# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222

# 1. SUBMISSION DETAILS

_publ_contact_author             
;
Dr. Darren Griffith
Centre for Synthesis & Chemical Biology
Department of Pharmaceutical & Medicinal Chemistry
Royal College of Surgeons in Ireland
123 St. Stephens Green
Dublin 2
Ireland.
;
_publ_contact_author_phone       '00353 1 402-2246'
_publ_contact_author_fax         '00353 1 402-2168'
_publ_contact_author_email       dgriffith@rcsi.ie
_publ_requested_coeditor_name    ?

loop_
_publ_author_name
_publ_author_address
'Darren Griffith'
; Centre for Synthesis & Chemical Biology
Department of Pharmaceutical & Medicinal Chemistry
Royal College of Surgeons in Ireland
123 St. Stephens Green
Dublin 2
Ireland.
;
'Atish Chopra'
; Centre for Synthesis & Chemical Biology
Department of Pharmaceutical & Medicinal Chemistry
Royal College of Surgeons in Ireland
123 St. Stephens Green
Dublin 2
Ireland.
;
'Celine Marmion'
; School of Chemistry and Chemical Biology
University College Dublin
Belfield
Dublin 4
Ireland
;
H.Muller-Bunz
; Centre for Synthesis & Chemical Biology
Department of Pharmaceutical & Medicinal Chemistry
Royal College of Surgeons in Ireland
123 St. Stephens Green
Dublin 2
Ireland.
;
_publ_contact_author_name        'Dr. Darren Griffith'
#===END_data_global

data_nol17
_database_code_depnum_ccdc_archive 'CCDC 690288'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C7 H5 N3 O4), 2 Na, 8 (H2 O)'
_chemical_formula_sum            'C7 H21 N3 O12 Na2'
_chemical_formula_weight         385.25

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1317(11)
_cell_length_b                   9.3823(15)
_cell_length_c                   12.482(2)
_cell_angle_alpha                80.310(2)
_cell_angle_beta                 87.568(2)
_cell_angle_gamma                79.188(2)
_cell_volume                     808.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7584
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             404
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7590
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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            13266
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3498
_reflns_number_gt                3171
_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^)+(0.0664P)^2^+0.1787P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3498
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1074
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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
N1 N 0.22958(16) 1.05929(12) 0.52266(9) 0.0236(2) Uani 1 1 d . . .
C1 C 0.27167(18) 0.95067(14) 0.46436(10) 0.0239(3) Uani 1 1 d . . .
C6 C 0.30949(18) 0.99446(14) 0.34461(10) 0.0242(3) Uani 1 1 d . . .
O11 O 0.34946(16) 0.90056(11) 0.28286(8) 0.0335(2) Uani 1 1 d . . .
N2 N 0.29082(17) 1.13684(12) 0.31272(9) 0.0249(2) Uani 1 1 d . . .
H1N2 H 0.264(2) 1.1952(19) 0.3557(14) 0.026(4) Uiso 1 1 d . . .
O12 O 0.30626(14) 1.19811(10) 0.20558(7) 0.0272(2) Uani 1 1 d . . .
C2 C 0.2757(2) 0.80389(16) 0.50816(12) 0.0330(3) Uani 1 1 d . . .
H2 H 0.307(3) 0.734(2) 0.4659(17) 0.045(5) Uiso 1 1 d . . .
C3 C 0.2324(2) 0.76943(16) 0.61730(12) 0.0355(3) Uani 1 1 d . . .
H3 H 0.230(3) 0.665(2) 0.6474(15) 0.043(5) Uiso 1 1 d . . .
C4 C 0.1884(2) 0.88071(16) 0.67882(11) 0.0297(3) Uani 1 1 d . . .
H4 H 0.161(3) 0.864(2) 0.7526(17) 0.043(5) Uiso 1 1 d . . .
C5 C 0.18871(18) 1.02465(14) 0.62836(10) 0.0243(3) Uani 1 1 d . . .
C7 C 0.14479(18) 1.14769(15) 0.69312(10) 0.0253(3) Uani 1 1 d . . .
N3 N 0.15254(19) 1.27991(13) 0.64125(11) 0.0304(3) Uani 1 1 d . . .
H1N3 H 0.173(3) 1.295(2) 0.5773(18) 0.039(5) Uiso 1 1 d . . .
O9 O 0.10897(15) 1.12175(11) 0.79389(8) 0.0326(2) Uani 1 1 d . . .
O10 O 0.13331(17) 1.39867(12) 0.69369(9) 0.0393(3) Uani 1 1 d . . .
O1 O 0.10051(16) 1.07953(12) 0.08163(9) 0.0331(2) Uani 1 1 d . . .
H1O1 H 0.039(3) 1.024(3) 0.1224(18) 0.050(6) Uiso 1 1 d . . .
H2O1 H 0.159(3) 1.114(2) 0.1265(17) 0.045(5) Uiso 1 1 d . . .
O2 O 0.40935(17) 0.93790(13) -0.09093(8) 0.0323(2) Uani 1 1 d . . .
H1O2 H 0.319(3) 0.985(2) -0.1287(17) 0.045(5) Uiso 1 1 d . . .
H2O2 H 0.487(3) 0.899(2) -0.1343(17) 0.044(5) Uiso 1 1 d . . .
O3 O 0.15813(16) 0.73633(12) 0.06962(11) 0.0358(3) Uani 1 1 d . . .
H1O3 H 0.089(4) 0.799(3) 0.016(3) 0.086(9) Uiso 1 1 d . . .
H2O3 H 0.102(3) 0.738(3) 0.130(2) 0.057(6) Uiso 1 1 d . . .
O4 O 0.50928(16) 0.56752(12) -0.13126(9) 0.0342(2) Uani 1 1 d . . .
H1O4 H 0.549(3) 0.646(3) -0.1633(18) 0.053(6) Uiso 1 1 d . . .
H2O4 H 0.522(3) 0.517(3) -0.179(2) 0.061(7) Uiso 1 1 d . . .
O5 O 0.30181(17) 0.29180(13) -0.08159(11) 0.0362(3) Uani 1 1 d . . .
H1O5 H 0.266(4) 0.302(3) -0.142(2) 0.069(8) Uiso 1 1 d . . .
H2O5 H 0.248(4) 0.231(3) -0.051(2) 0.082(9) Uiso 1 1 d . . .
O6 O 0.01320(17) 0.42810(13) 0.13711(9) 0.0364(3) Uani 1 1 d . . .
H1O6 H -0.005(4) 0.486(3) 0.182(2) 0.067(7) Uiso 1 1 d . . .
H2O6 H 0.097(3) 0.356(3) 0.1678(18) 0.052(6) Uiso 1 1 d . . .
O7 O 0.4783(2) 0.59582(14) 0.30596(11) 0.0445(3) Uani 1 1 d . . .
H1O7 H 0.591(4) 0.586(3) 0.310(2) 0.064(8) Uiso 1 1 d . . .
H2O7 H 0.437(4) 0.687(3) 0.300(2) 0.063(7) Uiso 1 1 d . . .
O8 O 0.1947(2) 0.41459(14) 0.40602(11) 0.0463(3) Uani 1 1 d . . .
H1O8 H 0.290(4) 0.463(3) 0.381(2) 0.075(8) Uiso 1 1 d . . .
H2O8 H 0.097(5) 0.467(4) 0.381(3) 0.101(11) Uiso 1 1 d . . .
Na1 Na 0.39520(8) 0.87308(6) 0.09512(4) 0.03063(16) Uani 1 1 d . . .
Na2 Na 0.24808(8) 0.52337(6) -0.01105(5) 0.03266(16) Uani 1 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
N1 0.0257(6) 0.0233(5) 0.0222(5) -0.0052(4) 0.0003(4) -0.0044(4)
C1 0.0258(6) 0.0241(6) 0.0220(6) -0.0046(5) -0.0002(5) -0.0044(5)
C6 0.0251(6) 0.0245(6) 0.0229(6) -0.0049(5) 0.0010(5) -0.0033(5)
O11 0.0526(7) 0.0239(5) 0.0234(5) -0.0076(4) 0.0029(4) -0.0029(4)
N2 0.0323(6) 0.0233(5) 0.0194(5) -0.0055(4) 0.0035(4) -0.0048(4)
O12 0.0352(5) 0.0234(4) 0.0216(5) -0.0010(3) 0.0027(4) -0.0051(4)
C2 0.0471(9) 0.0229(7) 0.0290(7) -0.0078(5) 0.0046(6) -0.0042(6)
C3 0.0490(9) 0.0235(7) 0.0316(7) -0.0002(6) 0.0033(6) -0.0058(6)
C4 0.0356(7) 0.0298(7) 0.0224(6) -0.0017(5) 0.0029(5) -0.0060(5)
C5 0.0239(6) 0.0269(6) 0.0224(6) -0.0057(5) 0.0002(5) -0.0037(5)
C7 0.0233(6) 0.0295(7) 0.0235(6) -0.0084(5) -0.0004(5) -0.0024(5)
N3 0.0397(7) 0.0276(6) 0.0256(6) -0.0109(5) 0.0030(5) -0.0054(5)
O9 0.0392(6) 0.0359(5) 0.0217(5) -0.0080(4) 0.0030(4) -0.0023(4)
O10 0.0509(7) 0.0293(5) 0.0416(6) -0.0196(5) 0.0025(5) -0.0054(5)
O1 0.0373(6) 0.0326(5) 0.0311(5) -0.0073(4) -0.0008(4) -0.0089(4)
O2 0.0316(6) 0.0386(6) 0.0258(5) -0.0082(4) 0.0008(4) -0.0015(4)
O3 0.0366(6) 0.0319(6) 0.0408(6) -0.0113(5) 0.0047(5) -0.0077(4)
O4 0.0405(6) 0.0298(5) 0.0353(6) -0.0070(5) 0.0026(4) -0.0130(4)
O5 0.0354(6) 0.0314(6) 0.0443(7) -0.0121(5) -0.0027(5) -0.0065(4)
O6 0.0381(6) 0.0324(6) 0.0363(6) -0.0064(5) -0.0065(5) 0.0018(5)
O7 0.0504(8) 0.0333(6) 0.0529(7) -0.0156(5) 0.0041(6) -0.0089(5)
O8 0.0537(8) 0.0326(6) 0.0505(7) -0.0038(5) 0.0028(6) -0.0056(6)
Na1 0.0313(3) 0.0334(3) 0.0288(3) -0.0086(2) 0.0021(2) -0.0076(2)
Na2 0.0308(3) 0.0321(3) 0.0364(3) -0.0105(2) -0.0010(2) -0.0046(2)

