# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1022773'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H40 Cu3 Mo24 N32 O84 P2'
_chemical_formula_weight         4579.92

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   12.8229(4)
_cell_length_b                   14.7384(5)
_cell_length_c                   25.0376(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3400(1)
_cell_angle_gamma                90.00
_cell_volume                     4730.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4314
_exptl_absorpt_coefficient_mu    3.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4685
_exptl_absorpt_correction_T_max  0.5103
_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  '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            23459
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8336
_reflns_number_gt                7790
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
 During the refinement, the restraint command 'ISOR' was used to refine the non-H atom 'O2W' with ADP problem. 
;

_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)+(0.1000P)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         8336
_refine_ls_number_parameters     731
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.049
_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 0.34737(4) 0.61094(3) 0.226250(17) 0.01745(13) Uani 1 1 d . . .
P1 P 0.23518(9) 0.66288(8) 0.35112(5) 0.0123(3) Uani 1 1 d . . .
O1 O 0.3485(3) 0.9657(3) 0.44266(15) 0.0244(8) Uani 1 1 d . . .
C1 C 0.6170(5) 1.1461(4) 0.4422(2) 0.0239(12) Uani 1 1 d . . .
H1 H 0.6824 1.1192 0.4455 0.029 Uiso 1 1 calc R . .
Cu1 Cu 0.5000 1.0000 0.5000 0.0180(2) Uani 1 2 d S . .
N1 N 0.5262(4) 1.1075(3) 0.45439(17) 0.0203(9) Uani 1 1 d . . .
O1W O 0.2491(5) 1.2852(4) 0.4492(3) 0.076(2) Uani 1 1 d . . .
Cu2 Cu 0.29479(5) 1.13492(5) 0.43716(3) 0.02194(17) Uani 1 1 d . . .
Mo2 Mo 0.42852(4) 0.80214(3) 0.292538(18) 0.01860(13) Uani 1 1 d . . .
C2 C 0.4925(5) 1.2434(4) 0.4254(2) 0.0296(13) Uani 1 1 d . . .
H2 H 0.4577 1.2963 0.4154 0.036 Uiso 1 1 calc R . .
N2 N 0.4481(4) 1.1695(3) 0.44277(19) 0.0262(11) Uani 1 1 d . . .
O2 O -0.0519(3) 0.5635(3) 0.34751(15) 0.0250(8) Uani 1 1 d . . .
O2W O 0.2315(8) 1.3483(7) 0.6157(4) 0.135(3) Uani 1 1 d U . .
H2WA H 0.1810 1.3782 0.6284 0.161 Uiso 1 1 d R . .
H2WB H 0.2332 1.3595 0.5824 0.161 Uiso 1 1 d R . .
Mo3 Mo 0.42370(4) 0.48733(3) 0.349403(18) 0.01933(13) Uani 1 1 d . . .
O3 O -0.1214(3) 0.6398(3) 0.24962(18) 0.0353(10) Uani 1 1 d . . .
N3 N 0.5976(4) 1.2309(3) 0.42434(18) 0.0242(10) Uani 1 1 d . . .
C3 C 0.3845(4) 1.0846(4) 0.5915(2) 0.0214(11) Uani 1 1 d . . .
H3 H 0.4334 1.0660 0.6173 0.026 Uiso 1 1 calc R . .
Mo4 Mo 0.15923(4) 0.45252(3) 0.289019(19) 0.02093(13) Uani 1 1 d . . .
O4 O -0.0456(4) 0.4572(3) 0.43811(18) 0.0391(11) Uani 1 1 d . . .
N4 N 0.6757(4) 1.2910(4) 0.4090(2) 0.0356(13) Uani 1 1 d . . .
H4A H 0.6642 1.3102 0.3766 0.043 Uiso 1 1 d R . .
H4B H 0.6772 1.3377 0.4302 0.043 Uiso 1 1 d R . .
C4 C 0.2473(4) 1.1421(4) 0.5544(2) 0.0249(12) Uani 1 1 d . . .
H4 H 0.1832 1.1710 0.5496 0.030 Uiso 1 1 calc R . .
N5 N 0.3924(3) 1.0713(3) 0.54053(17) 0.0182(9) Uani 1 1 d . . .
Mo5 Mo 0.29245(4) 0.87040(3) 0.415211(18) 0.01792(13) Uani 1 1 d . . .
C5 C 0.3192(5) 1.0884(5) 0.3193(3) 0.0339(14) Uani 1 1 d . . .
H5 H 0.3190 1.0255 0.3221 0.041 Uiso 1 1 calc R . .
O5 O 0.0427(3) 0.5184(3) 0.25863(15) 0.0238(8) Uani 1 1 d . . .
Mo6 Mo 0.18600(4) 0.79705(3) 0.234878(18) 0.02157(13) Uani 1 1 d . . .
O6 O 0.5030(3) 0.3984(3) 0.33773(15) 0.0253(9) Uani 1 1 d . . .
N6 N 0.3022(3) 1.1088(3) 0.51625(18) 0.0229(10) Uani 1 1 d . . .
C6 C 0.3293(5) 1.2247(5) 0.2890(3) 0.0411(17) Uani 1 1 d . . .
H6 H 0.3373 1.2735 0.2659 0.049 Uiso 1 1 calc R . .
Mo7 Mo 0.47964(4) 0.67849(3) 0.420905(19) 0.02087(13) Uani 1 1 d . . .
O7 O 0.3054(4) 0.4748(3) 0.52455(16) 0.0364(11) Uani 1 1 d . . .
N7 N 0.2954(4) 1.1292(3) 0.60172(18) 0.0262(11) Uani 1 1 d . . .
C7 C 0.0780(6) 1.1347(5) 0.3911(3) 0.0442(17) Uani 1 1 d . . .
H7 H 0.0953 1.1672 0.3607 0.053 Uiso 1 1 calc R . .
Mo8 Mo 0.04776(4) 0.84185(3) 0.360515(19) 0.02187(13) Uani 1 1 d . . .
O8 O 0.5227(3) 0.8772(3) 0.28074(16) 0.0272(9) Uani 1 1 d . . .
C8 C -0.0080(5) 1.0685(5) 0.4508(3) 0.0431(17) Uani 1 1 d . . .
H8 H -0.0634 1.0447 0.4696 0.052 Uiso 1 1 calc R . .
N8 N 0.2679(4) 1.1607(5) 0.6530(2) 0.0492(17) Uani 1 1 d . . .
H8A H 0.2391 1.2144 0.6450 0.059 Uiso 1 1 d R . .
H8B H 0.2115 1.1256 0.6601 0.059 Uiso 1 1 d R . .
Mo9 Mo 0.12027(4) 0.72670(3) 0.473870(18) 0.02232(13) Uani 1 1 d . . .
O9 O 0.4077(3) 0.5689(3) 0.17304(16) 0.0294(9) Uani 1 1 d . . .
N9 N 0.3061(4) 1.1445(3) 0.35833(19) 0.0281(11) Uani 1 1 d . . .
O10 O 0.1522(3) 0.3558(3) 0.25446(15) 0.0261(9) Uani 1 1 d . . .
Mo10 Mo 0.29962(4) 0.52961(3) 0.466116(18) 0.02301(14) Uani 1 1 d . . .
N10 N 0.3135(4) 1.2316(4) 0.3382(2) 0.0368(13) Uani 1 1 d . . .
Mo11 Mo 0.03666(4) 0.51843(3) 0.401683(19) 0.02377(14) Uani 1 1 d . . .
O11 O 0.1630(3) 0.9164(2) 0.38835(14) 0.0234(8) Uani 1 1 d . . .
N11 N 0.3333(4) 1.1355(4) 0.2741(2) 0.0406(14) Uani 1 1 d . . .
Mo12 Mo -0.00739(4) 0.63207(3) 0.28340(2) 0.02251(13) Uani 1 1 d . . .
O12 O 0.3916(3) 0.7799(3) 0.43676(15) 0.0220(8) Uani 1 1 d . . .
N12 N 0.3463(6) 1.0961(6) 0.2230(3) 0.069(2) Uani 1 1 d . . .
H12B H 0.4092 1.1076 0.2121 0.082 Uiso 1 1 d R . .
H12A H 0.3026 1.1190 0.1991 0.082 Uiso 1 1 d R . .
N13 N 0.1439(4) 1.1077(4) 0.4301(2) 0.0285(11) Uani 1 1 d . . .
O13 O 0.5189(3) 0.5695(2) 0.38389(15) 0.0209(8) Uani 1 1 d . . .
O14 O 0.2890(3) 0.4428(2) 0.32564(14) 0.0200(8) Uani 1 1 d . . .
N14 N 0.0895(4) 1.0678(4) 0.4685(2) 0.0412(14) Uani 1 1 d . . .
O15 O 0.0243(3) 0.8038(3) 0.43024(15) 0.0227(8) Uani 1 1 d . . .
N15 N -0.0181(4) 1.1061(4) 0.4039(2) 0.0341(12) Uani 1 1 d . . .
N16 N -0.1146(5) 1.1164(5) 0.3764(3) 0.0554(18) Uani 1 1 d . . .
H16A H -0.1628 1.0844 0.3913 0.066 Uiso 1 1 d R . .
H16B H -0.1330 1.1731 0.3771 0.066 Uiso 1 1 d R . .
O16 O -0.0124(3) 0.7375(3) 0.33021(15) 0.0234(8) Uani 1 1 d . . .
O17 O 0.2116(3) 0.8268(2) 0.47598(14) 0.0213(8) Uani 1 1 d . . .
O18 O 0.0430(3) 0.6276(3) 0.43874(15) 0.0251(8) Uani 1 1 d . . .
O19 O 0.0842(3) 0.4271(3) 0.34972(15) 0.0246(8) Uani 1 1 d . . .
O20 O 0.2425(3) 0.5303(3) 0.23896(14) 0.0222(8) Uani 1 1 d . . .
O21 O 0.4483(3) 0.7137(2) 0.24236(14) 0.0203(8) Uani 1 1 d . . .
O22 O 0.3498(3) 0.8678(2) 0.34922(14) 0.0213(8) Uani 1 1 d . . .
O23 O -0.0457(3) 0.9203(3) 0.35113(16) 0.0290(9) Uani 1 1 d . . .
O24 O 0.2252(3) 0.6412(3) 0.48587(14) 0.0255(9) Uani 1 1 d . . .
O25 O 0.3813(3) 0.4556(3) 0.42198(15) 0.0249(8) Uani 1 1 d . . .
O26 O 0.4250(3) 0.5538(2) 0.28612(14) 0.0213(8) Uani 1 1 d . . .
O27 O 0.2617(3) 0.7011(3) 0.19620(14) 0.0223(8) Uani 1 1 d . . .
O28 O 0.1232(3) 0.8480(3) 0.29300(15) 0.0235(8) Uani 1 1 d . . .
O29 O 0.0624(4) 0.7341(3) 0.53285(17) 0.0339(10) Uani 1 1 d . . .
O30 O 0.0815(3) 0.6979(3) 0.24218(15) 0.0248(9) Uani 1 1 d . . .
O31 O 0.3144(3) 0.8520(3) 0.24621(14) 0.0223(8) Uani 1 1 d . . .
O32 O 0.4848(3) 0.7366(3) 0.35021(15) 0.0231(8) Uani 1 1 d . . .
O33 O 0.4233(3) 0.6084(3) 0.47446(15) 0.0252(8) Uani 1 1 d . . .
O34 O 0.1745(3) 0.4925(3) 0.43631(15) 0.0250(9) Uani 1 1 d . . .
O35 O 0.1368(3) 0.8543(3) 0.18194(16) 0.0356(10) Uani 1 1 d . . .
O36 O 0.5941(3) 0.7111(3) 0.44866(17) 0.0289(9) Uani 1 1 d . . .
O37 O 0.1940(3) 0.7414(2) 0.38490(13) 0.0163(7) Uani 1 1 d . . .
O38 O 0.2801(3) 0.7015(2) 0.29947(14) 0.0157(7) Uani 1 1 d . . .
O39 O 0.3212(3) 0.6131(2) 0.38284(13) 0.0153(7) Uani 1 1 d . . .
O40 O 0.1461(3) 0.5969(2) 0.33765(13) 0.0161(7) Uani 1 1 d . . .


