# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bb
_audit_block_doi                 10.5517/ccdc.csd.cc1q9pb1
_database_code_depnum_ccdc_archive 'CCDC 1588233'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 Ag10 N16 O44 Si W12'
_chemical_formula_sum            'C4 H12 Ag10 N16 O44 Si W12'
_chemical_formula_weight         4301.10

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'
P P 0.1023 0.0942 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I-4m2 '

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

_cell_length_a                   14.198(5)
_cell_length_b                   14.198(5)
_cell_length_c                   12.297(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2479(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3371
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      28.41

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3728.0
_exptl_absorpt_coefficient_mu    31.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_T_max  0.022
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            9241
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         28.41
_reflns_number_total             1692
_reflns_number_gt                1621
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The restraint commands 'ISOR' were used to refine the non-H atoms with ADP problems. These atoms are as follows: O1 O3 O4 O5 C1 N1 and N2.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0502P)²+197.9268P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.376(19)
_refine_ls_number_reflns         1684
_refine_ls_number_parameters     112
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_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
W1 W 0.12934(4) 0.38255(4) 0.95299(4) 0.01009(15) Uani 1 1 d . . .
Si1 Si 0.0000 0.5000 0.7500 0.0009(15) Uani 1 8 d S . .
W2 W 0.0000 0.25241(5) 0.74194(7) 0.00910(17) Uani 1 2 d S . .
O2 O 0.1723(7) 0.3075(7) 1.0490(8) 0.014(2) Uani 1 1 d . . .
O1 O 0.1498(9) 0.5000 1.0263(11) 0.006(2) Uani 1 2 d SU . .
O8 O 0.0000 0.1350(9) 0.7677(14) 0.014(3) Uani 1 2 d S . .
O5 O 0.0930(7) 0.2965(7) 0.8410(7) 0.0056(18) Uani 1 1 d U . .
O3 O 0.0000 0.3868(9) 0.9898(10) 0.006(2) Uani 1 2 d SU . .
Ag1 Ag 0.11750(9) 0.11750(9) 0.5000 0.0118(3) Uani 1 2 d S . .
O6 O 0.0944(7) 0.2582(7) 0.6289(7) 0.0069(18) Uani 1 1 d . . .
Ag2 Ag 0.22981(8) 0.27019(8) 0.2500 0.0174(3) Uani 1 2 d S . .
N1 N 0.0775(8) 0.2172(8) 0.2706(9) 0.010(2) Uani 1 1 d U . .
C1 C 0.0000 0.2426(16) 0.2159(18) 0.017(5) Uani 1 2 d SU . .
H1 H 0.0000 0.2736 0.1493 0.020 Uiso 1 2 calc SR . .
N2 N 0.0465(8) 0.1696(8) 0.3564(9) 0.006(2) Uani 1 1 d U . .
O4 O 0.0936(9) 0.5000 0.8263(11) 0.004(2) Uani 1 2 d SU . .
O7 O 0.1104(13) 0.1104(13) 0.0000 0.044(6) Uani 1 2 d S . .
Ag3 Ag 0.0000 0.0000 0.8785(4) 0.091(2) Uani 1 4 d S . .

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
W1 0.0103(3) 0.0121(3) 0.0078(2) 0.0024(2) -0.0017(2) 0.00057(17)
Si1 0.001(2) 0.001(2) 0.002(4) 0.000 0.000 0.000
W2 0.0124(4) 0.0071(3) 0.0078(3) 0.0001(3) 0.000 0.000
O2 0.014(5) 0.015(5) 0.013(5) 0.000(4) -0.006(4) 0.002(4)
O1 0.006(3) 0.006(3) 0.006(3) 0.000 -0.0003(10) 0.000
O8 0.023(8) 0.005(6) 0.014(8) 0.001(6) 0.000 0.000
O5 0.0056(19) 0.0058(19) 0.005(2) -0.0001(10) -0.0002(10) -0.0001(10)
O3 0.006(3) 0.006(3) 0.006(3) -0.0002(10) 0.000 0.000
Ag1 0.0146(5) 0.0146(5) 0.0061(7) 0.0034(4) -0.0034(4) 0.0041(6)
O6 0.009(5) 0.007(4) 0.005(4) 0.001(4) 0.003(4) 0.001(3)
Ag2 0.0176(5) 0.0176(5) 0.0169(7) 0.0033(5) 0.0033(5) -0.0075(5)
N1 0.010(2) 0.010(2) 0.010(2) 0.0002(10) 0.0002(10) 0.0001(10)
C1 0.017(5) 0.017(5) 0.017(5) 0.0002(10) 0.000 0.000
N2 0.006(2) 0.006(2) 0.006(2) 0.0004(10) 0.0001(10) 0.0000(10)
O4 0.004(2) 0.004(2) 0.004(2) 0.000 0.0001(10) 0.000
O7 0.053(9) 0.053(9) 0.025(12) -0.005(7) 0.005(7) -0.006(14)
Ag3 0.190(8) 0.033(2) 0.049(3) 0.000 0.000 0.000

