# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012


data_global
_journal_name_full               'New J.Chem.'

_journal_coden_Cambridge         0440
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Prof. Hongjie Zhang'
_publ_contact_author_email       hongjie@ciac.jl.cn

_publ_section_title              
;
An unusual three-dimensional self-penetrating
network derived from cross-linking of twofold interpenetrating
nets via ligand-unsupported Ag-Ag bonds: synthesis, structure,
luminescence, and theoretical study
;
loop_
_publ_author_name
'Xuezhi Song'
'Chao Qin'
'Shuyan Song'
'Hongjie Zhang'

# Attachment '- 794548.cif'

data_p21na
_database_code_depnum_ccdc_archive 'CCDC 794548'
#TrackingRef '- 794548.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H40 Ag4 N6 O16'
_chemical_formula_weight         1220.20

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   p21/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   12.3937(7)
_cell_length_b                   19.3300(9)
_cell_length_c                   17.2992(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.75
_cell_angle_gamma                90.00
_cell_volume                     4123.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    187(2)
_cell_measurement_reflns_used    4897
_cell_measurement_theta_min      1.58
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2408
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_T_max  0.7143
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      187(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20933
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7260
_reflns_number_gt                4897
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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^)+(0.0332P)^2^+3.2563P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7260
_refine_ls_number_parameters     553
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0933
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.021
_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
Ag1 Ag 0.71681(4) 0.19839(3) 0.51668(3) 0.03655(15) Uani 1 1 d . . .
Ag2 Ag 0.75235(3) 0.04582(2) 0.50409(2) 0.02497(12) Uani 1 1 d . . .
Ag3 Ag 0.0000 0.0000 0.0000 0.03531(18) Uani 1 2 d S . .
Ag4 Ag 0.5000 0.0000 0.0000 0.03594(18) Uani 1 2 d S . .
Ag5 Ag 0.24984(4) 0.00182(2) 0.00670(3) 0.03048(13) Uani 1 1 d . . .
C1 C 0.6675(5) 0.2414(3) 0.6782(3) 0.0342(15) Uani 1 1 d . . .
H1 H 0.7428 0.2417 0.6857 0.041 Uiso 1 1 calc R . .
C2 C 0.6106(5) 0.2603(3) 0.7390(3) 0.0352(16) Uani 1 1 d . . .
H2 H 0.6473 0.2739 0.7860 0.042 Uiso 1 1 calc R . .
C3 C 0.4984(5) 0.2590(3) 0.7300(3) 0.0300(15) Uani 1 1 d . . .
C4 C 0.4464(5) 0.2401(3) 0.6581(3) 0.0313(15) Uani 1 1 d . . .
H4 H 0.3711 0.2397 0.6494 0.038 Uiso 1 1 calc R . .
C5 C 0.5106(6) 0.2218(3) 0.5995(3) 0.0344(16) Uani 1 1 d . . .
H5 H 0.4762 0.2085 0.5516 0.041 Uiso 1 1 calc R . .
C6 C 0.4167(5) 0.2828(3) 0.9313(3) 0.0360(16) Uani 1 1 d . . .
H9 H 0.4485 0.2780 0.9820 0.043 Uiso 1 1 calc R . .
C7 C 0.4774(5) 0.2687(3) 0.8715(3) 0.0367(16) Uani 1 1 d . . .
H10 H 0.5492 0.2547 0.8822 0.044 Uiso 1 1 calc R . .
C8 C 0.4333(5) 0.2750(3) 0.7957(3) 0.0281(14) Uani 1 1 d . . .
C9 C 0.3268(5) 0.2966(3) 0.7826(3) 0.0387(17) Uani 1 1 d . . .
H7 H 0.2940 0.3021 0.7322 0.046 Uiso 1 1 calc R . .
C10 C 0.2698(5) 0.3098(3) 0.8455(3) 0.0390(17) Uani 1 1 d . . .
H8 H 0.1979 0.3240 0.8360 0.047 Uiso 1 1 calc R . .
C11 C 0.5261(5) 0.0731(3) 0.4158(3) 0.0264(14) Uani 1 1 d . . .
C12 C 0.4280(4) 0.0374(3) 0.3742(3) 0.0247(14) Uani 1 1 d . . .
H12 H 0.3669 0.0396 0.4059 0.030 Uiso 1 1 calc R . .
C13 C 0.3937(4) 0.0668(3) 0.2924(3) 0.0249(13) Uani 1 1 d . . .
H13 H 0.3735 0.1157 0.2945 0.030 Uiso 1 1 calc R . .
C14 C 0.2965(4) 0.0214(3) 0.2601(3) 0.0268(14) Uani 1 1 d . . .
H14 H 0.2378 0.0242 0.2939 0.032 Uiso 1 1 calc R . .
C15 C 0.2556(4) 0.0416(3) 0.1772(3) 0.0274(14) Uani 1 1 d . . .
C16 C 0.3156(5) -0.0668(3) 0.1651(4) 0.0333(15) Uani 1 1 d . . .
C17 C 0.3325(4) -0.0531(3) 0.2518(3) 0.0261(14) Uani 1 1 d . . .
H17 H 0.2881 -0.0844 0.2800 0.031 Uiso 1 1 calc R . .