_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 O9 1.675(4) . ?
Mo1 O20 1.828(4) . ?
Mo1 O27 1.871(4) . ?
Mo1 O26 1.969(4) . ?
Mo1 O21 2.027(4) . ?
Mo1 O38 2.442(3) . ?
P1 O39 1.532(3) . ?
P1 O40 1.532(4) . ?
P1 O37 1.535(4) . ?
P1 O38 1.537(4) . ?
O1 Mo5 1.714(4) . ?
C1 N1 1.338(7) . ?
C1 N3 1.348(7) . ?
Cu1 N1 1.986(4) . ?
Cu1 N1 1.986(4) 3_676 ?
Cu1 N5 2.025(4) 3_676 ?
Cu1 N5 2.025(4) . ?
N1 N2 1.381(6) . ?
O1W Cu2 2.313(5) . ?
Cu2 N13 1.980(5) . ?
Cu2 N9 1.988(5) . ?
Cu2 N6 2.017(5) . ?
Cu2 N2 2.032(5) . ?
Mo2 O8 1.669(4) . ?
Mo2 O21 1.832(4) . ?
Mo2 O32 1.869(4) . ?
Mo2 O31 1.987(4) . ?
Mo2 O22 2.010(4) . ?
Mo2 O38 2.422(3) . ?
C2 N2 1.310(7) . ?
C2 N3 1.360(8) . ?
O2 Mo11 1.871(4) . ?
O2 Mo12 1.991(4) . ?
Mo3 O6 1.689(4) . ?
Mo3 O26 1.863(4) . ?
Mo3 O13 1.911(4) . ?
Mo3 O14 1.929(4) . ?
Mo3 O25 1.965(4) . ?
Mo3 O39 2.432(3) . ?
O3 Mo12 1.675(4) . ?
N3 N4 1.397(6) . ?
C3 N5 1.297(7) . ?
C3 N7 1.349(7) . ?
Mo4 O10 1.669(4) . ?
Mo4 O19 1.856(4) . ?
Mo4 O14 1.886(4) . ?
Mo4 O5 1.923(4) . ?
Mo4 O20 2.022(4) . ?
Mo4 O40 2.459(3) . ?
O4 Mo11 1.674(4) . ?
C4 N6 1.296(7) . ?
C4 N7 1.336(7) . ?
N5 N6 1.408(6) . ?
Mo5 O22 1.824(4) . ?
Mo5 O11 1.902(4) . ?
Mo5 O12 1.912(4) . ?
Mo5 O17 1.969(4) . ?
Mo5 O37 2.396(3) . ?
C5 N9 1.295(8) . ?
C5 N11 1.342(8) . ?
O5 Mo12 1.904(4) . ?
Mo6 O35 1.681(4) . ?
Mo6 O28 1.840(4) . ?
Mo6 O31 1.851(4) . ?
Mo6 O27 1.981(4) . ?
Mo6 O30 1.994(4) . ?
Mo6 O38 2.442(3) . ?
C6 N10 1.257(9) . ?
C6 N11 1.368(10) . ?
Mo7 O36 1.679(4) . ?
Mo7 O33 1.853(4) . ?
Mo7 O12 1.920(4) . ?
Mo7 O13 1.928(4) . ?
Mo7 O32 1.969(4) . ?
Mo7 O39 2.424(3) . ?
O7 Mo10 1.671(4) . ?
N7 N8 1.418(7) . ?
C7 N13 1.336(8) . ?
C7 N15 1.349(9) . ?
Mo8 O23 1.678(4) . ?
Mo8 O15 1.864(4) . ?
Mo8 O16 1.874(4) . ?
Mo8 O11 1.957(4) . ?
Mo8 O28 1.969(4) . ?
Mo8 O37 2.455(3) . ?
C8 N15 1.301(9) . ?
C8 N14 1.317(9) . ?
Mo9 O29 1.672(4) . ?
Mo9 O24 1.863(4) . ?
Mo9 O17 1.883(4) . ?
Mo9 O18 1.962(4) . ?
Mo9 O15 1.984(4) . ?
Mo9 O37 2.450(3) . ?
N9 N10 1.383(7) . ?
Mo10 O34 1.837(4) . ?
Mo10 O25 1.887(4) . ?
Mo10 O24 1.970(4) . ?
Mo10 O33 1.973(4) . ?
Mo10 O39 2.442(3) . ?
Mo11 O18 1.858(4) . ?
Mo11 O19 1.978(4) . ?
Mo11 O34 1.987(4) . ?
Mo11 O40 2.446(3) . ?
N11 N12 1.420(8) . ?
Mo12 O30 1.833(4) . ?
Mo12 O16 1.948(4) . ?
Mo12 O40 2.421(3) . ?
N13 N14 1.338(8) . ?
N15 N16 1.410(7) . ?

