# 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 2017

####################################################################### 
# 
# 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_zhn20140612_1223_0m
_database_code_depnum_ccdc_archive 'CCDC 1038934'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H28 Ag9 N12 O40 P W12'
_chemical_formula_sum            'C42 H28 Ag9 N12 O40 P W12'
_chemical_formula_weight         4548.65

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'
W W -0.8490 6.8722 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.080(2)
_cell_length_b                   12.781(3)
_cell_length_c                   15.660(3)
_cell_angle_alpha                80.391(4)
_cell_angle_beta                 71.443(4)
_cell_angle_gamma                74.048(4)
_cell_volume                     1832.1(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    14742
_cell_measurement_theta_min      1.38
_cell_measurement_theta_max      28.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2010
_exptl_absorpt_coefficient_mu    21.206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3156
_exptl_absorpt_correction_T_max  0.4184
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 Smart APEX 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            14742
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         28.50
_reflns_number_total             9229
_reflns_number_gt                7462
_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    SHELXP-97
_computing_publication_material  SHELXTL

_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. 
;

_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)+(0.0366P)²+605.1519P] 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_number_reflns         9229
_refine_ls_number_parameters     544
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0743
_refine_ls_wR_factor_ref         0.1229
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.062
_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
W1 W 0.23544(12) 0.98307(11) 0.63161(8) 0.0206(3) Uani 1 1 d U . .
W2 W 0.01240(14) 0.79580(10) 0.68005(8) 0.0220(3) Uani 1 1 d . . .
W3 W 0.30919(13) 0.78049(10) 0.48301(9) 0.0225(3) Uani 1 1 d D . .
W4 W 0.29036(13) 0.98064(13) 0.29976(8) 0.0258(3) Uani 1 1 d U . .
W5 W 0.23072(14) 1.18170(11) 0.44709(10) 0.0266(3) Uani 1 1 d U . .
W6 W 0.06807(16) 0.79463(11) 0.35746(9) 0.0260(3) Uani 1 1 d . . .
Ag1 Ag 0.3890(3) 0.8880(2) 0.85459(19) 0.0317(6) Uani 1 1 d . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0386(10) Uani 1 2 d S . .
Ag3 Ag 0.7453(3) 0.7660(3) 0.8967(2) 0.0363(7) Uani 1 1 d . . .
N2 N 0.523(3) 0.729(2) 0.8191(18) 0.0206(11) Uani 1 1 d U . .
C1 C 0.297(3) 1.062(3) 0.983(2) 0.0217(10) Uani 1 1 d U . .
O1 O 0.336(3) 1.271(2) 0.4228(17) 0.0301(11) Uani 1 1 d U . .
O2 O 0.4704(16) 0.6629(15) 0.476(3) 0.057(4) Uani 1 1 d DU . .
O3 O 0.020(2) 0.6988(19) 0.7683(16) 0.0265(11) Uani 1 1 d U . .
O4 O 0.428(3) 0.971(2) 0.2019(18) 0.035(7) Uani 1 1 d . . .
O5 O 0.100(3) 0.702(2) 0.2860(18) 0.048(8) Uani 1 1 d . . .
C2 C 0.492(4) 0.659(3) 0.778(3) 0.032(3) Uani 1 1 d U . .
C3 C 0.079(4) 1.157(3) 0.996(2) 0.0263(10) Uani 1 1 d U . .
C4 C 0.103(4) 1.092(3) 0.933(2) 0.0271(10) Uani 1 1 d U . .
C5 C 0.609(4) 0.571(3) 0.761(2) 0.0302(10) Uani 1 1 d U . .
N4 N 0.197(3) 1.141(3) 1.0274(19) 0.029(7) Uani 1 1 d . . .
N1 N 0.711(3) 0.592(2) 0.794(2) 0.0287(11) Uani 1 1 d U . .
C6 C 0.366(4) 0.662(3) 0.754(3) 0.034(3) Uani 1 1 d U . .
H1 H 0.2833 0.7186 0.7670 0.041 Uiso 1 1 calc R . .
C7 C 0.4927(19) 0.489(2) 0.691(2) 0.042(2) Uani 1 1 d DU . .
H2 H 0.4709 0.4189 0.6911 0.050 Uiso 1 1 calc R . .
C8 C 0.6086(13) 0.482(3) 0.718(2) 0.038(2) Uani 1 1 d DU . .
H3 H 0.6653 0.4099 0.7331 0.046 Uiso 1 1 calc R . .
C9 C -0.126(4) 1.161(3) 0.912(2) 0.030(3) Uani 1 1 d U . .
H4 H -0.1949 1.1635 0.8841 0.036 Uiso 1 1 calc R . .
C10 C -0.157(4) 1.238(3) 0.978(3) 0.0332(10) Uani 1 1 d U . .
H5 H -0.2450 1.2887 0.9916 0.040 Uiso 1 1 calc R . .
C11 C 0.001(4) 1.085(3) 0.891(2) 0.029(3) Uani 1 1 d U . .
H6 H 0.0198 1.0326 0.8511 0.035 Uiso 1 1 calc R . .
O6 O 0.337(3) 0.972(2) 0.698(2) 0.0439(11) Uani 1 1 d U . .
O7 O 0.127(4) 0.879(3) 0.702(2) 0.0538(11) Uani 1 1 d U . .
O8 O 0.197(4) 0.886(3) 0.284(3) 0.0731(11) Uani 1 1 d U . .
O9 O 0.377(4) 0.869(3) 0.375(3) 0.0609(11) Uani 1 1 d U . .
O10 O -0.106(4) 0.757(3) 0.625(3) 0.0652(11) Uani 1 1 d U . .
O11 O 0.300(4) 1.087(3) 0.529(3) 0.0596(11) Uani 1 1 d U . .
C16 C -0.057(4) 1.237(3) 1.020(2) 0.029(3) Uani 1 1 d U . .
H7 H -0.0751 1.2863 1.0629 0.034 Uiso 1 1 calc R . .
O12 O 0.179(4) 0.724(3) 0.591(2) 0.0527(11) Uani 1 1 d U . .
O13 O -0.160(5) 0.910(4) 0.737(3) 0.104(13) Uani 1 1 d . . .
O14 O 0.331(4) 1.076(3) 0.356(3) 0.0678(11) Uani 1 1 d U . .
O15 O 0.354(4) 0.864(3) 0.554(3) 0.0614(11) Uani 1 1 d U . .
O16 O 0.078(4) 1.097(3) 0.680(3) 0.0651(11) Uani 1 1 d U . .
O17 O 0.071(4) 1.248(3) 0.541(3) 0.0677(11) Uani 1 1 d U . .
O18 O 0.208(4) 0.735(3) 0.418(2) 0.0555(11) Uani 1 1 d U . .
Ag4 Ag 0.9238(3) 0.4904(3) 0.7831(3) 0.0487(9) Uani 1 1 d . . .
N3 N 0.246(3) 1.026(3) 0.9254(19) 0.026(6) Uani 1 1 d . . .
C12 C 0.653(3) 0.687(3) 0.830(2) 0.0246(10) Uani 1 1 d U . .
N6 N 1.127(4) 0.384(3) 0.787(3) 0.0433(11) Uani 1 1 d U . .
C13 C 1.206(5) 0.389(4) 0.845(4) 0.0552(10) Uani 1 1 d U . .
C14 C 1.197(6) 0.303(5) 0.744(4) 0.0632(10) Uani 1 1 d U . .
H14 H 1.1603 0.2753 0.7072 0.076 Uiso 1 1 calc R . .
C20 C 1.338(6) 0.304(5) 0.832(4) 0.0599(7) Uani 1 1 d U . .
N5 N 1.332(4) 0.257(3) 0.754(2) 0.0387(11) Uani 1 1 d U . .
H13 H 1.3988 0.2098 0.7215 0.046 Uiso 1 1 calc R . .
O20 O 0.109(4) 0.918(4) 0.553(3) 0.021(4) Uani 0.50 1 d PU . .
O21 O 0.132(8) 0.915(6) 0.431(5) 0.0602(11) Uani 0.50 1 d PU . .
Ag5 Ag 0.6388(3) 0.5540(3) 0.5454(3) 0.0565(8) Uani 1 1 d U . .
C21 C 0.3762(18) 0.574(2) 0.709(2) 0.035(3) Uani 1 1 d DU . .
H8 H 0.2974 0.5729 0.6910 0.042 Uiso 1 1 calc R . .
O19 O 0.096(6) 1.072(5) 0.418(4) 0.0417(11) Uani 0.50 1 d PU . .
C15 C 1.1853(15) 0.454(4) 0.917(3) 0.0588(10) Uani 1 1 d DU . .
H9 H 1.0998 0.5061 0.9365 0.071 Uiso 1 1 calc R . .
C18 C 1.439(6) 0.293(5) 0.872(4) 0.060(2) Uani 1 1 d U . .
H10 H 1.5244 0.2391 0.8585 0.072 Uiso 1 1 calc R . .
C17 C 1.4142(19) 0.359(3) 0.931(3) 0.0587(10) Uani 1 1 d DU . .
H11 H 1.4864 0.3531 0.9581 0.070 Uiso 1 1 calc R . .
C19 C 1.292(3) 0.438(3) 0.958(4) 0.0603(10) Uani 1 1 d DU . .
H12 H 1.2808 0.4807 1.0037 0.072 Uiso 1 1 calc R . .
P1 P 0.0000 1.0000 0.5000 0.014(2) Uani 1 2 d SU . .
O22 O -0.079(4) 0.929(3) 0.460(3) 0.0190(11) Uani 0.50 1 d PU . .


_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 O6 1.65(3) . ?
W1 O16 1.89(4) . ?
W1 O7 1.93(3) . ?
W1 O11 1.97(4) . ?
W1 O15 1.97(4) . ?
W1 O20 2.39(5) . ?
W1 O22 2.39(4) 2_576 ?
W2 O3 1.70(2) . ?
W2 O10 1.88(4) . ?
W2 O7 1.91(4) . ?
W2 O12 1.92(3) . ?
W2 O13 1.99(4) . ?
W2 O19 2.36(6) 2_576 ?
W2 O20 2.43(4) . ?
W3 O15 1.89(4) . ?
W3 O18 1.89(4) . ?
W3 O2 1.873(10) . ?
W3 O9 1.91(4) . ?
W3 O12 1.95(3) . ?
W3 O21 2.36(7) . ?
W3 O20 2.37(4) . ?
W4 O4 1.70(2) . ?
W4 O13 1.79(4) 2_576 ?
W4 O14 1.82(4) . ?
W4 O8 1.82(5) . ?
W4 O9 1.90(4) . ?
W4 O21 2.36(7) . ?
W4 O19 2.40(5) . ?
W5 O1 1.69(3) . ?
W5 O11 1.78(4) . ?
W5 O10 1.88(4) 2_576 ?
W5 O17 1.90(4) . ?
W5 O14 1.96(4) . ?
W5 O22 2.35(4) 2_576 ?
W5 O19 2.38(6) . ?
W6 O5 1.67(3) . ?
W6 O17 1.87(4) 2_576 ?
W6 O18 1.87(4) . ?
W6 O16 1.89(4) 2_576 ?
W6 O8 1.95(4) . ?
W6 O21 2.40(8) . ?
W6 O22 2.39(4) . ?
Ag1 N3 2.16(3) . ?
Ag1 N2 2.16(3) . ?
Ag2 C1 2.07(3) 2_677 ?
Ag2 C1 2.07(3) . ?
Ag3 N4 2.11(3) 2_677 ?
Ag3 C12 2.12(4) . ?
N2 C12 1.32(4) . ?
N2 C2 1.33(5) . ?
C1 N4 1.32(4) . ?
C1 N3 1.36(5) . ?
O1 Ag5 2.46(3) 2_676 ?
O2 Ag5 2.32(2) . ?
C2 C5 1.38(5) . ?
C2 C6 1.43(6) . ?
C3 C4 1.31(5) . ?
C3 N4 1.39(5) . ?
C3 C16 1.45(5) . ?
C4 C11 1.41(5) . ?
C4 N3 1.43(4) . ?
C5 N1 1.40(5) . ?
C5 C8 1.40(5) . ?
N4 Ag3 2.11(3) 2_677 ?
N1 C12 1.32(4) . ?
N1 Ag4 2.15(3) . ?
C6 C21 1.39(5) . ?
C7 C8 1.349(19) . ?
C7 C21 1.351(18) . ?
C7 Ag5 2.44(3) . ?
C8 Ag5 2.66(3) . ?
C9 C11 1.36(5) . ?
C9 C10 1.45(5) . ?
C10 C16 1.36(6) . ?
O10 W5 1.88(4) 2_576 ?
O13 W4 1.79(4) 2_576 ?
O16 W6 1.89(4) 2_576 ?
O17 W6 1.87(4) 2_576 ?
Ag4 N6 2.14(4) . ?
N6 C14 1.25(7) . ?
N6 C13 1.40(7) . ?
C13 C20 1.44(7) . ?
C13 C15 1.45(7) . ?
C14 N5 1.37(7) . ?
C20 C18 1.33(8) . ?
C20 N5 1.48(7) . ?
O20 P1 1.64(4) . ?
O21 P1 1.67(7) . ?
Ag5 O1 2.46(3) 2_676 ?
O19 P1 1.66(5) . ?
O19 W2 2.36(6) 2_576 ?
C15 C19 1.37(6) . ?
C18 C17 1.28(7) . ?
C17 C19 1.354(15) . ?
P1 O20 1.64(4) 2_576 ?
P1 O19 1.66(5) 2_576 ?
P1 O22 1.67(5) 2_576 ?
P1 O22 1.67(5) . ?
P1 O21 1.67(7) 2_576 ?
O22 W5 2.35(4) 2_576 ?
O22 W1 2.39(4) 2_576 ?