C18 C 0.4533(4) -0.0600(3) 0.2817(3) 0.0245(13) Uani 1 1 d . . .
H18 H 0.4794 -0.1074 0.2756 0.029 Uiso 1 1 calc R . .
C19 C 0.4655(4) -0.0378(3) 0.3672(3) 0.0251(13) Uani 1 1 d . . .
H19 H 0.4224 -0.0682 0.3974 0.030 Uiso 1 1 calc R . .
C20 C 0.5813(5) -0.0363(3) 0.4030(3) 0.0266(14) Uani 1 1 d . . .
C21 C 0.4842(4) 0.0557(3) 0.2422(3) 0.0216(13) Uani 1 1 d . . .
H21 H 0.5164 0.0917 0.2172 0.026 Uiso 1 1 calc R . .
C22 C 0.5142(4) -0.0093(3) 0.2364(3) 0.0261(14) Uani 1 1 d . . .
H22 H 0.5689 -0.0228 0.2066 0.031 Uiso 1 1 calc R . .
C23 C 0.9672(5) 0.0004(3) 0.5896(3) 0.0336(16) Uani 1 1 d . . .
C24 C 1.0701(5) 0.0236(3) 0.6360(3) 0.0311(15) Uani 1 1 d . . .
H24 H 1.1306 0.0221 0.6037 0.037 Uiso 1 1 calc R . .
C25 C 1.0968(5) -0.0196(3) 0.7097(4) 0.0345(16) Uani 1 1 d . . .
H25 H 1.1085 -0.0684 0.6976 0.041 Uiso 1 1 calc R . .
C26 C 1.1997(5) 0.0138(3) 0.7526(3) 0.0311(15) Uani 1 1 d . . .
H32 H 1.2593 0.0127 0.7194 0.037 Uiso 1 1 calc R . .
C27 C 1.1748(4) 0.0886(3) 0.7735(3) 0.0272(14) Uani 1 1 d . . .
H31 H 1.2242 0.1202 0.7502 0.033 Uiso 1 1 calc R . .
C28 C 1.0563(5) 0.1069(3) 0.7458(3) 0.0282(14) Uani 1 1 d . . .
H28 H 1.0375 0.1538 0.7613 0.034 Uiso 1 1 calc R . .
C29 C 1.0456(5) 0.0983(3) 0.6566(3) 0.0261(14) Uani 1 1 d . . .
H29 H 1.0962 0.1295 0.6340 0.031 Uiso 1 1 calc R . .
C30 C 0.9320(5) 0.1100(3) 0.6183(3) 0.0267(14) Uani 1 1 d . . .
C31 C 1.0061(5) -0.0107(3) 0.7612(4) 0.0370(17) Uani 1 1 d . . .
H26 H 0.9678 -0.0479 0.7790 0.044 Uiso 1 1 calc R . .
C32 C 0.9860(5) 0.0532(3) 0.7787(3) 0.0309(15) Uani 1 1 d . . .
H27 H 0.9316 0.0649 0.8096 0.037 Uiso 1 1 calc R . .
C33 C 0.1970(5) 0.0900(3) -0.1382(3) 0.0296(14) Uani 1 1 d . . .
C34 C 0.2348(5) -0.0194(3) -0.1704(4) 0.0324(15) Uani 1 1 d . . .
N1 N 0.6191(4) 0.2224(2) 0.6085(3) 0.0303(12) Uani 1 1 d . . .
N2 N 0.3122(4) 0.3034(3) 0.9197(3) 0.0341(13) Uani 1 1 d . . .
N3 N 0.8922(4) 0.0525(3) 0.5802(3) 0.0264(11) Uani 1 1 d . . .
N4 N 0.6092(4) 0.0273(2) 0.4331(3) 0.0237(11) Uani 1 1 d . . .
N5 N 0.2693(4) -0.0107(3) 0.1270(3) 0.0289(12) Uani 1 1 d . . .
N6 N 0.2291(4) 0.0271(3) -0.1104(3) 0.0282(12) Uani 1 1 d . . .
O1 O 0.6429(3) -0.0858(2) 0.4050(2) 0.0413(11) Uani 1 1 d . . .
O2 O 0.5315(3) 0.1344(2) 0.4338(2) 0.0380(11) Uani 1 1 d . . .
O3 O 0.2181(3) 0.0983(2) 0.1582(2) 0.0347(10) Uani 1 1 d . . .
O4 O 0.3409(4) -0.1206(2) 0.1345(2) 0.0446(12) Uani 1 1 d . . .
O5 O 0.2655(4) -0.0786(3) -0.1612(3) 0.0540(14) Uani 1 1 d . . .
O6 O 0.1811(4) 0.1410(2) -0.0983(2) 0.0400(11) Uani 1 1 d . . .
O7 O 0.9530(3) -0.0576(2) 0.5619(3) 0.0502(13) Uani 1 1 d . . .
O8 O 0.8828(3) 0.1647(2) 0.6213(2) 0.0404(11) Uani 1 1 d . . .
O1W O 0.5373(4) 0.1043(3) 0.0237(3) 0.0710(16) Uani 1 1 d D . .
H1A H 0.5850 0.1077 0.0624 0.106 Uiso 1 1 d RD . .
H1B H 0.5647 0.1242 -0.0135 0.106 Uiso 1 1 d RD . .
O2W O 0.0269(4) 0.1051(3) 0.0270(3) 0.0683(16) Uani 1 1 d D . .
H2B H -0.0333 0.1259 0.0283 0.102 Uiso 1 1 d RD . .
H2A H 0.0591 0.1251 -0.0080 0.102 Uiso 1 1 d RD . .
O3W O 0.3183(3) 0.1684(2) 0.0382(2) 0.0357(10) Uani 1 1 d D . .
H3A H 0.2886 0.1517 0.0762 0.054 Uiso 1 1 d RD . .
H3B H 0.3700 0.1415 0.0310 0.054 Uiso 1 1 d RD . .
O4W O 0.7969(4) 0.8526(3) 0.5055(3) 0.0685(16) Uani 1 1 d D . .
H4B H 0.8352 0.8816 0.5332 0.103 Uiso 1 1 d RD . .
H4A H 0.7458 0.8765 0.4824 0.103 Uiso 1 1 d RD . .
O5W O 0.0133(4) 0.2797(3) 0.6829(3) 0.0706(16) Uani 1 1 d D . .
H5A H -0.0308 0.2477 0.6678 0.106 Uiso 1 1 d RD . .
H5B H 0.0622 0.2796 0.6517 0.106 Uiso 1 1 d RD . .
O6W O 0.8167(4) 0.7372(3) 0.4115(4) 0.099(2) Uani 1 1 d D . .
H6B H 0.8456 0.7671 0.3839 0.148 Uiso 1 1 d RD . .
H6A H 0.8178 0.7554 0.4562 0.148 Uiso 1 1 d RD . .
O7W O 0.8102(5) 0.1614(4) 0.9947(5) 0.149(4) Uani 1 1 d D . .
H7A H 0.7513 0.1522 0.9672 0.224 Uiso 1 1 d RD . .
H7B H 0.8565 0.1644 0.9618 0.224 Uiso 1 1 d RD . .
O8W O 0.8206(8) 0.2863(6) 0.8951(5) 0.072(3) Uani 0.50 1 d PD . .
H8A H 0.7923 0.2471 0.9024 0.108 Uiso 0.50 1 d PRD . .
H8B H 0.8583 0.2801 0.8572 0.108 Uiso 0.50 1 d PRD . .
O9W O 1.0163(9) 0.2478(5) 0.8474(5) 0.062(3) Uani 0.50 1 d PD . .
H9A H 1.0559 0.2532 0.8104 0.093 Uiso 0.50 1 d PRD . .
H9B H 0.9524 0.2584 0.8288 0.093 Uiso 0.50 1 d PRD . .