_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
N1 C1 1.3322(18) . ?
N1 C5 1.3378(17) . ?
C1 C2 1.3891(19) . ?
C1 C6 1.5087(18) . ?
C6 O11 1.2519(16) . ?
C6 N2 1.3113(17) . ?
O11 Na1 2.4023(11) . ?
N2 O12 1.3724(14) . ?
N2 H1N2 0.822(18) . ?
C2 C3 1.382(2) . ?
C2 H2 0.90(2) . ?
C3 C4 1.380(2) . ?
C3 H3 0.99(2) . ?
C4 C5 1.3912(19) . ?
C4 H4 0.93(2) . ?
C5 C7 1.4970(18) . ?
C7 O9 1.2648(16) . ?
C7 N3 1.3090(19) . ?
N3 O10 1.3672(15) . ?
N3 H1N3 0.80(2) . ?
O1 Na1 2.5671(13) . ?
O1 H1O1 0.83(2) . ?
O1 H2O1 0.85(2) . ?
O2 Na1 2.3023(12) . ?
O2 Na1 2.4456(12) 2_675 ?
O2 H1O2 0.83(2) . ?
O2 H2O2 0.84(2) . ?
O3 Na2 2.3577(13) . ?
O3 Na1 2.3671(12) . ?
O3 H1O3 0.91(3) . ?
O3 H2O3 0.84(2) . ?
O4 Na2 2.3950(13) . ?
O4 Na2 2.4646(13) 2_665 ?
O4 H1O4 0.87(2) . ?
O4 H2O4 0.81(3) . ?
O5 Na1 2.4277(13) 2_665 ?
O5 Na2 2.4383(13) . ?
O5 H1O5 0.79(3) . ?
O5 H2O5 0.78(3) . ?
O6 Na2 2.4175(13) 2_565 ?
O6 Na2 2.6014(14) . ?
O6 H1O6 0.84(3) . ?
O6 H2O6 0.87(3) . ?
O7 H1O7 0.80(3) . ?
O7 H2O7 0.84(3) . ?
O8 H1O8 0.90(3) . ?
O8 H2O8 0.82(3) . ?
Na1 O5 2.4277(13) 2_665 ?
Na1 O2 2.4456(12) 2_675 ?
Na1 Na1 3.5603(12) 2_675 ?
Na1 Na2 4.0615(9) . ?
Na1 H2O1 2.63(2) . ?
Na1 H2O3 2.63(2) . ?
Na2 O6 2.4175(13) 2_565 ?
Na2 O4 2.4645(13) 2_665 ?
Na2 Na2 3.5542(12) 2_665 ?
Na2 Na2 3.6397(12) 2_565 ?

