag2 O21 70.1(2) 2 . ?
O13 Ag2 O21 138.2(3) . . ?
O21 Ag2 O21 85.5(3) 2 . ?
C6A N1A C2A 117.8(8) . . ?
C6A N1A Ag1 126.7(8) . . ?
C2A N1A Ag1 115.3(6) . . ?
C2A N2A Pd1 114.9(6) . 2 ?
C2A N2A Pd1 118.5(6) . . ?
Pd1 N2A Pd1 98.3(3) 2 . ?
C2A N2A H1 108.1 . . ?
Pd1 N2A H1 108.1 2 . ?
Pd1 N2A H1 108.1 . . ?
C8B N1B C7B 108.5(8) . . ?
C8B N1B C2B 106.4(9) . . ?
C7B N1B C2B 111.0(8) . . ?
C8B N1B Pd1 112.4(7) . . ?
C7B N1B Pd1 114.1(6) . . ?
C2B N1B Pd1 104.0(5) . . ?
C6B N4B C5B 108.2(8) . . ?
C6B N4B C3B 107.3(8) . . ?
C5B N4B C3B 109.6(8) . . ?
C6B N4B Pd1 114.6(6) . . ?
C5B N4B Pd1 109.2(7) . . ?
C3B N4B Pd1 107.8(6) . . ?
O11 N1N O13 130.0(15) . . ?
O11 N1N O12 120.8(15) . . ?
O13 N1N O12 107.8(11) . . ?
O22 N2N O23 122.7(9) . . ?
O22 N2N O21 122.9(9) . . ?
O23 N2N O21 114.5(8) . . ?
C3A C2A N2A 121.4(9) . . ?
C3A C2A N1A 120.3(9) . . ?
N2A C2A N1A 118.3(8) . . ?
C4A C3A C2A 118.4(10) . . ?
C4A C3A H4 120.8 . . ?
C2A C3A H4 120.8 . . ?
C3A C4A C5A 118.4(9) . . ?
C3A C4A H10 120.8 . . ?
C5A C4A H10 120.8 . . ?
C6A C5A C4A 121.4(9) . . ?
C6A C5A H3 119.3 . . ?
C4A C5A H3 119.3 . . ?
N1A C6A C5A 123.4(10) . . ?
N1A C6A H2 118.3 . . ?
C5A C6A H2 118.3 . . ?
N1B C2B C3B 109.6(9) . . ?
N1B C2B H5 109.8 . . ?
C3B C2B H5 109.8 . . ?
N1B C2B H6 109.8 . . ?
C3B C2B H6 109.8 . . ?
H5 C2B H6 108.2 . . ?
N4B C3B C2B 108.1(9) . . ?
N4B C3B H14 110.1 . . ?
C2B C3B H14 110.1 . . ?
N4B C3B H15 110.1 . . ?
C2B C3B H15 110.1 . . ?
H14 C3B H15 108.4 . . ?
N4B C5B H19 109.5 . . ?
N4B C5B H20 109.5 . . ?
H19 C5B H20 109.5 . . ?
N4B C5B H21 109.5 . . ?
H19 C5B H21 109.5 . . ?
H20 C5B H21 109.5 . . ?
N4B C6B H16 109.5 . . ?
N4B C6B H17 109.5 . . ?
H16 C6B H17 109.5 . . ?
N4B C6B H18 109.5 . . ?
H16 C6B H18 109.5 . . ?
H17 C6B H18 109.5 . . ?
N1B C7B H11 109.5 . . ?
N1B C7B H12 109.5 . . ?
H11 C7B H12 109.5 . . ?
N1B C7B H13 109.5 . . ?
H11 C7B H13 109.5 . . ?
H12 C7B H13 109.5 . . ?
N1B C8B H7 109.5 . . ?
N1B C8B H8 109.5 . . ?
H7 C8B H8 109.5 . . ?
N1B C8B H9 109.5 . . ?
H7 C8B H9 109.5 . . ?
H8 C8B H9 109.5 . . ?
N1N O13 Ag2 113.6(8) . . ?
N1N O13 Ag1 135.7(9) . . ?
Ag2 O13 Ag1 102.9(4) . . ?
N2N O21 Ag2 104.1(6) . 2 ?
N2N O21 Ag2 100.9(6) . . ?
Ag2 O21 Ag2 19.77(10) 2 . ?