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
Ag1 0.0586(3) 0.0314(3) 0.0230(3) 0.0011(2) 0.0211(2) 0.0033(2)
Ag2 0.0223(2) 0.0288(3) 0.0235(2) -0.0022(2) 0.00083(17) -0.0005(2)
Ag3 0.0238(4) 0.0346(4) 0.0463(4) -0.0051(3) -0.0025(3) 0.0027(3)
Ag4 0.0230(4) 0.0320(4) 0.0528(5) 0.0009(3) 0.0041(3) -0.0004(3)
Ag5 0.0222(2) 0.0376(3) 0.0310(3) 0.0108(2) -0.00041(19) 0.0037(2)
C1 0.049(4) 0.031(4) 0.024(4) -0.005(3) 0.011(3) -0.002(3)
C2 0.057(5) 0.032(4) 0.018(3) -0.004(3) 0.011(3) -0.004(3)
C3 0.054(4) 0.017(3) 0.021(3) 0.005(2) 0.016(3) 0.002(3)
C4 0.048(4) 0.023(4) 0.025(3) 0.000(3) 0.016(3) 0.006(3)
C5 0.060(5) 0.026(4) 0.019(3) 0.002(3) 0.011(3) 0.004(3)
C6 0.047(4) 0.043(4) 0.019(3) -0.001(3) 0.007(3) -0.002(3)
C7 0.047(4) 0.039(4) 0.026(4) -0.002(3) 0.016(3) 0.005(3)
C8 0.054(4) 0.016(3) 0.016(3) 0.000(2) 0.009(3) 0.003(3)
C9 0.067(5) 0.031(4) 0.020(3) 0.005(3) 0.014(3) 0.015(4)
C10 0.051(4) 0.039(4) 0.028(4) 0.008(3) 0.010(3) 0.010(3)
C11 0.033(4) 0.029(4) 0.018(3) 0.003(3) 0.008(3) 0.000(3)
C12 0.016(3) 0.037(4) 0.021(3) -0.001(3) 0.004(2) -0.006(3)
C13 0.028(3) 0.022(3) 0.024(3) -0.001(2) 0.001(3) 0.001(3)
C14 0.014(3) 0.040(4) 0.026(3) 0.011(3) -0.001(2) -0.001(3)
C15 0.016(3) 0.037(4) 0.029(4) 0.009(3) 0.001(3) 0.005(3)
C16 0.026(3) 0.034(4) 0.038(4) 0.013(3) -0.007(3) -0.001(3)
C17 0.021(3) 0.025(3) 0.031(3) 0.011(3) -0.003(3) -0.003(3)
C18 0.017(3) 0.024(3) 0.031(3) 0.002(3) -0.006(3) 0.003(2)
C19 0.023(3) 0.023(3) 0.029(3) 0.006(3) -0.002(3) -0.001(3)
C20 0.027(3) 0.029(4) 0.022(3) 0.006(3) -0.003(3) 0.000(3)
C21 0.017(3) 0.025(4) 0.023(3) 0.005(2) 0.001(2) -0.009(3)
C22 0.021(3) 0.038(4) 0.020(3) -0.004(3) 0.001(2) -0.003(3)
C23 0.025(3) 0.041(4) 0.034(4) -0.012(3) -0.001(3) 0.004(3)
C24 0.019(3) 0.043(4) 0.031(4) -0.009(3) 0.000(3) 0.004(3)
C25 0.021(3) 0.032(4) 0.048(4) -0.008(3) -0.013(3) 0.006(3)
C26 0.017(3) 0.047(4) 0.028(4) -0.008(3) -0.001(3) 0.000(3)
C27 0.024(3) 0.036(4) 0.022(3) -0.001(3) 0.005(3) -0.013(3)
C28 0.037(4) 0.030(4) 0.018(3) -0.002(3) 0.004(3) 0.009(3)
C29 0.030(3) 0.031(4) 0.018(3) 0.000(3) 0.006(3) -0.008(3)
C30 0.034(4) 0.032(4) 0.015(3) 0.001(3) 0.010(3) 0.001(3)
C31 0.022(3) 0.040(4) 0.046(4) 0.015(3) -0.010(3) -0.006(3)
C32 0.019(3) 0.049(5) 0.025(3) 0.006(3) 0.004(3) 0.000(3)
C33 0.027(3) 0.032(4) 0.030(4) 0.002(3) 0.003(3) -0.010(3)
C34 0.018(3) 0.033(4) 0.045(4) -0.006(3) -0.004(3) 0.008(3)
N1 0.042(3) 0.024(3) 0.026(3) 0.003(2) 0.013(2) 0.003(2)
N2 0.058(4) 0.024(3) 0.022(3) 0.000(2) 0.015(3) 0.002(3)
N3 0.023(3) 0.028(3) 0.028(3) 0.001(2) 0.002(2) 0.002(2)
N4 0.025(3) 0.025(3) 0.022(3) 0.002(2) 0.003(2) -0.003(2)
N5 0.023(3) 0.035(3) 0.027(3) 0.011(2) -0.005(2) -0.002(2)
N6 0.023(3) 0.037(3) 0.024(3) -0.002(2) 0.001(2) 0.002(2)
O1 0.037(3) 0.032(3) 0.051(3) -0.004(2) -0.016(2) 0.010(2)
O2 0.047(3) 0.030(3) 0.037(3) -0.004(2) 0.002(2) 0.004(2)
O3 0.031(2) 0.044(3) 0.029(2) 0.012(2) 0.0016(19) 0.009(2)
O4 0.061(3) 0.032(3) 0.038(3) -0.001(2) -0.010(2) 0.001(2)
O5 0.047(3) 0.048(3) 0.062(3) -0.016(3) -0.022(2) 0.017(3)
O6 0.062(3) 0.032(3) 0.025(2) -0.0014(19) -0.005(2) 0.001(2)
O7 0.042(3) 0.043(3) 0.060(3) -0.018(2) -0.020(2) 0.006(2)
O8 0.053(3) 0.034(3) 0.032(3) -0.001(2) -0.004(2) 0.014(2)
O1W 0.065(4) 0.056(4) 0.091(4) 0.006(3) 0.006(3) -0.010(3)
O2W 0.057(3) 0.053(4) 0.094(4) -0.004(3) 0.005(3) 0.005(3)
O3W 0.030(2) 0.036(3) 0.042(3) 0.008(2) 0.011(2) 0.006(2)
O4W 0.059(3) 0.068(4) 0.071(4) 0.007(3) -0.031(3) -0.011(3)
O5W 0.096(4) 0.047(4) 0.065(4) -0.007(3) -0.010(3) 0.005(3)
O6W 0.055(4) 0.052(4) 0.193(7) 0.009(4) 0.032(4) -0.011(3)
O7W 0.044(4) 0.120(7) 0.269(10) -0.125(6) -0.055(5) 0.029(4)
O8W 0.076(8) 0.103(10) 0.037(6) 0.009(6) 0.008(5) 0.032(7)
O9W 0.109(9) 0.036(6) 0.042(6) -0.012(5) 0.011(6) -0.007(6)