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
C1 N1 C5 118.11(12) . . ?
N1 C1 C2 123.16(12) . . ?
N1 C1 C6 116.61(12) . . ?
C2 C1 C6 120.20(12) . . ?
O11 C6 N2 124.48(12) . . ?
O11 C6 C1 121.46(12) . . ?
N2 C6 C1 114.02(11) . . ?
C6 O11 Na1 142.96(9) . . ?
C6 N2 O12 122.44(11) . . ?
C6 N2 H1N2 121.7(12) . . ?
O12 N2 H1N2 115.8(12) . . ?
C3 C2 C1 118.24(13) . . ?
C3 C2 H2 121.7(13) . . ?
C1 C2 H2 120.1(13) . . ?
C4 C3 C2 119.31(13) . . ?
C4 C3 H3 122.7(11) . . ?
C2 C3 H3 118.0(11) . . ?
C3 C4 C5 118.60(13) . . ?
C3 C4 H4 123.1(13) . . ?
C5 C4 H4 118.3(12) . . ?
N1 C5 C4 122.59(12) . . ?
N1 C5 C7 117.45(12) . . ?
C4 C5 C7 119.96(12) . . ?
O9 C7 N3 122.65(12) . . ?
O9 C7 C5 120.49(12) . . ?
N3 C7 C5 116.82(12) . . ?
C7 N3 O10 122.10(12) . . ?
C7 N3 H1N3 121.8(14) . . ?
O10 N3 H1N3 116.1(14) . . ?
Na1 O1 H1O1 90.3(15) . . ?
Na1 O1 H2O1 84.7(14) . . ?
H1O1 O1 H2O1 103(2) . . ?
Na1 O2 Na1 97.11(4) . 2_675 ?
Na1 O2 H1O2 124.3(14) . . ?
Na1 O2 H1O2 100.5(14) 2_675 . ?
Na1 O2 H2O2 127.7(14) . . ?
Na1 O2 H2O2 88.6(14) 2_675 . ?
H1O2 O2 H2O2 105(2) . . ?
Na2 O3 Na1 118.54(5) . . ?
Na2 O3 H1O3 101.7(18) . . ?
Na1 O3 H1O3 100.4(18) . . ?
Na2 O3 H2O3 124.1(16) . . ?
Na1 O3 H2O3 98.5(15) . . ?
H1O3 O3 H2O3 112(2) . . ?
Na2 O4 Na2 93.99(5) . 2_665 ?
Na2 O4 H1O4 134.2(15) . . ?
Na2 O4 H1O4 100.3(14) 2_665 . ?
Na2 O4 H2O4 112.1(17) . . ?
Na2 O4 H2O4 112.4(17) 2_665 . ?
H1O4 O4 H2O4 102(2) . . ?
Na1 O5 Na2 126.89(5) 2_665 . ?
Na1 O5 H1O5 99.9(19) 2_665 . ?
Na2 O5 H1O5 112.2(19) . . ?
Na1 O5 H2O5 95(2) 2_665 . ?
Na2 O5 H2O5 116(2) . . ?
H1O5 O5 H2O5 103(3) . . ?
Na2 O6 Na2 92.90(4) 2_565 . ?
Na2 O6 H1O6 111.2(18) 2_565 . ?
Na2 O6 H1O6 107.6(18) . . ?
Na2 O6 H2O6 140.0(14) 2_565 . ?
Na2 O6 H2O6 94.5(15) . . ?
H1O6 O6 H2O6 104(2) . . ?
H1O7 O7 H2O7 106(2) . . ?
H1O8 O8 H2O8 106(3) . . ?
O2 Na1 O3 87.84(5) . . ?
O2 Na1 O11 159.16(5) . . ?
O3 Na1 O11 102.31(5) . . ?
O2 Na1 O5 87.33(5) . 2_665 ?
O3 Na1 O5 105.56(5) . 2_665 ?
O11 Na1 O5 106.96(5) . 2_665 ?
O2 Na1 O2 82.89(4) . 2_675 ?
O3 Na1 O2 165.81(5) . 2_675 ?
O11 Na1 O2 83.40(4) . 2_675 ?
O5 Na1 O2 84.78(4) 2_665 2_675 ?
O2 Na1 O1 84.31(4) . . ?
O3 Na1 O1 80.66(4) . . ?
O11 Na1 O1 79.53(4) . . ?
O5 Na1 O1 169.40(5) 2_665 . ?
O2 Na1 O1 87.73(4) 2_675 . ?
O2 Na1 Na1 42.97(3) . 2_675 ?
O3 Na1 Na1 129.91(4) . 2_675 ?
O11 Na1 Na1 121.70(4) . 2_675 ?
O5 Na1 Na1 84.68(4) 2_665 2_675 ?
O2 Na1 Na1 39.92(3) 2_675 2_675 ?
O1 Na1 Na1 84.76(4) . 2_675 ?
O2 Na1 Na2 77.40(3) . . ?
O3 Na1 Na2 30.66(3) . . ?
O11 Na1 Na2 120.12(3) . . ?
O5 Na1 Na2 76.32(3) 2_665 . ?
O2 Na1 Na2 153.15(3) 2_675 . ?
O1 Na1 Na2 108.04(3) . . ?
Na1 Na1 Na2 118.15(3) 2_675 . ?
O2 Na1 H2O1 95.0(5) . . ?
O3 Na1 H2O1 96.5(5) . . ?
O11 Na1 H2O1 66.0(5) . . ?
O5 Na1 H2O1 157.8(5) 2_665 . ?
O2 Na1 H2O1 73.7(5) 2_675 . ?
O1 Na1 H2O1 18.9(5) . . ?
Na1 Na1 H2O1 82.2(4) 2_675 . ?
Na2 Na1 H2O1 125.7(5) . . ?
O2 Na1 H2O3 104.6(5) . . ?
O3 Na1 H2O3 18.5(5) . . ?
O11 Na1 H2O3 83.9(5) . . ?
O5 Na1 H2O3 113.6(5) 2_665 . ?
O2 Na1 H2O3 160.1(5) 2_675 . ?
O1 Na1 H2O3 74.9(5) . . ?
Na1 Na1 H2O3 143.9(5) 2_675 . ?
Na2 Na1 H2O3 45.7(5) . . ?
H2O1 Na1 H2O3 87.1(7) . . ?
O3 Na2 O4 105.87(5) . . ?
O3 Na2 O6 97.27(5) . 2_565 ?
O4 Na2 O6 101.33(5) . 2_565 ?
O3 Na2 O5 171.94(5) . . ?
O4 Na2 O5 82.14(5) . . ?
O6 Na2 O5 79.97(4) 2_565 . ?
O3 Na2 O4 87.98(5) . 2_665 ?
O4 Na2 O4 86.01(5) . 2_665 ?
O6 Na2 O4 169.36(5) 2_565 2_665 ?
O5 Na2 O4 93.57(5) . 2_665 ?
O3 Na2 O6 80.82(4) . . ?
O4 Na2 O6 168.28(5) . . ?
O6 Na2 O6 87.10(4) 2_565 . ?
O5 Na2 O6 91.45(5) . . ?
O4 Na2 O6 84.60(4) 2_665 . ?
O3 Na2 Na2 99.20(4) . 2_665 ?
O4 Na2 Na2 43.77(3) . 2_665 ?
O6 Na2 Na2 144.48(4) 2_565 2_665 ?
O5 Na2 Na2 87.19(3) . 2_665 ?
O4 Na2 Na2 42.24(3) 2_665 2_665 ?
O6 Na2 Na2 126.48(4) . 2_665 ?
O3 Na2 Na2 88.28(4) . 2_565 ?
O4 Na2 Na2 146.13(4) . 2_565 ?
O6 Na2 Na2 45.55(3) 2_565 2_565 ?
O5 Na2 Na2 84.40(4) . 2_565 ?
O4 Na2 Na2 125.84(4) 2_665 2_565 ?
O6 Na2 Na2 41.56(3) . 2_565 ?
Na2 Na2 Na2 164.92(4) 2_665 2_565 ?
O3 Na2 Na1 30.80(3) . . ?
O4 Na2 Na1 79.01(3) . . ?
O6 Na2 Na1 117.58(4) 2_565 . ?
O5 Na2 Na1 156.38(4) . . ?
O4 Na2 Na1 71.14(3) 2_665 . ?
O6 Na2 Na1 104.45(3) . . ?
Na2 Na2 Na1 69.349(19) 2_665 . ?
Na2 Na2 Na1 119.07(2) 2_565 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -0.2(2) . . . . ?
C5 N1 C1 C6 177.70(11) . . . . ?
N1 C1 C6 O11 -179.71(12) . . . . ?
C2 C1 C6 O11 -1.7(2) . . . . ?
N1 C1 C6 N2 -1.65(18) . . . . ?
C2 C1 C6 N2 176.34(13) . . . . ?
N2 C6 O11 Na1 -6.3(3) . . . . ?
C1 C6 O11 Na1 171.53(10) . . . . ?
O11 C6 N2 O12 2.7(2) . . . . ?
C1 C6 N2 O12 -175.30(11) . . . . ?
N1 C1 C2 C3 0.5(2) . . . . ?
C6 C1 C2 C3 -177.34(13) . . . . ?
C1 C2 C3 C4 -0.5(2) . . . . ?
C2 C3 C4 C5 0.2(2) . . . . ?
C1 N1 C5 C4 -0.1(2) . . . . ?
C1 N1 C5 C7 179.04(11) . . . . ?
C3 C4 C5 N1 0.1(2) . . . . ?
C3 C4 C5 C7 -178.99(13) . . . . ?
N1 C5 C7 O9 -178.51(12) . . . . ?
C4 C5 C7 O9 0.7(2) . . . . ?
N1 C5 C7 N3 -0.94(18) . . . . ?
C4 C5 C7 N3 178.24(13) . . . . ?
O9 C7 N3 O10 3.9(2) . . . . ?
C5 C7 N3 O10 -173.63(12) . . . . ?
Na1 O2 Na1 O3 169.23(5) 2_675 . . . ?
Na1 O2 Na1 O11 49.20(14) 2_675 . . . ?
Na1 O2 Na1 O5 -85.07(5) 2_675 . . 2_665 ?
Na1 O2 Na1 O2 0.000(2) 2_675 . . 2_675 ?
Na1 O2 Na1 O1 88.41(5) 2_675 . . . ?
Na1 O2 Na1 Na2 -161.65(4) 2_675 . . . ?
Na2 O3 Na1 O2 68.63(7) . . . . ?
Na2 O3 Na1 O11 -129.74(6) . . . . ?
Na2 O3 Na1 O5 -17.99(8) . . . 2_665 ?
Na2 O3 Na1 O2 117.75(17) . . . 2_675 ?
Na2 O3 Na1 O1 153.22(7) . . . . ?
Na2 O3 Na1 Na1 78.19(8) . . . 2_675 ?
C6 O11 Na1 O2 -2.1(2) . . . . ?
C6 O11 Na1 O3 -119.76(16) . . . . ?
C6 O11 Na1 O5 129.53(16) . . . 2_665 ?
C6 O11 Na1 O2 47.06(16) . . . 2_675 ?
C6 O11 Na1 O1 -41.83(16) . . . . ?
C6 O11 Na1 Na1 35.27(18) . . . 2_675 ?
C6 O11 Na1 Na2 -146.72(15) . . . . ?
Na1 O3 Na2 O4 -30.22(7) . . . . ?
Na1 O3 Na2 O6 -134.23(6) . . . 2_565 ?
Na1 O3 Na2 O5 156.3(3) . . . . ?
Na1 O3 Na2 O4 55.05(6) . . . 2_665 ?
Na1 O3 Na2 O6 139.91(7) . . . . ?
Na1 O3 Na2 Na2 14.18(7) . . . 2_665 ?
Na1 O3 Na2 Na2 -178.99(6) . . . 2_565 ?
Na2 O4 Na2 O3 86.76(5) 2_665 . . . ?
Na2 O4 Na2 O6 -172.22(5) 2_665 . . 2_565 ?
Na2 O4 Na2 O5 -94.16(5) 2_665 . . . ?
Na2 O4 Na2 O4 0.000(2) 2_665 . . 2_665 ?
Na2 O4 Na2 O6 -36.8(2) 2_665 . . . ?
Na2 O4 Na2 Na2 -161.68(7) 2_665 . . 2_565 ?
Na2 O4 Na2 Na1 71.54(3) 2_665 . . . ?
Na1 O5 Na2 O3 -137.2(3) 2_665 . . . ?
Na1 O5 Na2 O4 49.10(7) 2_665 . . . ?
Na1 O5 Na2 O6 152.16(8) 2_665 . . 2_565 ?
Na1 O5 Na2 O4 -36.36(8) 2_665 . . 2_665 ?
Na1 O5 Na2 O6 -121.04(7) 2_665 . . . ?
Na1 O5 Na2 Na2 5.41(7) 2_665 . . 2_665 ?
Na1 O5 Na2 Na2 -162.05(7) 2_665 . . 2_565 ?
Na1 O5 Na2 Na1 11.87(16) 2_665 . . . ?
Na2 O6 Na2 O3 97.85(5) 2_565 . . . ?
Na2 O6 Na2 O4 -136.4(2) 2_565 . . . ?
Na2 O6 Na2 O6 0.0 2_565 . . 2_565 ?
Na2 O6 Na2 O5 -79.88(5) 2_565 . . . ?
Na2 O6 Na2 O4 -173.33(5) 2_565 . . 2_665 ?
Na2 O6 Na2 Na2 -167.46(5) 2_565 . . 2_665 ?
Na2 O6 Na2 Na1 117.75(4) 2_565 . . . ?
O2 Na1 Na2 O3 -107.53(7) . . . . ?
O11 Na1 Na2 O3 60.29(7) . . . . ?
O5 Na1 Na2 O3 162.17(8) 2_665 . . . ?
O2 Na1 Na2 O3 -151.29(10) 2_675 . . . ?
O1 Na1 Na2 O3 -27.88(7) . . . . ?
Na1 Na1 Na2 O3 -121.62(7) 2_675 . . . ?
O2 Na1 Na2 O4 42.92(4) . . . . ?
O3 Na1 Na2 O4 150.45(7) . . . . ?
O11 Na1 Na2 O4 -149.25(5) . . . . ?
O5 Na1 Na2 O4 -47.38(5) 2_665 . . . ?
O2 Na1 Na2 O4 -0.84(8) 2_675 . . . ?
O1 Na1 Na2 O4 122.58(4) . . . . ?
Na1 Na1 Na2 O4 28.83(4) 2_675 . . . ?
O2 Na1 Na2 O6 -54.22(5) . . . 2_565 ?
O3 Na1 Na2 O6 53.31(7) . . . 2_565 ?
O11 Na1 Na2 O6 113.60(5) . . . 2_565 ?
O5 Na1 Na2 O6 -144.52(5) 2_665 . . 2_565 ?
O2 Na1 Na2 O6 -97.98(8) 2_675 . . 2_565 ?
O1 Na1 Na2 O6 25.43(5) . . . 2_565 ?
Na1 Na1 Na2 O6 -68.31(5) 2_675 . . 2_565 ?
O2 Na1 Na2 O5 80.55(10) . . . . ?
O3 Na1 Na2 O5 -171.92(12) . . . . ?
O11 Na1 Na2 O5 -111.63(10) . . . . ?
O5 Na1 Na2 O5 -9.75(13) 2_665 . . . ?
O2 Na1 Na2 O5 36.79(13) 2_675 . . . ?
O1 Na1 Na2 O5 160.20(10) . . . . ?
Na1 Na1 Na2 O5 66.46(10) 2_675 . . . ?
O2 Na1 Na2 O4 132.43(5) . . . 2_665 ?
O3 Na1 Na2 O4 -120.04(7) . . . 2_665 ?
O11 Na1 Na2 O4 -59.75(5) . . . 2_665 ?
O5 Na1 Na2 O4 42.13(5) 2_665 . . 2_665 ?
O2 Na1 Na2 O4 88.67(8) 2_675 . . 2_665 ?
O1 Na1 Na2 O4 -147.92(4) . . . 2_665 ?
Na1 Na1 Na2 O4 118.34(4) 2_675 . . 2_665 ?
O2 Na1 Na2 O6 -148.57(4) . . . . ?
O3 Na1 Na2 O6 -41.04(7) . . . . ?
O11 Na1 Na2 O6 19.26(5) . . . . ?
O5 Na1 Na2 O6 121.14(5) 2_665 . . . ?
O2 Na1 Na2 O6 167.67(8) 2_675 . . . ?
O1 Na1 Na2 O6 -68.91(4) . . . . ?
Na1 Na1 Na2 O6 -162.65(4) 2_675 . . . ?
O2 Na1 Na2 Na2 87.45(4) . . . 2_665 ?
O3 Na1 Na2 Na2 -165.02(7) . . . 2_665 ?
O11 Na1 Na2 Na2 -104.73(4) . . . 2_665 ?
O5 Na1 Na2 Na2 -2.85(4) 2_665 . . 2_665 ?
O2 Na1 Na2 Na2 43.69(8) 2_675 . . 2_665 ?
O1 Na1 Na2 Na2 167.10(4) . . . 2_665 ?
Na1 Na1 Na2 Na2 73.36(3) 2_675 . . 2_665 ?
O2 Na1 Na2 Na2 -106.37(4) . . . 2_565 ?
O3 Na1 Na2 Na2 1.16(7) . . . 2_565 ?
O11 Na1 Na2 Na2 61.45(5) . . . 2_565 ?
O5 Na1 Na2 Na2 163.33(5) 2_665 . . 2_565 ?
O2 Na1 Na2 Na2 -150.13(7) 2_675 . . 2_565 ?
O1 Na1 Na2 Na2 -26.72(4) . . . 2_565 ?
Na1 Na1 Na2 Na2 -120.46(3) 2_675 . . 2_565 ?