_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
W1 O2 1.704(10) . ?
W1 O3 1.892(3) . ?
W1 O5 1.913(9) . ?
W1 O6 1.916(9) 11_556 ?
W1 O1 1.918(7) . ?
W1 O4 2.338(9) . ?
Si1 O4 1.626(13) 11_556 ?
Si1 O4 1.626(13) . ?
Si1 O4 1.626(13) 12_456 ?
Si1 O4 1.626(13) 2_565 ?
W2 O8 1.697(14) . ?
W2 O5 1.902(9) . ?
W2 O5 1.902(9) 5 ?
W2 O6 1.933(9) 5 ?
W2 O6 1.933(9) . ?
W2 O4 2.342(13) 11_556 ?
O1 W1 1.918(7) 6_565 ?
O8 Ag3 2.352(15) . ?
O3 W1 1.892(3) 5 ?
Ag1 N2 2.163(11) . ?
Ag1 N2 2.163(11) 4_556 ?
Ag1 O6 2.571(10) . ?
Ag1 O6 2.571(10) 4_556 ?
Ag1 Ag1 3.336(3) 5 ?
Ag1 Ag1 3.336(3) 6 ?
O6 W1 1.916(9) 11_556 ?
Ag2 N1 2.303(11) 11 ?
Ag2 N1 2.303(11) . ?
N1 N2 1.328(16) . ?
N1 C1 1.339(16) . ?
C1 N1 1.339(16) 5 ?
N2 N2 1.32(2) 5 ?
O4 W1 2.338(9) 6_565 ?
O4 W2 2.342(13) 11_556 ?
Ag3 O8 2.352(15) 2 ?
Ag3 Ag3 2.988(10) 3_557 ?