#END


data_2692
_database_code_depnum_ccdc_archive 'CCDC 622575'

_audit_creation_date             2006-11-16T12:49:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_moiety         'C16 H28 N8 O8 Pd'
_chemical_formula_sum            'C16 H28 N8 O8 Pd'
_chemical_formula_weight         566.86

#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.175(4)
_cell_length_b                   12.672(3)
_cell_length_c                   20.633(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4752.1(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11594
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       cubes
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2320
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9209
_exptl_absorpt_correction_T_max  0.9209

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'profile fitled'
_diffrn_standards_number         N/A
_diffrn_reflns_number            11597
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         23.79
_diffrn_reflns_theta_full        23.79
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_reflns_number_total             3637
_reflns_number_gt                1661
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    nonref
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3637
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0817
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_restrained_S_all      0.801
_refine_ls_shift/su_max          0
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.337

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

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 0 '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 0.006 '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_
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Pd1 Pd 0.09337(2) 0.24732(4) 0.15198(2) 0.02983(14) Uani 1 d . . .
N1A N 0.0625(3) 0.1022(4) 0.1188(3) 0.0427(16) Uani 1 d . . .
N2A N 0.1695(4) 0.0748(5) 0.0664(3) 0.075(2) Uani 1 d . . .
H31 H 0.1866 0.1342 0.0826 0.09 Uiso 1 calc R . .
H30 H 0.1973 0.0362 0.0408 0.09 Uiso 1 calc R . .
N1B N 0.0523(3) 0.3087(4) 0.0675(3) 0.0338(14) Uani 1 d . . .
N2B N -0.0659(3) 0.3284(4) 0.1090(3) 0.0624(19) Uani 1 d . . .
H29 H -0.0499 0.3096 0.1476 0.075 Uiso 1 calc R . .
H28 H -0.1126 0.3442 0.1034 0.075 Uiso 1 calc R . .
N1N N 0.3991(3) 0.2775(4) 0.2153(3) 0.0426(16) Uani 1 d . . .
N2N N 0.2618(6) 0.0161(8) 0.4058(4) 0.105(4) Uani 1 d . . .
C2A C 0.1038(4) 0.0443(6) 0.0804(4) 0.057(2) Uani 1 d . . .
C3A C 0.0801(5) -0.0543(6) 0.0535(4) 0.074(3) Uani 1 d . . .
H23 H 0.111 -0.0965 0.0269 0.088 Uiso 1 calc R . .
C4A C 0.0114(6) -0.0827(6) 0.0686(5) 0.079(3) Uani 1 d . . .
H21 H -0.0072 -0.1474 0.0522 0.095 Uiso 1 calc R . .
C5A C -0.0323(5) -0.0235(6) 0.1060(5) 0.080(3) Uani 1 d . . .
H18 H -0.0808 -0.0475 0.1148 0.096 Uiso 1 calc R . .
C6A C -0.0099(4) 0.0689(5) 0.1316(4) 0.053(2) Uiso 1 d . . .
H13 H -0.0421 0.1103 0.1574 0.063 Uiso 1 calc R . .
C2B C -0.0191(4) 0.3329(5) 0.0588(4) 0.0429(18) Uani 1 d . . .
C3B C -0.0457(4) 0.3616(5) -0.0033(4) 0.0442(19) Uani 1 d . . .
H22 H -0.0965 0.3756 -0.01 0.053 Uiso 1 calc R . .
C4B C 0.0022(4) 0.3684(4) -0.0524(4) 0.048(2) Uani 1 d . . .
H19 H -0.0147 0.3883 -0.0942 0.058 Uiso 1 calc R . .
C5B C 0.0763(4) 0.3468(5) -0.0428(4) 0.053(2) Uani 1 d . . .
H17 H 0.1105 0.3521 -0.0774 0.063 Uiso 1 calc R . .
C6B C 0.0982(4) 0.3184(5) 0.0168(3) 0.0430(17) Uani 1 d . . .
H12 H 0.149 0.3043 0.0235 0.052 Uiso 1 calc R . .
N1T N 0.1257(2) 0.3924(4) 0.1863(3) 0.0343(14) Uani 1 d . . .
C2T C 0.1767(3) 0.3718(5) 0.2421(3) 0.0370(18) Uani 1 d . . .