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
O9 Mo1 O20 104.65(19) . . ?
O9 Mo1 O27 102.75(18) . . ?
O20 Mo1 O27 96.02(17) . . ?
O9 Mo1 O26 102.28(18) . . ?
O20 Mo1 O26 87.13(16) . . ?
O27 Mo1 O26 153.07(15) . . ?
O9 Mo1 O21 97.48(18) . . ?
O20 Mo1 O21 156.95(15) . . ?
O27 Mo1 O21 85.15(16) . . ?
O26 Mo1 O21 81.89(15) . . ?
O9 Mo1 O38 167.80(17) . . ?
O20 Mo1 O38 87.17(14) . . ?
O27 Mo1 O38 72.49(14) . . ?
O26 Mo1 O38 80.99(13) . . ?
O21 Mo1 O38 71.17(13) . . ?
O39 P1 O40 109.5(2) . . ?
O39 P1 O37 109.20(19) . . ?
O40 P1 O37 109.6(2) . . ?
O39 P1 O38 109.52(19) . . ?
O40 P1 O38 110.01(19) . . ?
O37 P1 O38 108.9(2) . . ?
N1 C1 N3 108.4(5) . . ?
N1 Cu1 N1 180.0 . 3_676 ?
N1 Cu1 N5 89.98(18) . 3_676 ?
N1 Cu1 N5 90.02(18) 3_676 3_676 ?
N1 Cu1 N5 90.03(18) . . ?
N1 Cu1 N5 89.97(18) 3_676 . ?
N5 Cu1 N5 180.0 3_676 . ?
C1 N1 N2 107.5(4) . . ?
C1 N1 Cu1 129.1(4) . . ?
N2 N1 Cu1 121.1(3) . . ?
N13 Cu2 N9 91.1(2) . . ?
N13 Cu2 N6 94.2(2) . . ?
N9 Cu2 N6 170.3(2) . . ?
N13 Cu2 N2 177.0(2) . . ?
N9 Cu2 N2 87.6(2) . . ?
N6 Cu2 N2 87.53(19) . . ?
N13 Cu2 O1W 87.5(2) . . ?
N9 Cu2 O1W 94.9(2) . . ?
N6 Cu2 O1W 93.5(2) . . ?
N2 Cu2 O1W 89.9(2) . . ?
O8 Mo2 O21 103.76(18) . . ?
O8 Mo2 O32 102.20(18) . . ?
O21 Mo2 O32 96.01(16) . . ?
O8 Mo2 O31 100.21(18) . . ?
O21 Mo2 O31 88.58(16) . . ?
O32 Mo2 O31 155.31(16) . . ?
O8 Mo2 O22 100.54(17) . . ?
O21 Mo2 O22 155.11(16) . . ?
O32 Mo2 O22 83.97(16) . . ?
O31 Mo2 O22 81.87(15) . . ?
O8 Mo2 O38 172.47(16) . . ?
O21 Mo2 O38 74.66(14) . . ?
O32 Mo2 O38 85.31(14) . . ?
O31 Mo2 O38 72.50(14) . . ?
O22 Mo2 O38 80.54(14) . . ?
N2 C2 N3 109.4(5) . . ?
C2 N2 N1 107.6(5) . . ?
C2 N2 Cu2 127.8(4) . . ?
N1 N2 Cu2 123.0(4) . . ?
Mo11 O2 Mo12 125.7(2) . . ?
O6 Mo3 O26 104.10(17) . . ?
O6 Mo3 O13 100.88(17) . . ?
O26 Mo3 O13 91.89(16) . . ?
O6 Mo3 O14 102.78(17) . . ?
O26 Mo3 O14 86.70(16) . . ?
O13 Mo3 O14 155.92(15) . . ?
O6 Mo3 O25 98.98(17) . . ?
O26 Mo3 O25 156.85(16) . . ?
O13 Mo3 O25 85.46(16) . . ?
O14 Mo3 O25 86.49(16) . . ?
O6 Mo3 O39 169.60(15) . . ?
O26 Mo3 O39 84.70(14) . . ?
O13 Mo3 O39 72.92(14) . . ?
O14 Mo3 O39 83.02(13) . . ?
O25 Mo3 O39 72.52(14) . . ?
C1 N3 C2 107.1(5) . . ?
C1 N3 N4 123.4(5) . . ?
C2 N3 N4 129.5(5) . . ?
N5 C3 N7 110.3(5) . . ?
O10 Mo4 O19 103.26(18) . . ?
O10 Mo4 O14 102.92(18) . . ?
O19 Mo4 O14 93.16(17) . . ?
O10 Mo4 O5 101.15(18) . . ?
O19 Mo4 O5 90.73(17) . . ?
O14 Mo4 O5 154.02(16) . . ?
O10 Mo4 O20 100.70(17) . . ?
O19 Mo4 O20 156.00(15) . . ?
O14 Mo4 O20 82.64(15) . . ?
O5 Mo4 O20 83.43(16) . . ?
O10 Mo4 O40 172.82(16) . . ?
O19 Mo4 O40 74.11(14) . . ?
O14 Mo4 O40 83.99(13) . . ?
O5 Mo4 O40 72.41(13) . . ?
O20 Mo4 O40 81.95(13) . . ?
N6 C4 N7 110.6(5) . . ?
C3 N5 N6 106.4(4) . . ?
C3 N5 Cu1 129.9(4) . . ?
N6 N5 Cu1 123.4(3) . . ?
O1 Mo5 O22 101.90(18) . . ?
O1 Mo5 O11 101.75(17) . . ?
O22 Mo5 O11 93.09(17) . . ?
O1 Mo5 O12 100.86(17) . . ?
O22 Mo5 O12 87.80(17) . . ?
O11 Mo5 O12 156.67(16) . . ?
O1 Mo5 O17 100.44(17) . . ?
O22 Mo5 O17 157.45(16) . . ?
O11 Mo5 O17 85.33(16) . . ?
O12 Mo5 O17 85.02(16) . . ?
O1 Mo5 O37 171.92(16) . . ?
O22 Mo5 O37 85.25(14) . . ?
O11 Mo5 O37 73.85(14) . . ?
O12 Mo5 O37 83.00(14) . . ?
O17 Mo5 O37 72.68(13) . . ?
N9 C5 N11 109.2(6) . . ?
Mo12 O5 Mo4 125.5(2) . . ?
O35 Mo6 O28 104.83(19) . . ?
O35 Mo6 O31 102.6(2) . . ?
O28 Mo6 O31 96.01(17) . . ?
O35 Mo6 O27 98.72(18) . . ?
O28 Mo6 O27 155.04(16) . . ?
O31 Mo6 O27 86.73(16) . . ?
O35 Mo6 O30 101.5(2) . . ?
O28 Mo6 O30 85.33(16) . . ?
O31 Mo6 O30 154.69(15) . . ?
O27 Mo6 O30 81.95(16) . . ?
O35 Mo6 O38 169.06(17) . . ?
O28 Mo6 O38 85.98(14) . . ?
O31 Mo6 O38 74.15(14) . . ?
O27 Mo6 O38 70.86(13) . . ?
O30 Mo6 O38 80.76(14) . . ?
C4 N6 N5 106.6(4) . . ?
C4 N6 Cu2 129.6(4) . . ?
N5 N6 Cu2 121.2(3) . . ?
N10 C6 N11 110.6(6) . . ?
O36 Mo7 O33 102.22(19) . . ?
O36 Mo7 O12 101.76(18) . . ?
O33 Mo7 O12 92.50(17) . . ?
O36 Mo7 O13 101.65(18) . . ?
O33 Mo7 O13 89.64(17) . . ?
O12 Mo7 O13 155.46(15) . . ?
O36 Mo7 O32 101.54(19) . . ?
O33 Mo7 O32 156.24(16) . . ?
O12 Mo7 O32 83.09(16) . . ?
O13 Mo7 O32 85.16(15) . . ?
O36 Mo7 O39 173.18(16) . . ?
O33 Mo7 O39 74.06(14) . . ?
O12 Mo7 O39 84.25(14) . . ?
O13 Mo7 O39 72.85(13) . . ?
O32 Mo7 O39 82.25(14) . . ?
C4 N7 C3 106.1(5) . . ?
C4 N7 N8 129.6(5) . . ?
