# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Hor, Andy'
_publ_contact_author_email       andyhor@nus.edu.sg

_publ_section_title              
;
Crystallographic Identification
of an Unusual Homoleptic Palladium Citrate [Na(OH2)6]
{[Na3(OH2)8]3[NaPd3(C6H4O7)3]2}\"i(H2O) Stabilised
by Intermetallic Aggregation with Sodium and Heavy Hydration
;
loop_
_publ_author_name
P.Gunari
S.Krishnasamy
S.Bai
A.Hor

# Attachment '- DT-COM-04-2010-000273-Rev-Cif.cif'

data_a7001
_database_code_depnum_ccdc_archive 'CCDC 692934'
#TrackingRef '- DT-COM-04-2010-000273-Rev-Cif.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H43 Na6 O36.50 Pd3'
_chemical_formula_weight         1300.66

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.8632(6)
_cell_length_b                   15.8632(6)
_cell_length_c                   28.772(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6270.1(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4515
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3882
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8223
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_process_details   'Not Measured'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11706
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2452
_reflns_number_gt                2304
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_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^)+(0.0152P)^2^+146.1366P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2452
_refine_ls_number_parameters     242
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_restrained_S_all      1.298
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

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
O1S O 0.8089(7) 0.9336(8) 0.3789(4) 0.103(3) Uani 1 1 d D . .
H1X H 0.866(6) 0.947(12) 0.366(4) 0.124 Uiso 1 1 d D . .
H1Y H 0.827(9) 0.934(11) 0.4086(14) 0.124 Uiso 1 1 d D . .
O2S O 0.5808(5) 0.6740(6) 0.3727(2) 0.0606(18) Uani 1 1 d D . .
H2X H 0.597(6) 0.660(7) 0.4003(18) 0.073 Uiso 1 1 d D . .
H2Y H 0.5161(16) 0.637(6) 0.375(3) 0.073 Uiso 1 1 d D . .
O3S O 0.6222(8) 0.4937(8) 0.3401(3) 0.098(3) Uani 1 1 d D . .
H3X H 0.620(10) 0.506(9) 0.3703(14) 0.117 Uiso 1 1 d D . .
H3Y H 0.632(13) 0.443(8) 0.343(4) 0.117 Uiso 1 1 d D . .
O4S O 0.4250(6) 0.4879(7) 0.2962(3) 0.089(3) Uani 1 1 d D . .
H4X H 0.406(8) 0.472(8) 0.3258(13) 0.107 Uiso 1 1 d D . .
H4Y H 0.372(6) 0.439(7) 0.283(3) 0.107 Uiso 1 1 d D . .
O5S O 0.1918(5) 0.5369(5) 0.1278(3) 0.0614(19) Uani 1 1 d D . .
H5X H 0.208(7) 0.491(5) 0.131(3) 0.074 Uiso 1 1 d D . .
H5Y H 0.235(6) 0.572(6) 0.105(3) 0.074 Uiso 1 1 d D . .
Pd1 Pd 0.97793(4) 0.87289(4) 0.138236(18) 0.02086(17) Uani 1 1 d . . .
Na1 Na 1.0000 1.0000 0.23679(18) 0.0326(12) Uani 1 3 d S . .
Na2 Na 0.6667 0.8333 0.3333 0.0622(15) Uani 1 2 d S . .
Na3 Na 0.5855(3) 0.6081(3) 0.29260(14) 0.0724(13) Uani 1 1 d . . .
Na4 Na 0.3333 0.6667 0.1667 0.052(2) Uani 1 6 d S . .
O1 O 0.8551(3) 0.7719(3) 0.10740(17) 0.0275(11) Uani 1 1 d . . .
O2 O 0.6964(4) 0.7018(4) 0.1150(2) 0.0458(15) Uani 1 1 d . . .
O3 O 0.8909(6) 0.8589(7) 0.2731(3) 0.046(4) Uani 0.74(3) 1 d PD . .
O3X O 0.857(2) 0.8907(13) 0.2706(9) 0.042(9) Uiso 0.26(3) 1 d PD . .
O4 O 0.7341(4) 0.7565(4) 0.2882(2) 0.0478(15) Uani 1 1 d . . .
O5 O 0.7636(3) 0.9407(4) 0.10927(18) 0.0310(12) Uani 1 1 d . . .