_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
Ag1 N1 2.142(5) . ?
Ag1 N2 2.147(5) 4_665 ?
Ag1 Ag2 2.9931(7) . ?
Ag2 N3 2.074(4) . ?
Ag2 N4 2.085(4) . ?
Ag3 O2W 2.103(5) . ?
Ag3 O2W 2.103(5) 3 ?
Ag3 Ag5 3.0872(5) 3 ?
Ag3 Ag5 3.0872(5) . ?
Ag4 O1W 2.100(5) . ?
Ag4 O1W 2.100(5) 3_655 ?
Ag4 Ag5 3.1143(5) . ?
Ag4 Ag5 3.1143(5) 3_655 ?
Ag5 N6 2.075(5) . ?
Ag5 N5 2.085(5) . ?
C1 N1 1.344(7) . ?
C1 C2 1.373(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(8) . ?
C3 C8 1.490(7) . ?
C4 C5 1.396(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.337(7) . ?
C5 H5 0.9300 . ?
C6 N2 1.350(7) . ?
C6 C7 1.367(8) . ?
C6 H9 0.9300 . ?
C7 C8 1.375(8) . ?
C7 H10 0.9300 . ?
C8 C9 1.382(8) . ?
C9 C10 1.379(8) . ?
C9 H7 0.9300 . ?
C10 N2 1.344(7) . ?
C10 H8 0.9300 . ?
C11 O2 1.224(7) . ?
C11 N4 1.369(7) . ?
C11 C12 1.516(8) . ?
C12 C19 1.535(8) . ?
C12 C13 1.544(7) . ?
C12 H12 0.9800 . ?
C13 C21 1.501(7) . ?
C13 C14 1.548(7) . ?
C13 H13 0.9800 . ?
C14 C17 1.518(8) . ?
C14 C15 1.524(7) . ?
C14 H14 0.9800 . ?
C15 O3 1.223(7) . ?
C15 N5 1.354(7) . ?
C16 O4 1.221(7) . ?
C16 N5 1.364(7) . ?
C16 C17 1.518(8) . ?
C17 C18 1.540(7) . ?
C17 H17 0.9800 . ?
C18 C22 1.504(8) . ?
C18 C19 1.533(7) . ?
C18 H18 0.9800 . ?
C19 C20 1.505(7) . ?
C19 H19 0.9800 . ?
C20 O1 1.222(7) . ?
C20 N4 1.366(7) . ?
C21 C22 1.316(8) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O7 1.224(7) . ?
C23 N3 1.369(7) . ?
C23 C24 1.506(8) . ?
C24 C29 1.525(8) . ?
C24 C25 1.533(8) . ?
C24 H24 0.9800 . ?
C25 C31 1.512(8) . ?
C25 C26 1.551(8) . ?
C25 H25 0.9800 . ?
C26 C34 1.503(8) 1_656 ?
C26 C27 1.528(8) . ?
C26 H32 0.9800 . ?
C27 C33 1.525(8) 1_656 ?
C27 C28 1.540(8) . ?
C27 H31 0.9800 . ?
C28 C32 1.503(8) . ?
C28 C29 1.544(7) . ?
C28 H28 0.9800 . ?
C29 C30 1.512(8) . ?
C29 H29 0.9800 . ?
C30 O8 1.224(7) . ?
C30 N3 1.358(7) . ?
C31 C32 1.301(8) . ?
C31 H26 0.9300 . ?
C32 H27 0.9300 . ?
C33 O6 1.232(7) . ?
C33 N6 1.352(7) . ?
C33 C27 1.525(8) 1_454 ?
C34 O5 1.211(7) . ?
C34 N6 1.381(7) . ?
C34 C26 1.503(8) 1_454 ?
N2 Ag1 2.147(5) 4_566 ?
O1W H1A 0.8500 . ?
O1W H1B 0.8500 . ?
O2W H2B 0.8500 . ?
O2W H2A 0.8500 . ?
O3W H3A 0.8491 . ?
O3W H3B 0.8447 . ?
O4W H4B 0.8502 . ?
O4W H4A 0.8512 . ?
O5W H5A 0.8499 . ?
O5W H5B 0.8500 . ?
O6W H6B 0.8500 . ?
O6W H6A 0.8499 . ?
O7W H7A 0.8499 . ?
O7W H7B 0.8498 . ?
O8W H8A 0.8498 . ?
O8W H8B 0.8500 . ?
O9W H9A 0.8501 . ?
O9W H9B 0.8500 . ?