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
O8 H2O8 O10 0.82(3) 2.03(3) 2.8401(19) 175(3) 2_576
O8 H1O8 O7 0.90(3) 2.09(3) 2.9839(19) 171(2) .
O7 H2O7 O11 0.84(3) 1.96(3) 2.8038(17) 178(2) .
O7 H1O7 O10 0.80(3) 1.99(3) 2.780(2) 169(3) 2_676
O6 H2O6 O12 0.87(3) 1.90(3) 2.7556(15) 168(2) 1_545
O6 H1O6 O10 0.84(3) 2.11(3) 2.9197(17) 161(2) 2_576
O5 H1O5 O10 0.79(3) 2.27(3) 3.0338(18) 163(3) 1_544
O4 H2O4 O7 0.81(3) 2.05(3) 2.8581(18) 173(2) 2_665
O4 H1O4 O12 0.87(2) 1.93(2) 2.7788(15) 164(2) 2_675
O3 H2O3 O9 0.84(2) 2.11(2) 2.8001(15) 139(2) 2_576
O3 H1O3 O1 0.91(3) 1.92(3) 2.8201(17) 168(3) 2_575
O2 H2O2 O12 0.84(2) 1.86(2) 2.6809(15) 168(2) 2_675
O2 H1O2 O9 0.83(2) 1.95(2) 2.7698(16) 171(2) 1_554
O1 H2O1 O12 0.85(2) 1.83(2) 2.6775(15) 172(2) .
O1 H1O1 O9 0.83(2) 2.01(2) 2.8436(16) 173(2) 2_576
N3 H1N3 O8 0.80(2) 2.25(2) 3.0210(19) 161.2(19) 1_565
N2 H1N2 O8 0.822(18) 2.214(19) 2.9833(18) 155.9(16) 1_565

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.060

#===END

data_nol21
_database_code_depnum_ccdc_archive 'CCDC 690289'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 N2 O8 Pd, 2 (H2 O)'
_chemical_formula_sum            'C14 H12 N2 O10 Pd'
_chemical_formula_weight         474.66

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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7526(8)
_cell_length_b                   10.2338(11)
_cell_length_c                   10.4818(11)
_cell_angle_alpha                85.176(2)
_cell_angle_beta                 88.064(2)
_cell_angle_gamma                73.046(2)
_cell_volume                     792.61(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5465
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      31.17

_exptl_crystal_description       yellow
_exptl_crystal_colour            plate
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             472
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_T_max  0.8865
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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            16408
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         30.00
_reflns_number_total             4567
_reflns_number_gt                4322
_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^)+(0.0379P)^2^+0.5329P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4567
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0690
_refine_ls_wR_factor_gt          0.0678
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001

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
O1 O 0.3136(2) 0.42390(17) 0.44904(15) 0.0182(3) Uani 1 1 d . . .
H1O1 H 0.374(5) 0.340(4) 0.438(3) 0.043(10) Uiso 1 1 d . . .
H2O1 H 0.363(5) 0.470(4) 0.419(3) 0.034(9) Uiso 1 1 d . . .
O2 O 0.6196(2) 0.02670(17) 0.12535(16) 0.0165(3) Uani 1 1 d . . .
H1O2 H 0.685(5) -0.044(4) 0.134(3) 0.038(10) Uiso 1 1 d . . .
H2O2 H 0.618(5) 0.052(4) 0.056(4) 0.037(10) Uiso 1 1 d . . .
Pd Pd 0.898269(17) 0.213109(13) 0.193560(13) 0.00993(5) Uani 1 1 d . . .
N1 N 0.8263(2) 0.39084(16) 0.08433(16) 0.0114(3) Uani 1 1 d . . .
C1 C 0.8960(2) 0.37620(19) -0.03514(18) 0.0120(3) Uani 1 1 d . . .
C6 C 1.0450(3) 0.24495(19) -0.04871(18) 0.0127(3) Uani 1 1 d . . .
O3 O 1.07975(19) 0.16204(15) 0.05335(13) 0.0145(3) Uani 1 1 d . . .
O4 O 1.1303(2) 0.22497(15) -0.14893(14) 0.0160(3) Uani 1 1 d . . .
C2 C 0.8412(3) 0.4764(2) -0.13415(19) 0.0138(3) Uani 1 1 d . . .
H2 H 0.893(4) 0.460(3) -0.210(3) 0.025(7) Uiso 1 1 d . . .
C3 C 0.7063(3) 0.5959(2) -0.1094(2) 0.0157(4) Uani 1 1 d . . .
H3 H 0.663(4) 0.662(3) -0.175(3) 0.019(7) Uiso 1 1 d . . .
C4 C 0.6384(3) 0.6126(2) 0.0142(2) 0.0145(4) Uani 1 1 d . . .
H4 H 0.548(4) 0.693(3) 0.040(3) 0.030(8) Uiso 1 1 d . . .
C5 C 0.7045(3) 0.5093(2) 0.11041(19) 0.0121(3) Uani 1 1 d . . .
C7 C 0.6471(3) 0.53354(19) 0.24733(19) 0.0131(3) Uani 1 1 d . . .
O5 O 0.7843(2) 0.50953(15) 0.32375(14) 0.0149(3) Uani 1 1 d . . .
H1O5 H 0.750(5) 0.522(4) 0.389(3) 0.038(10) Uiso 1 1 d . . .
O6 O 0.4892(2) 0.57685(16) 0.27638(15) 0.0179(3) Uani 1 1 d . . .
N2 N 0.9561(2) 0.03223(17) 0.29924(15) 0.0113(3) Uani 1 1 d . . .
C8 C 0.8202(3) 0.02466(19) 0.38047(18) 0.0123(3) Uani 1 1 d . . .
C13 C 0.6718(2) 0.15673(19) 0.38812(19) 0.0126(3) Uani 1 1 d . . .
O7 O 0.69490(19) 0.26044(14) 0.31819(14) 0.0146(3) Uani 1 1 d . . .
O8 O 0.5423(2) 0.16375(15) 0.46046(15) 0.0180(3) Uani 1 1 d . . .
C9 C 0.8204(3) -0.0931(2) 0.45527(19) 0.0136(3) Uani 1 1 d . . .
H9 H 0.722(3) -0.089(2) 0.508(2) 0.008(6) Uiso 1 1 d . . .
C10 C 0.9679(3) -0.2089(2) 0.44596(19) 0.0144(3) Uani 1 1 d . . .
H10 H 0.969(4) -0.286(3) 0.493(3) 0.017(7) Uiso 1 1 d . . .
C11 C 1.1086(3) -0.2011(2) 0.36403(19) 0.0138(3) Uani 1 1 d . . .
H11 H 1.215(4) -0.271(3) 0.355(3) 0.023(7) Uiso 1 1 d . . .
C12 C 1.0992(3) -0.07876(19) 0.29204(18) 0.0122(3) Uani 1 1 d . . .
C14 C 1.2553(2) -0.06820(19) 0.20628(18) 0.0130(3) Uani 1 1 d . . .
O9 O 1.3318(2) 0.01950(16) 0.24323(15) 0.0164(3) Uani 1 1 d . . .
H1O9 H 1.412(5) 0.020(3) 0.200(3) 0.033(9) Uiso 1 1 d . . .
O10 O 1.3006(2) -0.13996(15) 0.11686(15) 0.0174(3) Uani 1 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
O1 0.0167(7) 0.0173(7) 0.0169(7) -0.0027(6) 0.0057(6) 0.0003(6)
O2 0.0122(7) 0.0187(7) 0.0161(7) -0.0017(6) 0.0042(5) -0.0009(6)
Pd 0.00857(7) 0.00929(8) 0.01046(8) -0.00161(5) 0.00316(5) -0.00041(5)
N1 0.0102(7) 0.0112(7) 0.0121(7) -0.0026(5) 0.0029(6) -0.0019(6)
C1 0.0098(8) 0.0126(8) 0.0132(8) -0.0032(6) 0.0028(6) -0.0025(6)
C6 0.0125(8) 0.0124(8) 0.0132(8) -0.0037(6) 0.0015(7) -0.0030(6)
O3 0.0139(6) 0.0141(6) 0.0121(6) -0.0011(5) 0.0056(5) 0.0005(5)
O4 0.0165(7) 0.0172(7) 0.0128(6) -0.0036(5) 0.0042(5) -0.0026(5)
C2 0.0149(8) 0.0156(9) 0.0110(8) -0.0026(7) 0.0008(7) -0.0043(7)
C3 0.0157(9) 0.0145(9) 0.0154(9) 0.0001(7) -0.0015(7) -0.0020(7)
C4 0.0124(8) 0.0126(8) 0.0172(9) -0.0020(7) -0.0001(7) -0.0012(7)
C5 0.0095(8) 0.0125(8) 0.0140(8) -0.0024(6) 0.0021(6) -0.0025(6)
C7 0.0139(8) 0.0098(8) 0.0139(8) -0.0021(6) 0.0041(7) -0.0011(6)
O5 0.0142(6) 0.0172(7) 0.0125(7) -0.0037(5) 0.0031(5) -0.0028(5)
O6 0.0131(7) 0.0178(7) 0.0187(7) -0.0020(5) 0.0049(5) 0.0015(5)
N2 0.0099(7) 0.0121(7) 0.0110(7) -0.0029(5) 0.0028(6) -0.0018(6)
C8 0.0112(8) 0.0125(8) 0.0125(8) -0.0035(6) 0.0023(6) -0.0021(6)
C13 0.0096(8) 0.0123(8) 0.0149(8) -0.0028(6) 0.0024(6) -0.0015(6)
O7 0.0120(6) 0.0125(6) 0.0171(7) -0.0012(5) 0.0064(5) -0.0007(5)
O8 0.0130(6) 0.0162(7) 0.0229(7) -0.0024(6) 0.0085(6) -0.0020(5)
C9 0.0124(8) 0.0147(9) 0.0137(8) -0.0018(7) 0.0025(7) -0.0039(7)
C10 0.0154(9) 0.0122(8) 0.0153(9) -0.0004(7) 0.0018(7) -0.0037(7)
C11 0.0134(8) 0.0123(8) 0.0139(9) -0.0029(7) 0.0010(7) -0.0004(7)
C12 0.0107(8) 0.0122(8) 0.0122(8) -0.0036(6) 0.0023(6) -0.0008(6)
C14 0.0102(8) 0.0124(8) 0.0131(8) 0.0005(6) 0.0016(6) 0.0013(6)
O9 0.0113(6) 0.0226(7) 0.0156(7) -0.0035(5) 0.0048(5) -0.0052(6)
O10 0.0190(7) 0.0140(7) 0.0162(7) -0.0034(5) 0.0069(5) -0.0003(5)