C3 N7 N8 124.2(5) . . ?
N13 C7 N15 107.4(6) . . ?
O23 Mo8 O15 102.01(18) . . ?
O23 Mo8 O16 102.90(18) . . ?
O15 Mo8 O16 93.36(17) . . ?
O23 Mo8 O11 101.16(18) . . ?
O15 Mo8 O11 88.41(16) . . ?
O16 Mo8 O11 154.94(16) . . ?
O23 Mo8 O28 102.22(18) . . ?
O15 Mo8 O28 155.60(16) . . ?
O16 Mo8 O28 84.02(16) . . ?
O11 Mo8 O28 84.15(16) . . ?
O23 Mo8 O37 171.60(16) . . ?
O15 Mo8 O37 74.03(14) . . ?
O16 Mo8 O37 84.87(14) . . ?
O11 Mo8 O37 71.59(13) . . ?
O28 Mo8 O37 81.58(14) . . ?
N15 C8 N14 112.4(6) . . ?
O29 Mo9 O24 103.64(19) . . ?
O29 Mo9 O17 102.27(19) . . ?
O24 Mo9 O17 94.54(17) . . ?
O29 Mo9 O18 102.40(19) . . ?
O24 Mo9 O18 85.64(17) . . ?
O17 Mo9 O18 154.55(16) . . ?
O29 Mo9 O15 99.58(19) . . ?
O24 Mo9 O15 155.88(16) . . ?
O17 Mo9 O15 86.77(16) . . ?
O18 Mo9 O15 83.08(16) . . ?
O29 Mo9 O37 170.45(17) . . ?
O24 Mo9 O37 85.07(14) . . ?
O17 Mo9 O37 72.74(13) . . ?
O18 Mo9 O37 81.94(14) . . ?
O15 Mo9 O37 72.30(13) . . ?
C5 N9 N10 107.8(5) . . ?
C5 N9 Cu2 135.9(4) . . ?
N10 N9 Cu2 115.8(4) . . ?
O7 Mo10 O34 103.4(2) . . ?
O7 Mo10 O25 102.66(19) . . ?
O34 Mo10 O25 94.65(17) . . ?
O7 Mo10 O24 101.27(19) . . ?
O34 Mo10 O24 85.82(17) . . ?
O25 Mo10 O24 155.25(16) . . ?
O7 Mo10 O33 99.9(2) . . ?
O34 Mo10 O33 155.61(16) . . ?
O25 Mo10 O33 86.94(17) . . ?
O24 Mo10 O33 82.83(17) . . ?
O7 Mo10 O39 170.82(18) . . ?
O34 Mo10 O39 85.34(15) . . ?
O25 Mo10 O39 73.49(14) . . ?
O24 Mo10 O39 81.91(14) . . ?
O33 Mo10 O39 71.76(13) . . ?
C6 N10 N9 107.2(6) . . ?
O4 Mo11 O18 102.4(2) . . ?
O4 Mo11 O2 102.0(2) . . ?
O18 Mo11 O2 94.18(17) . . ?
O4 Mo11 O19 101.48(19) . . ?
O18 Mo11 O19 155.11(16) . . ?
O2 Mo11 O19 87.48(16) . . ?
O4 Mo11 O34 102.9(2) . . ?
O18 Mo11 O34 85.46(17) . . ?
O2 Mo11 O34 154.60(16) . . ?
O19 Mo11 O34 82.62(16) . . ?
O4 Mo11 O40 171.98(18) . . ?
O18 Mo11 O40 84.20(15) . . ?
O2 Mo11 O40 72.81(14) . . ?
O19 Mo11 O40 72.55(13) . . ?
O34 Mo11 O40 81.90(14) . . ?
Mo5 O11 Mo8 124.82(19) . . ?
C5 N11 C6 105.2(6) . . ?
C5 N11 N12 124.8(7) . . ?
C6 N11 N12 130.1(6) . . ?
O3 Mo12 O30 103.1(2) . . ?
O3 Mo12 O5 101.09(19) . . ?
O30 Mo12 O5 93.65(17) . . ?
O3 Mo12 O16 102.06(19) . . ?
O30 Mo12 O16 86.93(17) . . ?
O5 Mo12 O16 156.09(16) . . ?
O3 Mo12 O2 100.3(2) . . ?
O30 Mo12 O2 156.35(16) . . ?
O5 Mo12 O2 85.49(16) . . ?
O16 Mo12 O2 84.56(16) . . ?
O3 Mo12 O40 170.34(18) . . ?
O30 Mo12 O40 85.49(14) . . ?
O5 Mo12 O40 73.63(14) . . ?
O16 Mo12 O40 82.60(14) . . ?
O2 Mo12 O40 71.56(14) . . ?
Mo5 O12 Mo7 151.1(2) . . ?
C7 N13 N14 109.0(5) . . ?
C7 N13 Cu2 127.2(5) . . ?
N14 N13 Cu2 123.3(4) . . ?
Mo3 O13 Mo7 125.04(19) . . ?
Mo4 O14 Mo3 153.8(2) . . ?
C8 N14 N13 105.1(5) . . ?
Mo8 O15 Mo9 125.2(2) . . ?
C8 N15 C7 106.0(6) . . ?
C8 N15 N16 123.7(6) . . ?
C7 N15 N16 130.2(6) . . ?
Mo8 O16 Mo12 151.6(2) . . ?
Mo9 O17 Mo5 124.93(19) . . ?
Mo11 O18 Mo9 152.2(2) . . ?
Mo4 O19 Mo11 125.1(2) . . ?
Mo1 O20 Mo4 151.4(2) . . ?
Mo2 O21 Mo1 124.74(19) . . ?
Mo5 O22 Mo2 150.4(2) . . ?
Mo9 O24 Mo10 151.2(2) . . ?
Mo10 O25 Mo3 124.96(19) . . ?
Mo3 O26 Mo1 149.1(2) . . ?
Mo1 O27 Mo6 126.89(19) . . ?
Mo6 O28 Mo8 153.3(2) . . ?
Mo12 O30 Mo6 150.2(2) . . ?
Mo6 O31 Mo2 124.59(19) . . ?
Mo2 O32 Mo7 154.0(2) . . ?
Mo7 O33 Mo10 125.3(2) . . ?
Mo10 O34 Mo11 151.5(2) . . ?
P1 O37 Mo5 125.97(19) . . ?
P1 O37 Mo9 125.41(19) . . ?
Mo5 O37 Mo9 89.66(11) . . ?
P1 O37 Mo8 126.05(19) . . ?
Mo5 O37 Mo8 89.67(11) . . ?
Mo9 O37 Mo8 88.33(11) . . ?
P1 O38 Mo2 126.70(19) . . ?
P1 O38 Mo1 125.09(19) . . ?
Mo2 O38 Mo1 89.36(11) . . ?
P1 O38 Mo6 125.57(19) . . ?
Mo2 O38 Mo6 88.65(11) . . ?
Mo1 O38 Mo6 89.76(11) . . ?
P1 O39 Mo7 126.89(19) . . ?
P1 O39 Mo3 125.12(18) . . ?
Mo7 O39 Mo3 89.08(11) . . ?
P1 O39 Mo10 126.11(19) . . ?
Mo7 O39 Mo10 88.59(11) . . ?
Mo3 O39 Mo10 89.03(11) . . ?
P1 O40 Mo12 125.43(19) . . ?
P1 O40 Mo11 126.30(18) . . ?
Mo12 O40 Mo11 89.88(11) . . ?
P1 O40 Mo4 126.79(19) . . ?
Mo12 O40 Mo4 88.39(11) . . ?
Mo11 O40 Mo4 87.86(11) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.148
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.139
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1022774'
_audit_update_record             
;
2015-04-15 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H38 Cu2 N24 O47 Si W12'
_chemical_formula_weight         3631.03