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
O6 W1 O16 101.2(17) . . ?
O6 W1 O7 97.0(15) . . ?
O16 W1 O7 89.1(16) . . ?
O6 W1 O11 105.7(16) . . ?
O16 W1 O11 88.2(16) . . ?
O7 W1 O11 157.2(16) . . ?
O6 W1 O15 99.7(15) . . ?
O16 W1 O15 159.1(18) . . ?
O7 W1 O15 86.7(15) . . ?
O11 W1 O15 87.8(15) . . ?
O6 W1 O20 155.7(15) . . ?
O16 W1 O20 94.7(16) . . ?
O7 W1 O20 64.8(15) . . ?
O11 W1 O20 92.9(16) . . ?
O15 W1 O20 64.9(15) . . ?
O6 W1 O22 157.7(15) . 2_576 ?
O16 W1 O22 62.7(16) . 2_576 ?
O7 W1 O22 98.1(15) . 2_576 ?
O11 W1 O22 60.8(15) . 2_576 ?
O15 W1 O22 97.6(15) . 2_576 ?
O20 W1 O22 46.5(15) . 2_576 ?
O3 W2 O10 103.6(15) . . ?
O3 W2 O7 97.8(14) . . ?
O10 W2 O7 158.4(16) . . ?
O3 W2 O12 98.5(13) . . ?
O10 W2 O12 89.5(16) . . ?
O7 W2 O12 89.2(15) . . ?
O3 W2 O13 101.6(17) . . ?
O10 W2 O13 86.6(17) . . ?
O7 W2 O13 87.2(17) . . ?
O12 W2 O13 159.9(18) . . ?
O3 W2 O19 156.9(14) . 2_576 ?
O10 W2 O19 60.9(18) . 2_576 ?
O7 W2 O19 98.0(17) . 2_576 ?
O12 W2 O19 98.5(16) . 2_576 ?
O13 W2 O19 62.6(19) . 2_576 ?
O3 W2 O20 155.1(13) . . ?
O10 W2 O20 95.7(16) . . ?
O7 W2 O20 64.3(15) . . ?
O12 W2 O20 65.8(14) . . ?
O13 W2 O20 95.0(18) . . ?
O19 W2 O20 48.0(16) 2_576 . ?
O15 W3 O18 160.6(15) . . ?
O15 W3 O2 97.4(16) . . ?
O18 W3 O2 101.9(15) . . ?
O15 W3 O9 91.9(17) . . ?
O18 W3 O9 86.1(16) . . ?
O2 W3 O9 100.8(14) . . ?
O15 W3 O12 90.2(16) . . ?
O18 W3 O12 85.5(15) . . ?
O2 W3 O12 98.2(13) . . ?
O9 W3 O12 160.4(15) . . ?
O15 W3 O21 100(2) . . ?
O18 W3 O21 62(2) . . ?
O2 W3 O21 157(2) . . ?
O9 W3 O21 63(2) . . ?
O12 W3 O21 97(2) . . ?
O15 W3 O20 66.5(16) . . ?
O18 W3 O20 94.6(15) . . ?
O2 W3 O20 156.7(16) . . ?
O9 W3 O20 96.5(15) . . ?
O12 W3 O20 66.6(14) . . ?
O21 W3 O20 46(2) . . ?
O4 W4 O13 99.6(19) . 2_576 ?
O4 W4 O14 101.7(16) . . ?
O13 W4 O14 89.5(19) 2_576 . ?
O4 W4 O8 100.1(17) . . ?
O13 W4 O8 89(2) 2_576 . ?
O14 W4 O8 158.1(18) . . ?
O4 W4 O9 99.9(14) . . ?
O13 W4 O9 160(2) 2_576 . ?
O14 W4 O9 86.4(18) . . ?
O8 W4 O9 88.2(18) . . ?
O4 W4 O21 156(2) . . ?
O13 W4 O21 98(2) 2_576 . ?
O14 W4 O21 95(2) . . ?
O8 W4 O21 64(2) . . ?
O9 W4 O21 64(2) . . ?
O4 W4 O19 156.4(17) . . ?
O13 W4 O19 64(2) 2_576 . ?
O14 W4 O19 63.2(18) . . ?
O8 W4 O19 96.6(19) . . ?
O9 W4 O19 97.2(19) . . ?
O21 W4 O19 48(2) . . ?
O1 W5 O11 101.2(15) . . ?
O1 W5 O10 102.3(15) . 2_576 ?
O11 W5 O10 156.4(18) . 2_576 ?
O1 W5 O17 101.7(15) . . ?
O11 W5 O17 90.1(17) . . ?
O10 W5 O17 83.7(17) 2_576 . ?
O1 W5 O14 103.9(15) . . ?
O11 W5 O14 89.8(17) . . ?
O10 W5 O14 86.1(17) 2_576 . ?
O17 W5 O14 154.0(18) . . ?
O1 W5 O22 156.5(14) . 2_576 ?
O11 W5 O22 63.9(16) . 2_576 ?
O10 W5 O22 93.2(16) 2_576 2_576 ?
O17 W5 O22 62.3(16) . 2_576 ?
O14 W5 O22 94.6(16) . 2_576 ?
O1 W5 O19 156.9(16) . . ?
O11 W5 O19 97(2) . . ?
O10 W5 O19 61(2) 2_576 . ?
O17 W5 O19 92.1(18) . . ?
O14 W5 O19 62.1(17) . . ?
O22 W5 O19 46.4(17) 2_576 . ?
O5 W6 O17 103.5(17) . 2_576 ?
O5 W6 O18 102.9(15) . . ?
O17 W6 O18 89.5(17) 2_576 . ?
O5 W6 O16 99.6(16) . 2_576 ?
O17 W6 O16 89.9(17) 2_576 2_576 ?
O18 W6 O16 157.0(17) . 2_576 ?
O5 W6 O8 100.3(17) . . ?
O17 W6 O8 156.2(19) 2_576 . ?
O18 W6 O8 86.1(17) . . ?
O16 W6 O8 85.2(17) 2_576 . ?
O5 W6 O21 155(2) . . ?
O17 W6 O21 96(2) 2_576 . ?
O18 W6 O21 62(2) . . ?
O16 W6 O21 95(2) 2_576 . ?
O8 W6 O21 61(2) . . ?
O5 W6 O22 155.2(16) . . ?
O17 W6 O22 61.7(16) 2_576 . ?
O18 W6 O22 97.1(15) . . ?
O16 W6 O22 62.7(16) 2_576 . ?
O8 W6 O22 95.6(16) . . ?
O21 W6 O22 49(2) . . ?
N3 Ag1 N2 164.9(10) . . ?
C1 Ag2 C1 180.0(7) 2_677 . ?
N4 Ag3 C12 170.8(11) 2_677 . ?
C12 N2 C2 109(3) . . ?
C12 N2 Ag1 126(2) . . ?
C2 N2 Ag1 126(2) . . ?
N4 C1 N3 111(3) . . ?
N4 C1 Ag2 125(3) . . ?
N3 C1 Ag2 125(2) . . ?
W5 O1 Ag5 146.3(13) . 2_676 ?
W3 O2 Ag5 147(2) . . ?
N2 C2 C5 108(3) . . ?
N2 C2 C6 132(3) . . ?
C5 C2 C6 120(4) . . ?
C4 C3 N4 112(3) . . ?
C4 C3 C16 120(3) . . ?
N4 C3 C16 127(3) . . ?
C3 C4 C11 125(3) . . ?
C3 C4 N3 105(3) . . ?
C11 C4 N3 130(3) . . ?
C2 C5 N1 106(3) . . ?
C2 C5 C8 122(3) . . ?
N1 C5 C8 132(3) . . ?
C1 N4 C3 106(3) . . ?
C1 N4 Ag3 119(2) . 2_677 ?
C3 N4 Ag3 133(2) . 2_677 ?
C12 N1 C5 107(3) . . ?
C12 N1 Ag4 128(3) . . ?
C5 N1 Ag4 125(2) . . ?
C21 C6 C2 114(3) . . ?
C8 C7 C21 121(2) . . ?
C8 C7 Ag5 84.1(17) . . ?
C21 C7 Ag5 103(2) . . ?
C7 C8 C5 118(2) . . ?
C7 C8 Ag5 65.6(17) . . ?
C5 C8 Ag5 106(2) . . ?
C11 C9 C10 122(4) . . ?
C16 C10 C9 121(3) . . ?
C9 C11 C4 115(3) . . ?
W2 O7 W1 136(2) . . ?
W4 O8 W6 139(3) . . ?
W4 O9 W3 136(2) . . ?
W2 O10 W5 141(2) . 2_576 ?
W5 O11 W1 139(2) . . ?
C10 C16 C3 117(3) . . ?
W2 O12 W3 132.3(18) . . ?
W4 O13 W2 138(3) 2_576 . ?
W4 O14 W5 139(2) . . ?
W3 O15 W1 133(2) . . ?
W1 O16 W6 139(2) . 2_576 ?
W6 O17 W5 139(2) 2_576 . ?
W6 O18 W3 140(2) . . ?
N6 Ag4 N1 174.2(13) . . ?
C1 N3 C4 107(3) . . ?
C1 N3 Ag1 116(2) . . ?
C4 N3 Ag1 138(2) . . ?
N2 C12 N1 111(3) . . ?
N2 C12 Ag3 122(2) . . ?
N1 C12 Ag3 127(3) . . ?
C14 N6 C13 105(4) . . ?
C14 N6 Ag4 129(4) . . ?
C13 N6 Ag4 125(3) . . ?
N6 C13 C20 112(5) . . ?
N6 C13 C15 136(4) . . ?
C20 C13 C15 112(5) . . ?
N6 C14 N5 116(6) . . ?
C18 C20 C13 126(6) . . ?
C18 C20 N5 134(5) . . ?
C13 C20 N5 99(4) . . ?
C14 N5 C20 106(4) . . ?
P1 O20 W3 123(2) . . ?
P1 O20 W1 122(2) . . ?
W3 O20 W1 95.9(15) . . ?
P1 O20 W2 119(2) . . ?
W3 O20 W2 94.9(16) . . ?
W1 O20 W2 95.0(15) . . ?
P1 O21 W3 122(4) . . ?
P1 O21 W4 122(4) . . ?
W3 O21 W4 97(3) . . ?
P1 O21 W6 118(4) . . ?
W3 O21 W6 96(3) . . ?
W4 O21 W6 96(3) . . ?
O2 Ag5 C7 103.8(8) . . ?
O2 Ag5 O1 84.5(9) . 2_676 ?
C7 Ag5 O1 102.8(9) . 2_676 ?
O2 Ag5 C8 130.0(8) . . ?
C7 Ag5 C8 30.3(5) . . ?
O1 Ag5 C8 89.3(10) 2_676 . ?
C7 C21 C6 125(3) . . ?
P1 O19 W2 121(3) . 2_576 ?
P1 O19 W5 122(3) . . ?
W2 O19 W5 97(2) 2_576 . ?
P1 O19 W4 120(3) . . ?
W2 O19 W4 96(2) 2_576 . ?
W5 O19 W4 95.5(18) . . ?
C19 C15 C13 120(3) . . ?
C17 C18 C20 117(5) . . ?
C18 C17 C19 126(4) . . ?
C17 C19 C15 119(4) . . ?
O20 P1 O20 179.998(10) . 2_576 ?
O20 P1 O19 73(3) . 2_576 ?
O20 P1 O19 107(3) 2_576 2_576 ?
O20 P1 O19 107(3) . . ?
O20 P1 O19 73(3) 2_576 . ?
O19 P1 O19 180(4) 2_576 . ?
O20 P1 O22 70(2) . 2_576 ?
O20 P1 O22 110(2) 2_576 2_576 ?
O19 P1 O22 112(3) 2_576 2_576 ?
O19 P1 O22 68(3) . 2_576 ?
O20 P1 O22 110(2) . . ?
O20 P1 O22 70(2) 2_576 . ?
O19 P1 O22 68(3) 2_576 . ?
O19 P1 O22 112(3) . . ?
O22 P1 O22 180.000(7) 2_576 . ?
O20 P1 O21 68(3) . . ?
O20 P1 O21 112(3) 2_576 . ?
O19 P1 O21 109(3) 2_576 . ?
O19 P1 O21 71(3) . . ?
O22 P1 O21 106(3) 2_576 . ?
O22 P1 O21 74(3) . . ?
O20 P1 O21 112(3) . 2_576 ?
O20 P1 O21 68(3) 2_576 2_576 ?
O19 P1 O21 71(3) 2_576 2_576 ?
O19 P1 O21 109(3) . 2_576 ?
O22 P1 O21 74(3) 2_576 2_576 ?
O22 P1 O21 106(3) . 2_576 ?
O21 P1 O21 180(5) . 2_576 ?
P1 O22 W5 123(2) . 2_576 ?
P1 O22 W6 119(2) . . ?
W5 O22 W6 96.3(16) 2_576 . ?
P1 O22 W1 121(2) . 2_576 ?
W5 O22 W1 95.7(16) 2_576 2_576 ?
W6 O22 W1 95.3(16) . 2_576 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.127
_refine_diff_density_min         -2.288
_refine_diff_density_rms         0.297
####################################################################### 
# 
# 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_test_0m
_database_code_depnum_ccdc_archive 'CCDC 1002938'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H26 Cu7 Mo12 N18 O40 P'
_chemical_formula_sum            'C36 H26 Cu7 Mo12 N18 O40 P'
_chemical_formula_weight         2977.85

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.679(10)
_cell_length_b                   12.709(12)
_cell_length_c                   13.329(12)
_cell_angle_alpha                95.994(13)
_cell_angle_beta                 111.209(13)
_cell_angle_gamma                107.347(13)
_cell_volume                     1710(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8359
_cell_measurement_theta_min      1.69
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1410
_exptl_absorpt_coefficient_mu    4.372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4918
_exptl_absorpt_correction_T_max  0.7820
_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            8359
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5913
_reflns_number_gt                5514
_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 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. 
;

_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)+(0.1442P)²+79.1191P] 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     SHELXL
_refine_ls_extinction_coef       0.0093(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5913
_refine_ls_number_parameters     536
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1165
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.114
_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
Mo1 Mo 0.67517(16) 0.42572(15) 0.29868(14) 0.0327(5) Uani 1 1 d . . .
Mo2 Mo 0.93576(18) 0.63650(15) 0.27761(14) 0.0343(5) Uani 1 1 d . . .
Mo3 Mo 1.25358(17) 0.73232(14) 0.49741(15) 0.0337(5) Uani 1 1 d . . .
Mo4 Mo 0.98876(18) 0.77607(15) 0.54406(16) 0.0382(5) Uani 1 1 d U . .
Mo5 Mo 0.75581(18) 0.54671(17) 0.57865(16) 0.0385(5) Uani 1 1 d U . .
Mo6 Mo 1.08867(18) 0.65082(16) 0.77102(14) 0.0377(5) Uani 1 1 d U . .
Cu1 Cu 0.77635(17) 0.02594(17) -0.00219(17) 0.0212(5) Uani 1 1 d . . .
Cu2 Cu 1.2633(2) 0.39236(16) 0.13780(19) 0.0283(6) Uani 1 1 d . . .
P1 P 1.0000 0.5000 0.5000 0.0248(13) Uani 1 2 d S . .
O1 O 0.971(2) 0.585(2) 0.574(2) 0.030(6) Uani 0.50 1 d P . .
O2 O 0.852(3) 0.450(2) 0.476(2) 0.029(5) Uani 0.50 1 d PU . .
O3 O 1.1683(17) 0.806(2) 0.5512(15) 0.069(6) Uani 1 1 d . . .
O4 O 1.1281(16) 0.7180(14) 0.8995(15) 0.052(4) Uani 1 1 d . . .
O5 O 0.6428(18) 0.5717(17) 0.6139(15) 0.056(4) Uani 1 1 d . . .
O6 O 1.1187(17) 0.7041(18) 0.3505(14) 0.066(6) Uani 1 1 d . . .
O7 O 0.5223(18) 0.3851(15) 0.2064(17) 0.065(5) Uani 1 1 d . . .
O8 O 0.9296(18) 0.741(2) 0.3933(18) 0.084(8) Uani 1 1 d . . .
O9 O 0.940(2) 0.5052(14) 0.211(2) 0.079(7) Uani 1 1 d . . .
O10 O 0.8977(16) 0.5942(17) 0.7139(16) 0.063(4) Uani 1 1 d U . .
O11 O 0.749(2) 0.3413(13) 0.2228(19) 0.069(6) Uani 1 1 d . . .
O12 O 0.657(3) 0.2991(17) 0.3684(15) 0.074(7) Uani 1 1 d . . .
O13 O 0.9016(18) 0.7029(19) 0.1750(16) 0.064(5) Uani 1 1 d . . .
O14 O 1.274(2) 0.6018(16) 0.4245(14) 0.070(6) Uani 1 1 d . . .
O15 O 1.370(2) 0.8381(17) 0.4942(15) 0.074(7) Uani 1 1 d . . .
C1 C 0.380(2) 0.0082(18) -0.1676(18) 0.037(4) Uani 1 1 d . . .
N4 N 0.5800(18) 0.0039(16) -0.1003(16) 0.042(4) Uani 1 1 d . . .
N7 N 0.5058(19) -0.0924(17) -0.1667(17) 0.048(5) Uani 1 1 d . . .
C2 C 0.505(2) 0.0698(18) -0.0964(16) 0.036(4) Uani 1 1 d . . .
N5 N 0.3749(19) -0.0916(16) -0.2136(17) 0.049(5) Uani 1 1 d . . .
H1 H 0.3061 -0.1456 -0.2624 0.058 Uiso 1 1 calc R . .
N2 N 1.1702(18) 0.2138(15) 0.1129(16) 0.041(4) Uani 1 1 d . . .
N8 N 1.0477(17) 0.1702(15) 0.0460(15) 0.038(4) Uani 1 1 d . . .
C3 C 1.0737(18) 0.0667(16) 0.1638(16) 0.031(4) Uani 1 1 d . . .
C4 C 1.196(2) 0.1507(17) 0.1901(17) 0.036(4) Uani 1 1 d . . .
N1 N 0.9831(17) 0.0816(14) 0.0799(15) 0.038(4) Uani 1 1 d . . .
C5 C 1.390(2) 0.657(2) 0.238(2) 0.045(5) Uani 1 1 d . . .
N3 N 1.2861(19) 0.5646(16) 0.1636(18) 0.047(5) Uani 1 1 d . . .
C6 C 1.345(2) 0.7493(19) 0.2342(16) 0.037(5) Uani 1 1 d . . .
N9 N 1.188(2) 0.5992(17) 0.1235(16) 0.047(5) Uani 1 1 d . . .
O16 O 0.7570(19) 0.5534(14) 0.259(2) 0.072(6) Uani 1 1 d . . .
O17 O 1.0803(17) 0.7646(16) 0.7005(15) 0.063(4) Uani 1 1 d U . .
C7 C 1.069(2) -0.0150(18) 0.2336(18) 0.039(5) Uani 1 1 d . . .
H14 H 0.9900 -0.0725 0.2198 0.047 Uiso 1 1 calc R . .
C8 C 1.175(2) -0.005(2) 0.313(2) 0.046(5) Uani 1 1 d . . .
H3 H 1.1718 -0.0569 0.3574 0.055 Uiso 1 1 calc R . .
C9 C 1.307(2) 0.162(2) 0.277(2) 0.050(6) Uani 1 1 d . . .
H4 H 1.3843 0.2227 0.2938 0.060 Uiso 1 1 calc R . .
C10 C 0.543(2) 0.180(2) -0.0352(18) 0.049(6) Uani 1 1 d . . .
H5 H 0.6303 0.2220 0.0138 0.058 Uiso 1 1 calc R . .
C11 C 1.304(2) 0.085(2) 0.339(2) 0.049(6) Uani 1 1 d . . .
H6 H 1.3804 0.0877 0.3958 0.059 Uiso 1 1 calc R . .
C12 C 0.313(3) 0.160(2) -0.123(2) 0.055(6) Uani 1 1 d . . .
H7 H 0.2489 0.1919 -0.1285 0.066 Uiso 1 1 calc R . .
C13 C 0.275(2) 0.052(2) -0.186(2) 0.056(6) Uani 1 1 d . . .
H8 H 0.1881 0.0107 -0.2362 0.068 Uiso 1 1 calc R . .
C14 C 0.443(3) 0.223(2) -0.053(2) 0.059(7) Uani 1 1 d . . .
H9 H 0.4637 0.2969 -0.0157 0.071 Uiso 1 1 calc R . .
O18 O 0.916(3) 0.487(2) 0.382(2) 0.026(5) Uani 0.50 1 d P . .
O19 O 1.035(2) 0.612(2) 0.4671(19) 0.023(5) Uani 0.50 1 d P . .
O20 O 0.9929(18) 0.9057(13) 0.5738(15) 0.055(4) Uani 1 1 d . . .
O21 O 0.8400(17) 0.6868(16) 0.5458(16) 0.062(4) Uani 1 1 d U . .
C15 C 1.436(3) 0.859(2) 0.299(2) 0.052(6) Uani 1 1 d . . .
H10 H 1.4081 0.9206 0.2971 0.062 Uiso 1 1 calc R . .
C16 C 1.556(2) 0.875(2) 0.362(2) 0.050(6) Uani 1 1 d . . .
H11 H 1.6144 0.9464 0.4051 0.061 Uiso 1 1 calc R . .
C17 C 1.598(2) 0.782(3) 0.363(2) 0.067(8) Uani 1 1 d . . .
H12 H 1.6855 0.7972 0.4088 0.081 Uiso 1 1 calc R . .
C18 C 1.527(3) 0.675(3) 0.307(3) 0.078(10) Uani 1 1 d . . .
H13 H 1.5612 0.6178 0.3120 0.094 Uiso 1 1 calc R . .
O22 O 0.670(2) 0.5060(16) 0.4186(14) 0.068(6) Uani 1 1 d . . .
Cu3 Cu 1.0000 0.5000 0.0000 0.0270(7) Uani 1 2 d S . .
N6 N 1.2177(19) 0.7089(17) 0.1612(16) 0.045(4) Uani 1 1 d . . .
Cu4 Cu 1.0768(2) 0.7804(2) 0.08752(19) 0.0284(6) Uani 1 1 d U . .