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
N1 Ag1 N2 168.27(19) . 4_665 ?
N1 Ag1 Ag2 111.44(13) . . ?
N2 Ag1 Ag2 80.24(13) 4_665 . ?
N3 Ag2 N4 173.11(19) . . ?
N3 Ag2 Ag1 90.70(13) . . ?
N4 Ag2 Ag1 95.13(13) . . ?
O2W Ag3 O2W 180.0(3) . 3 ?
O2W Ag3 Ag5 98.95(13) . 3 ?
O2W Ag3 Ag5 81.05(13) 3 3 ?
O2W Ag3 Ag5 81.05(13) . . ?
O2W Ag3 Ag5 98.95(13) 3 . ?
Ag5 Ag3 Ag5 180.0 3 . ?
O1W Ag4 O1W 180.0(3) . 3_655 ?
O1W Ag4 Ag5 100.51(14) . . ?
O1W Ag4 Ag5 79.49(14) 3_655 . ?
O1W Ag4 Ag5 79.49(14) . 3_655 ?
O1W Ag4 Ag5 100.51(14) 3_655 3_655 ?
Ag5 Ag4 Ag5 180.0 . 3_655 ?
N6 Ag5 N5 173.0(2) . . ?
N6 Ag5 Ag3 86.60(12) . . ?
N5 Ag5 Ag3 92.96(12) . . ?
N6 Ag5 Ag4 89.57(12) . . ?
N5 Ag5 Ag4 91.12(12) . . ?
Ag3 Ag5 Ag4 175.546(17) . . ?
N1 C1 C2 122.9(6) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 119.8(6) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 118.4(5) . . ?
C2 C3 C8 121.7(5) . . ?
C4 C3 C8 119.9(6) . . ?
C3 C4 C5 117.9(6) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 123.6(6) . . ?
N1 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
N2 C6 C7 122.6(6) . . ?
N2 C6 H9 118.7 . . ?
C7 C6 H9 118.7 . . ?
C6 C7 C8 120.5(6) . . ?
C6 C7 H10 119.7 . . ?
C8 C7 H10 119.7 . . ?
C7 C8 C9 117.7(5) . . ?
C7 C8 C3 121.0(6) . . ?
C9 C8 C3 121.3(5) . . ?
C10 C9 C8 119.0(6) . . ?
C10 C9 H7 120.5 . . ?
C8 C9 H7 120.5 . . ?
N2 C10 C9 123.6(6) . . ?
N2 C10 H8 118.2 . . ?
C9 C10 H8 118.2 . . ?
O2 C11 N4 123.3(6) . . ?
O2 C11 C12 125.6(6) . . ?
N4 C11 C12 111.0(5) . . ?
C11 C12 C19 103.5(4) . . ?
C11 C12 C13 113.7(4) . . ?
C19 C12 C13 109.5(4) . . ?
C11 C12 H12 110.0 . . ?
C19 C12 H12 110.0 . . ?
C13 C12 H12 110.0 . . ?
C21 C13 C12 108.9(4) . . ?
C21 C13 C14 108.0(4) . . ?
C12 C13 C14 104.8(4) . . ?
C21 C13 H13 111.6 . . ?
C12 C13 H13 111.6 . . ?
C14 C13 H13 111.6 . . ?
C17 C14 C15 103.1(5) . . ?
C17 C14 C13 110.3(4) . . ?
C15 C14 C13 111.6(4) . . ?
C17 C14 H14 110.5 . . ?
C15 C14 H14 110.5 . . ?
C13 C14 H14 110.5 . . ?
O3 C15 N5 124.5(5) . . ?
O3 C15 C14 124.3(6) . . ?
N5 C15 C14 111.2(5) . . ?
O4 C16 N5 125.6(6) . . ?
O4 C16 C17 124.0(5) . . ?
N5 C16 C17 110.4(5) . . ?
C14 C17 C16 104.2(4) . . ?
C14 C17 C18 109.6(5) . . ?
C16 C17 C18 110.5(5) . . ?
C14 C17 H17 110.8 . . ?
C16 C17 H17 110.8 . . ?
C18 C17 H17 110.8 . . ?
C22 C18 C19 108.3(5) . . ?
C22 C18 C17 106.9(4) . . ?
C19 C18 C17 107.3(4) . . ?
C22 C18 H18 111.4 . . ?
C19 C18 H18 111.4 . . ?
C17 C18 H18 111.4 . . ?
C20 C19 C18 113.6(4) . . ?
C20 C19 C12 103.5(4) . . ?
C18 C19 C12 109.9(4) . . ?
C20 C19 H19 109.9 . . ?
C18 C19 H19 109.9 . . ?
C12 C19 H19 109.9 . . ?
O1 C20 N4 124.0(5) . . ?
O1 C20 C19 124.4(5) . . ?
N4 C20 C19 111.6(5) . . ?
C22 C21 C13 114.4(5) . . ?
C22 C21 H21 122.8 . . ?
C13 C21 H21 122.8 . . ?
C21 C22 C18 115.0(5) . . ?
C21 C22 H22 122.5 . . ?
C18 C22 H22 122.5 . . ?
O7 C23 N3 123.9(6) . . ?
O7 C23 C24 124.2(6) . . ?
N3 C23 C24 111.8(5) . . ?
C23 C24 C29 103.3(5) . . ?
C23 C24 C25 112.4(5) . . ?
C29 C24 C25 110.7(5) . . ?
C23 C24 H24 110.1 . . ?
C29 C24 H24 110.1 . . ?
C25 C24 H24 110.1 . . ?
C31 C25 C24 108.5(5) . . ?
C31 C25 C26 107.2(5) . . ?
C24 C25 C26 105.7(5) . . ?
C31 C25 H25 111.7 . . ?
C24 C25 H25 111.7 . . ?
C26 C25 H25 111.7 . . ?
C34 C26 C27 104.0(5) 1_656 . ?
C34 C26 C25 113.4(5) 1_656 . ?
C27 C26 C25 109.3(5) . . ?
C34 C26 H32 110.0 1_656 . ?
C27 C26 H32 110.0 . . ?
C25 C26 H32 110.0 . . ?
C33 C27 C26 103.5(5) 1_656 . ?
C33 C27 C28 112.2(4) 1_656 . ?
C26 C27 C28 110.6(5) . . ?
C33 C27 H31 110.1 1_656 . ?
C26 C27 H31 110.1 . . ?
C28 C27 H31 110.1 . . ?
C32 C28 C27 107.1(5) . . ?
C32 C28 C29 108.0(5) . . ?
C27 C28 C29 105.7(4) . . ?
C32 C28 H28 111.9 . . ?
C27 C28 H28 111.9 . . ?
C29 C28 H28 111.9 . . ?
C30 C29 C24 103.7(5) . . ?
C30 C29 C28 113.9(4) . . ?
C24 C29 C28 109.6(5) . . ?
C30 C29 H29 109.8 . . ?
C24 C29 H29 109.8 . . ?
C28 C29 H29 109.8 . . ?
O8 C30 N3 124.7(6) . . ?
O8 C30 C29 123.7(6) . . ?
N3 C30 C29 111.5(5) . . ?
C32 C31 C25 114.5(6) . . ?
C32 C31 H26 122.8 . . ?
C25 C31 H26 122.8 . . ?
C31 C32 C28 115.9(5) . . ?
C31 C32 H27 122.1 . . ?
C28 C32 H27 122.1 . . ?
O6 C33 N6 125.4(6) . . ?
O6 C33 C27 123.5(6) . 1_454 ?
N6 C33 C27 110.9(5) . 1_454 ?
O5 C34 N6 123.8(6) . . ?
O5 C34 C26 125.4(6) . 1_454 ?
N6 C34 C26 110.8(5) . 1_454 ?
C5 N1 C1 117.3(5) . . ?
C5 N1 Ag1 123.3(4) . . ?
C1 N1 Ag1 119.4(4) . . ?
C10 N2 C6 116.6(5) . . ?
C10 N2 Ag1 123.7(4) . 4_566 ?
C6 N2 Ag1 118.3(4) . 4_566 ?
C30 N3 C23 109.7(5) . . ?
C30 N3 Ag2 126.7(4) . . ?
C23 N3 Ag2 122.9(4) . . ?
C20 N4 C11 110.1(5) . . ?
C20 N4 Ag2 123.2(4) . . ?
C11 N4 Ag2 126.5(4) . . ?
C15 N5 C16 110.9(5) . . ?
C15 N5 Ag5 122.9(4) . . ?
C16 N5 Ag5 125.1(4) . . ?
C33 N6 C34 110.7(5) . . ?
C33 N6 Ag5 124.2(4) . . ?
C34 N6 Ag5 124.7(4) . . ?
Ag4 O1W H1A 110.5 . . ?
Ag4 O1W H1B 112.6 . . ?
H1A O1W H1B 105.3 . . ?
Ag3 O2W H2B 110.0 . . ?
Ag3 O2W H2A 110.9 . . ?
H2B O2W H2A 106.3 . . ?
H3A O3W H3B 105.9 . . ?
H4B O4W H4A 104.8 . . ?
H5A O5W H5B 106.4 . . ?
H6B O6W H6A 105.1 . . ?
H7A O7W H7B 103.8 . . ?
H8A O8W H8B 104.9 . . ?
H9A O9W H9B 105.8 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.125