_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
O1 H1O1 0.86(4) . ?
O1 H2O1 0.74(4) . ?
O2 H1O2 0.75(4) . ?
O2 H2O2 0.75(4) . ?
Pd O7 1.9872(14) . ?
Pd O3 1.9933(14) . ?
Pd N1 2.0078(16) . ?
Pd N2 2.0147(16) . ?
N1 C5 1.344(2) . ?
N1 C1 1.350(2) . ?
C1 C2 1.381(3) . ?
C1 C6 1.508(3) . ?
C6 O4 1.222(2) . ?
C6 O3 1.292(2) . ?
C2 C3 1.395(3) . ?
C2 H2 0.88(3) . ?
C3 C4 1.386(3) . ?
C3 H3 0.92(3) . ?
C4 C5 1.392(3) . ?
C4 H4 0.96(3) . ?
C5 C7 1.507(3) . ?
C7 O6 1.212(2) . ?
C7 O5 1.306(2) . ?
O5 H1O5 0.73(4) . ?
N2 C12 1.342(2) . ?
N2 C8 1.348(2) . ?
C8 C9 1.381(3) . ?
C8 C13 1.504(3) . ?
C13 O8 1.226(2) . ?
C13 O7 1.291(2) . ?
C9 C10 1.394(3) . ?
C9 H9 0.92(2) . ?
C10 C11 1.382(3) . ?
C10 H10 0.89(3) . ?
C11 C12 1.391(3) . ?
C11 H11 0.93(3) . ?
C12 C14 1.507(3) . ?
C14 O10 1.218(2) . ?
C14 O9 1.300(2) . ?
O9 H1O9 0.76(3) . ?

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
H1O1 O1 H2O1 109(4) . . ?
H1O2 O2 H2O2 109(4) . . ?
O7 Pd O3 172.73(6) . . ?
O7 Pd N1 96.62(6) . . ?
O3 Pd N1 81.71(6) . . ?
O7 Pd N2 81.95(6) . . ?
O3 Pd N2 99.28(6) . . ?
N1 Pd N2 176.28(6) . . ?
C5 N1 C1 119.31(16) . . ?
C5 N1 Pd 128.44(13) . . ?
C1 N1 Pd 111.57(12) . . ?
N1 C1 C2 122.47(17) . . ?
N1 C1 C6 114.17(16) . . ?
C2 C1 C6 123.28(17) . . ?
O4 C6 O3 123.91(18) . . ?
O4 C6 C1 120.55(17) . . ?
O3 C6 C1 115.44(16) . . ?
C6 O3 Pd 113.89(12) . . ?
C1 C2 C3 118.32(18) . . ?
C1 C2 H2 117.8(19) . . ?
C3 C2 H2 123.9(19) . . ?
C4 C3 C2 119.16(18) . . ?
C4 C3 H3 121.0(18) . . ?
C2 C3 H3 119.8(18) . . ?
C3 C4 C5 119.42(18) . . ?
C3 C4 H4 124.3(19) . . ?
C5 C4 H4 116.3(19) . . ?
N1 C5 C4 121.09(18) . . ?
N1 C5 C7 119.24(17) . . ?
C4 C5 C7 119.57(17) . . ?
O6 C7 O5 126.45(19) . . ?
O6 C7 C5 121.04(18) . . ?
O5 C7 C5 112.42(16) . . ?
C7 O5 H1O5 109(3) . . ?
C12 N2 C8 118.66(17) . . ?
C12 N2 Pd 129.37(13) . . ?
C8 N2 Pd 111.77(12) . . ?
N2 C8 C9 122.88(17) . . ?
N2 C8 C13 114.70(16) . . ?
C9 C8 C13 122.36(17) . . ?
O8 C13 O7 123.50(18) . . ?
O8 C13 C8 120.93(18) . . ?
O7 C13 C8 115.51(16) . . ?
C13 O7 Pd 114.28(12) . . ?
C8 C9 C10 118.33(18) . . ?
C8 C9 H9 117.2(15) . . ?
C10 C9 H9 124.4(15) . . ?
C11 C10 C9 119.00(18) . . ?
C11 C10 H10 121.8(18) . . ?
C9 C10 H10 119.2(18) . . ?
C10 C11 C12 119.40(18) . . ?
C10 C11 H11 125.1(18) . . ?
C12 C11 H11 115.5(18) . . ?
N2 C12 C11 121.70(18) . . ?
N2 C12 C14 118.68(17) . . ?
C11 C12 C14 119.59(17) . . ?
O10 C14 O9 127.18(19) . . ?
O10 C14 C12 120.75(18) . . ?
O9 C14 C12 112.03(16) . . ?
C14 O9 H1O9 110(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Pd N1 C5 13.43(17) . . . . ?
O3 Pd N1 C5 -173.71(17) . . . . ?
N2 Pd N1 C5 80.6(10) . . . . ?
O7 Pd N1 C1 -156.91(13) . . . . ?
O3 Pd N1 C1 15.96(13) . . . . ?
N2 Pd N1 C1 -89.7(9) . . . . ?
C5 N1 C1 C2 -3.0(3) . . . . ?
Pd N1 C1 C2 168.33(15) . . . . ?
C5 N1 C1 C6 173.87(17) . . . . ?
Pd N1 C1 C6 -14.81(19) . . . . ?
N1 C1 C6 O4 -173.38(18) . . . . ?
C2 C1 C6 O4 3.5(3) . . . . ?
N1 C1 C6 O3 3.1(2) . . . . ?
C2 C1 C6 O3 179.92(18) . . . . ?
O4 C6 O3 Pd -173.10(16) . . . . ?
C1 C6 O3 Pd 10.6(2) . . . . ?
O7 Pd O3 C6 62.5(5) . . . . ?
N1 Pd O3 C6 -14.68(13) . . . . ?
N2 Pd O3 C6 161.69(13) . . . . ?
N1 C1 C2 C3 -1.2(3) . . . . ?
C6 C1 C2 C3 -177.77(18) . . . . ?
C1 C2 C3 C4 3.0(3) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C1 N1 C5 C4 5.3(3) . . . . ?
Pd N1 C5 C4 -164.36(15) . . . . ?
C1 N1 C5 C7 -171.13(17) . . . . ?
Pd N1 C5 C7 19.2(3) . . . . ?
C3 C4 C5 N1 -3.4(3) . . . . ?
C3 C4 C5 C7 172.99(18) . . . . ?
N1 C5 C7 O6 -133.0(2) . . . . ?
C4 C5 C7 O6 50.5(3) . . . . ?
N1 C5 C7 O5 50.2(2) . . . . ?
C4 C5 C7 O5 -126.28(19) . . . . ?
O7 Pd N2 C12 -174.32(18) . . . . ?
O3 Pd N2 C12 12.92(18) . . . . ?
N1 Pd N2 C12 118.0(9) . . . . ?
O7 Pd N2 C8 10.99(13) . . . . ?
O3 Pd N2 C8 -161.77(13) . . . . ?
N1 Pd N2 C8 -56.6(10) . . . . ?
C12 N2 C8 C9 -1.1(3) . . . . ?
Pd N2 C8 C9 174.25(15) . . . . ?
C12 N2 C8 C13 176.15(16) . . . . ?
Pd N2 C8 C13 -8.5(2) . . . . ?
N2 C8 C13 O8 -178.59(18) . . . . ?
C9 C8 C13 O8 -1.4(3) . . . . ?
N2 C8 C13 O7 -1.3(3) . . . . ?
C9 C8 C13 O7 175.98(18) . . . . ?
O8 C13 O7 Pd -172.05(16) . . . . ?
C8 C13 O7 Pd 10.7(2) . . . . ?
O3 Pd O7 C13 88.2(4) . . . . ?
N1 Pd O7 C13 164.46(14) . . . . ?
N2 Pd O7 C13 -12.08(14) . . . . ?
N2 C8 C9 C10 0.0(3) . . . . ?
C13 C8 C9 C10 -177.04(18) . . . . ?
C8 C9 C10 C11 0.9(3) . . . . ?
C9 C10 C11 C12 -0.6(3) . . . . ?
C8 N2 C12 C11 1.3(3) . . . . ?
Pd N2 C12 C11 -173.05(14) . . . . ?
C8 N2 C12 C14 -176.92(17) . . . . ?
Pd N2 C12 C14 8.7(3) . . . . ?
C10 C11 C12 N2 -0.5(3) . . . . ?
C10 C11 C12 C14 177.74(18) . . . . ?
N2 C12 C14 O10 -119.0(2) . . . . ?
C11 C12 C14 O10 62.7(3) . . . . ?
N2 C12 C14 O9 63.2(2) . . . . ?
C11 C12 C14 O9 -115.1(2) . . . . ?