_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
Mo1 O7 1.642(17) . ?
Mo1 O22 1.837(18) . ?
Mo1 O16 1.855(18) . ?
Mo1 O12 1.937(18) . ?
Mo1 O11 1.972(16) . ?
Mo1 O2 2.43(3) . ?
Mo1 O18 2.45(3) . ?
Mo2 O13 1.670(16) . ?
Mo2 O9 1.828(17) . ?
Mo2 O6 1.864(18) . ?
Mo2 O16 1.948(16) . ?
Mo2 O8 1.965(18) . ?
Mo2 O19 2.47(2) . ?
Mo2 O18 2.47(2) . ?
Mo3 O15 1.618(17) . ?
Mo3 O3 1.820(16) . ?
Mo3 O12 1.868(18) 2_766 ?
Mo3 O6 1.932(17) . ?
Mo3 O14 1.954(18) . ?
Mo3 O2 2.41(3) 2_766 ?
Mo3 O19 2.41(2) . ?
Mo4 O20 1.636(16) . ?
Mo4 O21 1.779(18) . ?
Mo4 O8 1.83(2) . ?
Mo4 O3 1.980(17) . ?
Mo4 O17 2.014(17) . ?
Mo4 O1 2.46(3) . ?
Mo4 O19 2.52(2) . ?
Mo5 O5 1.652(17) . ?
Mo5 O14 1.808(18) 2_766 ?
Mo5 O10 1.837(17) . ?
Mo5 O22 1.934(17) . ?
Mo5 O21 1.938(17) . ?
Mo5 O1 2.44(2) . ?
Mo5 O2 2.50(3) . ?
Mo6 O4 1.662(17) . ?
Mo6 O17 1.813(17) . ?
Mo6 O11 1.834(18) 2_766 ?
Mo6 O10 1.942(17) . ?
Mo6 O9 1.964(19) 2_766 ?
Mo6 O1 2.39(3) . ?
Mo6 O18 2.52(2) 2_766 ?
Cu1 N4 2.102(19) . ?
Cu1 N1 2.106(18) . ?
Cu2 N3 2.100(19) . ?
Cu2 N2 2.133(18) . ?
P1 O18 1.49(2) . ?
P1 O18 1.49(2) 2_766 ?
P1 O19 1.51(2) . ?
P1 O19 1.51(2) 2_766 ?
P1 O2 1.54(3) 2_766 ?
P1 O2 1.54(3) . ?
P1 O1 1.58(3) 2_766 ?
P1 O1 1.58(3) . ?
O1 O18 1.79(4) 2_766 ?
O2 O19 1.71(3) 2_766 ?
O2 O18 1.72(3) . ?
O2 Mo3 2.41(3) 2_766 ?
O9 Mo6 1.964(19) 2_766 ?
O11 Mo6 1.834(18) 2_766 ?
O12 Mo3 1.868(18) 2_766 ?
O14 Mo5 1.808(18) 2_766 ?
C1 N5 1.33(3) . ?
C1 C2 1.34(3) . ?
C1 C13 1.45(3) . ?
N4 N7 1.27(3) . ?
N4 C2 1.39(3) . ?
N7 N5 1.43(3) . ?
C2 C10 1.40(3) . ?
N2 N8 1.28(3) . ?
N2 C4 1.37(3) . ?
N8 N1 1.38(2) . ?
N8 Cu4 2.141(17) 2_765 ?
C3 N1 1.31(3) . ?
C3 C4 1.40(3) . ?
C3 C7 1.47(3) . ?
C4 C9 1.34(3) . ?
C5 N3 1.37(3) . ?
C5 C6 1.42(3) . ?
C5 C18 1.47(3) . ?
N3 N9 1.31(3) . ?
C6 N6 1.34(3) . ?
C6 C15 1.42(3) . ?
N9 N6 1.32(3) . ?
N9 Cu3 2.10(2) . ?
C7 C8 1.26(3) . ?
C8 C11 1.49(3) . ?
C9 C11 1.35(3) . ?
C10 C14 1.40(4) . ?
C12 C13 1.38(4) . ?
C12 C14 1.38(4) . ?
O18 O19 1.70(3) . ?
O18 O1 1.79(4) 2_766 ?
O18 Mo6 2.52(2) 2_766 ?
O19 O2 1.71(3) 2_766 ?
C15 C16 1.29(4) . ?
C16 C17 1.40(4) . ?
C17 C18 1.32(4) . ?
Cu3 N9 2.10(2) 2_765 ?
N6 Cu4 2.099(18) . ?
Cu4 N8 2.140(17) 2_765 ?

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
O7 Mo1 O22 101.9(10) . . ?
O7 Mo1 O16 101.8(10) . . ?
O22 Mo1 O16 94.8(8) . . ?
O7 Mo1 O12 98.6(11) . . ?
O22 Mo1 O12 86.8(7) . . ?
O16 Mo1 O12 158.7(11) . . ?
O7 Mo1 O11 101.5(10) . . ?
O22 Mo1 O11 155.3(10) . . ?
O16 Mo1 O11 87.9(7) . . ?
O12 Mo1 O11 82.2(8) . . ?
O7 Mo1 O2 156.8(10) . . ?
O22 Mo1 O2 65.0(9) . . ?
O16 Mo1 O2 98.5(10) . . ?
O12 Mo1 O2 63.0(9) . . ?
O11 Mo1 O2 90.3(10) . . ?
O7 Mo1 O18 161.3(10) . . ?
O22 Mo1 O18 93.9(9) . . ?
O16 Mo1 O18 66.7(9) . . ?
O12 Mo1 O18 92.0(9) . . ?
O11 Mo1 O18 64.6(8) . . ?
O2 Mo1 O18 41.2(8) . . ?
O13 Mo2 O9 103.1(12) . . ?
O13 Mo2 O6 102.2(10) . . ?
O9 Mo2 O6 93.7(9) . . ?
O13 Mo2 O16 99.2(10) . . ?
O9 Mo2 O16 89.3(8) . . ?
O6 Mo2 O16 157.1(10) . . ?
O13 Mo2 O8 99.5(11) . . ?
O9 Mo2 O8 156.8(12) . . ?
O6 Mo2 O8 86.6(8) . . ?
O16 Mo2 O8 81.9(8) . . ?
O13 Mo2 O19 158.8(10) . . ?
O9 Mo2 O19 94.2(10) . . ?
O6 Mo2 O19 64.2(9) . . ?
O16 Mo2 O19 93.0(9) . . ?
O8 Mo2 O19 65.0(10) . . ?
O13 Mo2 O18 160.3(10) . . ?
O9 Mo2 O18 66.4(9) . . ?
O6 Mo2 O18 95.3(9) . . ?
O16 Mo2 O18 65.2(9) . . ?
O8 Mo2 O18 90.5(10) . . ?
O19 Mo2 O18 40.3(8) . . ?
O15 Mo3 O3 101.2(11) . . ?
O15 Mo3 O12 100.9(11) . 2_766 ?
O3 Mo3 O12 95.1(9) . 2_766 ?
O15 Mo3 O6 100.2(10) . . ?
O3 Mo3 O6 88.6(8) . . ?
O12 Mo3 O6 157.5(10) 2_766 . ?
O15 Mo3 O14 102.4(11) . . ?
O3 Mo3 O14 155.5(10) . . ?
O12 Mo3 O14 86.9(7) 2_766 . ?
O6 Mo3 O14 80.7(8) . . ?
O15 Mo3 O2 158.7(11) . 2_766 ?
O3 Mo3 O2 95.6(10) . 2_766 ?
O12 Mo3 O2 64.2(10) 2_766 2_766 ?
O6 Mo3 O2 93.3(10) . 2_766 ?
O14 Mo3 O2 63.4(9) . 2_766 ?
O15 Mo3 O19 159.5(11) . . ?
O3 Mo3 O19 66.5(9) . . ?
O12 Mo3 O19 96.6(10) 2_766 . ?
O6 Mo3 O19 64.6(9) . . ?
O14 Mo3 O19 89.0(9) . . ?
O2 Mo3 O19 41.6(8) 2_766 . ?
O20 Mo4 O21 105.6(10) . . ?
O20 Mo4 O8 103.9(10) . . ?
O21 Mo4 O8 95.3(10) . . ?
O20 Mo4 O3 100.8(9) . . ?
O21 Mo4 O3 152.0(10) . . ?
O8 Mo4 O3 87.2(8) . . ?
O20 Mo4 O17 97.5(9) . . ?
O21 Mo4 O17 86.9(8) . . ?
O8 Mo4 O17 157.0(10) . . ?
O3 Mo4 O17 80.5(8) . . ?
O20 Mo4 O1 155.2(9) . . ?
O21 Mo4 O1 61.3(8) . . ?
O8 Mo4 O1 98.4(10) . . ?
O3 Mo4 O1 90.8(9) . . ?
O17 Mo4 O1 62.7(8) . . ?
O20 Mo4 O19 159.5(9) . . ?
O21 Mo4 O19 93.2(9) . . ?
O8 Mo4 O19 65.5(9) . . ?
O3 Mo4 O19 62.4(8) . . ?
O17 Mo4 O19 91.6(8) . . ?
O1 Mo4 O19 43.7(8) . . ?
O5 Mo5 O14 104.3(10) . 2_766 ?
O5 Mo5 O10 101.0(9) . . ?
O14 Mo5 O10 93.2(9) 2_766 . ?
O5 Mo5 O22 102.6(9) . . ?
O14 Mo5 O22 88.6(8) 2_766 . ?
O10 Mo5 O22 155.1(10) . . ?
O5 Mo5 O21 104.1(9) . . ?
O14 Mo5 O21 151.0(10) 2_766 . ?
O10 Mo5 O21 87.2(8) . . ?
O22 Mo5 O21 79.5(8) . . ?
O5 Mo5 O1 157.2(9) . . ?
O14 Mo5 O1 94.0(10) 2_766 . ?
O10 Mo5 O1 63.8(9) . . ?
O22 Mo5 O1 91.3(9) . . ?
O21 Mo5 O1 60.3(9) . . ?
O5 Mo5 O2 158.8(9) . . ?
O14 Mo5 O2 62.8(9) 2_766 . ?
O10 Mo5 O2 96.6(9) . . ?
O22 Mo5 O2 62.3(9) . . ?
O21 Mo5 O2 88.3(9) . . ?
O1 Mo5 O2 43.8(9) . . ?
O4 Mo6 O17 100.5(9) . . ?
O4 Mo6 O11 101.5(9) . 2_766 ?
O17 Mo6 O11 95.0(9) . 2_766 ?
O4 Mo6 O10 100.3(9) . . ?
O17 Mo6 O10 88.5(8) . . ?
O11 Mo6 O10 156.9(9) 2_766 . ?
O4 Mo6 O9 100.3(10) . 2_766 ?
O17 Mo6 O9 158.2(10) . 2_766 ?
O11 Mo6 O9 87.2(8) 2_766 2_766 ?
O10 Mo6 O9 81.5(9) . 2_766 ?
O4 Mo6 O1 158.7(9) . . ?
O17 Mo6 O1 66.7(9) . . ?
O11 Mo6 O1 96.8(9) 2_766 . ?
O10 Mo6 O1 63.7(8) . . ?
O9 Mo6 O1 91.4(10) 2_766 . ?
O4 Mo6 O18 158.2(8) . 2_766 ?
O17 Mo6 O18 97.6(9) . 2_766 ?
O11 Mo6 O18 64.7(8) 2_766 2_766 ?
O10 Mo6 O18 92.2(9) . 2_766 ?
O9 Mo6 O18 63.7(9) 2_766 2_766 ?
O1 Mo6 O18 42.7(8) . 2_766 ?
N4 Cu1 N1 166.4(7) . . ?
N3 Cu2 N2 158.1(7) . . ?
O18 P1 O18 179.998(8) . 2_766 ?
O18 P1 O19 69.1(12) . . ?
O18 P1 O19 110.9(12) 2_766 . ?
O18 P1 O19 110.9(12) . 2_766 ?
O18 P1 O19 69.1(12) 2_766 2_766 ?
O19 P1 O19 179.999(4) . 2_766 ?
O18 P1 O2 110.9(13) . 2_766 ?
O18 P1 O2 69.1(13) 2_766 2_766 ?
O19 P1 O2 68.1(13) . 2_766 ?
O19 P1 O2 111.9(13) 2_766 2_766 ?
O18 P1 O2 69.1(13) . . ?
O18 P1 O2 110.9(13) 2_766 . ?
O19 P1 O2 111.9(13) . . ?
O19 P1 O2 68.1(13) 2_766 . ?
O2 P1 O2 179.999(3) 2_766 . ?
O18 P1 O1 71.2(13) . 2_766 ?
O18 P1 O1 108.8(13) 2_766 2_766 ?
O19 P1 O1 106.4(13) . 2_766 ?
O19 P1 O1 73.6(13) 2_766 2_766 ?
O2 P1 O1 72.2(13) 2_766 2_766 ?
O2 P1 O1 107.8(13) . 2_766 ?
O18 P1 O1 108.8(13) . . ?
O18 P1 O1 71.2(13) 2_766 . ?
O19 P1 O1 73.6(13) . . ?
O19 P1 O1 106.4(13) 2_766 . ?
O2 P1 O1 107.8(13) 2_766 . ?
O2 P1 O1 72.2(13) . . ?
O1 P1 O1 180.0(15) 2_766 . ?
P1 O1 O18 51.8(11) . 2_766 ?
P1 O1 Mo6 124.2(14) . . ?
O18 O1 Mo6 72.5(11) 2_766 . ?
P1 O1 Mo5 122.9(13) . . ?
O18 O1 Mo5 129.8(15) 2_766 . ?
Mo6 O1 Mo5 94.0(9) . . ?
P1 O1 Mo4 120.9(13) . . ?
O18 O1 Mo4 135.3(15) 2_766 . ?
Mo6 O1 Mo4 94.1(9) . . ?
Mo5 O1 Mo4 92.7(9) . . ?
P1 O2 O19 55.1(11) . 2_766 ?
P1 O2 O18 53.9(12) . . ?
O19 O2 O18 92.1(17) 2_766 . ?
P1 O2 Mo3 124.4(14) . 2_766 ?
O19 O2 Mo3 69.5(11) 2_766 2_766 ?
O18 O2 Mo3 131.9(15) . 2_766 ?
P1 O2 Mo1 123.9(14) . . ?
O19 O2 Mo1 138.6(16) 2_766 . ?
O18 O2 Mo1 70.1(12) . . ?
Mo3 O2 Mo1 94.5(9) 2_766 . ?
P1 O2 Mo5 121.0(13) . . ?
O19 O2 Mo5 125.4(15) 2_766 . ?
O18 O2 Mo5 131.9(15) . . ?
Mo3 O2 Mo5 92.4(9) 2_766 . ?
Mo1 O2 Mo5 91.9(9) . . ?
Mo3 O3 Mo4 138.2(12) . . ?
Mo2 O6 Mo3 137.7(13) . . ?
Mo4 O8 Mo2 138.6(14) . . ?
Mo2 O9 Mo6 138.6(13) . 2_766 ?
Mo5 O10 Mo6 138.1(11) . . ?
Mo6 O11 Mo1 138.6(11) 2_766 . ?
Mo3 O12 Mo1 138.0(14) 2_766 . ?
Mo5 O14 Mo3 140.7(12) 2_766 . ?
N5 C1 C2 108.9(19) . . ?
N5 C1 C13 129(2) . . ?
C2 C1 C13 122(2) . . ?
N7 N4 C2 109.6(18) . . ?
N7 N4 Cu1 117.7(15) . . ?
C2 N4 Cu1 131.9(15) . . ?
N4 N7 N5 107.4(18) . . ?
C1 C2 C10 123(2) . . ?
C1 C2 N4 107.1(18) . . ?
C10 C2 N4 130(2) . . ?
C1 N5 N7 107.0(18) . . ?
N8 N2 C4 109.4(18) . . ?
N8 N2 Cu2 116.1(14) . . ?
C4 N2 Cu2 126.7(15) . . ?
N2 N8 N1 110.1(16) . . ?
N2 N8 Cu4 134.1(14) . 2_765 ?
N1 N8 Cu4 115.1(13) . 2_765 ?
N1 C3 C4 109.7(18) . . ?
N1 C3 C7 132.9(18) . . ?
C4 C3 C7 117.3(18) . . ?
C9 C4 N2 132(2) . . ?
C9 C4 C3 124(2) . . ?
N2 C4 C3 104.2(18) . . ?
C3 N1 N8 106.3(16) . . ?
C3 N1 Cu1 139.7(15) . . ?
N8 N1 Cu1 113.5(13) . . ?
N3 C5 C6 106.6(18) . . ?
N3 C5 C18 133(2) . . ?
C6 C5 C18 120(2) . . ?
N9 N3 C5 105.9(18) . . ?
N9 N3 Cu2 122.8(15) . . ?
C5 N3 Cu2 130.0(15) . . ?
N6 C6 C5 107(2) . . ?
N6 C6 C15 134(2) . . ?
C5 C6 C15 118(2) . . ?
N3 N9 N6 114.0(19) . . ?
N3 N9 Cu3 125.6(16) . . ?
N6 N9 Cu3 120.2(15) . . ?
Mo1 O16 Mo2 136.0(13) . . ?
Mo6 O17 Mo4 136.2(11) . . ?
C8 C7 C3 118(2) . . ?
C7 C8 C11 123(2) . . ?
C4 C9 C11 119(2) . . ?
C2 C10 C14 115(2) . . ?
C9 C11 C8 118(2) . . ?
C13 C12 C14 122(2) . . ?
C12 C13 C1 115(2) . . ?
C12 C14 C10 123(2) . . ?
P1 O18 O19 56.2(12) . . ?
P1 O18 O2 57.1(12) . . ?
O19 O18 O2 95.5(16) . . ?
P1 O18 O1 56.9(12) . 2_766 ?
O19 O18 O1 90.5(17) . 2_766 ?
O2 O18 O1 92.1(16) . 2_766 ?
P1 O18 Mo1 125.6(13) . . ?
O19 O18 Mo1 131.4(14) . . ?
O2 O18 Mo1 68.7(12) . . ?
O1 O18 Mo1 133.8(15) 2_766 . ?
P1 O18 Mo2 125.9(14) . . ?
O19 O18 Mo2 69.8(11) . . ?
O2 O18 Mo2 138.2(15) . . ?
O1 O18 Mo2 125.6(15) 2_766 . ?
Mo1 O18 Mo2 91.5(8) . . ?
P1 O18 Mo6 121.6(13) . 2_766 ?
O19 O18 Mo6 131.4(15) . 2_766 ?
O2 O18 Mo6 124.8(14) . 2_766 ?
O1 O18 Mo6 64.8(11) 2_766 2_766 ?
Mo1 O18 Mo6 91.5(8) . 2_766 ?
Mo2 O18 Mo6 90.7(8) . 2_766 ?
P1 O19 O18 54.7(11) . . ?
P1 O19 O2 56.8(12) . 2_766 ?
O18 O19 O2 94.0(17) . 2_766 ?
P1 O19 Mo3 125.7(13) . . ?
O18 O19 Mo3 138.7(15) . . ?
O2 O19 Mo3 69.0(11) 2_766 . ?
P1 O19 Mo2 124.5(12) . . ?
O18 O19 Mo2 69.9(11) . . ?
O2 O19 Mo2 131.4(15) 2_766 . ?
Mo3 O19 Mo2 93.0(8) . . ?
P1 O19 Mo4 121.3(12) . . ?
O18 O19 Mo4 124.2(14) . . ?
O2 O19 Mo4 132.8(15) 2_766 . ?
Mo3 O19 Mo4 92.1(8) . . ?
Mo2 O19 Mo4 90.7(8) . . ?
Mo4 O21 Mo5 145.0(11) . . ?
C16 C15 C6 121(3) . . ?
C15 C16 C17 119(3) . . ?
C18 C17 C16 128(2) . . ?
C17 C18 C5 113(2) . . ?
Mo1 O22 Mo5 140.2(12) . . ?
N9 Cu3 N9 179.999(2) 2_765 . ?
N9 N6 C6 106.2(18) . . ?
N9 N6 Cu4 117.9(15) . . ?
C6 N6 Cu4 135.4(16) . . ?
N6 Cu4 N8 155.0(7) . 2_765 ?