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   I2/a

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

_cell_length_a                   18.331(12)
_cell_length_b                   13.2839(9)
_cell_length_c                   26.055(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.215(1)
_cell_angle_gamma                90
_cell_volume                     5991.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      25.10

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6452
_exptl_absorpt_coefficient_mu    23.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0997
_exptl_absorpt_correction_T_max  0.1153
_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  '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            15028
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5310
_reflns_number_gt                4931
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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. 
 During the refinement,the restraint command 'ISOR' was used to refine the non-H atoms 
 'C1,C2,C3,C4,C5,C6,N1,N2,N3,N4,N5,N6,N7,N8,N9,N10,N11,N12,O1W,O2W,O3W,O4W,Si1,
 O1,O2,O3,O4,O5,O6,O7,O8,O9,O10,O11,O12,O14,O15,O16,O17,O18,O19,O20,O21,O22' with ADP problems, 
 the command 'DFIX' was used to restrain the distances of N1 and N2,N3 and N4,N5 and N6 with longer bond lengths. 
;

_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)+(0.0000P)²+8508.7236P] 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         5310
_refine_ls_number_parameters     462
_refine_ls_number_restraints     403
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.1225
_refine_ls_wR_factor_ref         0.2838
_refine_ls_wR_factor_gt          0.2812
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.004
_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
Cu1 Cu 0.2660(3) 0.2992(4) -0.0644(2) 0.0201(11) Uani 1 1 d . . .
Si1 Si 0.2500 0.7500 -0.2500 0.024(4) Uani 1 2 d SU . .
W1 W 0.27511(14) 0.58109(16) -0.34738(8) 0.0354(6) Uani 1 1 d . . .
W2 W 0.39341(12) 0.76877(19) -0.12033(8) 0.0350(6) Uani 1 1 d . . .
W3 W 0.42011(12) 0.60604(16) -0.22041(10) 0.0350(6) Uani 1 1 d . . .
W4 W 0.13394(11) 0.53051(14) -0.28552(8) 0.0251(5) Uani 1 1 d . . .
W5 W 0.28097(12) 0.54764(14) -0.15741(8) 0.0241(5) Uani 1 1 d . . .
W6 W 0.11329(11) 0.69733(15) -0.18457(8) 0.0240(5) Uani 1 1 d . . .
N1 N 0.415(2) 0.275(3) -0.0882(18) 0.038(5) Uani 1 1 d DU . .
N2 N 0.356(2) 0.228(3) -0.0740(17) 0.033(5) Uani 1 1 d DU . .
N3 N 0.449(2) 0.120(3) -0.0654(18) 0.037(5) Uani 1 1 d DU . .
N4 N 0.496(3) 0.034(3) -0.0540(19) 0.045(7) Uani 1 1 d DU . .
H4B H 0.4796 -0.0203 -0.0434 0.054 Uiso 1 1 calc R . .
H4C H 0.5406 0.0357 -0.0577 0.054 Uiso 1 1 calc R . .
N5 N 0.165(2) 0.364(3) -0.0011(12) 0.019(5) Uani 1 1 d DU . .
N6 N 0.178(2) 0.371(3) -0.0511(12) 0.023(4) Uani 1 1 d DU . .
N7 N 0.073(2) 0.458(3) -0.0579(15) 0.020(5) Uani 1 1 d U . .
N8 N 0.009(2) 0.524(3) -0.0741(15) 0.025(6) Uani 1 1 d U . .
H8WB H 0.0258 0.5903 -0.0793 0.037 Uiso 1 1 d R . .
H8WC H -0.0275 0.5002 -0.1075 0.037 Uiso 1 1 d R . .
N9 N 0.196(2) 0.253(3) -0.1357(16) 0.028(4) Uani 1 1 d U . .
N10 N 0.124(2) 0.207(3) -0.1422(16) 0.026(4) Uani 1 1 d U . .
N11 N 0.144(2) 0.209(3) -0.2214(17) 0.029(5) Uani 1 1 d U . .
N12 N 0.138(2) 0.202(3) -0.2757(17) 0.033(6) Uani 1 1 d U . .
H12B H 0.1319 0.1327 -0.2867 0.050 Uiso 1 1 d R . .
H12C H 0.0932 0.2393 -0.2967 0.050 Uiso 1 1 d R . .
O1 O 0.500(2) 0.542(3) -0.2009(17) 0.050(10) Uani 1 1 d U . .
O1W O 0.2500 0.179(4) 0.0000 0.041(13) Uani 1 2 d SDU . .
H1WA H 0.2949 0.1378 0.0151 0.049 Uiso 1 1 d RD . .
O2 O 0.447(3) 0.692(5) -0.158(2) 0.082(16) Uani 1 1 d U . .
O2W O 0.388(5) 0.103(6) 0.053(3) 0.13(3) Uani 1 1 d U . .
H2WB H 0.4229 0.1419 0.0409 0.191 Uiso 1 1 d R . .
H2WA H 0.3958 0.1161 0.0905 0.191 Uiso 1 1 d R . .
O3 O 0.462(2) 0.773(3) -0.0586(16) 0.049(10) Uani 1 1 d U . .
O3W O 0.334(5) 0.840(7) -0.493(4) 0.15(3) Uani 1 1 d U . .
H3WA H 0.3023 0.8512 -0.5272 0.232 Uiso 1 1 d R . .
H3WB H 0.3510 0.9042 -0.4762 0.232 Uiso 1 1 d R . .
O4 O 0.446(3) 0.705(4) -0.263(2) 0.076(15) Uani 1 1 d U . .
O4W O 0.342(4) 0.622(6) -0.480(3) 0.12(2) Uani 1 1 d U . .
H4WB H 0.3430 0.6943 -0.4823 0.179 Uiso 1 1 d R . .
H4WA H 0.3588 0.5928 -0.5074 0.179 Uiso 1 1 d R . .
O5 O 0.414(3) 0.880(4) -0.155(2) 0.067(13) Uani 1 1 d U . .
O6 O 0.314(3) 0.850(4) -0.107(2) 0.062(12) Uani 1 1 d U . .
O7 O 0.351(3) 0.546(4) -0.284(2) 0.067(13) Uani 1 1 d U . .
O8 O 0.209(2) 0.511(3) -0.3230(15) 0.038(9) Uani 1 1 d U . .
O9 O 0.288(2) 0.499(3) -0.3954(15) 0.038(9) Uani 1 1 d U . .
O10 O 0.081(2) 0.423(3) -0.2995(17) 0.045(10) Uani 1 1 d U . .
O11 O 0.086(3) 0.603(3) -0.2436(17) 0.052(11) Uani 1 1 d U . .
O12 O 0.193(3) 0.613(3) -0.1456(18) 0.055(11) Uani 1 1 d U . .
O13 O 0.166(3) 0.811(3) -0.1428(19) 0.069(15) Uani 1 1 d . . .
O14 O 0.047(2) 0.668(3) -0.1556(15) 0.040(9) Uani 1 1 d U . .
O15 O 0.209(2) 0.490(3) -0.2205(15) 0.039(9) Uani 1 1 d U . .
O16 O 0.2934(19) 0.446(2) -0.1132(13) 0.027(7) Uani 1 1 d U . .
O17 O 0.368(3) 0.525(4) -0.181(2) 0.077(15) Uani 1 1 d U . .
O18 O 0.343(3) 0.642(4) -0.106(2) 0.070(14) Uani 1 1 d U . .
O19 O 0.299(3) 0.836(5) -0.202(2) 0.020(13) Uani 0.50 1 d PU . .
O20 O 0.311(3) 0.685(4) -0.202(2) 0.015(12) Uani 0.50 1 d PU . .
O21 O 0.213(3) 0.664(4) -0.229(2) 0.019(12) Uani 0.50 1 d PU . .
O22 O 0.185(3) 0.795(4) -0.223(2) 0.017(12) Uani 0.50 1 d PU . .
C1 C 0.464(3) 0.210(4) -0.090(2) 0.039(8) Uani 1 1 d U . .
H1A H 0.5035 0.2192 -0.1040 0.047 Uiso 1 1 calc R . .
C2 C 0.376(3) 0.137(4) -0.0628(19) 0.028(10) Uani 1 1 d U . .
H2A H 0.3452 0.0878 -0.0541 0.033 Uiso 1 1 calc R . .
C3 C 0.209(3) 0.250(4) -0.182(2) 0.039(13) Uani 1 1 d U . .
H3A H 0.2537 0.2710 -0.1872 0.047 Uiso 1 1 calc R . .
C4 C 0.096(3) 0.181(4) -0.1919(19) 0.025(10) Uani 1 1 d U . .
H4A H 0.0497 0.1472 -0.2067 0.031 Uiso 1 1 calc R . .
C5 C 0.126(2) 0.432(3) -0.0867(18) 0.020(9) Uani 1 1 d U . .
H5A H 0.1254 0.4523 -0.1211 0.024 Uiso 1 1 calc R . .
C6 C 0.096(2) 0.417(3) -0.0082(17) 0.017(9) Uani 1 1 d U . .
H6A H 0.0711 0.4228 0.0173 0.021 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
Cu1 N5 1.96(3) 2 ?
Cu1 N9 1.98(4) . ?
Cu1 N2 1.99(4) . ?
Cu1 N6 2.00(3) . ?
Cu1 O1W 2.40(4) . ?
Si1 O21 1.52(6) . ?
Si1 O21 1.52(6) 7_564 ?
Si1 O20 1.63(5) . ?
Si1 O20 1.63(5) 7_564 ?
Si1 O22 1.68(5) . ?
Si1 O22 1.68(5) 7_564 ?
Si1 O19 1.71(6) . ?
Si1 O19 1.71(6) 7_564 ?
W1 O9 1.74(4) . ?
W1 O8 1.80(4) . ?
W1 O7 1.84(5) . ?
W1 O13 1.87(5) 7_564 ?
W1 O6 1.91(5) 7_564 ?
W1 O22 2.40(6) 7_564 ?
W1 O19 2.42(6) 7_564 ?
W2 O3 1.69(4) . ?
W2 O5 1.83(5) . ?
W2 O2 1.90(6) . ?
W2 O6 1.94(5) . ?
W2 O18 2.00(5) . ?
W2 O19 2.42(6) . ?
W2 O20 2.43(5) . ?
W3 O1 1.63(4) . ?
W3 O4 1.89(6) . ?
W3 O7 1.89(5) . ?
W3 O2 1.90(6) . ?
W3 O17 1.95(6) . ?
W3 O22 2.40(6) 7_564 ?
W3 O20 2.44(5) . ?
W4 O10 1.70(4) . ?
W4 O15 1.88(4) . ?
W4 O11 1.88(4) . ?
W4 O5 1.93(5) 7_564 ?
W4 O8 1.95(3) . ?
W4 O19 2.24(6) 7_564 ?
W4 O21 2.44(6) . ?
W5 O16 1.74(3) . ?
W5 O15 1.90(4) . ?
W5 O17 1.91(5) . ?
W5 O18 1.92(5) . ?
W5 O12 1.94(4) . ?
W5 O20 2.31(5) . ?
W5 O21 2.43(6) . ?
W6 O14 1.68(4) . ?
W6 O12 1.86(4) . ?
W6 O11 1.92(4) . ?
W6 O13 1.92(4) . ?
W6 O4 1.93(5) 7_564 ?
W6 O22 2.30(5) . ?
W6 O21 2.50(6) . ?
N1 C1 1.25(7) . ?
N1 N2 1.401(10) . ?
N2 C2 1.27(6) . ?
N3 C2 1.38(6) . ?
N3 N4 1.401(10) . ?
N3 C1 1.42(7) . ?
N5 N6 1.400(10) . ?
N5 C6 1.40(5) . ?
N5 Cu1 1.96(3) 2 ?
N6 C5 1.35(6) . ?
N7 C6 1.34(6) . ?
N7 N8 1.42(5) . ?
N7 C5 1.45(6) . ?
N9 C3 1.29(7) . ?
N9 N10 1.41(6) . ?
N10 C4 1.28(6) . ?
N11 N12 1.38(6) . ?
N11 C3 1.40(7) . ?
N11 C4 1.40(6) . ?
O1W Cu1 2.40(4) 2 ?
O4 W6 1.93(5) 7_564 ?
O5 W4 1.93(5) 7_564 ?
O6 W1 1.91(5) 7_564 ?
O13 W1 1.87(5) 7_564 ?
O19 O21 1.73(8) 7_564 ?
O19 W4 2.24(6) 7_564 ?
O19 W1 2.42(6) 7_564 ?
O20 O21 1.73(8) . ?
O21 O19 1.73(8) 7_564 ?
O22 W1 2.40(6) 7_564 ?
O22 W3 2.40(6) 7_564 ?