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
O1 H1O1 O8 0.86(4) 1.89(4) 2.730(2) 162(3) .
O1 H2O1 O6 0.74(4) 2.15(4) 2.860(2) 162(4) .
O2 H1O2 O4 0.75(4) 1.98(4) 2.733(2) 176(4) 2_755
O2 H2O2 O10 0.75(4) 2.11(4) 2.826(2) 159(4) 2_755
O5 H1O5 O1 0.73(4) 1.84(4) 2.561(2) 170(4) 2_666
O9 H1O9 O2 0.76(3) 1.78(4) 2.531(2) 170(4) 1_655

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.116

#===END

data_nol24
_database_code_depnum_ccdc_archive 'CCDC 690290'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H7 N3 O4'
_chemical_formula_weight         197.16
_chemical_absolute_configuration unk

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   4.9425(5)
_cell_length_b                   9.6524(9)
_cell_length_c                   15.7170(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     749.81(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9425
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      31.79

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             408
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8374
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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            16788
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         31.97
_reflns_number_total             1485
_reflns_number_gt                1435
_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^)+(0.0639P)^2^+0.2310P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1485
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.003

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
N1 N 0.3276(3) 0.86271(12) 0.33818(7) 0.0094(2) Uani 1 1 d . . .
C1 C 0.5153(3) 0.86983(13) 0.39926(8) 0.0090(2) Uani 1 1 d . . .
C6 C 0.5062(3) 0.98980(13) 0.45978(8) 0.0094(2) Uani 1 1 d . . .
O1 O 0.6723(2) 0.99829(10) 0.51854(7) 0.0133(2) Uani 1 1 d . . .
N2 N 0.3030(3) 1.07763(12) 0.44807(7) 0.0112(2) Uani 1 1 d . . .
H1N2 H 0.194(6) 1.085(2) 0.4059(15) 0.021(6) Uiso 1 1 d . . .
O2 O 0.2655(2) 1.18215(11) 0.50793(7) 0.0125(2) Uani 1 1 d . . .
H1O2 H 0.393(7) 1.231(3) 0.506(2) 0.037(8) Uiso 1 1 d . . .
C2 C 0.7094(3) 0.76841(14) 0.41313(8) 0.0108(2) Uani 1 1 d . . .
H2 H 0.835(5) 0.779(2) 0.4554(13) 0.011(5) Uiso 1 1 d . . .
C3 C 0.7041(3) 0.65069(15) 0.36256(9) 0.0121(3) Uani 1 1 d . . .
H3 H 0.826(6) 0.579(2) 0.3712(14) 0.024(6) Uiso 1 1 d . . .
C4 C 0.5118(3) 0.64100(14) 0.29875(9) 0.0110(2) Uani 1 1 d . . .
H4 H 0.502(5) 0.565(2) 0.2632(13) 0.014(5) Uiso 1 1 d . . .
C5 C 0.3298(3) 0.74946(13) 0.28875(8) 0.0092(2) Uani 1 1 d . . .
C7 C 0.1195(3) 0.73882(14) 0.22055(8) 0.0100(2) Uani 1 1 d . . .
O3 O 0.0898(2) 0.63074(11) 0.17904(7) 0.0135(2) Uani 1 1 d . . .
N3 N -0.0251(3) 0.85432(13) 0.20957(7) 0.0112(2) Uani 1 1 d . . .
H1N3 H -0.013(6) 0.918(2) 0.2434(15) 0.023(6) Uiso 1 1 d . . .
O4 O -0.2519(2) 0.84890(11) 0.15754(7) 0.0122(2) Uani 1 1 d . . .
H1O4 H -0.215(6) 0.892(3) 0.1146(16) 0.026(6) Uiso 1 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
N1 0.0107(5) 0.0087(5) 0.0088(5) -0.0005(4) -0.0010(4) -0.0003(4)
C1 0.0103(6) 0.0082(5) 0.0085(5) -0.0005(4) -0.0002(5) -0.0003(5)
C6 0.0105(5) 0.0079(5) 0.0097(5) -0.0002(4) 0.0014(5) -0.0004(5)
O1 0.0137(5) 0.0148(5) 0.0115(4) -0.0036(3) -0.0033(4) 0.0020(4)
N2 0.0130(5) 0.0107(5) 0.0100(5) -0.0037(4) -0.0025(4) 0.0022(5)
O2 0.0137(5) 0.0097(4) 0.0140(4) -0.0053(3) -0.0002(4) 0.0004(4)
C2 0.0114(6) 0.0117(5) 0.0093(5) -0.0009(4) -0.0008(5) 0.0009(5)
C3 0.0135(6) 0.0106(5) 0.0124(6) 0.0000(5) 0.0004(5) 0.0032(5)
C4 0.0131(6) 0.0094(5) 0.0106(5) -0.0006(4) 0.0013(5) 0.0012(5)
C5 0.0100(5) 0.0088(5) 0.0089(5) -0.0002(4) -0.0004(4) -0.0007(5)
C7 0.0107(6) 0.0107(6) 0.0086(5) 0.0013(4) 0.0001(5) -0.0010(5)
O3 0.0150(5) 0.0120(5) 0.0137(4) -0.0038(3) -0.0027(4) 0.0002(4)
N3 0.0138(5) 0.0100(5) 0.0099(5) -0.0010(4) -0.0031(4) 0.0005(5)
O4 0.0118(5) 0.0145(4) 0.0103(4) 0.0028(3) -0.0026(4) -0.0019(4)

_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
N1 C1 1.3366(17) . ?
N1 C5 1.3412(16) . ?
C1 C2 1.3880(19) . ?
C1 C6 1.4992(18) . ?
C6 O1 1.2385(17) . ?
C6 N2 1.3272(18) . ?
N2 O2 1.3919(15) . ?
N2 H1N2 0.86(3) . ?
O2 H1O2 0.79(4) . ?
C2 C3 1.3869(19) . ?
C2 H2 0.92(2) . ?
C3 C4 1.385(2) . ?
C3 H3 0.93(3) . ?
C4 C5 1.3890(19) . ?
C4 H4 0.93(2) . ?
C5 C7 1.4967(19) . ?
C7 O3 1.2391(17) . ?
C7 N3 1.3354(18) . ?
N3 O4 1.3886(16) . ?
N3 H1N3 0.81(2) . ?
O4 H1O4 0.81(3) . ?