H25 H 0.1798 0.4351 0.27 0.044 Uiso 1 calc R . .
H24 H 0.2266 0.3555 0.2257 0.044 Uiso 1 calc R . .
C3T C 0.1474(3) 0.2801(4) 0.2802(3) 0.0351(18) Uani 1 d . . .
H27 H 0.182 0.2622 0.3156 0.042 Uiso 1 calc R . .
H26 H 0.0995 0.2991 0.2999 0.042 Uiso 1 calc R . .
N4T N 0.1379(2) 0.1876(4) 0.2366(3) 0.0323(14) Uani 1 d . . .
C5T C 0.1657(3) 0.4581(4) 0.1378(3) 0.0456(19) Uani 1 d . . .
H16 H 0.1793 0.5257 0.1575 0.068 Uiso 1 calc R . .
H15 H 0.1339 0.4708 0.1003 0.068 Uiso 1 calc R . .
H14 H 0.2103 0.421 0.1238 0.068 Uiso 1 calc R . .
C6T C 0.0606(3) 0.4544(4) 0.2087(3) 0.0438(19) Uani 1 d . . .
H11 H 0.077 0.5233 0.2247 0.066 Uiso 1 calc R . .
H10 H 0.0357 0.4161 0.2437 0.066 Uiso 1 calc R . .
H9 H 0.0265 0.4644 0.1725 0.066 Uiso 1 calc R . .
C7T C 0.2104(3) 0.1377(5) 0.2233(3) 0.0413(19) Uani 1 d . . .
H8 H 0.2308 0.1096 0.2638 0.062 Uiso 1 calc R . .
H7 H 0.2441 0.1904 0.2054 0.062 Uiso 1 calc R . .
H6 H 0.204 0.0801 0.1921 0.062 Uiso 1 calc R . .
C8T C 0.0913(3) 0.1072(4) 0.2700(3) 0.0427(17) Uani 1 d . . .
H5 H 0.1162 0.0831 0.3095 0.064 Uiso 1 calc R . .
H4 H 0.0833 0.047 0.241 0.064 Uiso 1 calc R . .
H3 H 0.0438 0.1387 0.2814 0.064 Uiso 1 calc R . .
O11 O 0.3596(2) 0.3555(4) 0.2217(3) 0.0764(19) Uani 1 d . . .
O12 O 0.3903(2) 0.2162(3) 0.1688(3) 0.0535(15) Uani 1 d . . .
O13 O 0.4503(2) 0.2577(4) 0.2553(2) 0.0649(13) Uani 1 d . . .
O21 O 0.2779(4) 0.0918(6) 0.3729(3) 0.113(2) Uani 1 d . . .
O22 O 0.2385(4) 0.0283(6) 0.4630(4) 0.135(3) Uani 1 d . . .
O23 O 0.2795(5) -0.0726(6) 0.3896(4) 0.175(4) Uani 1 d . . .
O1W O 0.27042(19) 0.2546(4) 0.0846(2) 0.0564(12) Uani 1 d . . .
O2W O 0.2868(2) 0.2680(5) 0.4532(3) 0.0887(17) Uani 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0327(2) 0.0312(2) 0.0256(2) -0.0005(4) -0.0011(2) 0.0001(3)
N1A 0.066(4) 0.042(3) 0.021(4) -0.002(3) 0.002(3) 0.018(3)
N2A 0.107(6) 0.062(5) 0.056(6) -0.016(4) 0.004(5) 0.023(4)
N1B 0.030(3) 0.038(3) 0.034(4) 0.002(3) -0.007(3) 0.000(3)
N2B 0.039(3) 0.090(5) 0.058(6) 0.016(4) -0.011(3) 0.004(3)
N1N 0.037(3) 0.052(5) 0.039(4) -0.005(3) 0.006(3) -0.008(3)
N2N 0.188(10) 0.096(8) 0.033(5) 0.009(6) -0.020(8) 0.033(7)
C2A 0.068(6) 0.060(6) 0.042(6) 0.025(4) 0.001(5) -0.015(5)
C3A 0.141(8) 0.042(5) 0.038(6) -0.007(4) -0.018(6) 0.011(6)
C4A 0.141(10) 0.040(6) 0.056(8) 0.006(5) -0.034(7) -0.020(6)
C5A 0.106(7) 0.058(6) 0.075(8) 0.018(5) -0.035(6) -0.026(5)
C2B 0.050(5) 0.040(4) 0.038(6) 0.003(4) 0.002(4) -0.008(4)
C3B 0.044(5) 0.044(4) 0.045(6) 0.007(4) -0.013(4) -0.008(3)
C4B 0.070(6) 0.029(4) 0.045(6) 0.004(4) -0.019(5) -0.011(4)
C5B 0.070(6) 0.058(5) 0.030(5) 0.002(4) 0.002(4) -0.005(4)
C6B 0.053(4) 0.047(4) 0.029(5) 0.000(4) 0.006(4) 0.000(4)
N1T 0.037(3) 0.033(3) 0.033(4) 0.002(3) -0.001(3) -0.005(3)
C2T 0.040(4) 0.042(4) 0.029(5) -0.003(4) -0.013(4) 0.000(3)
C3T 0.042(4) 0.036(5) 0.028(4) -0.003(3) -0.002(3) 0.002(3)
N4T 0.031(3) 0.036(3) 0.030(4) -0.005(3) 0.003(3) 0.000(3)
C5T 0.050(4) 0.043(4) 0.043(6) 0.008(4) -0.002(4) -0.012(4)
C6T 0.052(4) 0.034(4) 0.045(5) -0.009(4) 0.008(4) 0.005(3)
C7T 0.044(4) 0.052(4) 0.027(5) 0.003(4) 0.000(4) 0.012(4)
C8T 0.052(4) 0.040(4) 0.036(5) 0.001(3) 0.001(4) 0.002(4)
O11 0.061(3) 0.057(3) 0.111(6) -0.032(3) -0.009(3) 0.021(3)
O12 0.060(3) 0.052(3) 0.048(4) -0.010(3) 0.000(3) 0.003(2)
O13 0.051(3) 0.093(3) 0.051(3) -0.010(4) -0.017(2) 0.003(4)
O21 0.151(6) 0.129(6) 0.058(5) 0.025(4) -0.027(4) -0.035(5)
O22 0.148(7) 0.180(8) 0.078(6) 0.027(6) 0.021(5) 0.095(5)
O23 0.339(12) 0.107(6) 0.079(7) -0.019(5) 0.095(7) -0.009(7)
O1W 0.044(2) 0.078(3) 0.048(3) -0.002(3) 0.002(2) 0.001(3)
O2W 0.068(3) 0.138(5) 0.059(4) -0.017(4) 0.004(3) 0.005(4)