# Attachment '- 794549.cif'

data_p21nb
_database_code_depnum_ccdc_archive 'CCDC 794549'
#TrackingRef '- 794549.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H15 N3 O6'
_chemical_formula_weight         369.33

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   p21/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   7.6395(4)
_cell_length_b                   21.1972(11)
_cell_length_c                   9.8455(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.6830(10)
_cell_angle_gamma                90.00
_cell_volume                     1580.03(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2361
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.9629
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7922
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2768
_reflns_number_gt                2361
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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^)+(0.1388P)^2^+3.4434P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2768
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.2431
_refine_ls_wR_factor_gt          0.2350
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
C1 C 0.8593(5) 0.14815(19) -0.1112(4) 0.0296(9) Uani 1 1 d . . .
C2 C 0.7582(5) 0.18047(17) -0.0082(4) 0.0256(8) Uani 1 1 d . . .
H2A H 0.8406 0.2076 0.0540 0.031 Uiso 1 1 calc R . .
C3 C 0.6038(5) 0.22087(17) -0.0782(4) 0.0248(8) Uani 1 1 d . . .
H3A H 0.6460 0.2544 -0.1376 0.030 Uiso 1 1 calc R . .
C4 C 0.5188(5) 0.24974(17) 0.0425(4) 0.0250(8) Uani 1 1 d . . .
H4A H 0.6082 0.2748 0.1036 0.030 Uiso 1 1 calc R . .
C5 C 0.3619(5) 0.29020(18) -0.0084(4) 0.0292(9) Uani 1 1 d . . .
C6 C 0.2491(5) 0.20921(18) 0.1093(4) 0.0270(8) Uani 1 1 d . . .
C7 C 0.4436(5) 0.19612(18) 0.1244(4) 0.0255(8) Uani 1 1 d . . .
H7A H 0.4953 0.1983 0.2231 0.031 Uiso 1 1 calc R . .
C8 C 0.4842(5) 0.13099(17) 0.0631(4) 0.0251(8) Uani 1 1 d . . .
H8A H 0.4343 0.0955 0.1128 0.030 Uiso 1 1 calc R . .
C9 C 0.6892(5) 0.12692(17) 0.0744(4) 0.0251(8) Uani 1 1 d . . .
H9A H 0.7426 0.1300 0.1726 0.030 Uiso 1 1 calc R . .
C10 C 0.7517(5) 0.06710(18) 0.0110(4) 0.0301(9) Uani 1 1 d . . .
C11 C 0.4106(5) 0.13165(18) -0.0860(4) 0.0262(8) Uani 1 1 d . . .
H11A H 0.3278 0.1012 -0.1256 0.031 Uiso 1 1 calc R . .
C12 C 0.4701(5) 0.17810(18) -0.1587(4) 0.0266(8) Uani 1 1 d . . .
H12A H 0.4314 0.1838 -0.2536 0.032 Uiso 1 1 calc R . .
O1 O 0.7224(4) 0.01301(13) 0.0394(4) 0.0451(8) Uani 1 1 d . . .
O2 O 0.9322(4) 0.17363(14) -0.1981(3) 0.0420(8) Uani 1 1 d . . .
O3 O 0.3572(4) 0.33758(14) -0.0774(3) 0.0401(8) Uani 1 1 d . . .
O4 O 0.1356(4) 0.17710(14) 0.1539(3) 0.0344(7) Uani 1 1 d . . .
N1 N 0.8526(5) 0.08453(16) -0.0908(3) 0.0322(8) Uani 1 1 d . . .
H1 H 0.9047 0.0593 -0.1533 0.039 Uiso 1 1 d R . .
N2 N 0.2131(4) 0.26336(15) 0.0348(3) 0.0287(8) Uani 1 1 d . . .
H2 H 0.0985 0.2806 0.0269 0.034 Uiso 1 1 d R . .
N3 N 0.1923(5) 0.09413(16) 0.3887(5) 0.0478(11) Uani 1 1 d . . .
H3 H 0.1806 0.1232 0.2855 0.057 Uiso 0.50 1 d PR . .
H3' H 0.0846 0.1177 0.4026 0.057 Uiso 0.50 1 d PR . .
O8 O 0.3831(4) 0.16907(12) 0.4882(3) 0.0337(7) Uani 1 1 d . . .
O9 O 0.0523(4) 0.00585(13) 0.2958(3) 0.0364(7) Uani 1 1 d . . .
C19 C 0.5921(5) 0.04646(17) 0.5576(4) 0.0255(8) Uani 1 1 d . . .
H19A H 0.6734 0.0826 0.5981 0.031 Uiso 1 1 d R . .
C13 C 0.3393(5) 0.11657(18) 0.4567(4) 0.0311(9) Uani 1 1 d . . .
C14 C 0.1724(6) 0.0341(2) 0.3587(5) 0.0398(11) Uani 1 1 d . . .
C15 C 0.2814(9) 0.0025(3) 0.4966(7) 0.0221(15) Uani 0.50 1 d P . .
H15A H 0.2115 -0.0131 0.5683 0.027 Uiso 0.50 1 d PR . .
C21 C 0.6219(10) 0.0304(3) 0.4205(8) 0.0250(15) Uani 0.50 1 d P . .
H21A H 0.7105 0.0545 0.3687 0.030 Uiso 0.50 1 d PR . .
C17 C 0.4797(10) 0.0704(3) 0.4159(7) 0.0223(15) Uani 0.50 1 d P . .
H17A H 0.5671 0.0880 0.3578 0.027 Uiso 0.50 1 d PR . .
C20 C 0.4746(10) 0.0168(3) 0.6391(7) 0.0236(15) Uani 0.50 1 d P . .
H20A H 0.4857 0.0325 0.7351 0.028 Uiso 0.50 1 d PR . .
C16 C 0.3917(10) 0.0582(3) 0.5623(7) 0.0231(15) Uani 0.50 1 d P . .
H16A H 0.3691 0.0727 0.6606 0.028 Uiso 0.50 1 d PR . .
C18 C 0.3726(10) 0.0157(3) 0.3475(7) 0.0236(15) Uani 0.50 1 d P . .
H18A H 0.4020 0.0040 0.2398 0.028 Uiso 0.50 1 d PR . .

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
C1 0.028(2) 0.032(2) 0.028(2) 0.0019(17) 0.0030(16) 0.0004(16)
C2 0.0263(19) 0.0227(18) 0.0276(19) -0.0020(15) 0.0026(15) -0.0031(15)
C3 0.0275(19) 0.0223(18) 0.0248(18) 0.0023(14) 0.0038(15) -0.0042(15)
C4 0.0274(19) 0.0188(17) 0.0295(19) -0.0005(15) 0.0067(15) -0.0017(15)
C5 0.033(2) 0.027(2) 0.0268(19) -0.0011(16) 0.0049(16) 0.0007(16)
C6 0.034(2) 0.030(2) 0.0174(17) 0.0001(15) 0.0038(15) -0.0036(17)
C7 0.0289(19) 0.028(2) 0.0199(17) 0.0027(15) 0.0025(14) -0.0005(15)
C8 0.028(2) 0.0222(18) 0.0251(19) 0.0059(14) 0.0032(15) -0.0024(15)
C9 0.030(2) 0.0218(18) 0.0224(18) 0.0016(14) 0.0009(15) 0.0000(15)
C10 0.029(2) 0.027(2) 0.033(2) 0.0000(16) -0.0028(16) 0.0014(16)
C11 0.0254(19) 0.0264(19) 0.0261(19) -0.0056(15) 0.0011(15) -0.0032(15)
C12 0.029(2) 0.029(2) 0.0217(18) -0.0024(15) 0.0015(15) 0.0009(16)
O1 0.0479(19) 0.0214(16) 0.067(2) 0.0070(14) 0.0131(16) -0.0008(13)
O2 0.0451(18) 0.0397(18) 0.0454(18) 0.0076(14) 0.0219(15) 0.0044(14)
O3 0.0406(17) 0.0293(16) 0.0517(18) 0.0141(14) 0.0110(14) 0.0034(13)
O4 0.0346(16) 0.0381(16) 0.0317(15) 0.0065(12) 0.0086(12) -0.0049(13)
N1 0.0372(19) 0.0264(17) 0.0332(18) -0.0048(14) 0.0060(15) -0.0004(14)
N2 0.0261(17) 0.0295(17) 0.0314(17) 0.0046(14) 0.0073(13) 0.0011(13)
N3 0.039(2) 0.0219(18) 0.073(3) 0.0055(17) -0.026(2) 0.0024(15)
O8 0.0367(16) 0.0202(14) 0.0412(16) 0.0042(12) -0.0054(13) 0.0006(12)
O9 0.0300(16) 0.0344(16) 0.0420(17) -0.0107(13) -0.0057(13) 0.0009(12)
C19 0.0256(19) 0.0190(18) 0.030(2) -0.0036(15) -0.0019(15) -0.0002(15)
C13 0.031(2) 0.025(2) 0.036(2) -0.0064(17) -0.0029(17) 0.0068(17)
C14 0.031(2) 0.032(2) 0.054(3) -0.011(2) -0.005(2) 0.0081(18)
C15 0.019(3) 0.021(3) 0.026(4) -0.001(3) 0.002(3) -0.003(3)
C21 0.022(4) 0.024(4) 0.029(4) 0.006(3) 0.004(3) 0.004(3)
C17 0.029(4) 0.019(4) 0.019(3) -0.001(3) 0.005(3) -0.002(3)
C20 0.027(4) 0.021(4) 0.022(3) 0.001(3) 0.002(3) 0.015(3)
C16 0.030(4) 0.021(4) 0.019(3) -0.005(3) 0.005(3) 0.003(3)
C18 0.029(4) 0.020(4) 0.022(4) -0.002(3) 0.002(3) 0.002(3)