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 W1 O3 101.7(5) . . ?
O2 W1 O5 101.3(4) . . ?
O3 W1 O5 86.0(5) . . ?
O2 W1 O6 99.9(5) . 11_556 ?
O3 W1 O6 158.3(5) . 11_556 ?
O5 W1 O6 87.5(4) . 11_556 ?
O2 W1 O1 99.4(5) . . ?
O3 W1 O1 90.4(6) . . ?
O5 W1 O1 159.3(4) . . ?
O6 W1 O1 88.4(5) 11_556 . ?
O2 W1 O4 170.3(5) . . ?
O3 W1 O4 85.7(5) . . ?
O5 W1 O4 85.2(4) . . ?
O6 W1 O4 73.1(4) 11_556 . ?
O1 W1 O4 74.1(4) . . ?
O4 Si1 O4 109.4(5) 11_556 . ?
O4 Si1 O4 109.6(9) 11_556 12_456 ?
O4 Si1 O4 109.4(5) . 12_456 ?
O4 Si1 O4 109.4(5) 11_556 2_565 ?
O4 Si1 O4 109.6(9) . 2_565 ?
O4 Si1 O4 109.4(5) 12_456 2_565 ?
O8 W2 O5 101.7(5) . . ?
O8 W2 O5 101.7(5) . 5 ?
O5 W2 O5 87.9(6) . 5 ?
O8 W2 O6 100.1(5) . 5 ?
O5 W2 O6 158.1(4) . 5 ?
O5 W2 O6 88.0(4) 5 5 ?
O8 W2 O6 100.1(5) . . ?
O5 W2 O6 88.0(4) . . ?
O5 W2 O6 158.1(4) 5 . ?
O6 W2 O6 87.8(6) 5 . ?
O8 W2 O4 169.8(7) . 11_556 ?
O5 W2 O4 85.5(4) . 11_556 ?
O5 W2 O4 85.5(4) 5 11_556 ?
O6 W2 O4 72.7(4) 5 11_556 ?
O6 W2 O4 72.7(4) . 11_556 ?
W1 O1 W1 120.8(7) . 6_565 ?
W2 O8 Ag3 155.3(9) . . ?
W2 O5 W1 149.2(5) . . ?
W1 O3 W1 152.1(8) . 5 ?
N2 Ag1 N2 170.0(6) . 4_556 ?
N2 Ag1 O6 100.3(4) . . ?
N2 Ag1 O6 84.4(4) 4_556 . ?
N2 Ag1 O6 84.4(4) . 4_556 ?
N2 Ag1 O6 100.3(4) 4_556 4_556 ?
O6 Ag1 O6 125.3(4) . 4_556 ?
N2 Ag1 Ag1 62.2(3) . 5 ?
N2 Ag1 Ag1 110.0(3) 4_556 5 ?
O6 Ag1 Ag1 82.7(2) . 5 ?
O6 Ag1 Ag1 141.0(2) 4_556 5 ?
N2 Ag1 Ag1 110.0(3) . 6 ?
N2 Ag1 Ag1 62.2(3) 4_556 6 ?
O6 Ag1 Ag1 141.0(2) . 6 ?
O6 Ag1 Ag1 82.7(2) 4_556 6 ?
Ag1 Ag1 Ag1 90.0 5 6 ?
W1 O6 W2 122.1(5) 11_556 . ?
W1 O6 Ag1 107.6(4) 11_556 . ?
W2 O6 Ag1 119.9(4) . . ?
N1 Ag2 N1 128.7(6) 11 . ?
N2 N1 C1 105.3(12) . . ?
N2 N1 Ag2 124.4(8) . . ?
C1 N1 Ag2 128.9(10) . . ?
N1 C1 N1 110.6(18) 5 . ?
N2 N2 N1 109.3(7) 5 . ?
N2 N2 Ag1 117.8(3) 5 . ?
N1 N2 Ag1 131.9(9) . . ?
Si1 O4 W1 124.2(4) . 6_565 ?
Si1 O4 W1 124.2(4) . . ?
W1 O4 W1 91.0(5) 6_565 . ?
Si1 O4 W2 123.8(7) . 11_556 ?
W1 O4 W2 92.1(4) 6_565 11_556 ?
W1 O4 W2 92.1(4) . 11_556 ?
O8 Ag3 O8 109.2(8) 2 . ?
O8 Ag3 Ag3 125.4(4) 2 3_557 ?
O8 Ag3 Ag3 125.4(4) . 3_557 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.978
_refine_diff_density_min         -4.731
_refine_diff_density_rms         0.616
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_llllll
_audit_block_doi                 10.5517/ccdc.csd.cc1q9vb6
_database_code_depnum_ccdc_archive 'CCDC 1588388'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 Ag10 N16 O44 P W12'
_chemical_formula_sum            'C4 H12 Ag10 N16 O44 P W12'
_chemical_formula_weight         4303.98

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'
P P 0.1023 0.0942 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I-4m2 '

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

_cell_length_a                   14.182(5)
_cell_length_b                   14.182(5)
_cell_length_c                   12.331(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2480.(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5024
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      28.41