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
N5 H1 O3 0.86 2.31 3.02(3) 140.7 1_444
N5 H1 O17 0.86 2.38 3.07(3) 138.4 1_444
N5 H1 O12 0.86 2.52 3.01(3) 117.4 2_655
N5 H1 O11 0.86 2.54 3.04(3) 117.9 2_655

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.748
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.334
####################################################################### 
# 
# 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_test_0m_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1038931'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mo12 O40 Si, 4(C7 H7 N2)'
_chemical_formula_sum            'C28 H28 Mo12 N8 O40 Si'
_chemical_formula_weight         2295.95

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'
Mo Mo -1.6832 0.6857 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9145(16)
_cell_length_b                   11.2727(19)
_cell_length_c                   13.766(2)
_cell_angle_alpha                69.701(3)
_cell_angle_beta                 82.052(3)
_cell_angle_gamma                71.665(2)
_cell_volume                     1369.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7650
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      27.04

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1090
_exptl_absorpt_coefficient_mu    2.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71068
_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            7650
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0913
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         27.04
_reflns_number_total             5868
_reflns_number_gt                3522
_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 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. 
;

_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)+(0.2000P)²+0.0000P] 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_number_reflns         5868
_refine_ls_number_parameters     403
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.1226
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.092
_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
Mo1 Mo 0.0745(2) 0.2638(2) 0.24964(16) 0.0316(6) Uani 1 1 d . . .
Mo2 Mo 0.3286(2) 0.2447(2) 0.04017(16) 0.0320(6) Uani 1 1 d . . .
Mo3 Mo 0.2484(3) 0.4799(2) -0.21038(18) 0.0415(7) Uani 1 1 d . . .
Mo4 Mo 0.0575(3) 0.2408(2) -0.10335(19) 0.0522(8) Uani 1 1 d . . .
Mo5 Mo 0.1954(3) 0.7357(2) -0.1016(2) 0.0498(8) Uani 1 1 d . . .
Mo6 Mo 0.2676(2) 0.5003(2) 0.14873(17) 0.0375(7) Uani 1 1 d . . .
Si1 Si 0.0000 0.5000 0.0000 0.0212(17) Uani 1 2 d S . .
O1 O 0.2282(17) 0.1898(17) 0.1734(13) 0.041(2) Uani 1 1 d U . .
O2 O 0.285(2) 0.8476(19) -0.1561(16) 0.051(4) Uani 1 1 d U . .
O3 O 0.362(2) 0.468(2) -0.3103(15) 0.055(5) Uani 1 1 d U . .
O4 O 0.1751(17) 0.3877(18) 0.2437(15) 0.043(3) Uani 1 1 d U . .
O5 O 0.112(3) 0.157(2) 0.3683(15) 0.063(5) Uani 1 1 d U . .
O6 O 0.166(3) 0.349(2) -0.2009(16) 0.059(3) Uani 1 1 d U . .
O7 O 0.476(2) 0.1203(19) 0.0644(16) 0.058(5) Uani 1 1 d U . .
O8 O -0.050(2) 0.179(2) 0.0184(18) 0.057(3) Uani 1 1 d U . .
O9 O -0.0417(18) 0.201(2) 0.2018(19) 0.051(3) Uani 1 1 d U . .
O10 O 0.0952(18) 0.1166(18) -0.1496(14) 0.043(4) Uani 1 1 d U . .
C13 C 0.095(3) 0.782(4) 0.435(2) 0.057(8) Uani 1 1 d . . .
H9 H 0.0322 0.7867 0.4907 0.069 Uiso 1 1 calc R . .
C12 C 0.215(4) 0.682(4) 0.450(3) 0.069(10) Uani 1 1 d . . .
H10 H 0.2292 0.6179 0.5149 0.083 Uiso 1 1 calc R . .
O11 O 0.281(2) 0.606(2) -0.1631(17) 0.057(3) Uani 1 1 d U . .
O12 O 0.388(2) 0.504(2) 0.2178(17) 0.054(4) Uani 1 1 d U . .
O13 O -0.090(2) 0.389(2) 0.283(2) 0.054(3) Uani 1 1 d U . .
O14 O -0.053(3) 0.415(3) 0.108(2) 0.032(3) Uani 0.50 1 d PU . .
C9 C 0.059(3) 0.881(3) 0.339(3) 0.057(9) Uani 1 1 d . . .
H8 H -0.0265 0.9477 0.3289 0.069 Uiso 1 1 calc R . .
C14 C 0.318(3) 0.672(3) 0.373(2) 0.051(7) Uani 1 1 d . . .
H11 H 0.4027 0.6034 0.3848 0.061 Uiso 1 1 calc R . .
O15 O 0.370(3) 0.350(2) -0.0961(15) 0.056(3) Uani 1 1 d U . .
O16 O 0.292(2) 0.629(2) 0.0131(18) 0.062(3) Uani 1 1 d U . .
C11 C 0.2890(18) 0.7664(18) 0.2795(13) 0.048(8) Uani 1 1 d G . .
C8 C 0.1610(15) 0.8716(19) 0.2621(13) 0.049(7) Uani 1 1 d G . .
N4 N 0.1615(19) 0.9501(16) 0.1561(14) 0.054(7) Uani 1 1 d G . .
H12 H 0.0956 1.0198 0.1263 0.064 Uiso 1 1 calc R . .
C10 C 0.290(2) 0.893(2) 0.1080(13) 0.078(12) Uani 1 1 d G . .
H13 H 0.3174 0.9251 0.0387 0.094 Uiso 1 1 calc R . .
N3 N 0.3687(16) 0.7799(19) 0.1843(17) 0.062(8) Uani 1 1 d G . .
H14 H 0.4504 0.7283 0.1745 0.074 Uiso 1 1 calc R . .
O17 O 0.110(3) 0.421(3) 0.069(2) 0.036(2) Uani 0.50 1 d PU . .
O18 O 0.223(3) 0.175(2) -0.0115(14) 0.056(3) Uani 1 1 d U . .
O22 O 0.3625(17) 0.3667(18) 0.0937(14) 0.041(2) Uani 1 1 d U . .
C5 C 0.328(5) 0.931(5) 0.494(4) 0.096(5) Uani 1 1 d U . .
H7 H 0.2441 0.9968 0.4705 0.116 Uiso 1 1 calc R . .
C7 C 0.450(3) 0.757(3) 0.615(2) 0.065(10) Uani 1 1 d D . .
H5 H 0.4548 0.6960 0.6814 0.078 Uiso 1 1 calc R . .
C4 C 0.344(5) 0.851(5) 0.592(4) 0.107(14) Uani 1 1 d U . .
H6 H 0.2755 0.8676 0.6431 0.128 Uiso 1 1 calc R . .
O19 O 0.118(3) 0.399(3) -0.042(2) 0.039(3) Uani 0.50 1 d PU . .
O20 O -0.082(3) 0.423(3) -0.035(2) 0.039(3) Uani 0.50 1 d PU . .
O21 O -0.107(2) 0.358(2) -0.1660(19) 0.064(3) Uani 1 1 d U . .
C6 C 0.600(3) 0.920(3) 0.2784(18) 0.107(7) Uani 1 1 d GU . .
H2 H 0.6336 0.9480 0.2104 0.128 Uiso 1 1 calc R . .
N1 N 0.675(2) 0.814(3) 0.361(2) 0.106(6) Uani 1 1 d GU . .
H3 H 0.7599 0.7638 0.3572 0.127 Uiso 1 1 calc R . .
C2 C 0.585(3) 0.804(3) 0.4518(18) 0.097(5) Uani 1 1 d GDU . .
C3 C 0.455(3) 0.905(3) 0.425(2) 0.096(5) Uani 1 1 d GDU . .
N2 N 0.464(3) 0.976(3) 0.318(2) 0.102(7) Uani 1 1 d GU . .
H1 H 0.3980 1.0422 0.2830 0.122 Uiso 1 1 calc R . .
C1 C 0.559(4) 0.739(4) 0.549(2) 0.097(5) Uani 1 1 d DU . .
H4 H 0.6329 0.6631 0.5765 0.116 Uiso 1 1 calc R . .


_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
Mo1 O5 1.67(2) . ?
Mo1 O9 1.822(19) . ?
Mo1 O1 1.867(16) . ?
Mo1 O13 1.914(19) . ?
Mo1 O4 1.931(17) . ?
Mo1 O14 2.31(3) . ?
Mo2 O7 1.652(18) . ?
Mo2 O18 1.821(19) . ?
Mo2 O22 1.899(16) . ?
Mo2 O15 1.91(2) . ?
Mo2 O1 1.958(17) . ?
Mo2 O19 2.38(3) . ?
Mo3 O3 1.667(18) . ?
Mo3 O6 1.86(2) . ?
Mo3 O11 1.88(2) . ?
Mo3 O13 1.90(2) 2_565 ?
Mo3 O15 1.98(2) . ?
Mo3 O14 2.47(3) 2_565 ?
Mo3 O19 2.51(3) . ?
Mo4 O10 1.651(17) . ?
Mo4 O21 1.84(2) . ?
Mo4 O8 1.90(2) . ?
Mo4 O6 1.93(2) . ?
Mo4 O18 2.00(2) . ?
Mo4 O19 2.47(3) . ?
Mo4 O20 2.49(3) . ?
Mo5 O2 1.67(2) . ?
Mo5 O16 1.80(2) . ?
Mo5 O11 1.86(2) . ?
Mo5 O8 1.94(2) 2_565 ?
Mo5 O9 1.99(2) 2_565 ?
Mo6 O12 1.641(19) . ?
Mo6 O22 1.852(16) . ?
Mo6 O4 1.847(19) . ?
Mo6 O21 1.92(2) 2_565 ?
Mo6 O16 1.97(2) . ?
Mo6 O20 2.33(3) 2_565 ?
Si1 O17 1.40(3) . ?
Si1 O17 1.40(3) 2_565 ?
Si1 O19 1.56(3) 2_565 ?
Si1 O19 1.56(3) . ?
Si1 O14 1.58(3) . ?
Si1 O14 1.58(3) 2_565 ?
Si1 O20 1.58(3) . ?
Si1 O20 1.58(3) 2_565 ?
O8 Mo5 1.94(2) 2_565 ?
O9 Mo5 1.99(2) 2_565 ?
C13 C12 1.34(5) . ?
C13 C9 1.40(5) . ?
C13 H9 0.9300 . ?
C12 C14 1.37(4) . ?
C12 H10 0.9300 . ?
O13 Mo3 1.90(2) 2_565 ?
O14 O17 1.64(4) . ?
O14 Mo3 2.47(3) 2_565 ?
C9 C8 1.37(3) . ?
C9 H8 0.9300 . ?
C14 C11 1.36(4) . ?
C14 H11 0.9300 . ?
C11 N3 1.4200 . ?
C11 C8 1.4200 . ?
C8 N4 1.4200 . ?
N4 C10 1.4200 . ?
N4 H12 0.8600 . ?
C10 N3 1.4200 . ?
C10 H13 0.9300 . ?
N3 H14 0.8600 . ?
O17 O20 1.60(4) 2_565 ?
O17 O19 1.63(4) . ?
C5 C4 1.34(6) . ?
C5 C3 1.48(5) . ?
C5 H7 0.9300 . ?
C7 C4 1.22(5) . ?
C7 C1 1.33(2) . ?
C7 H5 0.9300 . ?
C4 H6 0.9300 . ?
O20 O17 1.60(4) 2_565 ?
O20 Mo6 2.33(3) 2_565 ?
O21 Mo6 1.92(2) 2_565 ?
C6 N1 1.4200 . ?
C6 N2 1.4200 . ?
C6 H2 0.9300 . ?
N1 C2 1.4200 . ?
N1 H3 0.8600 . ?
C2 C1 1.32(2) . ?
C2 C3 1.4200 . ?
C3 N2 1.4200 . ?
N2 H1 0.8600 . ?
C1 H4 0.9300 . ?