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
C1 N1 C5 116.89(12) . . ?
N1 C1 C2 123.80(12) . . ?
N1 C1 C6 118.33(12) . . ?
C2 C1 C6 117.76(12) . . ?
O1 C6 N2 124.25(13) . . ?
O1 C6 C1 120.29(12) . . ?
N2 C6 C1 115.35(12) . . ?
C6 N2 O2 118.04(12) . . ?
C6 N2 H1N2 129.6(16) . . ?
O2 N2 H1N2 112.2(16) . . ?
N2 O2 H1O2 108(2) . . ?
C3 C2 C1 118.35(13) . . ?
C3 C2 H2 121.2(14) . . ?
C1 C2 H2 120.4(14) . . ?
C4 C3 C2 118.89(13) . . ?
C4 C3 H3 120.0(15) . . ?
C2 C3 H3 121.1(15) . . ?
C3 C4 C5 118.39(13) . . ?
C3 C4 H4 121.7(16) . . ?
C5 C4 H4 119.9(16) . . ?
N1 C5 C4 123.64(13) . . ?
N1 C5 C7 117.73(12) . . ?
C4 C5 C7 118.62(12) . . ?
O3 C7 N3 124.85(13) . . ?
O3 C7 C5 121.14(12) . . ?
N3 C7 C5 114.01(12) . . ?
C7 N3 O4 118.46(11) . . ?
C7 N3 H1N3 120.4(19) . . ?
O4 N3 H1N3 118(2) . . ?
N3 O4 H1O4 106.7(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.6(2) . . . . ?
C5 N1 C1 C6 -175.56(12) . . . . ?
N1 C1 C6 O1 178.18(13) . . . . ?
C2 C1 C6 O1 1.8(2) . . . . ?
N1 C1 C6 N2 1.85(18) . . . . ?
C2 C1 C6 N2 -174.53(13) . . . . ?
O1 C6 N2 O2 -3.3(2) . . . . ?
C1 C6 N2 O2 172.84(11) . . . . ?
N1 C1 C2 C3 -2.1(2) . . . . ?
C6 C1 C2 C3 174.10(12) . . . . ?
C1 C2 C3 C4 2.0(2) . . . . ?
C2 C3 C4 C5 -0.7(2) . . . . ?
C1 N1 C5 C4 0.9(2) . . . . ?
C1 N1 C5 C7 179.39(12) . . . . ?
C3 C4 C5 N1 -0.8(2) . . . . ?
C3 C4 C5 C7 -179.31(12) . . . . ?
N1 C5 C7 O3 -171.68(13) . . . . ?
C4 C5 C7 O3 6.9(2) . . . . ?
N1 C5 C7 N3 8.74(18) . . . . ?
C4 C5 C7 N3 -172.70(13) . . . . ?
O3 C7 N3 O4 10.3(2) . . . . ?
C5 C7 N3 O4 -170.11(11) . . . . ?

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
O4 H1O4 O1 0.81(3) 1.86(3) 2.6652(15) 172(3) 2_574
N2 H1N2 O3 0.86(3) 1.99(3) 2.8325(17) 169(2) 3
O2 H1O2 O2 0.79(4) 2.04(4) 2.8080(11) 167(3) 4_576

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        31.97
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.066

#===END

data_nol32
_database_code_depnum_ccdc_archive 'CCDC 690291'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 N O8 Pt, 2 (H2 O)'
_chemical_formula_sum            'C14 H12 N2 O10 Pt'
_chemical_formula_weight         563.35

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8165(11)
_cell_length_b                   10.2605(15)
_cell_length_c                   10.4094(15)
_cell_angle_alpha                84.536(3)
_cell_angle_beta                 88.206(3)
_cell_angle_gamma                72.512(3)
_cell_volume                     792.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5442
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      28.13

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    8.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5510
_exptl_absorpt_correction_T_max  0.8418
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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            18597
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         31.65
_reflns_number_total             4957
_reflns_number_gt                4429
_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^)+(0.0437P)^2^+0.6863P] 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         4957
_refine_ls_number_parameters     258
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_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
O1 O 0.3159(5) 0.4239(4) 0.4495(3) 0.0162(7) Uani 1 1 d D . .
H1O1 H 0.390(7) 0.345(3) 0.458(7) 0.024 Uiso 1 1 d D . .
H2O1 H 0.365(8) 0.481(5) 0.417(6) 0.024 Uiso 1 1 d D . .
O2 O 0.6160(5) 0.0204(4) 0.1265(4) 0.0159(7) Uani 1 1 d D . .
H1O2 H 0.684(7) -0.060(3) 0.130(6) 0.024 Uiso 1 1 d D . .
H2O2 H 0.637(9) 0.058(6) 0.056(4) 0.024 Uiso 1 1 d D . .
Pt Pt 0.89552(2) 0.213148(17) 0.191138(16) 0.00909(6) Uani 1 1 d U . .
N1 N 0.8238(5) 0.3915(4) 0.0810(4) 0.0110(7) Uani 1 1 d U . .
C1 C 0.8970(5) 0.3837(5) -0.0349(4) 0.0102(8) Uani 1 1 d U . .
C6 C 1.0444(6) 0.2489(5) -0.0521(5) 0.0116(8) Uani 1 1 d U . .
O3 O 1.0787(5) 0.1646(4) 0.0506(3) 0.0143(7) Uani 1 1 d U . .
O4 O 1.1308(5) 0.2297(4) -0.1526(3) 0.0159(7) Uani 1 1 d U . .
C2 C 0.8431(7) 0.4824(5) -0.1381(5) 0.0138(9) Uani 1 1 d U . .
H2 H 0.8953 0.4695 -0.2214 0.017 Uiso 1 1 calc R . .
C3 C 0.7074(7) 0.6025(5) -0.1131(5) 0.0159(9) Uani 1 1 d U . .
H3 H 0.6637 0.6736 -0.1799 0.019 Uiso 1 1 calc R . .
C4 C 0.6381(7) 0.6155(5) 0.0108(5) 0.0152(9) Uani 1 1 d U . .
H4 H 0.5466 0.6962 0.0297 0.018 Uiso 1 1 calc R . .
C5 C 0.7027(6) 0.5103(5) 0.1068(5) 0.0126(8) Uani 1 1 d U . .
C7 C 0.6438(7) 0.5330(5) 0.2449(5) 0.0138(8) Uani 1 1 d U . .
O5 O 0.7783(5) 0.5096(4) 0.3227(3) 0.0150(7) Uani 1 1 d U . .
H1O5 H 0.7399 0.5291 0.3969 0.023 Uiso 1 1 calc R . .
O6 O 0.4859(5) 0.5757(4) 0.2726(4) 0.0201(8) Uani 1 1 d U . .
N2 N 0.9524(5) 0.0327(4) 0.2970(4) 0.0105(7) Uani 1 1 d U . .
C8 C 0.8228(7) 0.0221(5) 0.3821(4) 0.0130(8) Uani 1 1 d U . .
C13 C 0.6710(6) 0.1551(5) 0.3881(5) 0.0137(8) Uani 1 1 d U . .
O7 O 0.6931(4) 0.2589(3) 0.3174(3) 0.0142(7) Uani 1 1 d U . .
O8 O 0.5426(5) 0.1623(4) 0.4614(4) 0.0170(7) Uani 1 1 d U . .
C9 C 0.8227(6) -0.0946(5) 0.4575(5) 0.0133(8) Uani 1 1 d U . .
H9 H 0.7257 -0.0967 0.5141 0.016 Uiso 1 1 calc R . .
C10 C 0.9703(7) -0.2103(5) 0.4482(5) 0.0149(9) Uani 1 1 d U . .
H10 H 0.9760 -0.2936 0.4987 0.018 Uiso 1 1 calc R . .
C11 C 1.1093(7) -0.2021(5) 0.3641(5) 0.0144(9) Uani 1 1 d U . .
H11 H 1.2113 -0.2796 0.3566 0.017 Uiso 1 1 calc R . .
C12 C 1.0968(6) -0.0796(5) 0.2916(5) 0.0125(8) Uani 1 1 d U . .
C14 C 1.2507(6) -0.0689(5) 0.2044(5) 0.0133(8) Uani 1 1 d U . .
O9 O 1.3293(5) 0.0160(4) 0.2424(3) 0.0171(7) Uani 1 1 d U . .
H1O9 H 1.4233 0.0104 0.1990 0.026 Uiso 1 1 calc R . .
O10 O 1.2942(5) -0.1387(4) 0.1139(3) 0.0176(7) Uani 1 1 d U . .

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
O1 0.0223(18) 0.0089(16) 0.0135(16) -0.0051(13) 0.0053(14) 0.0019(13)
O2 0.0094(16) 0.0203(18) 0.0167(17) -0.0017(14) 0.0032(13) -0.0026(13)
Pt 0.00874(8) 0.00842(9) 0.00924(9) -0.00063(5) 0.00229(5) -0.00154(6)
N1 0.0087(17) 0.0122(17) 0.0117(17) -0.0011(13) 0.0014(13) -0.0026(13)
C1 0.0008(17) 0.0112(19) 0.0138(19) 0.0096(15) 0.0019(14) 0.0017(14)
C6 0.010(2) 0.0105(19) 0.015(2) -0.0011(15) 0.0006(15) -0.0037(15)
O3 0.0149(16) 0.0142(16) 0.0113(15) -0.0019(12) 0.0043(12) -0.0007(13)
O4 0.0157(17) 0.0179(18) 0.0128(16) -0.0042(13) 0.0049(13) -0.0029(14)
C2 0.016(2) 0.016(2) 0.0097(19) 0.0005(16) -0.0014(16) -0.0051(17)
C3 0.018(2) 0.013(2) 0.016(2) -0.0004(17) -0.0041(18) -0.0046(17)
C4 0.013(2) 0.015(2) 0.017(2) -0.0011(17) -0.0019(17) -0.0023(17)
C5 0.011(2) 0.015(2) 0.0135(19) -0.0028(16) 0.0005(16) -0.0048(16)
C7 0.016(2) 0.011(2) 0.0129(19) 0.0012(16) 0.0032(16) -0.0028(17)
O5 0.0150(16) 0.0176(17) 0.0120(16) -0.0038(13) 0.0031(12) -0.0039(13)
O6 0.0161(16) 0.0191(18) 0.0203(18) -0.0018(15) 0.0050(14) 0.0012(14)
N2 0.0099(17) 0.0106(16) 0.0108(18) -0.0027(13) 0.0027(13) -0.0026(13)
C8 0.029(2) 0.0078(18) 0.0047(18) -0.0045(14) 0.0034(16) -0.0080(16)
C13 0.013(2) 0.0125(19) 0.015(2) -0.0002(17) 0.0031(16) -0.0044(16)
O7 0.0113(16) 0.0112(15) 0.0186(17) -0.0002(13) 0.0066(12) -0.0022(12)
O8 0.0122(16) 0.0155(17) 0.0221(18) -0.0007(14) 0.0091(13) -0.0034(13)
C9 0.011(2) 0.016(2) 0.014(2) -0.0014(16) 0.0022(16) -0.0049(16)
C10 0.015(2) 0.012(2) 0.017(2) 0.0018(17) 0.0003(17) -0.0043(16)
C11 0.014(2) 0.0096(19) 0.019(2) -0.0030(16) 0.0012(17) -0.0020(17)
C12 0.0123(19) 0.0124(19) 0.012(2) -0.0055(16) 0.0023(15) -0.0021(15)
C14 0.011(2) 0.010(2) 0.013(2) 0.0019(15) 0.0011(15) 0.0040(15)
O9 0.0111(16) 0.0246(19) 0.0168(17) -0.0038(14) 0.0050(13) -0.0068(14)
O10 0.0210(18) 0.0149(17) 0.0144(16) -0.0003(13) 0.0055(14) -0.0023(14)