O6 O 0.6083(4) 0.8625(4) 0.1267(2) 0.0466(15) Uani 1 1 d . . .
O7 O 0.8880(3) 0.9082(3) 0.17102(16) 0.0211(10) Uani 1 1 d . . .
C1 C 0.7941(5) 0.8202(5) 0.1736(2) 0.0244(15) Uani 1 1 d . . .
C2 C 0.7785(5) 0.7603(5) 0.1290(3) 0.0272(16) Uani 1 1 d . . .
C3 C 0.7952(6) 0.7546(6) 0.2131(3) 0.0335(18) Uani 1 1 d . . .
H3B H 0.849(6) 0.748(6) 0.206(3) 0.040 Uiso 1 1 d . . .
H3A H 0.739(6) 0.697(6) 0.209(3) 0.040 Uiso 1 1 d . . .
C4 C 0.8035(6) 0.7981(7) 0.2616(3) 0.045(2) Uani 1 1 d D . .
C5 C 0.7137(5) 0.8443(5) 0.1792(3) 0.0284(16) Uani 1 1 d . . .
H5B H 0.654(6) 0.787(6) 0.188(3) 0.034 Uiso 1 1 d . . .
H5A H 0.738(5) 0.883(6) 0.210(3) 0.034 Uiso 1 1 d . . .
C6 C 0.6923(5) 0.8833(5) 0.1364(3) 0.0309(17) Uani 1 1 d . . .
O6S O 0.3333 0.6667 0.0141(8) 0.102(11) Uani 0.50 3 d SP . .

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
O1S 0.098(7) 0.110(7) 0.103(7) 0.002(7) -0.039(6) 0.052(7)
O2S 0.053(4) 0.076(5) 0.055(4) 0.016(4) 0.002(3) 0.034(4)
O3S 0.102(7) 0.127(9) 0.060(5) -0.008(5) 0.004(5) 0.054(7)
O4S 0.068(5) 0.094(7) 0.061(5) -0.002(5) 0.018(4) 0.006(5)
O5S 0.055(4) 0.044(4) 0.085(6) -0.002(4) -0.008(4) 0.024(3)
Pd1 0.0198(3) 0.0193(3) 0.0239(3) -0.0016(2) 0.0000(2) 0.0101(2)
Na1 0.0295(16) 0.0295(16) 0.039(3) 0.000 0.000 0.0147(8)
Na2 0.089(4) 0.061(3) 0.054(3) -0.005(3) -0.001(3) 0.050(3)
Na3 0.056(2) 0.066(3) 0.053(2) -0.009(2) 0.0098(19) -0.002(2)
Na4 0.039(3) 0.039(3) 0.076(7) 0.000 0.000 0.0197(14)
O1 0.027(3) 0.025(3) 0.029(3) -0.009(2) -0.007(2) 0.012(2)
O2 0.034(3) 0.044(3) 0.048(4) -0.013(3) -0.010(3) 0.011(3)
O3 0.038(5) 0.040(6) 0.039(5) 0.006(4) -0.010(4) 0.003(4)
O4 0.043(3) 0.049(4) 0.041(3) 0.003(3) 0.006(3) 0.015(3)
O5 0.024(3) 0.031(3) 0.033(3) -0.001(2) -0.008(2) 0.010(2)
O6 0.032(3) 0.048(4) 0.057(4) 0.004(3) -0.008(3) 0.018(3)
O7 0.014(2) 0.018(2) 0.028(2) -0.0013(19) 0.0001(19) 0.0055(19)
C1 0.017(3) 0.023(4) 0.027(4) 0.004(3) 0.004(3) 0.005(3)
C2 0.026(4) 0.030(4) 0.031(4) -0.001(3) -0.002(3) 0.018(3)
C3 0.030(4) 0.031(4) 0.039(5) 0.004(4) -0.001(4) 0.015(4)
C4 0.039(5) 0.048(5) 0.027(4) 0.005(4) -0.005(4) 0.004(4)
C5 0.025(4) 0.022(4) 0.036(4) -0.002(3) 0.002(3) 0.010(3)
C6 0.028(4) 0.026(4) 0.036(4) -0.011(3) -0.005(3) 0.011(3)
O6S 0.142(18) 0.142(18) 0.022(13) 0.000 0.000 0.071(9)

_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
O1S Na2 2.399(9) . ?