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
O5 Mo1 O9 103.6(11) . . ?
O5 Mo1 O1 100.5(9) . . ?
O9 Mo1 O1 90.5(8) . . ?
O5 Mo1 O13 99.0(11) . . ?
O9 Mo1 O13 88.8(8) . . ?
O1 Mo1 O13 160.1(10) . . ?
O5 Mo1 O4 101.0(10) . . ?
O9 Mo1 O4 155.4(9) . . ?
O1 Mo1 O4 86.8(7) . . ?
O13 Mo1 O4 85.5(8) . . ?
O5 Mo1 O14 160.8(11) . . ?
O9 Mo1 O14 66.0(10) . . ?
O1 Mo1 O14 95.8(8) . . ?
O13 Mo1 O14 65.8(10) . . ?
O4 Mo1 O14 89.9(9) . . ?
O7 Mo2 O18 99.5(12) . . ?
O7 Mo2 O22 103.7(10) . . ?
O18 Mo2 O22 156.2(10) . . ?
O7 Mo2 O15 101.5(11) . . ?
O18 Mo2 O15 91.1(8) . . ?
O22 Mo2 O15 89.2(8) . . ?
O7 Mo2 O1 98.1(8) . . ?
O18 Mo2 O1 87.5(8) . . ?
O22 Mo2 O1 84.3(7) . . ?
O15 Mo2 O1 160.3(10) . . ?
O7 Mo2 O19 160.7(10) . . ?
O18 Mo2 O19 65.1(11) . . ?
O22 Mo2 O19 93.0(9) . . ?
O15 Mo2 O19 68.8(11) . . ?
O1 Mo2 O19 92.9(9) . . ?
O3 Mo3 O6 99.6(11) . . ?
O3 Mo3 O11 106.6(11) . . ?
O6 Mo3 O11 153.5(10) . . ?
O3 Mo3 O13 99.2(10) . 2_565 ?
O6 Mo3 O13 90.4(10) . 2_565 ?
O11 Mo3 O13 89.2(9) . 2_565 ?
O3 Mo3 O15 99.3(10) . . ?
O6 Mo3 O15 87.4(9) . . ?
O11 Mo3 O15 84.7(9) . . ?
O13 Mo3 O15 161.4(10) 2_565 . ?
O3 Mo3 O14 158.0(10) . 2_565 ?
O6 Mo3 O14 93.1(10) . 2_565 ?
O11 Mo3 O14 63.4(9) . 2_565 ?
O13 Mo3 O14 62.6(9) 2_565 2_565 ?
O15 Mo3 O14 99.1(9) . 2_565 ?
O3 Mo3 O19 156.8(10) . . ?
O6 Mo3 O19 64.2(10) . . ?
O11 Mo3 O19 89.6(10) . . ?
O13 Mo3 O19 97.5(10) 2_565 . ?
O15 Mo3 O19 65.0(10) . . ?
O14 Mo3 O19 44.9(10) 2_565 . ?
O10 Mo4 O21 105.4(10) . . ?
O10 Mo4 O8 100.7(10) . . ?
O21 Mo4 O8 89.7(10) . . ?
O10 Mo4 O6 100.2(10) . . ?
O21 Mo4 O6 89.6(10) . . ?
O8 Mo4 O6 158.6(9) . . ?
O10 Mo4 O18 98.7(9) . . ?
O21 Mo4 O18 155.9(10) . . ?
O8 Mo4 O18 86.6(9) . . ?
O6 Mo4 O18 85.4(8) . . ?
O10 Mo4 O19 154.2(9) . . ?
O21 Mo4 O19 95.4(10) . . ?
O8 Mo4 O19 94.4(10) . . ?
O6 Mo4 O19 64.4(9) . . ?
O18 Mo4 O19 61.2(9) . . ?
O10 Mo4 O20 160.5(9) . . ?
O21 Mo4 O20 59.9(10) . . ?
O8 Mo4 O20 68.4(10) . . ?
O6 Mo4 O20 92.9(10) . . ?
O18 Mo4 O20 96.8(10) . . ?
O19 Mo4 O20 45.3(10) . . ?
O2 Mo5 O16 103.8(10) . . ?
O2 Mo5 O11 103.2(10) . . ?
O16 Mo5 O11 88.3(10) . . ?
O2 Mo5 O8 102.2(10) . 2_565 ?
O16 Mo5 O8 90.0(10) . 2_565 ?
O11 Mo5 O8 154.3(10) . 2_565 ?
O2 Mo5 O9 100.7(9) . 2_565 ?
O16 Mo5 O9 155.6(10) . 2_565 ?
O11 Mo5 O9 86.6(9) . 2_565 ?
O8 Mo5 O9 84.4(9) 2_565 2_565 ?
O12 Mo6 O22 103.8(8) . . ?
O12 Mo6 O4 103.2(10) . . ?
O22 Mo6 O4 89.5(8) . . ?
O12 Mo6 O21 102.1(10) . 2_565 ?
O22 Mo6 O21 154.1(9) . 2_565 ?
O4 Mo6 O21 86.5(9) . 2_565 ?
O12 Mo6 O16 102.8(10) . . ?
O22 Mo6 O16 88.5(9) . . ?
O4 Mo6 O16 153.7(9) . . ?
O21 Mo6 O16 84.0(10) 2_565 . ?
O12 Mo6 O20 159.1(11) . 2_565 ?
O22 Mo6 O20 92.0(9) . 2_565 ?
O4 Mo6 O20 90.4(9) . 2_565 ?
O21 Mo6 O20 62.5(10) 2_565 2_565 ?
O16 Mo6 O20 63.5(10) . 2_565 ?
O17 Si1 O17 179.998(4) . 2_565 ?
O17 Si1 O19 113.7(16) . 2_565 ?
O17 Si1 O19 66.3(16) 2_565 2_565 ?
O17 Si1 O19 66.3(16) . . ?
O17 Si1 O19 113.7(16) 2_565 . ?
O19 Si1 O19 179.999(3) 2_565 . ?
O17 Si1 O14 66.5(15) . . ?
O17 Si1 O14 113.5(15) 2_565 . ?
O19 Si1 O14 74.5(15) 2_565 . ?
O19 Si1 O14 105.5(15) . . ?
O17 Si1 O14 113.5(15) . 2_565 ?
O17 Si1 O14 66.5(15) 2_565 2_565 ?
O19 Si1 O14 105.5(15) 2_565 2_565 ?
O19 Si1 O14 74.5(15) . 2_565 ?
O14 Si1 O14 180(2) . 2_565 ?
O17 Si1 O20 115.7(16) . . ?
O17 Si1 O20 64.3(16) 2_565 . ?
O19 Si1 O20 105.4(16) 2_565 . ?
O19 Si1 O20 74.6(16) . . ?
O14 Si1 O20 78.2(15) . . ?
O14 Si1 O20 101.8(15) 2_565 . ?
O17 Si1 O20 64.3(16) . 2_565 ?
O17 Si1 O20 115.7(16) 2_565 2_565 ?
O19 Si1 O20 74.6(16) 2_565 2_565 ?
O19 Si1 O20 105.4(16) . 2_565 ?
O14 Si1 O20 101.8(15) . 2_565 ?
O14 Si1 O20 78.2(15) 2_565 2_565 ?
O20 Si1 O20 180.0(14) . 2_565 ?
Mo1 O1 Mo2 138.4(9) . . ?
Mo6 O4 Mo1 140.1(10) . . ?
Mo3 O6 Mo4 140.0(12) . . ?
Mo4 O8 Mo5 134.1(13) . 2_565 ?
Mo1 O9 Mo5 139.9(12) . 2_565 ?
C12 C13 C9 124(3) . . ?
C12 C13 H9 118.2 . . ?
C9 C13 H9 117.7 . . ?
C13 C12 C14 122(3) . . ?
C13 C12 H10 119.1 . . ?
C14 C12 H10 118.7 . . ?
Mo5 O11 Mo3 144.1(13) . . ?
Mo3 O13 Mo1 135.7(14) 2_565 . ?
Si1 O14 O17 51.4(13) . . ?
Si1 O14 Mo1 130.0(14) . . ?
O17 O14 Mo1 78.6(14) . . ?
Si1 O14 Mo3 121.0(14) . 2_565 ?
O17 O14 Mo3 136.9(18) . 2_565 ?
Mo1 O14 Mo3 95.1(10) . 2_565 ?
C8 C9 C13 114(3) . . ?
C8 C9 H8 122.2 . . ?
C13 C9 H8 123.4 . . ?
C11 C14 C12 116(3) . . ?
C11 C14 H11 121.8 . . ?
C12 C14 H11 122.2 . . ?
Mo2 O15 Mo3 132.6(14) . . ?
Mo5 O16 Mo6 141.0(13) . . ?
C14 C11 N3 129.8(17) . . ?
C14 C11 C8 122.1(17) . . ?
N3 C11 C8 108.0 . . ?
C9 C8 N4 131(2) . . ?
C9 C8 C11 121(2) . . ?
N4 C8 C11 108.0 . . ?
C10 N4 C8 108.0 . . ?
C10 N4 H12 126.0 . . ?
C8 N4 H12 126.0 . . ?
N4 C10 N3 108.0 . . ?
N4 C10 H13 126.0 . . ?
N3 C10 H13 126.0 . . ?
C11 N3 C10 108.0 . . ?
C11 N3 H14 126.0 . . ?
C10 N3 H14 126.0 . . ?
Si1 O17 O20 63.3(15) . 2_565 ?
Si1 O17 O19 61.6(15) . . ?
O20 O17 O19 102(2) 2_565 . ?
Si1 O17 O14 62.0(14) . . ?
O20 O17 O14 99(2) 2_565 . ?
O19 O17 O14 100(2) . . ?
Mo2 O18 Mo4 137.9(13) . . ?
Mo6 O22 Mo2 141.4(9) . . ?
C4 C5 C3 114(4) . . ?
C4 C5 H7 122.5 . . ?
C3 C5 H7 123.3 . . ?
C4 C7 C1 122(4) . . ?
C4 C7 H5 118.6 . . ?
C1 C7 H5 118.9 . . ?
C7 C4 C5 119(5) . . ?
C7 C4 H6 119.5 . . ?
C5 C4 H6 121.0 . . ?
Si1 O19 O17 52.1(14) . . ?
Si1 O19 Mo2 128.0(16) . . ?
O17 O19 Mo2 75.9(15) . . ?
Si1 O19 Mo4 121.0(17) . . ?
O17 O19 Mo4 135(2) . . ?
Mo2 O19 Mo4 94.8(11) . . ?
Si1 O19 Mo3 119.5(16) . . ?
O17 O19 Mo3 132(2) . . ?
Mo2 O19 Mo3 93.2(11) . . ?
Mo4 O19 Mo3 91.4(10) . . ?
Si1 O20 O17 52.4(14) . 2_565 ?
Si1 O20 Mo6 130.6(17) . 2_565 ?
O17 O20 Mo6 78.3(15) 2_565 2_565 ?
Si1 O20 Mo4 119.0(15) . . ?
O17 O20 Mo4 137(2) 2_565 . ?
Mo6 O20 Mo4 95.2(11) 2_565 . ?
Mo4 O21 Mo6 141.9(14) . 2_565 ?
N1 C6 N2 108.0 . . ?
N1 C6 H2 126.1 . . ?
N2 C6 H2 125.9 . . ?
C2 N1 C6 108.0 . . ?
C2 N1 H3 126.0 . . ?
C6 N1 H3 126.0 . . ?
C1 C2 N1 149(3) . . ?
C1 C2 C3 102(3) . . ?
N1 C2 C3 108.0 . . ?
N2 C3 C2 108.0 . . ?
N2 C3 C5 125(3) . . ?
C2 C3 C5 127(3) . . ?
C3 N2 C6 108.0 . . ?
C3 N2 H1 126.0 . . ?
C6 N2 H1 126.0 . . ?
C2 C1 C7 134(4) . . ?
C2 C1 H4 113.6 . . ?
C7 C1 H4 112.7 . . ?

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
N2 H1 O1 0.86 2.25 3.10(3) 169.0 1_565
N4 H12 O9 0.86 2.53 3.12(2) 126.1 1_565
N4 H12 O8 0.86 2.15 2.99(3) 165.7 1_565

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.04
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         2.866
_refine_diff_density_min         -2.828
_refine_diff_density_rms         0.317
####################################################################### 
# 
# 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_zhn20140605_1227_0m
_database_code_depnum_ccdc_archive 'CCDC 1038933'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H26 Ag7 As N18 O40 W12'
_chemical_formula_sum            'C36 H26 Ag7 As N18 O40 W12'
_chemical_formula_weight         4386.84

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6544(8)
_cell_length_b                   12.8654(9)
_cell_length_c                   13.5532(9)
_cell_angle_alpha                95.9940(10)
_cell_angle_beta                 111.0330(10)
_cell_angle_gamma                106.860(2)
_cell_volume                     1765.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    14695
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1938
_exptl_absorpt_coefficient_mu    21.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0353
_exptl_absorpt_correction_T_max  0.0529
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 Smart APEX 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            14695
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         28.28
_reflns_number_total             8726
_reflns_number_gt                7726
_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 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. 
;

_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)+(0.0374P)²+41.5594P] 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     SHELXL
_refine_ls_extinction_coef       0.00109(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8726
_refine_ls_number_parameters     536
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0741
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.081
_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 0.67502(8) -0.07695(7) 0.79809(7) 0.0177(2) Uani 1 1 d . . .
W3 W 1.25577(8) 0.22772(7) 0.99501(7) 0.0179(2) Uani 1 1 d . . .
W6 W 0.92212(9) -0.13629(8) 0.73101(7) 0.0243(2) Uani 1 1 d . . .
W4 W 0.99843(9) 0.27644(7) 1.05444(8) 0.0236(2) Uani 1 1 d U . .
W2 W 0.93383(9) 0.14377(7) 0.78673(7) 0.0189(2) Uani 1 1 d . . .
W5 W 0.74946(9) 0.04884(9) 1.07072(8) 0.0242(2) Uani 1 1 d U . .
Ag1 Ag 0.21892(19) 0.47153(19) 0.50334(18) 0.0373(5) Uani 1 1 d . . .
Ag3 Ag 0.0000 0.0000 0.5000 0.0455(8) Uani 1 2 d S . .
Ag2 Ag -0.2697(3) 0.10337(19) 0.3541(2) 0.0465(6) Uani 1 1 d . . .
Ag4 Ag 0.0686(3) 0.2728(2) 0.5803(2) 0.0476(6) Uani 1 1 d . . .
C1 C -0.598(4) -0.286(3) 0.139(3) 0.057(9) Uani 1 1 d . . .
H12 H -0.6862 -0.3014 0.0964 0.068 Uiso 1 1 calc R . .
O3 O 1.1688(19) 0.2994(18) 1.0554(16) 0.040(3) Uani 1 1 d U . .
O6 O 1.1176(19) 0.2046(18) 0.8565(17) 0.040(2) Uani 1 1 d U . .
O8 O 0.9317(19) 0.2419(18) 0.9013(16) 0.040(2) Uani 1 1 d U . .
O16 O 0.761(2) 0.0548(17) 0.7678(18) 0.041(2) Uani 1 1 d U . .
O22 O 0.670(2) 0.0073(16) 0.9159(16) 0.038(3) Uani 1 1 d U . .
O21 O 0.836(2) 0.1882(19) 1.0494(18) 0.045(3) Uani 1 1 d U . .
O4 O 0.8831(19) -0.2001(16) 0.6026(15) 0.036(4) Uani 1 1 d U . .
O5 O 0.635(2) 0.0728(18) 1.1062(17) 0.037(4) Uani 1 1 d U . .
O13 O 0.904(2) 0.210(2) 0.6850(17) 0.041(4) Uani 1 1 d U . .
O20 O 1.002(2) 0.4059(16) 1.0821(18) 0.041(4) Uani 1 1 d U . .
O15 O 1.375(2) 0.3359(19) 0.9949(18) 0.050(5) Uani 1 1 d U . .
O7 O 0.5218(19) -0.1148(17) 0.7042(18) 0.042(4) Uani 1 1 d U . .
O11 O 0.7552(19) -0.1509(17) 0.7262(18) 0.040(3) Uani 1 1 d U . .
O9 O 0.9437(19) 0.0145(17) 0.7178(18) 0.042(3) Uani 1 1 d U . .
O12 O 1.339(2) 0.1988(17) 1.1319(16) 0.040(3) Uani 1 1 d U . .
N2 N -0.176(2) 0.2799(18) 0.3790(18) 0.028(4) Uani 1 1 d . . .
N9 N -0.050(2) 0.3255(17) 0.4482(17) 0.027(4) Uani 1 1 d . . .
N1 N 0.012(2) 0.4164(17) 0.4226(17) 0.026(4) Uani 1 1 d . . .
C2 C -0.076(2) 0.4308(18) 0.3348(19) 0.021(4) Uani 1 1 d . . .
C3 C -0.196(2) 0.3439(18) 0.304(2) 0.023(4) Uani 1 1 d . . .
C4 C -0.308(2) 0.334(2) 0.213(2) 0.030(5) Uani 1 1 d . . .
H4 H -0.3867 0.2752 0.1916 0.036 Uiso 1 1 calc R . .
N3 N -0.290(2) -0.067(2) 0.331(2) 0.040(6) Uani 1 1 d . . .
N8 N -0.185(2) -0.097(2) 0.376(2) 0.033(5) Uani 1 1 d . . .
C5 C -0.389(3) -0.161(2) 0.263(2) 0.032(6) Uani 1 1 d . . .
N6 N -0.213(2) -0.2051(19) 0.3399(18) 0.030(5) Uani 1 1 d . . .
C6 C -0.067(3) 0.515(2) 0.275(2) 0.027(5) Uani 1 1 d . . .
H14 H 0.0122 0.5733 0.2943 0.033 Uiso 1 1 calc R . .
C7 C -0.177(3) 0.506(2) 0.188(2) 0.034(6) Uani 1 1 d . . .
H3 H -0.1737 0.5614 0.1489 0.041 Uiso 1 1 calc R . .
C8 C -0.422(3) -0.357(2) 0.206(2) 0.032(6) Uani 1 1 d . . .
H10 H -0.3916 -0.4167 0.2087 0.038 Uiso 1 1 calc R . .
C9 C -0.340(3) -0.248(2) 0.268(2) 0.032(5) Uani 1 1 d . . .
C10 C -0.296(3) 0.416(2) 0.157(2) 0.034(6) Uani 1 1 d . . .
H6 H -0.3681 0.4116 0.0957 0.041 Uiso 1 1 calc R . .
O14 O 0.718(2) -0.1029(18) 1.0693(16) 0.042(3) Uani 1 1 d U . .
O10 O 1.108(2) -0.0855(19) 0.7931(19) 0.048(3) Uani 1 1 d U . .
C11 C -0.550(3) -0.371(3) 0.143(3) 0.048(8) Uani 1 1 d . . .
H11 H -0.6062 -0.4423 0.1006 0.057 Uiso 1 1 calc R . .
C12 C -0.521(4) -0.180(3) 0.196(3) 0.057(9) Uani 1 1 d . . .
H13 H -0.5536 -0.1221 0.1916 0.069 Uiso 1 1 calc R . .
O17 O 0.9217(19) -0.254(2) 0.8017(19) 0.048(3) Uani 1 1 d U . .
As1 As 1.0000 0.0000 1.0000 0.0222(5) Uani 1 2 d S . .
O18 O 0.916(3) -0.007(3) 0.879(3) 0.030(2) Uani 0.50 1 d PU . .
O2 O 1.148(3) 0.049(3) 1.026(3) 0.027(3) Uani 0.50 1 d PU . .
O19 O 1.034(3) 0.111(3) 0.969(3) 0.030(2) Uani 0.50 1 d PU . .
O1 O 0.966(3) 0.084(3) 1.071(3) 0.028(2) Uani 0.50 1 d PU . .
N4 N 0.416(2) 0.4992(18) 0.5993(17) 0.026(4) Uani 1 1 d . . .
C13 C 0.488(2) 0.431(2) 0.5925(19) 0.024(5) Uani 1 1 d . . .
N7 N 0.502(3) 0.595(2) 0.670(2) 0.047(6) Uani 1 1 d . . .
C14 C 0.620(2) 0.492(2) 0.662(2) 0.027(5) Uani 1 1 d . . .
C15 C 0.451(3) 0.324(2) 0.537(2) 0.033(6) Uani 1 1 d . . .
H5 H 0.3630 0.2825 0.4937 0.040 Uiso 1 1 calc R . .
C16 C 0.719(3) 0.446(2) 0.677(2) 0.036(6) Uani 1 1 d . . .
H8 H 0.8059 0.4851 0.7246 0.044 Uiso 1 1 calc R . .
C17 C 0.678(3) 0.337(3) 0.616(3) 0.047(8) Uani 1 1 d . . .
H7 H 0.7393 0.3029 0.6224 0.056 Uiso 1 1 calc R . .
C18 C 0.547(3) 0.279(3) 0.547(3) 0.048(7) Uani 1 1 d . . .
H9 H 0.5236 0.2082 0.5057 0.058 Uiso 1 1 calc R . .
N5 N 0.623(2) 0.5916(19) 0.7088(18) 0.031(5) Uani 1 1 d . . .
H1 H 0.6922 0.6443 0.7559 0.038 Uiso 1 1 calc R . .