_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
C1 O2 1.209(5) . ?
C1 N1 1.365(5) . ?
C1 C2 1.517(5) . ?
C2 C9 1.530(5) . ?
C2 C3 1.543(5) . ?
C2 H2A 1.0000 . ?
C3 C12 1.509(5) . ?
C3 C4 1.553(5) . ?
C3 H3A 1.0000 . ?
C4 C5 1.504(5) . ?
C4 C7 1.548(5) . ?
C4 H4A 1.0000 . ?
C5 O3 1.210(5) . ?
C5 N2 1.388(5) . ?
C6 O4 1.228(5) . ?
C6 N2 1.370(5) . ?
C6 C7 1.499(5) . ?
C7 C8 1.555(5) . ?
C7 H7A 1.0000 . ?
C8 C11 1.500(5) . ?
C8 C9 1.558(5) . ?
C8 H8A 1.0000 . ?
C9 C10 1.518(5) . ?
C9 H9A 1.0000 . ?
C10 O1 1.208(5) . ?
C10 N1 1.393(5) . ?
C11 C12 1.332(5) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
N1 H1 0.9424 . ?
N2 H2 0.9422 . ?
N3 C14 1.311(6) . ?
N3 C13 1.317(5) . ?
N3 H3 1.1818 . ?
N3 H3' 0.9881 . ?
O8 C13 1.191(5) . ?
O9 C14 1.196(5) . ?
C19 C20 1.427(9) . ?
C19 C21 1.440(8) . ?
C19 C16 1.558(8) . ?
C19 C15 1.561(8) 3_656 ?
C19 C18 1.617(8) 3_656 ?
C19 C17 1.619(8) . ?
C19 H19A 1.0326 . ?
C13 C17 1.545(8) . ?
C13 C16 1.631(8) . ?
C14 C18 1.596(8) . ?
C14 C15 1.637(8) . ?
C15 C21 1.240(10) 3_656 ?
C15 C16 1.541(10) . ?
C15 C19 1.561(8) 3_656 ?
C15 C18 1.729(10) . ?
C15 C20 1.920(10) . ?
C15 H15A 0.9962 . ?
C21 C15 1.240(10) 3_656 ?
C21 C20 1.331(11) 3_656 ?
C21 C17 1.374(10) . ?
C21 C16 1.889(10) 3_656 ?
C21 C18 1.968(11) . ?
C21 H21A 1.0353 . ?
C21 H17A 1.4069 . ?
C17 C18 1.522(10) . ?
C17 C16 1.690(10) . ?
C17 C20 1.970(10) 3_656 ?
C17 H17A 1.0074 . ?
C20 C16 1.271(10) . ?
C20 C21 1.331(11) 3_656 ?
C20 C18 1.347(10) 3_656 ?
C20 C17 1.970(10) 3_656 ?
C20 H20A 0.9948 . ?
C20 H16A 1.4643 . ?
C16 C21 1.889(10) 3_656 ?
C16 H16A 1.0518 . ?
C18 C20 1.347(10) 3_656 ?
C18 C19 1.617(8) 3_656 ?
C18 H18A 1.1406 . ?