O1S Na3 2.610(12) 16_665 ?
O2S Na2 2.467(7) . ?
O2S Na3 2.547(8) . ?
O3S Na3 2.560(11) . ?
O4S Na3 2.296(9) . ?
O5S Na4 2.431(7) . ?
Pd1 O7 1.991(5) 2_765 ?
Pd1 O5 2.003(5) 2_765 ?
Pd1 O1 2.008(5) . ?
Pd1 O7 2.009(4) . ?
Pd1 Pd1 3.2321(9) 2_765 ?
Pd1 Pd1 3.2321(9) 3_675 ?
Pd1 Na1 3.394(4) . ?
Na1 O3X 2.27(2) 3_675 ?
Na1 O3X 2.27(2) 2_765 ?
Na1 O3X 2.27(2) . ?
Na1 O3 2.285(8) 2_765 ?
Na1 O3 2.285(8) . ?
Na1 O3 2.285(8) 3_675 ?
Na1 O7 2.504(6) . ?
Na1 O7 2.504(6) 2_765 ?
Na1 O7 2.504(6) 3_675 ?
Na1 Pd1 3.394(4) 3_675 ?
Na1 Pd1 3.394(4) 2_765 ?
Na2 O4 2.371(6) 16_665 ?
Na2 O4 2.371(6) . ?
Na2 O1S 2.399(9) 16_665 ?
Na2 O2S 2.467(7) 16_665 ?
Na2 Na3 3.347(4) 16_665 ?
Na2 Na3 3.347(4) . ?
Na3 O4 2.359(7) . ?
Na3 O6 2.595(7) 14_455 ?
Na3 O1S 2.610(12) 16_665 ?
Na3 O5 2.635(6) 14_455 ?
Na3 C6 2.985(9) 14_455 ?
Na4 O5S 2.431(7) 15 ?
Na4 O5S 2.431(7) 3_565 ?
Na4 O5S 2.431(7) 2_665 ?
Na4 O5S 2.431(7) 13_565 ?
Na4 O5S 2.431(7) 14_455 ?
O1 C2 1.293(8) . ?
O2 C2 1.229(9) . ?
O3 O3X 0.90(3) . ?
O3 C4 1.275(11) . ?
O3X C4 1.303(17) . ?
O4 C4 1.227(10) . ?
O5 C6 1.299(9) . ?
O5 Pd1 2.003(5) 3_675 ?
O5 Na3 2.635(6) 15 ?
O6 C6 1.234(9) . ?
O6 Na3 2.595(7) 15 ?
O7 C1 1.447(8) . ?
O7 Pd1 1.991(4) 3_675 ?
C1 C5 1.511(10) . ?
C1 C2 1.541(10) . ?
C1 C3 1.547(10) . ?
C3 C4 1.532(12) . ?
C5 C6 1.491(11) . ?
C6 Na3 2.985(9) 15 ?

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
Na2 O1S Na3 83.7(3) . 16_665 ?
Na2 O2S Na3 83.7(2) . . ?
O7 Pd1 O5 92.53(19) 2_765 2_765 ?
O7 Pd1 O1 173.91(18) 2_765 . ?
O5 Pd1 O1 93.5(2) 2_765 . ?
O7 Pd1 O7 90.5(2) 2_765 . ?
O5 Pd1 O7 173.4(2) 2_765 . ?
O1 Pd1 O7 83.61(18) . . ?
O7 Pd1 Pd1 36.30(13) 2_765 2_765 ?
O5 Pd1 Pd1 101.61(15) 2_765 2_765 ?
O1 Pd1 Pd1 140.81(14) . 2_765 ?
O7 Pd1 Pd1 84.26(12) . 2_765 ?
O7 Pd1 Pd1 84.52(12) 2_765 3_675 ?
O5 Pd1 Pd1 150.30(15) 2_765 3_675 ?
O1 Pd1 Pd1 89.79(14) . 3_675 ?
O7 Pd1 Pd1 35.92(13) . 3_675 ?
Pd1 Pd1 Pd1 60.0 2_765 3_675 ?
O7 Pd1 Na1 47.02(13) 2_765 . ?
O5 Pd1 Na1 133.39(15) 2_765 . ?