_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 O7 1.667(19) . ?
W1 O22 1.864(19) . ?
W1 O16 1.87(2) . ?
W1 O12 1.91(2) 2_757 ?
W1 O11 1.924(19) . ?
W1 O2 2.44(3) 2_757 ?
W1 O18 2.46(3) . ?
W3 O15 1.658(18) . ?
W3 O3 1.878(19) . ?
W3 O12 1.893(19) . ?
W3 O14 1.90(2) 2_757 ?
W3 O6 1.91(2) . ?
W3 O2 2.43(3) . ?
W3 O19 2.46(3) . ?
W6 O4 1.681(17) . ?
W6 O11 1.876(19) . ?
W6 O17 1.88(2) . ?
W6 O10 1.89(2) . ?
W6 O9 1.92(2) . ?
W6 O1 2.44(3) 2_757 ?
W6 O18 2.50(3) . ?
W4 O20 1.655(18) . ?
W4 O21 1.88(2) . ?
W4 O8 1.89(2) . ?
W4 O3 1.916(19) . ?
W4 O17 1.93(2) 2_757 ?
W4 O1 2.44(3) . ?
W2 O13 1.682(19) . ?
W2 O9 1.88(2) . ?
W2 O6 1.87(2) . ?
W2 O8 1.908(19) . ?
W2 O16 1.92(2) . ?
W2 O18 2.42(3) . ?
W2 O19 2.47(3) . ?
W5 O5 1.666(17) . ?
W5 O14 1.88(2) . ?
W5 O10 1.89(2) 2_757 ?
W5 O21 1.89(2) . ?
W5 O22 1.905(19) . ?
W5 O1 2.43(3) . ?
Ag1 N4 2.10(2) . ?
Ag1 N1 2.11(2) . ?
Ag1 Ag4 3.156(3) . ?
Ag3 N8 2.10(3) 2_556 ?
Ag3 N8 2.10(3) . ?
Ag3 Ag4 3.330(3) . ?
Ag3 Ag4 3.331(3) 2_556 ?
Ag2 N3 2.12(2) . ?
Ag2 N2 2.14(2) . ?
Ag4 N6 2.12(2) 2_556 ?
Ag4 N9 2.15(2) . ?
C1 C12 1.36(5) . ?
C1 C11 1.37(5) . ?
O12 W1 1.91(2) 2_757 ?
N2 N9 1.33(3) . ?
N2 C3 1.37(3) . ?
N9 N1 1.34(3) . ?
N1 C2 1.34(3) . ?
C2 C3 1.40(3) . ?
C2 C6 1.42(3) . ?
C3 C4 1.40(3) . ?
C4 C10 1.36(4) . ?
N3 N8 1.35(3) . ?
N3 C5 1.35(4) . ?
N8 N6 1.32(3) . ?
C5 C9 1.39(3) . ?
C5 C12 1.41(5) . ?
N6 C9 1.35(4) . ?
N6 Ag4 2.12(2) 2_556 ?
C6 C7 1.36(4) . ?
C7 C10 1.41(4) . ?
C8 C11 1.37(4) . ?
C8 C9 1.41(4) . ?
O14 W3 1.90(2) 2_757 ?
O10 W5 1.89(2) 2_757 ?
O17 W4 1.93(2) 2_757 ?
As1 O19 1.51(3) . ?
As1 O19 1.51(3) 2_757 ?
As1 O2 1.55(3) 2_757 ?
As1 O2 1.55(3) . ?
As1 O18 1.55(3) . ?
As1 O18 1.55(3) 2_757 ?
As1 O1 1.60(3) 2_757 ?
As1 O1 1.60(3) . ?
O18 O19 1.70(5) . ?
O18 O2 1.77(4) 2_757 ?
O2 O19 1.73(4) . ?
O2 O18 1.77(4) 2_757 ?
O2 W1 2.44(3) 2_757 ?
O1 W6 2.44(3) 2_757 ?
N4 N7 1.34(3) . ?
N4 C13 1.40(3) . ?
C13 C15 1.36(4) . ?
C13 C14 1.40(3) . ?
N7 N5 1.34(3) . ?
C14 N5 1.36(3) . ?
C14 C16 1.40(4) . ?
C15 C18 1.37(4) . ?
C16 C17 1.40(4) . ?
C17 C18 1.39(5) . ?

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
O7 W1 O22 102.6(10) . . ?
O7 W1 O16 102.4(10) . . ?
O22 W1 O16 89.7(9) . . ?
O7 W1 O12 101.0(10) . 2_757 ?
O22 W1 O12 88.1(8) . 2_757 ?
O16 W1 O12 156.3(10) . 2_757 ?
O7 W1 O11 102.6(10) . . ?
O22 W1 O11 154.6(9) . . ?
O16 W1 O11 87.5(8) . . ?
O12 W1 O11 84.6(9) 2_757 . ?
O7 W1 O2 158.3(11) . 2_757 ?
O22 W1 O2 64.2(9) . 2_757 ?
O16 W1 O2 95.0(10) . 2_757 ?
O12 W1 O2 63.0(10) 2_757 2_757 ?
O11 W1 O2 90.9(10) . 2_757 ?
O7 W1 O18 159.3(11) . . ?
O22 W1 O18 92.2(10) . . ?
O16 W1 O18 62.8(10) . . ?
O12 W1 O18 93.8(10) 2_757 . ?
O11 W1 O18 64.2(10) . . ?
O2 W1 O18 42.4(11) 2_757 . ?
O15 W3 O3 101.4(11) . . ?
O15 W3 O12 101.1(11) . . ?
O3 W3 O12 89.0(9) . . ?
O15 W3 O14 103.3(12) . 2_757 ?
O3 W3 O14 155.2(10) . 2_757 ?
O12 W3 O14 87.8(8) . 2_757 ?
O15 W3 O6 102.2(11) . . ?
O3 W3 O6 87.4(8) . . ?
O12 W3 O6 156.6(10) . . ?
O14 W3 O6 85.9(8) 2_757 . ?
O15 W3 O2 159.4(12) . . ?
O3 W3 O2 92.1(10) . . ?
O12 W3 O2 63.3(10) . . ?
O14 W3 O2 64.5(10) 2_757 . ?
O6 W3 O2 93.7(10) . . ?
O15 W3 O19 159.0(12) . . ?
O3 W3 O19 64.3(10) . . ?
O12 W3 O19 94.2(11) . . ?
O14 W3 O19 91.4(11) 2_757 . ?
O6 W3 O19 63.5(10) . . ?
O2 W3 O19 41.5(11) . . ?
O4 W6 O11 101.0(9) . . ?
O4 W6 O17 102.1(11) . . ?
O11 W6 O17 89.2(9) . . ?
O4 W6 O10 102.8(10) . . ?
O11 W6 O10 156.1(11) . . ?
O17 W6 O10 88.7(9) . . ?
O4 W6 O9 101.0(10) . . ?
O11 W6 O9 87.5(9) . . ?
O17 W6 O9 156.9(11) . . ?
O10 W6 O9 85.2(9) . . ?
O4 W6 O1 158.2(10) . 2_757 ?
O11 W6 O1 95.4(10) . 2_757 ?
O17 W6 O1 63.6(11) . 2_757 ?
O10 W6 O1 62.5(10) . 2_757 ?
O9 W6 O1 93.9(10) . 2_757 ?
O4 W6 O18 156.7(10) . . ?
O11 W6 O18 63.8(10) . . ?
O17 W6 O18 95.4(11) . . ?
O10 W6 O18 92.7(11) . . ?
O9 W6 O18 62.7(10) . . ?
O1 W6 O18 45.0(11) 2_757 . ?
O20 W4 O21 104.0(11) . . ?
O20 W4 O8 102.2(10) . . ?
O21 W4 O8 91.0(9) . . ?
O20 W4 O3 102.2(10) . . ?
O21 W4 O3 153.5(10) . . ?
O8 W4 O3 87.3(8) . . ?
O20 W4 O17 101.5(11) . 2_757 ?
O21 W4 O17 87.5(9) . 2_757 ?
O8 W4 O17 155.9(10) . 2_757 ?
O3 W4 O17 83.5(9) . 2_757 ?
O20 W4 O1 157.7(11) . . ?
O21 W4 O1 61.5(10) . . ?
O8 W4 O1 95.3(10) . . ?
O3 W4 O1 92.3(10) . . ?
O17 W4 O1 63.1(11) 2_757 . ?
O13 W2 O9 100.8(11) . . ?
O13 W2 O6 101.5(10) . . ?
O9 W2 O6 90.2(9) . . ?
O13 W2 O8 102.5(11) . . ?
O9 W2 O8 156.7(10) . . ?
O6 W2 O8 87.0(8) . . ?
O13 W2 O16 102.7(10) . . ?
O9 W2 O16 87.6(8) . . ?
O6 W2 O16 155.7(10) . . ?
O8 W2 O16 85.6(9) . . ?
O13 W2 O18 159.1(12) . . ?
O9 W2 O18 65.0(10) . . ?
O6 W2 O18 94.1(11) . . ?
O8 W2 O18 92.1(11) . . ?
O16 W2 O18 63.1(10) . . ?
O13 W2 O19 160.2(12) . . ?
O9 W2 O19 92.8(11) . . ?
O6 W2 O19 63.7(10) . . ?
O8 W2 O19 65.2(10) . . ?
O16 W2 O19 92.2(10) . . ?
O18 W2 O19 40.8(12) . . ?
O5 W5 O14 102.9(10) . . ?
O5 W5 O10 101.7(11) . 2_757 ?
O14 W5 O10 89.0(10) . 2_757 ?
O5 W5 O21 103.2(11) . . ?
O14 W5 O21 153.8(11) . . ?
O10 W5 O21 87.4(9) 2_757 . ?
O5 W5 O22 104.8(10) . . ?
O14 W5 O22 87.9(8) . . ?
O10 W5 O22 153.3(10) 2_757 . ?
O21 W5 O22 83.7(9) . . ?
O5 W5 O1 157.2(11) . . ?
O14 W5 O1 93.9(11) . . ?
O10 W5 O1 62.8(11) 2_757 . ?
O21 W5 O1 61.6(11) . . ?
O22 W5 O1 90.9(10) . . ?
N4 Ag1 N1 168.2(8) . . ?
N4 Ag1 Ag4 102.5(6) . . ?
N1 Ag1 Ag4 65.7(6) . . ?
N8 Ag3 N8 179.999(2) 2_556 . ?
N8 Ag3 Ag4 61.2(6) 2_556 . ?
N8 Ag3 Ag4 118.8(6) . . ?
N8 Ag3 Ag4 118.8(6) 2_556 2_556 ?
N8 Ag3 Ag4 61.2(6) . 2_556 ?
Ag4 Ag3 Ag4 180.0 . 2_556 ?
N3 Ag2 N2 157.8(9) . . ?
N6 Ag4 N9 156.1(8) 2_556 . ?
N6 Ag4 Ag1 104.2(6) 2_556 . ?
N9 Ag4 Ag1 63.6(6) . . ?
N6 Ag4 Ag3 62.1(7) 2_556 . ?
N9 Ag4 Ag3 108.0(6) . . ?
Ag1 Ag4 Ag3 128.68(9) . . ?
C12 C1 C11 122(4) . . ?
W3 O3 W4 140.6(12) . . ?
W2 O6 W3 139.8(13) . . ?
W4 O8 W2 139.2(12) . . ?
W1 O16 W2 139.7(13) . . ?
W1 O22 W5 141.5(11) . . ?
W4 O21 W5 142.1(14) . . ?
W6 O11 W1 139.5(12) . . ?
W2 O9 W6 139.2(12) . . ?
W3 O12 W1 138.9(12) . 2_757 ?
N9 N2 C3 106.9(19) . . ?
N9 N2 Ag2 117.3(15) . . ?
C3 N2 Ag2 127.8(17) . . ?
N2 N9 N1 111.5(19) . . ?
N2 N9 Ag4 132.1(16) . . ?
N1 N9 Ag4 116.2(16) . . ?
C2 N1 N9 107(2) . . ?
C2 N1 Ag1 137.1(17) . . ?
N9 N1 Ag1 114.0(15) . . ?
N1 C2 C3 108(2) . . ?
N1 C2 C6 132(2) . . ?
C3 C2 C6 120(2) . . ?
N2 C3 C4 132(2) . . ?
N2 C3 C2 106(2) . . ?
C4 C3 C2 122(2) . . ?
C10 C4 C3 117(2) . . ?
N8 N3 C5 106(2) . . ?
N8 N3 Ag2 120.1(19) . . ?
C5 N3 Ag2 132.8(18) . . ?
N6 N8 N3 111(2) . . ?
N6 N8 Ag3 120.2(17) . . ?
N3 N8 Ag3 128.4(19) . . ?
N3 C5 C9 108(2) . . ?
N3 C5 C12 131(3) . . ?
C9 C5 C12 121(3) . . ?
N8 N6 C9 108(2) . . ?
N8 N6 Ag4 116.5(17) . 2_556 ?
C9 N6 Ag4 135.1(19) . 2_556 ?
C7 C6 C2 118(2) . . ?
C6 C7 C10 121(2) . . ?
C11 C8 C9 116(3) . . ?
N6 C9 C5 107(3) . . ?
N6 C9 C8 132(2) . . ?
C5 C9 C8 121(3) . . ?
C4 C10 C7 122(2) . . ?
W5 O14 W3 140.5(13) . 2_757 ?
W5 O10 W6 140.3(14) 2_757 . ?
C8 C11 C1 123(3) . . ?
C1 C12 C5 117(3) . . ?
W6 O17 W4 138.9(14) . 2_757 ?
O19 As1 O19 179.998(8) . 2_757 ?
O19 As1 O2 111.0(17) . 2_757 ?
O19 As1 O2 69.0(17) 2_757 2_757 ?
O19 As1 O2 69.0(17) . . ?
O19 As1 O2 111.0(17) 2_757 . ?
O2 As1 O2 180.000(9) 2_757 . ?
O19 As1 O18 67.3(18) . . ?
O19 As1 O18 112.7(18) 2_757 . ?
O2 As1 O18 69.6(17) 2_757 . ?
O2 As1 O18 110.4(17) . . ?
O19 As1 O18 112.7(18) . 2_757 ?
O19 As1 O18 67.3(18) 2_757 2_757 ?
O2 As1 O18 110.4(17) 2_757 2_757 ?
O2 As1 O18 69.6(17) . 2_757 ?
O18 As1 O18 179.998(14) . 2_757 ?
O19 As1 O1 107.8(17) . 2_757 ?
O19 As1 O1 72.2(17) 2_757 2_757 ?
O2 As1 O1 108.5(17) 2_757 2_757 ?
O2 As1 O1 71.5(17) . 2_757 ?
O18 As1 O1 73.7(17) . 2_757 ?
O18 As1 O1 106.3(17) 2_757 2_757 ?
O19 As1 O1 72.2(17) . . ?
O19 As1 O1 107.8(17) 2_757 . ?
O2 As1 O1 71.5(17) 2_757 . ?
O2 As1 O1 108.5(17) . . ?
O18 As1 O1 106.3(17) . . ?
O18 As1 O1 73.7(17) 2_757 . ?
O1 As1 O1 179.999(15) 2_757 . ?
As1 O18 O19 55.2(16) . . ?
As1 O18 O2 55.0(15) . 2_757 ?
O19 O18 O2 93(2) . 2_757 ?
As1 O18 W2 126.4(19) . . ?
O19 O18 W2 71.2(16) . . ?
O2 O18 W2 137(2) 2_757 . ?
As1 O18 W1 123.3(17) . . ?
O19 O18 W1 134(2) . . ?
O2 O18 W1 68.2(15) 2_757 . ?
W2 O18 W1 93.7(11) . . ?
As1 O18 W6 120.0(17) . . ?
O19 O18 W6 131(2) . . ?
O2 O18 W6 125(2) 2_757 . ?
W2 O18 W6 92.6(11) . . ?
W1 O18 W6 92.0(12) . . ?
As1 O2 O19 54.6(15) . . ?
As1 O2 O18 55.4(15) . 2_757 ?
O19 O2 O18 94(2) . 2_757 ?
As1 O2 W3 124.7(17) . . ?
O19 O2 W3 70.1(15) . . ?
O18 O2 W3 135(2) 2_757 . ?
As1 O2 W1 124.8(16) . 2_757 ?
O19 O2 W1 137(2) . 2_757 ?
O18 O2 W1 69.4(15) 2_757 2_757 ?
W3 O2 W1 94.0(11) . 2_757 ?
As1 O19 O18 57.5(16) . . ?
As1 O19 O2 56.4(15) . . ?
O18 O19 O2 96(2) . . ?
As1 O19 W3 124.8(18) . . ?
O18 O19 W3 135(2) . . ?
O2 O19 W3 68.4(15) . . ?
As1 O19 W2 125.5(19) . . ?
O18 O19 W2 68.1(16) . . ?
O2 O19 W2 134(2) . . ?
W3 O19 W2 92.3(11) . . ?
As1 O1 W4 122.4(17) . . ?
As1 O1 W6 121.1(16) . 2_757 ?
W4 O1 W6 93.8(11) . 2_757 ?
As1 O1 W5 123.8(18) . . ?
W4 O1 W5 94.2(11) . . ?
W6 O1 W5 93.7(11) 2_757 . ?
N7 N4 C13 107(2) . . ?
N7 N4 Ag1 124.6(17) . . ?
C13 N4 Ag1 128.1(16) . . ?
C15 C13 N4 132(2) . . ?
C15 C13 C14 121(2) . . ?
N4 C13 C14 107(2) . . ?
N5 N7 N4 111(2) . . ?
N5 C14 C13 106(2) . . ?
N5 C14 C16 132(2) . . ?
C13 C14 C16 122(2) . . ?
C13 C15 C18 118(3) . . ?
C17 C16 C14 115(2) . . ?
C18 C17 C16 121(3) . . ?
C15 C18 C17 122(3) . . ?
N7 N5 C14 109(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
N5 H1 O11 0.86 2.65 3.17(3) 119.8 1_565
N5 H1 O12 0.86 2.59 3.09(3) 118.4 2_767
N5 H1 O17 0.86 2.43 3.16(3) 142.9 1_565
N5 H1 O3 0.86 2.37 3.10(3) 142.9 2_767

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.347
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.278
####################################################################### 
# 
# 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_x
_database_code_depnum_ccdc_archive 'CCDC 1038932'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mo12 O40 P, C7 H6 N2, 3(C7 H7 N2)'
_chemical_formula_sum            'C28 H27 Mo12 N8 O40 P'
_chemical_formula_weight         2297.83

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'
Mo Mo -1.6832 0.6857 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.4090(8)
_cell_length_b                   14.8977(10)
_cell_length_c                   17.3674(11)
_cell_angle_alpha                65.9480(10)
_cell_angle_beta                 80.8140(10)
_cell_angle_gamma                69.9220(10)
_cell_volume                     2753.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22060
_cell_measurement_theta_min      1.28
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2180
_exptl_absorpt_coefficient_mu    2.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_T_max  0.590
_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  'Bruker Smart APEX 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            22060
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         28.28
_reflns_number_total             13584
_reflns_number_gt                10359
_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    SHELXP-97
_computing_publication_material  SHELXTL

_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. 
;