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3730.0
_exptl_absorpt_coefficient_mu    31.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_T_max  0.022
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            9219
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         28.42
_reflns_number_total             1690
_reflns_number_gt                1649
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The restraint commands 'ISOR' were used to refine the non-H atoms with ADP problems. These atoms are as follows: O1 O3 O6 O7 N1 N2 C1 and Ag1.Furthermore, the data was not of the best quality, resulting in poor thermal parameters for the lighter atom (P1). Thus, the P1 atom was left isotropic, however the overall structural connectivity is still clearly visible.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0773P)²+894.5024P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.58(2)
_refine_ls_number_reflns         1688
_refine_ls_number_parameters     111
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1228
_refine_ls_wR_factor_gt          0.1219
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_restrained_S_all      0.816
_refine_ls_shift/su_max          0.000
_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
W1 W 0.74975(7) 0.5000 1.00665(9) 0.0097(2) Uani 1 2 d S . .
W2 W 0.61964(5) 0.62915(5) 0.79662(5) 0.01030(18) Uani 1 1 d . . .
O2 O 0.7056(9) 0.5934(9) 0.9074(9) 0.006(2) Uani 1 1 d . . .
Ag1 Ag 0.61826(11) 0.88174(11) 0.7500 0.0100(4) Uani 1 2 d SU . .
O1 O 0.8662(12) 0.5000 0.9839(16) 0.010(3) Uani 1 2 d SU . .
O4 O 0.6924(9) 0.6738(9) 0.7003(10) 0.012(2) Uani 1 1 d . . .
O7 O 0.5000 0.5888(11) 0.9280(13) 0.002(3) Uani 1 2 d SU . .
O3 O 0.6160(12) 0.5000 0.7599(13) 0.005(3) Uani 1 2 d SU . .
O5 O 0.5000 0.6472(13) 0.7288(13) 0.007(3) Uani 1 2 d S . .
O6 O 0.5939(9) 0.7404(8) 0.8794(9) 0.006(2) Uani 1 1 d U . .
Ag3 Ag 1.0000 0.5000 0.8653(7) 0.100(3) Uani 1 4 d S . .
Ag2 Ag 0.73095(10) 0.73095(10) 0.5000 0.0149(4) Uani 1 2 d S . .
O8 O 0.8909(15) 0.6091(15) 0.7500 0.035(7) Uani 1 2 d S . .
N2 N 0.5781(10) 0.7831(10) 0.5195(12) 0.012(3) Uani 1 1 d U . .
N1 N 0.5469(9) 0.8294(10) 0.6077(11) 0.004(2) Uani 1 1 d U . .
C1 C 0.5000 0.757(2) 0.464(2) 0.018(6) Uani 1 2 d SU . .
H1 H 0.5000 0.7258 0.3975 0.022 Uiso 1 2 calc SR . .
P1 P 0.5000 0.5000 1.0000 0.0001(16) Uiso 1 8 d S . .

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
W1 0.0072(4) 0.0129(4) 0.0089(4) 0.000 -0.0002(4) 0.000
W2 0.0127(3) 0.0103(3) 0.0079(3) 0.0017(3) 0.0027(3) -0.0008(2)
O2 0.009(6) 0.005(5) 0.004(5) 0.001(4) -0.001(4) -0.001(4)
Ag1 0.0114(5) 0.0114(5) 0.0070(7) -0.0027(4) -0.0027(4) -0.0027(6)
O1 0.010(4) 0.010(4) 0.010(4) 0.000 0.0001(10) 0.000
O4 0.013(6) 0.013(6) 0.011(5) 0.006(5) -0.001(5) -0.002(5)
O7 0.003(3) 0.002(3) 0.002(3) -0.0001(10) 0.000 0.000
O3 0.005(3) 0.005(3) 0.005(3) 0.000 -0.0002(10) 0.000
O5 0.002(7) 0.012(8) 0.006(8) 0.001(6) 0.000 0.000
O6 0.006(2) 0.006(2) 0.005(2) -0.0001(10) 0.0002(10) -0.0001(10)
Ag3 0.048(4) 0.188(11) 0.064(4) 0.000 0.000 0.000
Ag2 0.0149(5) 0.0149(5) 0.0151(8) -0.0023(6) 0.0023(6) 0.0070(6)
O8 0.047(10) 0.047(10) 0.011(11) -0.008(8) -0.008(8) 0.004(15)
N2 0.011(3) 0.012(3) 0.012(3) -0.0003(10) 0.0002(10) 0.0000(10)
N1 0.004(3) 0.004(3) 0.004(3) -0.0001(10) -0.0001(10) -0.0001(10)
C1 0.018(6) 0.018(6) 0.018(6) -0.0001(10) 0.000 0.000