_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
O1 H1O1 0.84(2) . ?
O1 H2O1 0.83(2) . ?
O2 H1O2 0.84(2) . ?
O2 H2O2 0.83(2) . ?
Pt N2 1.997(4) . ?
Pt O7 1.998(3) . ?
Pt N1 2.000(4) . ?
Pt O3 2.005(3) . ?
N1 C1 1.318(6) . ?
N1 C5 1.344(6) . ?
C1 C2 1.387(6) . ?
C1 C6 1.532(6) . ?
C6 O4 1.228(6) . ?
C6 O3 1.290(6) . ?
C2 C3 1.403(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(7) . ?
C4 H4 0.9500 . ?
C5 C7 1.514(7) . ?
C7 O6 1.214(6) . ?
C7 O5 1.297(6) . ?
O5 H1O5 0.8400 . ?
N2 C8 1.347(6) . ?
N2 C12 1.353(6) . ?
C8 C9 1.368(6) . ?
C8 C13 1.521(7) . ?
C13 O8 1.230(6) . ?
C13 O7 1.288(6) . ?
C9 C10 1.393(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(7) . ?
C11 H11 0.9500 . ?
C12 C14 1.508(7) . ?
C14 O10 1.216(6) . ?
C14 O9 1.302(6) . ?
O9 H1O9 0.8400 . ?

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
H1O1 O1 H2O1 111(7) . . ?
H1O2 O2 H2O2 106(6) . . ?
N2 Pt O7 81.36(14) . . ?
N2 Pt N1 176.17(15) . . ?
O7 Pt N1 97.15(15) . . ?
N2 Pt O3 99.81(15) . . ?
O7 Pt O3 173.57(14) . . ?
N1 Pt O3 81.27(15) . . ?
C1 N1 C5 118.0(4) . . ?
C1 N1 Pt 113.3(3) . . ?
C5 N1 Pt 128.4(3) . . ?
N1 C1 C2 125.0(4) . . ?
N1 C1 C6 114.4(4) . . ?
C2 C1 C6 120.6(4) . . ?
O4 C6 O3 123.7(4) . . ?
O4 C6 C1 121.7(4) . . ?
O3 C6 C1 114.4(4) . . ?
C6 O3 Pt 114.1(3) . . ?
C1 C2 C3 116.4(4) . . ?
C1 C2 H2 121.8 . . ?
C3 C2 H2 121.8 . . ?
C4 C3 C2 118.9(5) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 119.7(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C7 119.3(4) . . ?
C4 C5 C7 119.1(4) . . ?
O6 C7 O5 126.5(5) . . ?
O6 C7 C5 120.9(5) . . ?
O5 C7 C5 112.5(4) . . ?
C7 O5 H1O5 109.5 . . ?
C8 N2 C12 116.7(4) . . ?
C8 N2 Pt 113.8(3) . . ?
C12 N2 Pt 129.5(3) . . ?
N2 C8 C9 125.0(4) . . ?
N2 C8 C13 113.4(4) . . ?
C9 C8 C13 121.6(4) . . ?
O8 C13 O7 123.5(4) . . ?
O8 C13 C8 121.3(4) . . ?
O7 C13 C8 115.1(4) . . ?
C13 O7 Pt 114.8(3) . . ?
C8 C9 C10 117.5(4) . . ?
C8 C9 H9 121.2 . . ?
C10 C9 H9 121.2 . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N2 C12 C11 122.5(4) . . ?
N2 C12 C14 118.3(4) . . ?
C11 C12 C14 119.2(4) . . ?
O10 C14 O9 126.9(5) . . ?
O10 C14 C12 121.0(5) . . ?
O9 C14 C12 112.0(4) . . ?
C14 O9 H1O9 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Pt N1 C1 -94(2) . . . . ?
O7 Pt N1 C1 -160.4(3) . . . . ?
O3 Pt N1 C1 13.3(3) . . . . ?
N2 Pt N1 C5 80(2) . . . . ?
O7 Pt N1 C5 13.6(4) . . . . ?
O3 Pt N1 C5 -172.7(4) . . . . ?
C5 N1 C1 C2 -8.6(7) . . . . ?
Pt N1 C1 C2 166.1(4) . . . . ?
C5 N1 C1 C6 175.2(4) . . . . ?
Pt N1 C1 C6 -10.1(5) . . . . ?
N1 C1 C6 O4 -176.3(4) . . . . ?
C2 C1 C6 O4 7.3(7) . . . . ?
N1 C1 C6 O3 -2.0(6) . . . . ?
C2 C1 C6 O3 -178.3(4) . . . . ?
O4 C6 O3 Pt -172.7(4) . . . . ?
C1 C6 O3 Pt 13.1(5) . . . . ?
N2 Pt O3 C6 161.6(3) . . . . ?
O7 Pt O3 C6 61.7(13) . . . . ?
N1 Pt O3 C6 -14.6(3) . . . . ?
N1 C1 C2 C3 4.0(7) . . . . ?
C6 C1 C2 C3 180.0(4) . . . . ?
C1 C2 C3 C4 0.6(7) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C1 N1 C5 C4 8.5(7) . . . . ?
Pt N1 C5 C4 -165.2(4) . . . . ?
C1 N1 C5 C7 -167.8(4) . . . . ?
Pt N1 C5 C7 18.4(6) . . . . ?
C3 C4 C5 N1 -4.3(7) . . . . ?
C3 C4 C5 C7 172.1(4) . . . . ?
N1 C5 C7 O6 -132.0(5) . . . . ?
C4 C5 C7 O6 51.5(7) . . . . ?
N1 C5 C7 O5 51.7(6) . . . . ?
C4 C5 C7 O5 -124.8(5) . . . . ?
O7 Pt N2 C8 9.4(3) . . . . ?
N1 Pt N2 C8 -58(2) . . . . ?
O3 Pt N2 C8 -164.2(3) . . . . ?
O7 Pt N2 C12 -173.5(4) . . . . ?
N1 Pt N2 C12 119(2) . . . . ?
O3 Pt N2 C12 13.0(4) . . . . ?
C12 N2 C8 C9 -3.4(7) . . . . ?
Pt N2 C8 C9 174.1(4) . . . . ?
C12 N2 C8 C13 176.4(4) . . . . ?
Pt N2 C8 C13 -6.0(5) . . . . ?
N2 C8 C13 O8 -179.8(5) . . . . ?
C9 C8 C13 O8 0.0(8) . . . . ?
N2 C8 C13 O7 -3.6(6) . . . . ?
C9 C8 C13 O7 176.2(4) . . . . ?
O8 C13 O7 Pt -172.3(4) . . . . ?
C8 C13 O7 Pt 11.6(5) . . . . ?
N2 Pt O7 C13 -11.7(3) . . . . ?
N1 Pt O7 C13 164.7(3) . . . . ?
O3 Pt O7 C13 89.3(12) . . . . ?
N2 C8 C9 C10 1.8(7) . . . . ?
C13 C8 C9 C10 -178.0(4) . . . . ?
C8 C9 C10 C11 0.1(7) . . . . ?
C9 C10 C11 C12 -0.3(7) . . . . ?
C8 N2 C12 C11 3.2(7) . . . . ?
Pt N2 C12 C11 -173.9(4) . . . . ?
C8 N2 C12 C14 -175.8(4) . . . . ?
Pt N2 C12 C14 7.1(6) . . . . ?
C10 C11 C12 N2 -1.4(7) . . . . ?
C10 C11 C12 C14 177.5(5) . . . . ?
N2 C12 C14 O10 -117.5(5) . . . . ?
C11 C12 C14 O10 63.5(6) . . . . ?
N2 C12 C14 O9 65.4(6) . . . . ?
C11 C12 C14 O9 -113.6(5) . . . . ?

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
O1 H1O1 O8 0.84(2) 1.89(2) 2.730(5) 173(7) .
O1 H2O1 O6 0.83(2) 2.07(3) 2.851(5) 156(7) .
O2 H1O2 O4 0.84(2) 1.90(2) 2.724(5) 169(7) 2_755
O2 H2O2 O10 0.83(2) 2.01(2) 2.838(5) 175(7) 2_755
O5 H1O5 O1 0.84 1.72 2.555(5) 172.9 2_666
O9 H1O9 O2 0.84 1.69 2.522(5) 170.2 1_655

_diffrn_measured_fraction_theta_max 0.926
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         4.841
_refine_diff_density_min         -2.855
_refine_diff_density_rms         0.258