O1 Pd1 Na1 127.87(14) . . ?
O7 Pd1 Na1 47.08(13) . . ?
Pd1 Pd1 Na1 61.57(4) 2_765 . ?
Pd1 Pd1 Na1 61.57(4) 3_675 . ?
O3X Na1 O3X 103.0(8) 3_675 2_765 ?
O3X Na1 O3X 103.0(8) 3_675 . ?
O3X Na1 O3X 103.0(8) 2_765 . ?
O3X Na1 O3 82.4(5) 3_675 2_765 ?
O3X Na1 O3 22.9(7) 2_765 2_765 ?
O3X Na1 O3 117.8(7) . 2_765 ?
O3X Na1 O3 117.8(7) 3_675 . ?
O3X Na1 O3 82.4(5) 2_765 . ?
O3X Na1 O3 22.9(6) . . ?
O3 Na1 O3 100.8(3) 2_765 . ?
O3X Na1 O3 22.9(7) 3_675 3_675 ?
O3X Na1 O3 117.8(7) 2_765 3_675 ?
O3X Na1 O3 82.4(5) . 3_675 ?
O3 Na1 O3 100.8(3) 2_765 3_675 ?
O3 Na1 O3 100.8(3) . 3_675 ?
O3X Na1 O7 130.4(5) 3_675 . ?
O3X Na1 O7 126.2(9) 2_765 . ?
O3X Na1 O7 74.5(6) . . ?
O3 Na1 O7 143.7(3) 2_765 . ?
O3 Na1 O7 78.8(2) . . ?
O3 Na1 O7 115.1(3) 3_675 . ?
O3X Na1 O7 126.2(9) 3_675 2_765 ?
O3X Na1 O7 74.5(6) 2_765 2_765 ?
O3X Na1 O7 130.4(5) . 2_765 ?
O3 Na1 O7 78.8(2) 2_765 2_765 ?
O3 Na1 O7 115.1(3) . 2_765 ?
O3 Na1 O7 143.7(3) 3_675 2_765 ?
O7 Na1 O7 69.1(2) . 2_765 ?
O3X Na1 O7 74.5(6) 3_675 3_675 ?
O3X Na1 O7 130.4(6) 2_765 3_675 ?
O3X Na1 O7 126.2(9) . 3_675 ?
O3 Na1 O7 115.1(3) 2_765 3_675 ?
O3 Na1 O7 143.7(3) . 3_675 ?
O3 Na1 O7 78.8(2) 3_675 3_675 ?
O7 Na1 O7 69.1(2) . 3_675 ?
O7 Na1 O7 69.1(2) 2_765 3_675 ?
O3X Na1 Pd1 148.6(7) 3_675 . ?
O3X Na1 Pd1 94.7(8) 2_765 . ?
O3X Na1 Pd1 97.9(5) . . ?
O3 Na1 Pd1 108.2(2) 2_765 . ?
O3 Na1 Pd1 89.8(3) . . ?
O3 Na1 Pd1 146.7(3) 3_675 . ?
O7 Na1 Pd1 35.99(12) . . ?
O7 Na1 Pd1 35.57(12) 2_765 . ?
O7 Na1 Pd1 74.27(16) 3_675 . ?
O3X Na1 Pd1 97.9(5) 3_675 3_675 ?
O3X Na1 Pd1 148.6(7) 2_765 3_675 ?
O3X Na1 Pd1 94.7(8) . 3_675 ?
O3 Na1 Pd1 146.7(3) 2_765 3_675 ?
O3 Na1 Pd1 108.2(2) . 3_675 ?
O3 Na1 Pd1 89.8(3) 3_675 3_675 ?
O7 Na1 Pd1 35.57(12) . 3_675 ?
O7 Na1 Pd1 74.27(16) 2_765 3_675 ?
O7 Na1 Pd1 35.99(12) 3_675 3_675 ?
Pd1 Na1 Pd1 56.86(8) . 3_675 ?
O3X Na1 Pd1 94.7(8) 3_675 2_765 ?
O3X Na1 Pd1 97.9(5) 2_765 2_765 ?
O3X Na1 Pd1 148.6(7) . 2_765 ?
O3 Na1 Pd1 89.8(3) 2_765 2_765 ?
O3 Na1 Pd1 146.7(3) . 2_765 ?