_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
W1 O1 1.675(17) . ?
W1 O2 1.909(12) 6_565 ?
W1 O2 1.909(12) . ?
W1 O6 1.940(12) 4_557 ?
W1 O6 1.940(12) 8_567 ?
W1 O7 2.421(16) 4_557 ?
W2 O4 1.696(12) . ?
W2 O3 1.888(4) . ?
W2 O2 1.900(12) . ?
W2 O5 1.909(8) . ?
W2 O6 1.914(12) . ?
W2 O7 2.415(11) . ?
Ag1 N1 2.157(14) 11_666 ?
Ag1 N1 2.157(14) . ?
Ag1 O6 2.586(12) 11_666 ?
Ag1 O6 2.586(12) . ?
Ag1 Ag1 3.354(3) 6_575 ?
Ag1 Ag1 3.354(3) 5_655 ?
O1 Ag3 2.395(18) . ?
O7 P1 1.541(16) . ?
O7 W1 2.421(16) 4_557 ?
O7 W2 2.415(11) 5_655 ?
O3 W2 1.888(4) 6_565 ?
O5 W2 1.909(8) 5_655 ?
O6 W1 1.940(12) 4_557 ?
Ag3 O1 2.395(19) 2_765 ?
Ag3 O8 2.61(3) 6_565 ?
Ag3 O8 2.61(3) . ?
Ag3 O8 2.61(3) 5_755 ?
Ag3 O8 2.61(3) 2_765 ?
Ag3 Ag3 2.845(16) 11_666 ?
Ag2 N2 2.303(14) 4_556 ?
Ag2 N2 2.303(14) . ?
O8 Ag3 2.61(3) 11_666 ?
N2 N1 1.345(19) . ?
N2 C1 1.35(2) . ?
N1 N1 1.33(3) 5_655 ?
C1 N2 1.35(2) 5_655 ?
P1 O7 1.541(16) 4_557 ?
P1 O7 1.541(16) 3_667 ?
P1 O7 1.541(16) 2_665 ?