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
N5 Cu1 N9 171.8(16) 2 . ?
N5 Cu1 N2 89.9(16) 2 . ?
N9 Cu1 N2 92.3(17) . . ?
N5 Cu1 N6 87.9(13) 2 . ?
N9 Cu1 N6 90.1(15) . . ?
N2 Cu1 N6 177.4(16) . . ?
N5 Cu1 O1W 82.8(12) 2 . ?
N9 Cu1 O1W 104.9(14) . . ?
N2 Cu1 O1W 94.0(13) . . ?
N6 Cu1 O1W 84.5(12) . . ?
O21 Si1 O21 180.000(11) . 7_564 ?
O21 Si1 O20 66(3) . . ?
O21 Si1 O20 114(3) 7_564 . ?
O21 Si1 O20 114(3) . 7_564 ?
O21 Si1 O20 66(3) 7_564 7_564 ?
O20 Si1 O20 180(4) . 7_564 ?
O21 Si1 O22 70(3) . . ?
O21 Si1 O22 110(3) 7_564 . ?
O20 Si1 O22 105(3) . . ?
O20 Si1 O22 75(3) 7_564 . ?
O21 Si1 O22 110(3) . 7_564 ?
O21 Si1 O22 70(3) 7_564 7_564 ?
O20 Si1 O22 75(3) . 7_564 ?
O20 Si1 O22 105(3) 7_564 7_564 ?
O22 Si1 O22 180(3) . 7_564 ?
O21 Si1 O19 115(3) . . ?
O21 Si1 O19 65(3) 7_564 . ?
O20 Si1 O19 74(3) . . ?
O20 Si1 O19 106(3) 7_564 . ?
O22 Si1 O19 75(3) . . ?
O22 Si1 O19 105(3) 7_564 . ?
O21 Si1 O19 65(3) . 7_564 ?
O21 Si1 O19 115(3) 7_564 7_564 ?
O20 Si1 O19 106(3) . 7_564 ?
O20 Si1 O19 74(3) 7_564 7_564 ?
O22 Si1 O19 105(3) . 7_564 ?
O22 Si1 O19 75(3) 7_564 7_564 ?
O19 Si1 O19 180(3) . 7_564 ?
O9 W1 O8 101.3(18) . . ?
O9 W1 O7 104(2) . . ?
O8 W1 O7 87(2) . . ?
O9 W1 O13 99(2) . 7_564 ?
O8 W1 O13 159(2) . 7_564 ?
O7 W1 O13 91(2) . 7_564 ?
O9 W1 O6 98.2(19) . 7_564 ?
O8 W1 O6 86.3(18) . 7_564 ?
O7 W1 O6 157(2) . 7_564 ?
O13 W1 O6 88(2) 7_564 7_564 ?
O9 W1 O22 154.9(18) . 7_564 ?
O8 W1 O22 99.1(18) . 7_564 ?
O7 W1 O22 62(2) . 7_564 ?
O13 W1 O22 62(2) 7_564 7_564 ?
O6 W1 O22 98(2) 7_564 7_564 ?
O9 W1 O19 154.7(19) . 7_564 ?
O8 W1 O19 59.4(19) . 7_564 ?
O7 W1 O19 92(2) . 7_564 ?
O13 W1 O19 100(2) 7_564 7_564 ?
O6 W1 O19 66.5(19) 7_564 7_564 ?
O22 W1 O19 50.4(19) 7_564 7_564 ?
O3 W2 O5 103(2) . . ?
O3 W2 O2 100(2) . . ?
O5 W2 O2 87(2) . . ?
O3 W2 O6 100(2) . . ?
O5 W2 O6 86(2) . . ?
O2 W2 O6 160(2) . . ?
O3 W2 O18 96(2) . . ?
O5 W2 O18 161(2) . . ?
O2 W2 O18 89(2) . . ?
O6 W2 O18 91(2) . . ?
O3 W2 O19 156(2) . . ?
O5 W2 O19 59(2) . . ?
O2 W2 O19 95(2) . . ?
O6 W2 O19 66(2) . . ?
O18 W2 O19 103(2) . . ?
O3 W2 O20 154(2) . . ?
O5 W2 O20 97(2) . . ?
O2 W2 O20 65(2) . . ?
O6 W2 O20 97(2) . . ?
O18 W2 O20 65.5(19) . . ?
O19 W2 O20 49.1(19) . . ?
O1 W3 O4 100(2) . . ?
O1 W3 O7 109(2) . . ?
O4 W3 O7 90(2) . . ?
O1 W3 O2 95(2) . . ?
O4 W3 O2 92(2) . . ?
O7 W3 O2 154(2) . . ?
O1 W3 O17 95(2) . . ?
O4 W3 O17 165(2) . . ?
O7 W3 O17 86(2) . . ?
O2 W3 O17 85(2) . . ?
O1 W3 O22 160(2) . 7_564 ?
O4 W3 O22 64(2) . 7_564 ?
O7 W3 O22 62(2) . 7_564 ?
O2 W3 O22 97(2) . 7_564 ?
O17 W3 O22 101(2) . 7_564 ?
O1 W3 O20 151(2) . . ?
O4 W3 O20 102(2) . . ?
O7 W3 O20 90(2) . . ?
O2 W3 O20 65(2) . . ?
O17 W3 O20 64(2) . . ?
O22 W3 O20 48.9(18) 7_564 . ?
O10 W4 O15 98.4(18) . . ?
O10 W4 O11 102(2) . . ?
O15 W4 O11 88.1(17) . . ?
O10 W4 O5 105(2) . 7_564 ?
O15 W4 O5 156(2) . 7_564 ?
O11 W4 O5 89(2) . 7_564 ?
O10 W4 O8 103.1(18) . . ?
O15 W4 O8 89.3(15) . . ?
O11 W4 O8 154.4(18) . . ?
O5 W4 O8 83.6(18) 7_564 . ?
O10 W4 O19 159(2) . 7_564 ?
O15 W4 O19 95.1(19) . 7_564 ?
O11 W4 O19 93(2) . 7_564 ?
O5 W4 O19 62(2) 7_564 7_564 ?
O8 W4 O19 61.5(19) . 7_564 ?
O10 W4 O21 157.1(19) . . ?
O15 W4 O21 63.6(18) . . ?
O11 W4 O21 65(2) . . ?
O5 W4 O21 94(2) 7_564 . ?
O8 W4 O21 91.3(18) . . ?
O19 W4 O21 43(2) 7_564 . ?
O16 W5 O15 99.1(16) . . ?
O16 W5 O17 98(2) . . ?
O15 W5 O17 95(2) . . ?
O16 W5 O18 98(2) . . ?
O15 W5 O18 163(2) . . ?
O17 W5 O18 87(2) . . ?
O16 W5 O12 100.1(17) . . ?
O15 W5 O12 86.4(17) . . ?
O17 W5 O12 161(2) . . ?
O18 W5 O12 86(2) . . ?
O16 W5 O20 159.8(17) . . ?
O15 W5 O20 95.8(18) . . ?
O17 W5 O20 67(2) . . ?
O18 W5 O20 69(2) . . ?
O12 W5 O20 94.4(19) . . ?
O16 W5 O21 157.5(17) . . ?
O15 W5 O21 63.6(18) . . ?
O17 W5 O21 97(2) . . ?
O18 W5 O21 99(2) . . ?
O12 W5 O21 66(2) . . ?
O20 W5 O21 42.7(18) . . ?
O14 W6 O12 100(2) . . ?
O14 W6 O11 100.0(19) . . ?
O12 W6 O11 89.7(19) . . ?
O14 W6 O13 103(2) . . ?
O12 W6 O13 91(2) . . ?
O11 W6 O13 156(2) . . ?
O14 W6 O4 98(2) . 7_564 ?
O12 W6 O4 162(2) . 7_564 ?
O11 W6 O4 86(2) . 7_564 ?
O13 W6 O4 86(2) . 7_564 ?
O14 W6 O22 159(2) . . ?
O12 W6 O22 97(2) . . ?
O11 W6 O22 93(2) . . ?
O13 W6 O22 64(2) . . ?
O4 W6 O22 66(2) 7_564 . ?
O14 W6 O21 156.2(19) . . ?
O12 W6 O21 65.5(19) . . ?
O11 W6 O21 63.1(18) . . ?
O13 W6 O21 96(2) . . ?
O4 W6 O21 97(2) 7_564 . ?
O22 W6 O21 44.6(19) . . ?
C1 N1 N2 109(4) . . ?
C2 N2 N1 107(4) . . ?
C2 N2 Cu1 128(3) . . ?
N1 N2 Cu1 125(3) . . ?
C2 N3 N4 131(5) . . ?
C2 N3 C1 103(4) . . ?
N4 N3 C1 126(4) . . ?
N6 N5 C6 105(3) . . ?
N6 N5 Cu1 126(3) . 2 ?
C6 N5 Cu1 129(2) . 2 ?
C5 N6 N5 113(3) . . ?
C5 N6 Cu1 126(3) . . ?
N5 N6 Cu1 121(3) . . ?
C6 N7 N8 120(4) . . ?
C6 N7 C5 111(4) . . ?
N8 N7 C5 129(4) . . ?
C3 N9 N10 109(4) . . ?
C3 N9 Cu1 128(4) . . ?
N10 N9 Cu1 123(3) . . ?
C4 N10 N9 106(4) . . ?
N12 N11 C3 124(4) . . ?
N12 N11 C4 133(4) . . ?
C3 N11 C4 103(4) . . ?
Cu1 O1W Cu1 97(2) 2 . ?
W2 O2 W3 137(3) . . ?
W3 O4 W6 134(3) . 7_564 ?
W2 O5 W4 141(3) . 7_564 ?
W1 O6 W2 134(3) 7_564 . ?
W1 O7 W3 140(3) . . ?
W1 O8 W4 141(2) . . ?
W4 O11 W6 139(2) . . ?
W6 O12 W5 137(3) . . ?
W1 O13 W6 137(3) 7_564 . ?
W4 O15 W5 139(2) . . ?
W5 O17 W3 133(3) . . ?
W5 O18 W2 129(3) . . ?
Si1 O19 O21 52(3) . 7_564 ?
Si1 O19 W4 127(3) . 7_564 ?
O21 O19 W4 75(3) 7_564 7_564 ?
Si1 O19 W2 117(3) . . ?
O21 O19 W2 136(4) 7_564 . ?
W4 O19 W2 99(2) 7_564 . ?
Si1 O19 W1 116(3) . 7_564 ?
O21 O19 W1 130(4) 7_564 7_564 ?
W4 O19 W1 98(2) 7_564 7_564 ?
W2 O19 W1 94(2) . 7_564 ?
Si1 O20 O21 54(3) . . ?
Si1 O20 W5 126(3) . . ?
O21 O20 W5 72(3) . . ?
Si1 O20 W2 120(3) . . ?
O21 O20 W2 134(4) . . ?
W5 O20 W2 96.3(19) . . ?
Si1 O20 W3 118(3) . . ?
O21 O20 W3 131(4) . . ?
W5 O20 W3 96(2) . . ?
W2 O20 W3 93.2(18) . . ?
Si1 O21 O20 60(3) . . ?
Si1 O21 O19 63(3) . 7_564 ?
O20 O21 O19 101(4) . 7_564 ?
Si1 O21 W5 125(3) . . ?
O20 O21 W5 65(3) . . ?
O19 O21 W5 131(4) 7_564 . ?
Si1 O21 W4 125(3) . . ?
O20 O21 W4 134(4) . . ?
O19 O21 W4 62(3) 7_564 . ?
W5 O21 W4 93(2) . . ?
Si1 O21 W6 121(3) . . ?
O20 O21 W6 127(3) . . ?
O19 O21 W6 128(3) 7_564 . ?
W5 O21 W6 91.4(19) . . ?
W4 O21 W6 91.8(18) . . ?
Si1 O22 W6 125(3) . . ?
Si1 O22 W1 119(3) . 7_564 ?
W6 O22 W1 97(2) . 7_564 ?
Si1 O22 W3 118(3) . 7_564 ?
W6 O22 W3 96.7(19) . 7_564 ?
W1 O22 W3 94(2) 7_564 7_564 ?
N1 C1 N3 109(5) . . ?
N2 C2 N3 110(4) . . ?
N9 C3 N11 110(5) . . ?
N10 C4 N11 112(4) . . ?
N6 C5 N7 103(3) . . ?
N7 C6 N5 108(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.201
_refine_diff_density_min         -4.052
_refine_diff_density_rms         0.694