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
O2 C1 N1 125.1(4) . . ?
O2 C1 C2 126.5(4) . . ?
N1 C1 C2 108.4(3) . . ?
C1 C2 C9 105.2(3) . . ?
C1 C2 C3 112.3(3) . . ?
C9 C2 C3 110.6(3) . . ?
C1 C2 H2A 109.5 . . ?
C9 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C12 C3 C2 108.9(3) . . ?
C12 C3 C4 108.4(3) . . ?
C2 C3 C4 104.5(3) . . ?
C12 C3 H3A 111.6 . . ?
C2 C3 H3A 111.6 . . ?
C4 C3 H3A 111.6 . . ?
C5 C4 C7 104.9(3) . . ?
C5 C4 C3 111.5(3) . . ?
C7 C4 C3 109.4(3) . . ?
C5 C4 H4A 110.3 . . ?
C7 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
O3 C5 N2 123.2(4) . . ?
O3 C5 C4 128.5(4) . . ?
N2 C5 C4 108.3(3) . . ?
O4 C6 N2 123.7(4) . . ?
O4 C6 C7 126.8(4) . . ?
N2 C6 C7 109.5(3) . . ?
C6 C7 C4 104.1(3) . . ?
C6 C7 C8 111.8(3) . . ?
C4 C7 C8 110.0(3) . . ?
C6 C7 H7A 110.2 . . ?
C4 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
C11 C8 C7 107.7(3) . . ?
C11 C8 C9 108.2(3) . . ?
C7 C8 C9 105.8(3) . . ?
C11 C8 H8A 111.6 . . ?
C7 C8 H8A 111.6 . . ?
C9 C8 H8A 111.6 . . ?
C10 C9 C2 104.6(3) . . ?
C10 C9 C8 112.7(3) . . ?
C2 C9 C8 109.6(3) . . ?
C10 C9 H9A 110.0 . . ?
C2 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
O1 C10 N1 123.7(4) . . ?
O1 C10 C9 128.3(4) . . ?
N1 C10 C9 108.0(3) . . ?
C12 C11 C8 115.0(3) . . ?
C12 C11 H11A 122.5 . . ?
C8 C11 H11A 122.5 . . ?
C11 C12 C3 114.7(3) . . ?
C11 C12 H12A 122.7 . . ?
C3 C12 H12A 122.7 . . ?
C1 N1 C10 113.8(3) . . ?
C1 N1 H1 115.9 . . ?
C10 N1 H1 129.9 . . ?
C6 N2 C5 113.2(3) . . ?
C6 N2 H2 119.1 . . ?
C5 N2 H2 127.4 . . ?
C14 N3 C13 122.1(4) . . ?
C14 N3 H3 108.7 . . ?
C13 N3 H3 102.1 . . ?
C14 N3 H3' 116.6 . . ?
C13 N3 H3' 114.6 . . ?
H3 N3 H3' 83.5 . . ?
C20 C19 C21 127.8(5) . . ?
C20 C19 C16 50.2(4) . . ?
C21 C19 C16 110.2(5) . . ?
C20 C19 C15 111.3(4) . 3_656 ?
C21 C19 C15 48.6(4) . 3_656 ?
C16 C19 C15 140.6(4) . 3_656 ?
C20 C19 C18 52.1(4) . 3_656 ?
C21 C19 C18 108.3(4) . 3_656 ?
C16 C19 C18 101.6(4) . 3_656 ?
C15 C19 C18 65.9(4) 3_656 3_656 ?
C20 C19 C17 108.8(4) . . ?
C21 C19 C17 53.0(4) . . ?
C16 C19 C17 64.3(4) . . ?
C15 C19 C17 101.3(4) 3_656 . ?
C18 C19 C17 141.4(4) 3_656 . ?
C20 C19 H19A 120.1 . . ?
C21 C19 H19A 112.0 . . ?
C16 C19 H19A 114.4 . . ?
C15 C19 H19A 104.9 3_656 . ?
C18 C19 H19A 109.6 3_656 . ?
C17 C19 H19A 108.8 . . ?
O8 C13 N3 131.4(4) . . ?
O8 C13 C17 118.6(4) . . ?
N3 C13 C17 102.3(4) . . ?
O8 C13 C16 120.4(4) . . ?
N3 C13 C16 99.8(4) . . ?
C17 C13 C16 64.2(4) . . ?
O9 C14 N3 131.3(4) . . ?
O9 C14 C18 121.2(4) . . ?
N3 C14 C18 99.7(4) . . ?
O9 C14 C15 119.7(4) . . ?
N3 C14 C15 100.3(4) . . ?
C18 C14 C15 64.6(4) . . ?
C21 C15 C16 84.8(6) 3_656 . ?
C21 C15 C19 60.6(5) 3_656 3_656 ?
C16 C15 C19 108.9(5) . 3_656 ?
C21 C15 C14 165.4(7) 3_656 . ?
C16 C15 C14 103.0(5) . . ?
C19 C15 C14 105.0(5) 3_656 . ?
C21 C15 C18 112.2(6) 3_656 . ?
C16 C15 C18 88.4(5) . . ?
C19 C15 C18 58.6(4) 3_656 . ?
C14 C15 C18 56.5(4) . . ?
C21 C15 C20 43.5(5) 3_656 . ?
C16 C15 C20 41.3(4) . . ?
C19 C15 C20 84.5(4) 3_656 . ?
C14 C15 C20 142.9(5) . . ?
C18 C15 C20 103.7(5) . . ?
C21 C15 H15A 71.0 3_656 . ?
C16 C15 H15A 105.7 . . ?
C19 C15 H15A 115.9 3_656 . ?
C14 C15 H15A 117.5 . . ?
C18 C15 H15A 165.8 . . ?
C20 C15 H15A 88.1 . . ?
C15 C21 C20 96.6(6) 3_656 3_656 ?
C15 C21 C17 140.1(8) 3_656 . ?
C20 C21 C17 93.4(6) 3_656 . ?
C15 C21 C19 70.8(5) 3_656 . ?
C20 C21 C19 116.3(6) 3_656 . ?
C17 C21 C19 70.2(5) . . ?
C15 C21 C16 54.3(5) 3_656 3_656 ?
C20 C21 C16 42.2(4) 3_656 3_656 ?
C17 C21 C16 124.3(6) . 3_656 ?
C19 C21 C16 97.7(5) . 3_656 ?
C15 C21 C18 127.9(6) 3_656 . ?
C20 C21 C18 43.0(4) 3_656 . ?
C17 C21 C18 50.4(4) . . ?
C19 C21 C18 96.5(5) . . ?
C16 C21 C18 79.3(4) 3_656 . ?
C15 C21 H21A 103.4 3_656 . ?
C20 C21 H21A 121.0 3_656 . ?
C17 C21 H21A 104.1 . . ?
C19 C21 H21A 122.7 . . ?
C16 C21 H21A 125.7 3_656 . ?
C18 C21 H21A 124.2 . . ?
C15 C21 H17A 153.3 3_656 . ?
C20 C21 H17A 110.1 3_656 . ?
C17 C21 H17A 42.5 . . ?
C19 C21 H17A 97.5 . . ?
C16 C21 H17A 152.3 3_656 . ?
C18 C21 H17A 76.1 . . ?
H21A C21 H17A 62.0 . . ?
C21 C17 C18 85.5(6) . . ?
C21 C17 C13 163.0(6) . . ?
C18 C17 C13 104.3(5) . . ?
C21 C17 C19 56.8(4) . . ?
C18 C17 C19 109.5(5) . . ?
C13 C17 C19 106.3(4) . . ?
C21 C17 C16 106.3(6) . . ?
C18 C17 C16 90.5(5) . . ?
C13 C17 C16 60.4(4) . . ?
C19 C17 C16 56.1(4) . . ?
C21 C17 C20 42.4(4) . 3_656 ?
C18 C17 C20 43.0(4) . 3_656 ?
C13 C17 C20 145.2(5) . 3_656 ?
C19 C17 C20 81.4(4) . 3_656 ?
C16 C17 C20 101.3(5) . 3_656 ?
C21 C17 H17A 70.5 . . ?
C18 C17 H17A 112.9 . . ?
C13 C17 H17A 116.7 . . ?
C19 C17 H17A 106.9 . . ?
C16 C17 H17A 155.6 . . ?
C20 C17 H17A 92.1 3_656 . ?
C16 C20 C21 93.1(6) . 3_656 ?
C16 C20 C18 140.2(8) . 3_656 ?
C21 C20 C18 94.6(6) 3_656 3_656 ?
C16 C20 C19 70.2(5) . . ?
C21 C20 C19 115.8(6) 3_656 . ?
C18 C20 C19 71.2(5) 3_656 . ?
C16 C20 C15 53.1(5) . . ?
C21 C20 C15 39.9(4) 3_656 . ?
C18 C20 C15 124.2(6) 3_656 . ?
C19 C20 C15 97.9(5) . . ?
C16 C20 C17 125.2(6) . 3_656 ?
C21 C20 C17 44.1(4) 3_656 3_656 ?
C18 C20 C17 50.5(4) 3_656 3_656 ?
C19 C20 C17 96.4(4) . 3_656 ?
C15 C20 C17 78.4(4) . 3_656 ?
C16 C20 H20A 107.9 . . ?
C21 C20 H20A 129.9 3_656 . ?
C18 C20 H20A 96.7 3_656 . ?
C19 C20 H20A 114.0 . . ?
C15 C20 H20A 134.9 . . ?
C17 C20 H20A 125.4 3_656 . ?
C16 C20 H16A 44.5 . . ?
C21 C20 H16A 112.8 3_656 . ?
C18 C20 H16A 152.5 3_656 . ?
C19 C20 H16A 97.1 . . ?
C15 C20 H16A 81.3 . . ?
C17 C20 H16A 156.9 3_656 . ?
H20A C20 H16A 64.5 . . ?
C20 C16 C15 85.6(6) . . ?
C20 C16 C19 59.6(5) . . ?
C15 C16 C19 110.5(5) . . ?
C20 C16 C13 164.4(7) . . ?
C15 C16 C13 103.9(5) . . ?
C19 C16 C13 105.1(5) . . ?
C20 C16 C17 112.9(6) . . ?
C15 C16 C17 91.0(5) . . ?
C19 C16 C17 59.6(4) . . ?
C13 C16 C17 55.4(4) . . ?
C20 C16 C21 44.7(5) . 3_656 ?
C15 C16 C21 40.8(4) . 3_656 ?
C19 C16 C21 84.8(4) . 3_656 ?
C13 C16 C21 143.1(5) . 3_656 ?
C17 C16 C21 105.2(5) . 3_656 ?
C20 C16 H16A 77.5 . . ?
C15 C16 H16A 117.5 . . ?
C19 C16 H16A 110.9 . . ?
C13 C16 H16A 108.0 . . ?
C17 C16 H16A 150.9 . . ?
C21 C16 H16A 100.9 3_656 . ?
C20 C18 C17 86.5(6) 3_656 . ?
C20 C18 C14 160.7(7) 3_656 . ?
C17 C18 C14 104.3(5) . . ?
C20 C18 C19 56.7(4) 3_656 3_656 ?
C17 C18 C19 109.1(5) . 3_656 ?
C14 C18 C19 104.3(5) . 3_656 ?
C20 C18 C15 106.1(6) 3_656 . ?
C17 C18 C15 90.1(5) . . ?
C14 C18 C15 58.8(4) . . ?
C19 C18 C15 55.5(3) 3_656 . ?
C20 C18 C21 42.4(4) 3_656 . ?
C17 C18 C21 44.1(4) . . ?
C14 C18 C21 145.7(5) . . ?
C19 C18 C21 80.7(4) 3_656 . ?
C15 C18 C21 101.3(5) . . ?
C20 C18 H18A 72.8 3_656 . ?
C17 C18 H18A 114.5 . . ?
C14 C18 H18A 115.3 . . ?
C19 C18 H18A 108.8 3_656 . ?
C15 C18 H18A 155.0 . . ?
C21 C18 H18A 94.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.064