O3 Na1 Pd1 108.2(2) 3_675 2_765 ?
O7 Na1 Pd1 74.27(16) . 2_765 ?
O7 Na1 Pd1 35.99(12) 2_765 2_765 ?
O7 Na1 Pd1 35.57(12) 3_675 2_765 ?
Pd1 Na1 Pd1 56.86(8) . 2_765 ?
Pd1 Na1 Pd1 56.86(8) 3_675 2_765 ?
O4 Na2 O4 179.999(1) 16_665 . ?
O4 Na2 O1S 82.9(3) 16_665 . ?
O4 Na2 O1S 97.1(3) . . ?
O4 Na2 O1S 97.1(3) 16_665 16_665 ?
O4 Na2 O1S 82.9(3) . 16_665 ?
O1S Na2 O1S 179.998(1) . 16_665 ?
O4 Na2 O2S 96.6(2) 16_665 . ?
O4 Na2 O2S 83.4(2) . . ?
O1S Na2 O2S 106.4(3) . . ?
O1S Na2 O2S 73.6(3) 16_665 . ?
O4 Na2 O2S 83.4(2) 16_665 16_665 ?
O4 Na2 O2S 96.6(2) . 16_665 ?
O1S Na2 O2S 73.6(3) . 16_665 ?
O1S Na2 O2S 106.4(3) 16_665 16_665 ?
O2S Na2 O2S 179.998(1) . 16_665 ?
O4 Na2 Na3 44.82(16) 16_665 16_665 ?
O4 Na2 Na3 135.18(16) . 16_665 ?
O1S Na2 Na3 50.8(3) . 16_665 ?
O1S Na2 Na3 129.2(3) 16_665 16_665 ?
O2S Na2 Na3 130.84(19) . 16_665 ?
O2S Na2 Na3 49.16(19) 16_665 16_665 ?
O4 Na2 Na3 135.18(16) 16_665 . ?
O4 Na2 Na3 44.82(16) . . ?
O1S Na2 Na3 129.2(3) . . ?
O1S Na2 Na3 50.8(3) 16_665 . ?
O2S Na2 Na3 49.16(19) . . ?
O2S Na2 Na3 130.84(19) 16_665 . ?
Na3 Na2 Na3 180.0 16_665 . ?
O4S Na3 O4 166.1(4) . . ?
O4S Na3 O2S 93.0(3) . . ?
O4 Na3 O2S 81.9(2) . . ?
O4S Na3 O3S 86.5(4) . . ?
O4 Na3 O3S 105.6(3) . . ?
O2S Na3 O3S 82.6(3) . . ?
O4S Na3 O6 76.7(3) . 14_455 ?
O4 Na3 O6 100.6(2) . 14_455 ?
O2S Na3 O6 146.6(3) . 14_455 ?
O3S Na3 O6 127.3(3) . 14_455 ?
O4S Na3 O1S 87.4(4) . 16_665 ?
O4 Na3 O1S 78.7(3) . 16_665 ?
O2S Na3 O1S 68.8(3) . 16_665 ?
O3S Na3 O1S 150.4(4) . 16_665 ?
O6 Na3 O1S 79.0(3) 14_455 16_665 ?
O4S Na3 O5 87.9(3) . 14_455 ?
O4 Na3 O5 100.8(2) . 14_455 ?
O2S Na3 O5 163.3(3) . 14_455 ?
O3S Na3 O5 80.8(3) . 14_455 ?
O6 Na3 O5 49.54(18) 14_455 14_455 ?
O1S Na3 O5 127.9(3) 16_665 14_455 ?
O4S Na3 C6 77.7(3) . 14_455 ?
O4 Na3 C6 105.5(2) . 14_455 ?
O2S Na3 C6 168.3(3) . 14_455 ?
O3S Na3 C6 103.7(3) . 14_455 ?
O6 Na3 C6 24.28(19) 14_455 14_455 ?
O1S Na3 C6 103.2(3) 16_665 14_455 ?
O5 Na3 C6 25.78(18) 14_455 14_455 ?
O4S Na3 Na2 123.0(3) . . ?
O4 Na3 Na2 45.10(17) . . ?
O2S Na3 Na2 47.12(18) . . ?
O3S Na3 Na2 117.9(3) . . ?
O6 Na3 Na2 113.1(2) 14_455 . ?