#------------------ MOLECULAR GEOMETRY --------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1A 2.040(5) . ?
Pd1 N1B 2.049(5) . ?
Pd1 N1T 2.055(5) . ?
Pd1 N4T 2.069(5) . ?
N1A C2A 1.316(8) . ?
N1A C6A 1.407(7) . ?
N2A C2A 1.288(8) . ?
N2A H31 0.88 . ?
N2A H30 0.88 . ?
N1B C6B 1.344(8) . ?
N1B C2B 1.346(7) . ?
N2B C2B 1.341(8) . ?
N2B H29 0.88 . ?
N2B H28 0.88 . ?
N1N O11 1.228(5) . ?
N1N O12 1.246(6) . ?
N1N O13 1.269(6) . ?
N2N O21 1.212(9) . ?
N2N O23 1.216(10) . ?
N2N O22 1.262(10) . ?
C2A C3A 1.433(10) . ?
C3A C4A 1.337(10) . ?
C3A H23 0.95 . ?
C4A C5A 1.337(11) . ?
C4A H21 0.95 . ?
C5A C6A 1.347(9) . ?
C5A H18 0.95 . ?
C6A H13 0.95 . ?
C2B C3B 1.418(9) . ?
C3B C4B 1.337(9) . ?
C3B H22 0.95 . ?
C4B C5B 1.388(8) . ?
C4B H19 0.95 . ?
C5B C6B 1.341(9) . ?
C5B H17 0.95 . ?
C6B H12 0.95 . ?
N1T C5T 1.492(7) . ?
N1T C6T 1.493(6) . ?
N1T C2T 1.501(7) . ?
C2T C3T 1.501(7) . ?
C2T H25 0.99 . ?
C2T H24 0.99 . ?
C3T N4T 1.488(7) . ?
C3T H27 0.99 . ?
C3T H26 0.99 . ?
N4T C7T 1.486(6) . ?
N4T C8T 1.494(7) . ?
C5T H16 0.98 . ?
C5T H15 0.98 . ?
C5T H14 0.98 . ?
C6T H11 0.98 . ?
C6T H10 0.98 . ?
C6T H9 0.98 . ?
C7T H8 0.98 . ?
C7T H7 0.98 . ?
C7T H6 0.98 . ?
C8T H5 0.98 . ?
C8T H4 0.98 . ?
C8T H3 0.98 . ?