_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)+(0.2001P)²+180.0966P] 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_number_reflns         13584
_refine_ls_number_parameters     790
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.1368
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.123
_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
N1 N 0.724(3) 1.074(3) 0.066(2) 0.090(9) Uani 1 1 d U . .
H1 H 0.6927 1.1320 0.0734 0.108 Uiso 1 1 calc R . .
Mo1 Mo 0.71790(13) 0.60459(12) 0.90605(10) 0.0254(3) Uani 1 1 d . . .
Mo2 Mo 0.79507(13) 0.37314(12) 0.60621(10) 0.0258(3) Uani 1 1 d . . .
Mo3 Mo 1.02524(11) 0.53587(11) 0.68733(9) 0.0217(3) Uani 1 1 d . . .
Mo4 Mo 0.50454(12) 0.70344(11) 0.74522(10) 0.0240(3) Uani 1 1 d . . .
Mo5 Mo 0.95824(12) 0.40085(11) 0.90941(9) 0.0230(3) Uani 1 1 d . . .
Mo6 Mo 0.78563(13) 0.74108(11) 0.68458(10) 0.0260(3) Uani 1 1 d . . .
Mo7 Mo 0.99782(12) 0.27856(12) 0.75607(9) 0.0240(3) Uani 1 1 d . . .
Mo8 Mo 0.69348(14) 0.36338(12) 0.96741(9) 0.0259(3) Uani 1 1 d . . .
Mo9 Mo 0.73485(13) 0.24194(11) 0.81490(9) 0.0238(3) Uani 1 1 d . . .
Mo10 Mo 0.54099(11) 0.58955(11) 0.60086(9) 0.0224(3) Uani 1 1 d . . .
Mo11 Mo 0.82171(14) 0.63327(12) 0.53840(9) 0.0257(3) Uani 1 1 d . . .
Mo12 Mo 0.47738(11) 0.46063(11) 0.81019(9) 0.0219(3) Uani 1 1 d . . .
P1 P 0.7547(2) 0.4928(2) 0.75260(18) 0.0069(6) Uani 1 1 d . . .
O2 O 0.7751(9) 0.4739(9) 0.8445(7) 0.021(2) Uani 1 1 d . . .
O3 O 0.6256(9) 0.5418(9) 0.7347(7) 0.022(2) Uani 1 1 d . . .
O4 O 0.8214(9) 0.5669(9) 0.6934(7) 0.022(2) Uani 1 1 d . . .
O5 O 0.7997(9) 0.3919(9) 0.7394(7) 0.021(2) Uani 1 1 d . . .
O6 O 0.7860(12) 0.7456(10) 0.5698(9) 0.034(3) Uani 1 1 d . . .
O7 O 0.6571(11) 0.6436(10) 0.5507(9) 0.035(3) Uani 1 1 d . . .
O8 O 0.9756(10) 0.5868(10) 0.5721(8) 0.027(2) Uani 1 1 d . . .
O9 O 0.8377(12) 0.6894(11) 0.4340(8) 0.032(3) Uani 1 1 d . . .
O10 O 0.6381(10) 0.4586(10) 0.6060(9) 0.032(3) Uani 1 1 d . . .
O11 O 0.4732(12) 0.6973(10) 0.6432(8) 0.032(3) Uani 1 1 d . . .
O12 O 0.6264(10) 0.7535(10) 0.6897(8) 0.029(3) Uani 1 1 d . . .
O13 O 0.9485(10) 0.6782(9) 0.6790(8) 0.027(2) Uani 1 1 d . . .
O14 O 0.9433(10) 0.2928(11) 0.6545(8) 0.032(3) Uani 1 1 d . . .
O15 O 0.7404(11) 0.2662(10) 0.6995(8) 0.030(3) Uani 1 1 d . . .
O16 O 0.3579(11) 0.4277(11) 0.8490(9) 0.031(3) Uani 1 1 d . . .
O17 O 0.4518(11) 0.5138(9) 0.6945(8) 0.028(2) Uani 1 1 d . . .
O18 O 0.5612(11) 0.4231(10) 0.9117(9) 0.032(3) Uani 1 1 d . . .
O19 O 0.8624(11) 0.3306(10) 0.9870(9) 0.032(3) Uani 1 1 d . . .
O20 O 1.0093(11) 0.4907(9) 0.8031(7) 0.026(2) Uani 1 1 d . . .
O21 O 0.9948(11) 0.3067(9) 0.8544(8) 0.028(2) Uani 1 1 d . . .
O22 O 1.0419(10) 0.4009(8) 0.6965(7) 0.023(2) Uani 1 1 d . . .
O23 O 0.7429(11) 0.2690(9) 0.9142(8) 0.027(3) Uani 1 1 d . . .
O24 O 1.1229(11) 0.1869(10) 0.7647(9) 0.032(3) Uani 1 1 d . . .
O25 O 1.0746(11) 0.3547(11) 0.9674(8) 0.033(3) Uani 1 1 d . . .
O26 O 0.4513(12) 0.6294(11) 0.5242(9) 0.038(3) Uani 1 1 d . . .
O27 O 0.8796(10) 0.5221(10) 0.9334(8) 0.029(3) Uani 1 1 d . . .
O28 O 0.5861(10) 0.6556(10) 0.8460(8) 0.030(3) Uani 1 1 d . . .
O29 O 0.4268(10) 0.6004(9) 0.8048(7) 0.024(2) Uani 1 1 d . . .
O30 O 0.7851(12) 0.8624(10) 0.6611(11) 0.039(3) Uani 1 1 d . . .
O31 O 0.7849(10) 0.6834(10) 0.8014(8) 0.028(2) Uani 1 1 d . . .
O32 O 0.5871(10) 0.3378(9) 0.8044(8) 0.028(3) Uani 1 1 d . . .
O33 O 0.6607(12) 0.2899(11) 1.0643(7) 0.031(3) Uani 1 1 d . . .
O34 O 0.3999(11) 0.8080(10) 0.7456(9) 0.032(3) Uani 1 1 d . . .
O35 O 0.8015(11) 0.3323(11) 0.5284(8) 0.030(3) Uani 1 1 d . . .
O36 O 0.9014(11) 0.1930(11) 0.8169(9) 0.033(3) Uani 1 1 d . . .
O37 O 1.1600(11) 0.5429(11) 0.6678(9) 0.033(3) Uani 1 1 d . . .
O38 O 0.7086(12) 0.1288(10) 0.8599(10) 0.037(3) Uani 1 1 d . . .
O39 O 0.6795(12) 0.4883(11) 0.9851(9) 0.036(3) Uani 1 1 d . . .
O40 O 0.8366(11) 0.4912(9) 0.5568(8) 0.029(3) Uani 1 1 d . . .
O1 O 0.6966(12) 0.6779(12) 0.9611(9) 0.036(3) Uani 1 1 d . . .
C1 C 0.838(3) 1.037(3) 0.0423(18) 0.065(7) Uani 1 1 d . . .
H2 H 0.8936 1.0697 0.0319 0.078 Uiso 1 1 calc R . .
N2 N 0.3113(13) 0.3064(13) 0.6733(11) 0.032(3) Uani 1 1 d . . .
H3 H 0.2378 0.3214 0.6786 0.038 Uiso 1 1 calc R . .
C2 C 0.3891(16) 0.2116(15) 0.6716(12) 0.030(4) Uani 1 1 d . . .
N3 N 0.4811(14) 0.3217(14) 0.6590(14) 0.043(5) Uani 1 1 d . . .
H4 H 0.5343 0.3488 0.6538 0.052 Uiso 1 1 calc R . .
C3 C 0.3705(17) 0.3659(16) 0.6653(15) 0.038(5) Uani 1 1 d . . .
H5 H 0.3384 0.4328 0.6641 0.046 Uiso 1 1 calc R . .
C4 C 0.4971(17) 0.2220(16) 0.6624(16) 0.039(5) Uani 1 1 d . . .
C5 C 0.593(2) 0.149(2) 0.660(3) 0.072(10) Uani 1 1 d . . .
H6 H 0.6649 0.1585 0.6507 0.087 Uiso 1 1 calc R . .
C6 C 0.576(3) 0.057(3) 0.671(3) 0.098(15) Uani 1 1 d . . .
H7 H 0.6403 0.0020 0.6721 0.117 Uiso 1 1 calc R . .
C7 C 0.372(3) 0.1212(18) 0.6815(18) 0.054(6) Uani 1 1 d . . .
H8 H 0.2998 0.1136 0.6880 0.064 Uiso 1 1 calc R . .
C8 C 0.473(3) 0.042(3) 0.681(3) 0.083(10) Uani 1 1 d . . .
H9 H 0.4684 -0.0224 0.6877 0.099 Uiso 1 1 calc R . .
N4 N 0.1887(11) 0.6807(12) 0.8290(10) 0.026(3) Uani 1 1 d . . .
H10 H 0.2611 0.6702 0.8184 0.031 Uiso 1 1 calc R . .
C9 C 0.1344(14) 0.6082(15) 0.8519(12) 0.028(3) Uani 1 1 d . . .
H11 H 0.1685 0.5387 0.8610 0.033 Uiso 1 1 calc R . .
C10 C 0.1110(14) 0.7721(16) 0.8252(10) 0.030(4) Uani 1 1 d . . .
N5 N 0.0229(13) 0.6557(13) 0.8591(12) 0.034(3) Uani 1 1 d . . .
H12 H -0.0303 0.6270 0.8710 0.040 Uiso 1 1 calc R . .
C11 C 0.0056(14) 0.7568(13) 0.8446(11) 0.024(3) Uani 1 1 d . . .
C12 C -0.0935(18) 0.8324(18) 0.8519(17) 0.046(5) Uani 1 1 d . . .
H13 H -0.1636 0.8195 0.8679 0.056 Uiso 1 1 calc R . .
C13 C 0.1280(19) 0.8662(15) 0.8118(14) 0.038(4) Uani 1 1 d . . .
H14 H 0.2003 0.8751 0.8011 0.045 Uiso 1 1 calc R . .
C14 C 0.029(2) 0.9455(17) 0.8159(16) 0.048(5) Uani 1 1 d . . .
H15 H 0.0349 1.0095 0.8067 0.058 Uiso 1 1 calc R . .
C15 C -0.082(2) 0.9313(19) 0.8336(19) 0.055(6) Uani 1 1 d . . .
H16 H -0.1470 0.9864 0.8332 0.066 Uiso 1 1 calc R . .
N6 N 0.0915(15) 0.8086(13) 0.6129(11) 0.037(4) Uani 1 1 d . . .
H17 H 0.0429 0.7748 0.6259 0.044 Uiso 1 1 calc R . .
C16 C 0.0689(15) 0.9094(12) 0.6044(11) 0.026(3) Uani 1 1 d . . .
C17 C 0.206(2) 0.7730(17) 0.5964(16) 0.049(6) Uani 1 1 d . . .
H18 H 0.2463 0.7064 0.5990 0.059 Uiso 1 1 calc R . .
C18 C -0.0319(17) 0.9834(15) 0.6157(13) 0.036(4) Uani 1 1 d . . .
H19 H -0.1004 0.9674 0.6311 0.043 Uiso 1 1 calc R . .
C19 C 0.1696(19) 0.9367(18) 0.5786(14) 0.041(5) Uani 1 1 d . . .
C20 C -0.029(2) 1.0750(17) 0.6043(16) 0.047(5) Uani 1 1 d . . .
H20 H -0.0972 1.1242 0.6097 0.056 Uiso 1 1 calc R . .
C21 C 0.068(3) 1.101(2) 0.585(2) 0.067(8) Uani 1 1 d . . .
H21 H 0.0658 1.1664 0.5795 0.081 Uiso 1 1 calc R . .
C22 C 0.180(3) 1.028(2) 0.5724(19) 0.065(8) Uani 1 1 d . . .
H22 H 0.2495 1.0429 0.5616 0.078 Uiso 1 1 calc R . .
N7 N 0.250(2) 0.847(3) 0.576(2) 0.097(13) Uani 1 1 d . . .
H23 H 0.3217 0.8409 0.5633 0.117 Uiso 1 1 calc R . .
C23 C 0.676(2) 1.0098(17) 0.0764(14) 0.091(14) Uani 1 1 d G . .
C24 C 0.7516(16) 0.925(2) 0.0613(14) 0.071(8) Uani 1 1 d GU . .
C25 C 0.715(2) 0.8423(18) 0.0716(18) 0.097(11) Uani 1 1 d GU . .
H24 H 0.7657 0.7854 0.0615 0.117 Uiso 1 1 calc R . .
C26 C 0.602(2) 0.8447(19) 0.0970(18) 0.117(14) Uani 1 1 d GU . .
H25 H 0.5777 0.7894 0.1039 0.140 Uiso 1 1 calc R . .
C27 C 0.5263(18) 0.930(2) 0.1121(18) 0.080(9) Uani 1 1 d GU . .
H26 H 0.4509 0.9312 0.1291 0.096 Uiso 1 1 calc R . .
C28 C 0.563(2) 1.0122(18) 0.1018(17) 0.138(16) Uani 1 1 d GU . .
H27 H 0.5122 1.0690 0.1119 0.165 Uiso 1 1 calc R . .
N8 N 0.851(3) 0.952(2) 0.0370(19) 0.077(7) Uani 1 1 d U . .


_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 C23 1.24(4) . ?
N1 C1 1.39(4) . ?
N1 H1 0.8600 . ?
Mo1 O1 1.658(12) . ?
Mo1 O28 1.840(12) . ?
Mo1 O39 1.880(15) . ?
Mo1 O31 1.955(13) . ?
Mo1 O27 1.974(13) . ?
Mo1 O2 2.438(11) . ?
Mo2 O35 1.675(11) . ?
Mo2 O40 1.829(13) . ?
Mo2 O14 1.918(13) . ?
Mo2 O10 1.926(12) . ?
Mo2 O15 1.978(12) . ?
Mo2 O5 2.452(11) . ?
Mo3 O37 1.683(13) . ?
Mo3 O20 1.842(11) . ?
Mo3 O22 1.890(11) . ?
Mo3 O8 1.949(12) . ?
Mo3 O13 1.958(12) . ?
Mo3 O4 2.403(11) . ?
Mo4 O34 1.652(12) . ?
Mo4 O12 1.870(12) . ?
Mo4 O28 1.910(12) . ?
Mo4 O11 1.918(13) . ?
Mo4 O29 1.939(12) . ?
Mo4 O3 2.425(11) . ?
Mo5 O25 1.670(12) . ?
Mo5 O19 1.875(13) . ?
Mo5 O21 1.898(11) . ?
Mo5 O27 1.914(13) . ?
Mo5 O20 1.948(12) . ?
Mo5 O2 2.396(11) . ?
Mo6 O30 1.682(13) . ?
Mo6 O31 1.852(13) . ?
Mo6 O12 1.911(12) . ?
Mo6 O13 1.919(12) . ?
Mo6 O6 1.966(14) . ?
Mo6 O4 2.420(11) . ?
Mo7 O24 1.657(13) . ?
Mo7 O14 1.896(13) . ?
Mo7 O21 1.910(12) . ?
Mo7 O22 1.913(11) . ?
Mo7 O36 1.928(14) . ?
Mo7 O5 2.441(11) . ?
Mo8 O33 1.667(12) . ?
Mo8 O18 1.796(13) . ?
Mo8 O23 1.869(11) . ?
Mo8 O39 1.953(14) . ?
Mo8 O19 2.034(14) . ?
Mo8 O2 2.426(11) . ?
Mo9 O38 1.667(13) . ?
Mo9 O32 1.879(12) . ?
Mo9 O15 1.880(12) . ?
Mo9 O36 1.942(12) . ?
Mo9 O23 1.948(12) . ?
Mo9 O5 2.422(11) . ?
Mo10 O26 1.655(13) . ?
Mo10 O7 1.819(13) . ?
Mo10 O10 1.883(12) . ?
Mo10 O11 1.913(13) . ?
Mo10 O17 1.982(13) . ?
Mo10 O3 2.435(11) . ?
Mo11 O9 1.670(12) . ?
Mo11 O6 1.859(13) . ?
Mo11 O8 1.893(12) . ?
Mo11 O40 1.953(12) . ?
Mo11 O7 1.978(13) . ?
Mo11 O4 2.461(11) . ?
Mo12 O16 1.675(12) . ?
Mo12 O17 1.870(12) . ?
Mo12 O32 1.899(12) . ?
Mo12 O29 1.924(12) . ?
Mo12 O18 1.971(13) . ?
Mo12 O3 2.456(12) . ?
P1 O5 1.513(11) . ?
P1 O3 1.538(11) . ?
P1 O4 1.547(11) . ?
P1 O2 1.550(11) . ?
C1 N8 1.27(4) . ?
C1 H2 0.9300 . ?
N2 C3 1.29(2) . ?
N2 C2 1.42(2) . ?
N2 H3 0.8600 . ?
C2 C7 1.37(3) . ?
C2 C4 1.38(3) . ?
N3 C3 1.31(3) . ?
N3 C4 1.41(2) . ?
N3 H4 0.8600 . ?
C3 H5 0.9300 . ?
C4 C5 1.32(3) . ?
C5 C6 1.39(5) . ?
C5 H6 0.9300 . ?
C6 C8 1.35(5) . ?
C6 H7 0.9300 . ?
C7 C8 1.39(4) . ?
C7 H8 0.9300 . ?
C8 H9 0.9300 . ?
N4 C10 1.35(2) . ?
N4 C9 1.36(2) . ?
N4 H10 0.8600 . ?
C9 N5 1.33(2) . ?
C9 H11 0.9300 . ?
C10 C11 1.37(2) . ?
C10 C13 1.41(3) . ?
N5 C11 1.36(2) . ?
N5 H12 0.8600 . ?
C11 C12 1.38(2) . ?
C12 C15 1.43(4) . ?
C12 H13 0.9300 . ?
C13 C14 1.40(3) . ?
C13 H14 0.9300 . ?
C14 C15 1.43(4) . ?
C14 H15 0.9300 . ?
C15 H16 0.9300 . ?
N6 C17 1.37(3) . ?
N6 C16 1.38(2) . ?
N6 H17 0.8600 . ?
C16 C19 1.40(3) . ?
C16 C18 1.40(2) . ?
C17 N7 1.30(4) . ?
C17 H18 0.9300 . ?
C18 C20 1.31(3) . ?
C18 H19 0.9300 . ?
C19 C22 1.37(3) . ?
C19 N7 1.38(3) . ?
C20 C21 1.35(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.49(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N7 H23 0.8600 . ?
C23 C24 1.3900 . ?
C23 C28 1.3900 . ?
C24 N8 1.38(3) . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C25 H24 0.9300 . ?
C26 C27 1.3900 . ?
C26 H25 0.9300 . ?
C27 C28 1.3900 . ?
C27 H26 0.9300 . ?
C28 H27 0.9300 . ?