O1S Na3 Na2 45.4(2) 16_665 . ?
O5 Na3 Na2 142.78(18) 14_455 . ?
C6 Na3 Na2 133.2(2) 14_455 . ?
O5S Na4 O5S 179.998(1) 15 3_565 ?
O5S Na4 O5S 79.5(2) 15 . ?
O5S Na4 O5S 100.5(2) 3_565 . ?
O5S Na4 O5S 79.5(2) 15 2_665 ?
O5S Na4 O5S 100.5(2) 3_565 2_665 ?
O5S Na4 O5S 100.5(2) . 2_665 ?
O5S Na4 O5S 100.5(2) 15 13_565 ?
O5S Na4 O5S 79.5(2) 3_565 13_565 ?
O5S Na4 O5S 179.998(1) . 13_565 ?
O5S Na4 O5S 79.5(2) 2_665 13_565 ?
O5S Na4 O5S 100.5(2) 15 14_455 ?
O5S Na4 O5S 79.5(2) 3_565 14_455 ?
O5S Na4 O5S 79.5(2) . 14_455 ?
O5S Na4 O5S 179.999(1) 2_665 14_455 ?
O5S Na4 O5S 100.5(2) 13_565 14_455 ?
C2 O1 Pd1 111.7(4) . . ?
O3X O3 C4 71.2(11) . . ?
O3X O3 Na1 77.7(15) . . ?
C4 O3 Na1 128.9(7) . . ?
O3 O3X C4 67.8(12) . . ?
O3 O3X Na1 79.4(17) . . ?
C4 O3X Na1 128.0(17) . . ?
C4 O4 Na3 138.6(6) . . ?
C4 O4 Na2 125.4(6) . . ?
Na3 O4 Na2 90.1(2) . . ?
C6 O5 Pd1 117.6(5) . 3_675 ?
C6 O5 Na3 92.3(4) . 15 ?
Pd1 O5 Na3 147.6(3) 3_675 15 ?
C6 O6 Na3 95.8(5) . 15 ?
C1 O7 Pd1 117.6(4) . 3_675 ?
C1 O7 Pd1 106.7(4) . . ?
Pd1 O7 Pd1 107.8(2) 3_675 . ?
C1 O7 Na1 127.7(4) . . ?
Pd1 O7 Na1 97.41(17) 3_675 . ?
Pd1 O7 Na1 96.93(17) . . ?
O7 C1 C5 110.7(6) . . ?
O7 C1 C2 108.8(5) . . ?
C5 C1 C2 110.4(6) . . ?
O7 C1 C3 109.5(6) . . ?
C5 C1 C3 112.8(6) . . ?
C2 C1 C3 104.5(6) . . ?
O2 C2 O1 121.0(7) . . ?
O2 C2 C1 121.4(6) . . ?
O1 C2 C1 117.6(6) . . ?
C4 C3 C1 113.2(7) . . ?
O4 C4 O3 126.2(8) . . ?
O4 C4 O3X 112.8(13) . . ?
O3 C4 O3X 41.0(12) . . ?
O4 C4 C3 118.2(7) . . ?
O3 C4 C3 113.1(8) . . ?
O3X C4 C3 123.3(12) . . ?
C6 C5 C1 114.4(6) . . ?
O6 C6 O5 119.8(7) . . ?
O6 C6 C5 121.0(7) . . ?
O5 C6 C5 119.2(6) . . ?
O6 C6 Na3 59.9(4) . 15 ?
O5 C6 Na3 61.9(4) . 15 ?
C5 C6 Na3 166.6(5) . 15 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4S H4Y O2 0.90(2) 2.42(10) 3.049(11) 127(10) 14_455
O4S H4X O3 0.90(2) 2.63(9) 3.320(12) 134(11) 18_545
O4S H4X O4 0.90(2) 2.03(5) 2.880(10) 157(10) 18_545
O3S H3Y O3S 0.90(2) 2.63(17) 2.986(11) 105(12) 18_545
O3S H3X O1 0.90(2) 2.10(6) 2.945(10) 158(12) 6_565
O2S H2Y O3 0.89(2) 2.14(3) 3.024(15) 169(9) 18_545
O2S H2X O2 0.90(2) 1.97(3) 2.832(9) 160(8) 6_565

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.825
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.129