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
N1A Pd1 N1B 87.53(19) . . ?
N1A Pd1 N1T 179.1(2) . . ?
N1B Pd1 N1T 93.30(19) . . ?
N1A Pd1 N4T 93.5(2) . . ?
N1B Pd1 N4T 178.21(19) . . ?
N1T Pd1 N4T 85.67(19) . . ?
C2A N1A C6A 118.6(6) . . ?
C2A N1A Pd1 123.2(5) . . ?
C6A N1A Pd1 117.7(4) . . ?
C2A N2A H31 120 . . ?
C2A N2A H30 120 . . ?
H31 N2A H30 120 . . ?
C6B N1B C2B 118.3(6) . . ?
C6B N1B Pd1 118.1(4) . . ?
C2B N1B Pd1 123.4(5) . . ?
C2B N2B H29 120 . . ?
C2B N2B H28 120 . . ?
H29 N2B H28 120 . . ?
O11 N1N O12 120.6(6) . . ?
O11 N1N O13 121.2(7) . . ?
O12 N1N O13 118.1(5) . . ?
O21 N2N O23 120.9(11) . . ?
O21 N2N O22 120.5(10) . . ?
O23 N2N O22 117.3(10) . . ?
N2A C2A N1A 119.8(7) . . ?
N2A C2A C3A 117.0(8) . . ?
N1A C2A C3A 123.3(7) . . ?
C4A C3A C2A 115.1(8) . . ?
C4A C3A H23 122.4 . . ?
C2A C3A H23 122.4 . . ?
C5A C4A C3A 122.6(9) . . ?
C5A C4A H21 118.7 . . ?
C3A C4A H21 118.7 . . ?
C4A C5A C6A 122.2(9) . . ?
C4A C5A H18 118.9 . . ?
C6A C5A H18 118.9 . . ?
C5A C6A N1A 118.1(7) . . ?
C5A C6A H13 121 . . ?
N1A C6A H13 121 . . ?
N2B C2B N1B 119.9(7) . . ?
N2B C2B C3B 119.6(7) . . ?
N1B C2B C3B 120.5(7) . . ?
C4B C3B C2B 118.7(7) . . ?
C4B C3B H22 120.7 . . ?
C2B C3B H22 120.7 . . ?
C3B C4B C5B 120.6(7) . . ?
C3B C4B H19 119.7 . . ?
C5B C4B H19 119.7 . . ?
C6B C5B C4B 118.2(7) . . ?
C6B C5B H17 120.9 . . ?
C4B C5B H17 120.9 . . ?
C5B C6B N1B 123.6(7) . . ?
C5B C6B H12 118.2 . . ?
N1B C6B H12 118.2 . . ?
C5T N1T C6T 107.5(4) . . ?
C5T N1T C2T 108.0(4) . . ?
C6T N1T C2T 110.1(5) . . ?
C5T N1T Pd1 114.1(4) . . ?
C6T N1T Pd1 110.6(3) . . ?
C2T N1T Pd1 106.6(3) . . ?
N1T C2T C3T 108.5(5) . . ?
N1T C2T H25 110 . . ?
C3T C2T H25 110 . . ?
N1T C2T H24 110 . . ?
C3T C2T H24 110 . . ?
H25 C2T H24 108.4 . . ?
N4T C3T C2T 109.5(5) . . ?
N4T C3T H27 109.8 . . ?
C2T C3T H27 109.8 . . ?
N4T C3T H26 109.8 . . ?
C2T C3T H26 109.8 . . ?
H27 C3T H26 108.2 . . ?
C7T N4T C3T 110.2(5) . . ?
C7T N4T C8T 107.3(4) . . ?
C3T N4T C8T 108.9(5) . . ?
C7T N4T Pd1 110.3(4) . . ?
C3T N4T Pd1 105.5(4) . . ?
C8T N4T Pd1 114.6(4) . . ?
N1T C5T H16 109.5 . . ?
N1T C5T H15 109.5 . . ?
H16 C5T H15 109.5 . . ?
N1T C5T H14 109.5 . . ?
H16 C5T H14 109.5 . . ?
H15 C5T H14 109.5 . . ?
N1T C6T H11 109.5 . . ?
N1T C6T H10 109.5 . . ?
H11 C6T H10 109.5 . . ?
N1T C6T H9 109.5 . . ?
H11 C6T H9 109.5 . . ?
H10 C6T H9 109.5 . . ?
N4T C7T H8 109.5 . . ?
N4T C7T H7 109.5 . . ?
H8 C7T H7 109.5 . . ?
N4T C7T H6 109.5 . . ?
H8 C7T H6 109.5 . . ?
H7 C7T H6 109.5 . . ?
N4T C8T H5 109.5 . . ?
N4T C8T H4 109.5 . . ?
H5 C8T H4 109.5 . . ?
N4T C8T H3 109.5 . . ?
H5 C8T H3 109.5 . . ?
H4 C8T H3 109.5 . . ?