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
O1 W1 O2 102.5(6) . 6_565 ?
O1 W1 O2 102.5(6) . . ?
O2 W1 O2 87.9(7) 6_565 . ?
O1 W1 O6 100.9(6) . 4_557 ?
O2 W1 O6 156.6(6) 6_565 4_557 ?
O2 W1 O6 88.0(5) . 4_557 ?
O1 W1 O6 100.9(6) . 8_567 ?
O2 W1 O6 88.0(5) 6_565 8_567 ?
O2 W1 O6 156.6(6) . 8_567 ?
O6 W1 O6 86.7(7) 4_557 8_567 ?
O1 W1 O7 170.2(8) . 4_557 ?
O2 W1 O7 84.5(5) 6_565 4_557 ?
O2 W1 O7 84.5(5) . 4_557 ?
O6 W1 O7 72.2(4) 4_557 4_557 ?
O6 W1 O7 72.2(4) 8_567 4_557 ?
O4 W2 O3 102.2(7) . . ?
O4 W2 O2 102.3(5) . . ?
O3 W2 O2 86.1(6) . . ?
O4 W2 O5 100.6(6) . . ?
O3 W2 O5 90.0(7) . . ?
O2 W2 O5 157.1(6) . . ?
O4 W2 O6 100.5(6) . . ?
O3 W2 O6 157.3(6) . . ?
O2 W2 O6 87.6(5) . . ?
O5 W2 O6 87.4(7) . . ?
O4 W2 O7 170.3(5) . . ?
O3 W2 O7 84.9(6) . . ?
O2 W2 O7 84.6(5) . . ?
O5 W2 O7 72.6(5) . . ?
O6 W2 O7 72.8(5) . . ?
W2 O2 W1 148.9(7) . . ?
N1 Ag1 N1 169.9(7) 11_666 . ?
N1 Ag1 O6 100.0(5) 11_666 11_666 ?
N1 Ag1 O6 84.7(5) . 11_666 ?
N1 Ag1 O6 84.7(5) 11_666 . ?
N1 Ag1 O6 100.0(5) . . ?
O6 Ag1 O6 126.0(5) 11_666 . ?
N1 Ag1 Ag1 62.0(4) 11_666 6_575 ?
N1 Ag1 Ag1 110.1(4) . 6_575 ?
O6 Ag1 Ag1 82.3(3) 11_666 6_575 ?
O6 Ag1 Ag1 140.8(3) . 6_575 ?
N1 Ag1 Ag1 110.1(4) 11_666 5_655 ?
N1 Ag1 Ag1 62.0(4) . 5_655 ?
O6 Ag1 Ag1 140.8(3) 11_666 5_655 ?
O6 Ag1 Ag1 82.3(3) . 5_655 ?
Ag1 Ag1 Ag1 90.0 6_575 5_655 ?
W1 O1 Ag3 152.0(11) . . ?
P1 O7 W1 125.4(9) . 4_557 ?
P1 O7 W2 125.5(5) . 5_655 ?
W1 O7 W2 90.0(5) 4_557 5_655 ?
P1 O7 W2 125.5(5) . . ?
W1 O7 W2 90.0(5) 4_557 . ?
W2 O7 W2 89.3(5) 5_655 . ?
W2 O3 W2 152.0(10) . 6_565 ?
W2 O5 W2 125.5(9) . 5_655 ?
W2 O6 W1 125.0(6) . 4_557 ?
W2 O6 Ag1 106.5(5) . . ?
W1 O6 Ag1 119.0(5) 4_557 . ?
O1 Ag3 O1 104.8(9) 2_765 . ?
O1 Ag3 O8 143.35(14) 2_765 6_565 ?
O1 Ag3 O8 82.1(5) . 6_565 ?
O1 Ag3 O8 143.35(14) 2_765 . ?
O1 Ag3 O8 82.1(5) . . ?
O8 Ag3 O8 72.7(4) 6_565 . ?
O1 Ag3 O8 82.1(5) 2_765 5_755 ?
O1 Ag3 O8 143.35(14) . 5_755 ?
O8 Ag3 O8 114.0(8) 6_565 5_755 ?
O8 Ag3 O8 72.7(4) . 5_755 ?
O1 Ag3 O8 82.1(5) 2_765 2_765 ?
O1 Ag3 O8 143.35(14) . 2_765 ?
O8 Ag3 O8 72.7(4) 6_565 2_765 ?
O8 Ag3 O8 114.0(8) . 2_765 ?
O8 Ag3 O8 72.7(4) 5_755 2_765 ?
O1 Ag3 Ag3 127.6(5) 2_765 11_666 ?
O1 Ag3 Ag3 127.6(5) . 11_666 ?
O8 Ag3 Ag3 57.0(4) 6_565 11_666 ?
O8 Ag3 Ag3 57.0(4) . 11_666 ?
O8 Ag3 Ag3 57.0(4) 5_755 11_666 ?
O8 Ag3 Ag3 57.0(4) 2_765 11_666 ?
N2 Ag2 N2 128.0(7) 4_556 . ?
Ag3 O8 Ag3 66.0(8) . 11_666 ?
N1 N2 C1 105.9(15) . . ?
N1 N2 Ag2 123.4(10) . . ?
C1 N2 Ag2 129.0(13) . . ?
N1 N1 N2 109.2(8) 5_655 . ?
N1 N1 Ag1 118.0(4) 5_655 . ?
N2 N1 Ag1 132.2(11) . . ?
N2 C1 N2 110(2) . 5_655 ?
O7 P1 O7 109.6(12) 4_557 3_667 ?
O7 P1 O7 109.4(6) 4_557 2_665 ?
O7 P1 O7 109.4(6) 3_667 2_665 ?
O7 P1 O7 109.4(6) 4_557 . ?
O7 P1 O7 109.4(6) 3_667 . ?
O7 P1 O7 109.6(12) 2_665 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.42
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.939
_refine_diff_density_min         -4.803
_refine_diff_density_rms         0.608