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
C23 N1 C1 108(3) . . ?
C23 N1 H1 126.0 . . ?
C1 N1 H1 126.0 . . ?
O1 Mo1 O28 105.0(7) . . ?
O1 Mo1 O39 102.4(7) . . ?
O28 Mo1 O39 93.9(6) . . ?
O1 Mo1 O31 101.0(7) . . ?
O28 Mo1 O31 85.9(5) . . ?
O39 Mo1 O31 155.8(5) . . ?
O1 Mo1 O27 99.4(6) . . ?
O28 Mo1 O27 154.8(6) . . ?
O39 Mo1 O27 86.7(6) . . ?
O31 Mo1 O27 83.5(5) . . ?
O1 Mo1 O2 169.5(6) . . ?
O28 Mo1 O2 84.7(5) . . ?
O39 Mo1 O2 72.7(5) . . ?
O31 Mo1 O2 83.2(5) . . ?
O27 Mo1 O2 71.4(4) . . ?
O35 Mo2 O40 105.3(6) . . ?
O35 Mo2 O14 100.9(6) . . ?
O40 Mo2 O14 92.3(6) . . ?
O35 Mo2 O10 103.7(6) . . ?
O40 Mo2 O10 88.3(5) . . ?
O14 Mo2 O10 154.3(6) . . ?
O35 Mo2 O15 99.3(6) . . ?
O40 Mo2 O15 155.4(5) . . ?
O14 Mo2 O15 84.9(6) . . ?
O10 Mo2 O15 84.0(6) . . ?
O35 Mo2 O5 167.3(5) . . ?
O40 Mo2 O5 85.4(5) . . ?
O14 Mo2 O5 71.2(5) . . ?
O10 Mo2 O5 83.3(5) . . ?
O15 Mo2 O5 70.6(4) . . ?
O37 Mo3 O20 104.0(6) . . ?
O37 Mo3 O22 103.6(6) . . ?
O20 Mo3 O22 88.5(5) . . ?
O37 Mo3 O8 99.6(6) . . ?
O20 Mo3 O8 156.2(6) . . ?
O22 Mo3 O8 88.2(5) . . ?
O37 Mo3 O13 97.4(6) . . ?
O20 Mo3 O13 89.7(5) . . ?
O22 Mo3 O13 158.7(5) . . ?
O8 Mo3 O13 85.0(5) . . ?
O37 Mo3 O4 166.8(6) . . ?
O20 Mo3 O4 83.6(5) . . ?
O22 Mo3 O4 87.2(5) . . ?
O8 Mo3 O4 72.7(5) . . ?
O13 Mo3 O4 71.5(5) . . ?
O34 Mo4 O12 103.9(6) . . ?
O34 Mo4 O28 104.8(6) . . ?
O12 Mo4 O28 85.5(5) . . ?
O34 Mo4 O11 100.5(6) . . ?
O12 Mo4 O11 89.4(6) . . ?
O28 Mo4 O11 154.7(6) . . ?
O34 Mo4 O29 99.4(6) . . ?
O12 Mo4 O29 156.7(5) . . ?
O28 Mo4 O29 87.9(5) . . ?
O11 Mo4 O29 87.0(5) . . ?
O34 Mo4 O3 167.5(6) . . ?
O12 Mo4 O3 84.9(5) . . ?
O28 Mo4 O3 84.6(5) . . ?
O11 Mo4 O3 70.3(5) . . ?
O29 Mo4 O3 72.2(4) . . ?
O25 Mo5 O19 100.4(7) . . ?
O25 Mo5 O21 100.9(6) . . ?
O19 Mo5 O21 90.5(5) . . ?
O25 Mo5 O27 99.8(6) . . ?
O19 Mo5 O27 90.5(5) . . ?
O21 Mo5 O27 158.8(6) . . ?
O25 Mo5 O20 100.8(6) . . ?
O19 Mo5 O20 158.8(6) . . ?
O21 Mo5 O20 84.1(5) . . ?
O27 Mo5 O20 87.4(5) . . ?
O25 Mo5 O2 171.0(5) . . ?
O19 Mo5 O2 74.2(5) . . ?
O21 Mo5 O2 86.6(5) . . ?
O27 Mo5 O2 73.3(5) . . ?
O20 Mo5 O2 84.9(5) . . ?
O30 Mo6 O31 103.9(7) . . ?
O30 Mo6 O12 103.6(6) . . ?
O31 Mo6 O12 88.3(5) . . ?
O30 Mo6 O13 98.1(6) . . ?
O31 Mo6 O13 91.4(5) . . ?
O12 Mo6 O13 157.7(6) . . ?
O30 Mo6 O6 99.4(7) . . ?
O31 Mo6 O6 156.7(6) . . ?
O12 Mo6 O6 86.0(6) . . ?
O13 Mo6 O6 85.4(5) . . ?
O30 Mo6 O4 166.7(6) . . ?
O31 Mo6 O4 85.4(5) . . ?
O12 Mo6 O4 86.0(5) . . ?
O13 Mo6 O4 71.7(5) . . ?
O6 Mo6 O4 71.7(5) . . ?
O24 Mo7 O14 101.7(6) . . ?
O24 Mo7 O21 101.6(6) . . ?
O14 Mo7 O21 156.8(6) . . ?
O24 Mo7 O22 101.6(6) . . ?
O14 Mo7 O22 89.8(5) . . ?
O21 Mo7 O22 85.6(5) . . ?
O24 Mo7 O36 99.2(6) . . ?
O14 Mo7 O36 88.2(6) . . ?
O21 Mo7 O36 88.1(6) . . ?
O22 Mo7 O36 159.1(5) . . ?
O24 Mo7 O5 169.5(6) . . ?
O14 Mo7 O5 71.8(5) . . ?
O21 Mo7 O5 85.2(5) . . ?
O22 Mo7 O5 86.7(4) . . ?
O36 Mo7 O5 72.9(5) . . ?
O33 Mo8 O18 105.1(7) . . ?
O33 Mo8 O23 101.6(6) . . ?
O18 Mo8 O23 90.3(5) . . ?
O33 Mo8 O39 100.1(6) . . ?
O18 Mo8 O39 92.2(6) . . ?
O23 Mo8 O39 156.7(6) . . ?
O33 Mo8 O19 97.0(6) . . ?
O18 Mo8 O19 157.9(6) . . ?
O23 Mo8 O19 86.1(5) . . ?
O39 Mo8 O19 82.9(5) . . ?
O33 Mo8 O2 166.0(5) . . ?
O18 Mo8 O2 87.0(5) . . ?
O23 Mo8 O2 85.1(5) . . ?
O39 Mo8 O2 71.8(5) . . ?
O19 Mo8 O2 71.1(5) . . ?
O38 Mo9 O32 102.7(6) . . ?
O38 Mo9 O15 102.4(7) . . ?
O32 Mo9 O15 90.8(6) . . ?
O38 Mo9 O36 99.5(7) . . ?
O32 Mo9 O36 157.0(6) . . ?
O15 Mo9 O36 90.2(6) . . ?
O38 Mo9 O23 100.7(7) . . ?
O32 Mo9 O23 84.7(5) . . ?
O15 Mo9 O23 156.9(5) . . ?
O36 Mo9 O23 85.5(5) . . ?
O38 Mo9 O5 170.8(6) . . ?
O32 Mo9 O5 85.3(5) . . ?
O15 Mo9 O5 72.7(5) . . ?
O36 Mo9 O5 73.1(5) . . ?
O23 Mo9 O5 84.4(5) . . ?
O26 Mo10 O7 105.0(7) . . ?
O26 Mo10 O10 105.2(7) . . ?
O7 Mo10 O10 89.5(5) . . ?
O26 Mo10 O11 99.4(7) . . ?
O7 Mo10 O11 90.7(6) . . ?
O10 Mo10 O11 154.4(6) . . ?
O26 Mo10 O17 97.8(6) . . ?
O7 Mo10 O17 157.1(6) . . ?
O10 Mo10 O17 86.2(5) . . ?
O11 Mo10 O17 83.8(5) . . ?
O26 Mo10 O3 164.7(6) . . ?
O7 Mo10 O3 86.6(6) . . ?
O10 Mo10 O3 84.4(5) . . ?
O11 Mo10 O3 70.1(5) . . ?
O17 Mo10 O3 70.6(4) . . ?
O9 Mo11 O6 101.0(7) . . ?
O9 Mo11 O8 100.6(6) . . ?
O6 Mo11 O8 91.8(6) . . ?
O9 Mo11 O40 103.8(6) . . ?
O6 Mo11 O40 154.7(6) . . ?
O8 Mo11 O40 88.5(5) . . ?
O9 Mo11 O7 101.9(6) . . ?
O6 Mo11 O7 88.9(6) . . ?
O8 Mo11 O7 156.9(6) . . ?
O40 Mo11 O7 81.1(5) . . ?
O9 Mo11 O4 169.6(5) . . ?
O6 Mo11 O4 72.3(5) . . ?
O8 Mo11 O4 72.1(5) . . ?
O40 Mo11 O4 83.8(5) . . ?
O7 Mo11 O4 86.1(5) . . ?
O16 Mo12 O17 100.3(6) . . ?
O16 Mo12 O32 104.5(6) . . ?
O17 Mo12 O32 91.2(5) . . ?
O16 Mo12 O29 100.1(6) . . ?
O17 Mo12 O29 88.2(5) . . ?
O32 Mo12 O29 155.1(5) . . ?
O16 Mo12 O18 103.7(6) . . ?
O17 Mo12 O18 156.0(6) . . ?
O32 Mo12 O18 83.5(5) . . ?
O29 Mo12 O18 86.9(5) . . ?
O16 Mo12 O3 168.3(6) . . ?
O17 Mo12 O3 71.7(5) . . ?
O32 Mo12 O3 84.5(5) . . ?
O29 Mo12 O3 71.7(4) . . ?
O18 Mo12 O3 84.4(5) . . ?
O5 P1 O3 110.1(6) . . ?
O5 P1 O4 109.3(6) . . ?
O3 P1 O4 110.3(6) . . ?
O5 P1 O2 110.0(6) . . ?
O3 P1 O2 109.6(6) . . ?
O4 P1 O2 107.4(6) . . ?
P1 O2 Mo5 125.5(6) . . ?
P1 O2 Mo8 123.6(6) . . ?
Mo5 O2 Mo8 91.2(4) . . ?
P1 O2 Mo1 126.0(6) . . ?
Mo5 O2 Mo1 90.6(4) . . ?
Mo8 O2 Mo1 89.2(4) . . ?
P1 O3 Mo4 125.8(6) . . ?
P1 O3 Mo10 124.8(6) . . ?
Mo4 O3 Mo10 90.7(4) . . ?
P1 O3 Mo12 124.9(6) . . ?
Mo4 O3 Mo12 89.8(4) . . ?
Mo10 O3 Mo12 90.0(4) . . ?
P1 O4 Mo3 127.0(6) . . ?
P1 O4 Mo6 124.5(6) . . ?
Mo3 O4 Mo6 91.2(4) . . ?
P1 O4 Mo11 124.6(6) . . ?
Mo3 O4 Mo11 89.3(4) . . ?
Mo6 O4 Mo11 88.9(4) . . ?
P1 O5 Mo9 125.9(6) . . ?
P1 O5 Mo7 126.0(6) . . ?
Mo9 O5 Mo7 89.4(4) . . ?
P1 O5 Mo2 125.1(6) . . ?
Mo9 O5 Mo2 90.0(4) . . ?
Mo7 O5 Mo2 89.0(4) . . ?
Mo11 O6 Mo6 126.8(7) . . ?
Mo10 O7 Mo11 151.0(8) . . ?
Mo11 O8 Mo3 125.6(7) . . ?
Mo10 O10 Mo2 145.2(7) . . ?
Mo10 O11 Mo4 128.9(7) . . ?
Mo4 O12 Mo6 149.1(8) . . ?
Mo6 O13 Mo3 125.5(7) . . ?
Mo7 O14 Mo2 128.1(7) . . ?
Mo9 O15 Mo2 126.6(7) . . ?
Mo12 O17 Mo10 127.7(7) . . ?
Mo8 O18 Mo12 149.2(7) . . ?
Mo5 O19 Mo8 123.5(7) . . ?
Mo3 O20 Mo5 150.1(7) . . ?
Mo5 O21 Mo7 150.8(7) . . ?
Mo3 O22 Mo7 146.6(7) . . ?
Mo8 O23 Mo9 146.9(7) . . ?
Mo5 O27 Mo1 124.2(6) . . ?
Mo1 O28 Mo4 153.3(8) . . ?
Mo12 O29 Mo4 126.1(6) . . ?
Mo6 O31 Mo1 148.1(7) . . ?
Mo9 O32 Mo12 153.9(7) . . ?
Mo7 O36 Mo9 124.2(8) . . ?
Mo1 O39 Mo8 126.0(7) . . ?
Mo2 O40 Mo11 153.3(7) . . ?
N8 C1 N1 108(3) . . ?
N8 C1 H2 126.2 . . ?
N1 C1 H2 126.2 . . ?
C3 N2 C2 107.7(15) . . ?
C3 N2 H3 126.1 . . ?
C2 N2 H3 126.1 . . ?
C7 C2 C4 122(2) . . ?
C7 C2 N2 131.7(19) . . ?
C4 C2 N2 106.0(16) . . ?
C3 N3 C4 107.7(16) . . ?
C3 N3 H4 126.2 . . ?
C4 N3 H4 126.2 . . ?
N2 C3 N3 112.5(17) . . ?
N2 C3 H5 123.8 . . ?
N3 C3 H5 123.8 . . ?
C5 C4 C2 124(2) . . ?
C5 C4 N3 130(2) . . ?
C2 C4 N3 106.1(17) . . ?
C4 C5 C6 113(3) . . ?
C4 C5 H6 123.4 . . ?
C6 C5 H6 123.4 . . ?
C8 C6 C5 125(3) . . ?
C8 C6 H7 117.3 . . ?
C5 C6 H7 117.3 . . ?
C2 C7 C8 115(3) . . ?
C2 C7 H8 122.5 . . ?
C8 C7 H8 122.5 . . ?
C6 C8 C7 120(3) . . ?
C6 C8 H9 120.1 . . ?
C7 C8 H9 120.1 . . ?
C10 N4 C9 109.3(14) . . ?
C10 N4 H10 125.3 . . ?
C9 N4 H10 125.3 . . ?
N5 C9 N4 107.0(16) . . ?
N5 C9 H11 126.5 . . ?
N4 C9 H11 126.5 . . ?
N4 C10 C11 107.1(17) . . ?
N4 C10 C13 129.9(16) . . ?
C11 C10 C13 122.8(18) . . ?
C9 N5 C11 109.9(15) . . ?
C9 N5 H12 125.1 . . ?
C11 N5 H12 125.1 . . ?
N5 C11 C10 106.7(16) . . ?
N5 C11 C12 130.1(18) . . ?
C10 C11 C12 123.0(19) . . ?
C11 C12 C15 116(2) . . ?
C11 C12 H13 121.8 . . ?
C15 C12 H13 121.8 . . ?
C14 C13 C10 115.4(19) . . ?
C14 C13 H14 122.3 . . ?
C10 C13 H14 122.3 . . ?
C13 C14 C15 122(2) . . ?
C13 C14 H15 118.9 . . ?
C15 C14 H15 118.9 . . ?
C12 C15 C14 120(2) . . ?
C12 C15 H16 120.0 . . ?
C14 C15 H16 120.0 . . ?
C17 N6 C16 106.5(17) . . ?
C17 N6 H17 126.8 . . ?
C16 N6 H17 126.8 . . ?
N6 C16 C19 108.9(17) . . ?
N6 C16 C18 132.3(18) . . ?
C19 C16 C18 118.8(17) . . ?
N7 C17 N6 109.0(19) . . ?
N7 C17 H18 125.5 . . ?
N6 C17 H18 125.5 . . ?
C20 C18 C16 119.8(19) . . ?
C20 C18 H19 120.1 . . ?
C16 C18 H19 120.1 . . ?
C22 C19 N7 132(2) . . ?
C22 C19 C16 124(2) . . ?
N7 C19 C16 103.6(19) . . ?
C18 C20 C21 123(2) . . ?
C18 C20 H20 118.7 . . ?
C21 C20 H20 118.7 . . ?
C20 C21 C22 122(2) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C19 C22 C21 112(2) . . ?
C19 C22 H22 123.9 . . ?
C21 C22 H22 123.9 . . ?
C17 N7 C19 112(2) . . ?
C17 N7 H23 124.0 . . ?
C19 N7 H23 124.0 . . ?
N1 C23 C24 111(2) . . ?
N1 C23 C28 129(2) . . ?
C24 C23 C28 120.0 . . ?
N8 C24 C23 103(2) . . ?
N8 C24 C25 137(2) . . ?
C23 C24 C25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H24 120.0 . . ?
C24 C25 H24 120.0 . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H25 120.0 . . ?
C27 C26 H25 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H26 120.0 . . ?
C26 C27 H26 120.0 . . ?
C27 C28 C23 120.0 . . ?
C27 C28 H27 120.0 . . ?
C23 C28 H27 120.0 . . ?
C1 N8 C24 111(3) . . ?

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
N6 H17 O13 0.86 2.01 2.85(2) 167.9 1_455
N5 H12 O20 0.86 2.62 3.050(19) 112.6 1_455
N5 H12 O31 0.86 2.48 3.11(2) 130.4 1_455
N5 H12 O27 0.86 2.07 2.90(2) 160.2 1_455
N2 H3 O9 0.86 2.38 2.80(2) 110.0 2_666
N2 H3 O22 0.86 2.34 3.181(19) 164.7 1_455
N1 H1 O33 0.86 2.19 3.02(4) 161.2 1_564
N7 H23 O11 0.86 2.38 2.94(3) 122.6 .
N4 H10 O29 0.86 1.99 2.815(18) 161.7 .
N3 H4 O17 0.86 2.66 3.058(19) 110.0 .
N3 H4 O15 0.86 2.53 3.15(2) 130.7 .
N3 H4 O10 0.86 2.24 3.07(2) 161.8 .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.421
_refine_diff_density_min         -2.561
_refine_diff_density_rms         0.304