####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1022775'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H29 Cr Cu2 Mo6 N16 O28'
_chemical_formula_weight         1552.19

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'
Cr Cr 0.3209 0.6236 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   13.4466(11)
_cell_length_b                   13.4785(11)
_cell_length_c                   13.8805(12)
_cell_angle_alpha                64.4500(1)
_cell_angle_beta                 61.8190(1)
_cell_angle_gamma                78.750(2)
_cell_volume                     2000.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      26.66

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1494
_exptl_absorpt_coefficient_mu    3.227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_T_max  0.7179
_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  '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            11694
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         26.66
_reflns_number_total             8262
_reflns_number_gt                5471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
 During the refinement, the command 'ISOR' was used to refine atom N8 with ADP problem, 
 and the command 'DFIX' was used to restrain the distance between N7 and N8 with longer bond length. 
;

_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)+(0.0767P)²+13.7110P] 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         8262
_refine_ls_number_parameters     557
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1641
_refine_ls_wR_factor_gt          0.1430
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
Mo1 Mo 0.29730(7) -0.20580(7) 0.54161(8) 0.0225(2) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.0000 0.5000 0.0166(4) Uani 1 2 d S . .
Cr1 Cr 0.30650(12) -0.39812(12) 0.45319(13) 0.0152(3) Uani 1 1 d . . .
O1 O 0.4104(7) -0.1236(6) 0.4813(8) 0.040(2) Uani 1 1 d . . .
N1 N 0.4932(6) 0.1088(6) 0.3517(7) 0.0173(17) Uani 1 1 d . . .
C1 C 0.4066(8) 0.1412(9) 0.3265(9) 0.025(2) Uani 1 1 d . . .
H1 H 0.3315 0.1335 0.3825 0.030 Uiso 1 1 calc R . .
O1W O 0.6524(9) 0.5089(9) -0.0050(10) 0.078(3) Uani 1 1 d . . .
H1WA H 0.6132 0.5666 -0.0171 0.094 Uiso 1 1 d R . .
H1WB H 0.6412 0.4693 -0.0329 0.094 Uiso 1 1 d R . .
Mo2 Mo 0.27993(7) -0.47931(7) 0.72074(7) 0.0213(2) Uani 1 1 d . . .
Cu2 Cu 0.73809(9) 0.06260(10) 0.24140(10) 0.0179(3) Uani 1 1 d . . .
N2 N 0.5881(6) 0.1335(7) 0.2436(7) 0.0199(18) Uani 1 1 d . . .
O2 O 0.2004(7) -0.1769(7) 0.6595(7) 0.039(2) Uani 1 1 d . . .
C2 C 0.5562(8) 0.1808(8) 0.1604(8) 0.024(2) Uani 1 1 d . . .
H2 H 0.6041 0.2069 0.0794 0.029 Uiso 1 1 calc R . .
O2W O -0.0063(9) -0.3562(12) 0.6725(11) 0.106(5) Uani 1 1 d . . .
H2WA H 0.0479 -0.3464 0.6827 0.127 Uiso 1 1 d R . .
H2WB H 0.0111 -0.3242 0.5986 0.127 Uiso 1 1 d R . .
Mo3 Mo 0.30043(7) -0.66001(7) 0.61857(8) 0.0198(2) Uani 1 1 d . . .
Cu3 Cu 1.0000 0.0000 0.0000 0.0192(4) Uani 1 2 d S . .
O3 O 0.3758(6) -0.5500(6) 0.7756(6) 0.0302(17) Uani 1 1 d . . .
N3 N 0.4417(6) 0.1867(7) 0.2089(7) 0.0202(18) Uani 1 1 d . . .
C3 C 0.8071(9) 0.2928(8) 0.0730(9) 0.024(2) Uani 1 1 d . . .
H3 H 0.7453 0.3218 0.1213 0.029 Uiso 1 1 calc R . .
O3W O -0.0062(10) -0.5313(15) 0.6185(14) 0.148(7) Uani 1 1 d . . .
H3WA H -0.0352 -0.5954 0.6622 0.178 Uiso 1 1 d R . .
H3WB H 0.0643 -0.5383 0.5805 0.178 Uiso 1 1 d R . .
Mo4 Mo 0.32042(7) -0.58640(7) 0.34936(8) 0.0210(2) Uani 1 1 d . . .
O4 O 0.3946(6) -0.7299(6) 0.6766(6) 0.0285(17) Uani 1 1 d . . .
C4 C 0.9613(9) 0.2801(10) -0.0689(10) 0.036(3) Uani 1 1 d . . .
H4 H 1.0284 0.2983 -0.1385 0.044 Uiso 1 1 calc R . .
N4 N 0.3683(8) 0.2279(9) 0.1563(9) 0.040(3) Uani 1 1 d . . .
H4A H 0.3900 0.2067 0.0987 0.048 Uiso 1 1 d R . .
H4B H 0.3002 0.2035 0.2076 0.048 Uiso 1 1 d R . .
Mo5 Mo 0.32793(7) -0.32416(7) 0.18074(7) 0.0209(2) Uani 1 1 d . . .
N5 N 0.8270(6) 0.1905(7) 0.0964(7) 0.0191(17) Uani 1 1 d . . .
O5 O 0.2022(6) -0.7552(6) 0.6691(7) 0.0332(18) Uani 1 1 d . . .
C5 C 0.9797(8) 0.1253(8) -0.2285(8) 0.019(2) Uani 1 1 d . . .
H5 H 0.9165 0.1628 -0.1936 0.023 Uiso 1 1 calc R . .
Mo6 Mo 0.31664(7) -0.12989(7) 0.27239(8) 0.0213(2) Uani 1 1 d . . .
O6 O 0.2248(6) -0.6861(6) 0.4070(7) 0.0339(19) Uani 1 1 d . . .
C6 C 1.1150(8) 0.0692(8) -0.3568(9) 0.021(2) Uani 1 1 d . . .
H6 H 1.1635 0.0603 -0.4273 0.025 Uiso 1 1 calc R . .
N6 N 0.9256(7) 0.1791(7) 0.0061(7) 0.027(2) Uani 1 1 d . . .
O7 O 0.4306(6) -0.6039(6) 0.2289(7) 0.0328(18) Uani 1 1 d . . .
N7 N 0.8890(8) 0.3521(7) -0.0319(8) 0.033(2) Uani 1 1 d D . .
C7 C 1.1799(8) 0.1086(10) -0.0064(9) 0.027(2) Uani 1 1 d . . .
H7 H 1.1292 0.1373 0.0491 0.033 Uiso 1 1 calc R . .
O8 O 0.4385(6) -0.3548(6) 0.0693(6) 0.036(2) Uani 1 1 d . . .
C8 C 1.3335(8) 0.0701(8) -0.1359(9) 0.023(2) Uani 1 1 d . . .
H8 H 1.4092 0.0678 -0.1870 0.028 Uiso 1 1 calc R . .
N8 N 0.9006(10) 0.4687(8) -0.0885(11) 0.058(3) Uani 1 1 d DU . .
H8A H 0.8797 0.4947 -0.1452 0.070 Uiso 1 1 d R . .
H8B H 0.8581 0.4967 -0.0364 0.070 Uiso 1 1 d R . .
O9 O 0.2381(6) -0.2510(6) 0.1206(7) 0.0311(18) Uani 1 1 d . . .
N9 N 1.0351(6) 0.0535(6) -0.1751(7) 0.0168(17) Uani 1 1 d . . .
N10 N 1.1222(6) 0.0166(7) -0.2566(7) 0.0191(17) Uani 1 1 d . . .
O10 O 0.4159(6) -0.0331(6) 0.2158(8) 0.036(2) Uani 1 1 d . . .
N11 N 1.0283(6) 0.1375(6) -0.3434(7) 0.0185(17) Uani 1 1 d . . .
O11 O 0.3722(6) -0.3350(6) 0.6306(6) 0.0266(16) Uani 1 1 d . . .
N12 N 0.9936(7) 0.2135(8) -0.4313(8) 0.029(2) Uani 1 1 d . . .
H12A H 1.0516 0.2579 -0.4911 0.035 Uiso 1 1 d R . .
H12B H 0.9718 0.1771 -0.4588 0.035 Uiso 1 1 d R . .
O12 O 0.2076(6) -0.5923(6) 0.7331(6) 0.0257(16) Uani 1 1 d . . .
N13 N 1.1529(6) 0.0492(7) -0.0434(7) 0.0231(19) Uani 1 1 d . . .
O13 O 0.3921(6) -0.6524(6) 0.4574(6) 0.0244(16) Uani 1 1 d . . .
N14 N 1.2497(6) 0.0231(7) -0.1256(7) 0.0205(18) Uani 1 1 d . . .
O14 O 0.2461(5) -0.4624(6) 0.2742(6) 0.0233(15) Uani 1 1 d . . .
O15 O 0.4009(6) -0.2048(6) 0.1680(6) 0.0273(17) Uani 1 1 d . . .
N15 N 1.2917(7) 0.1223(8) -0.0602(8) 0.032(2) Uani 1 1 d . . .
O16 O 0.2297(6) -0.1351(5) 0.4353(6) 0.0238(16) Uani 1 1 d . . .
N16 N 1.3519(8) 0.1878(10) -0.0486(9) 0.046(3) Uani 1 1 d . . .
H16A H 1.4176 0.1581 -0.0551 0.055 Uiso 1 1 d R . .
H16B H 1.3637 0.2549 -0.1033 0.055 Uiso 1 1 d R . .
O17 O 0.2184(6) -0.3610(6) 0.5925(6) 0.0231(15) Uani 1 1 d . . .
O18 O 0.3835(6) -0.4986(5) 0.5485(6) 0.0199(14) Uani 1 1 d . . .
O19 O 0.2224(5) -0.5329(5) 0.5071(6) 0.0199(14) Uani 1 1 d . . .
O20 O 0.4007(5) -0.4317(5) 0.3106(5) 0.0150(13) Uani 1 1 d . . .
O21 O 0.2296(5) -0.2967(5) 0.3548(6) 0.0192(14) Uani 1 1 d . . .
O22 O 0.3916(5) -0.2637(5) 0.3899(6) 0.0196(14) Uani 1 1 d . . .
O23 O 0.1717(6) -0.4450(6) 0.8315(7) 0.0339(18) Uani 1 1 d . . .
O24 O 0.2195(6) -0.0618(6) 0.2227(7) 0.0339(19) Uani 1 1 d . . .
O25 O 0.6495(5) -0.0381(5) 0.4013(5) 0.0177(14) Uani 1 1 d . . .


_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 O2 1.693(7) . ?
Mo1 O1 1.702(7) . ?
Mo1 O16 1.905(7) . ?
Mo1 O11 2.052(7) . ?
Mo1 O17 2.210(7) . ?
Mo1 O22 2.272(7) . ?
Cu1 O25 1.945(6) 2_656 ?
Cu1 O25 1.945(6) . ?
Cu1 N1 1.980(8) . ?
Cu1 N1 1.980(8) 2_656 ?
Cu1 O1 2.397(7) . ?
Cu1 O1 2.397(7) 2_656 ?
Cr1 O17 1.958(7) . ?
Cr1 O22 1.962(6) . ?
Cr1 O18 1.964(6) . ?
Cr1 O20 1.977(6) . ?
Cr1 O19 1.992(6) . ?
Cr1 O21 1.994(7) . ?
N1 C1 1.313(12) . ?
N1 N2 1.385(10) . ?
C1 N3 1.336(12) . ?
Mo2 O23 1.712(7) . ?
Mo2 O3 1.725(7) . ?
Mo2 O12 1.868(7) . ?
Mo2 O11 2.065(7) . ?
Mo2 O17 2.195(7) . ?
Mo2 O18 2.230(7) . ?
Mo2 Mo3 3.2198(13) . ?
Cu2 O25 1.929(6) . ?
Cu2 N5 1.998(8) . ?
Cu2 N10 2.028(8) 2_755 ?
Cu2 N2 2.049(8) . ?
Cu2 N14 2.286(8) 2_755 ?
N2 C2 1.284(12) . ?
C2 N3 1.360(12) . ?
Mo3 O5 1.700(7) . ?
Mo3 O4 1.728(7) . ?
Mo3 O13 1.945(7) . ?
Mo3 O12 1.962(7) . ?
Mo3 O19 2.230(7) . ?
Mo3 O18 2.241(6) . ?
Cu3 N13 2.012(8) 2_755 ?
Cu3 N13 2.012(8) . ?
Cu3 N9 2.047(8) . ?
Cu3 N9 2.047(8) 2_755 ?
Cu3 N6 2.447(9) . ?
Cu3 N6 2.447(9) 2_755 ?
N3 N4 1.390(11) . ?
C3 N5 1.277(13) . ?
C3 N7 1.341(13) . ?
Mo4 O6 1.695(7) . ?
Mo4 O7 1.706(7) . ?
Mo4 O14 1.926(7) . ?
Mo4 O13 1.962(7) . ?
Mo4 O20 2.273(6) . ?
Mo4 O19 2.306(7) . ?
C4 N6 1.315(14) . ?
C4 N7 1.320(15) . ?
Mo5 O9 1.705(7) . ?
Mo5 O8 1.707(7) . ?
Mo5 O14 1.933(7) . ?
Mo5 O15 1.946(7) . ?
Mo5 O20 2.273(6) . ?
Mo5 O21 2.299(7) . ?
N5 N6 1.367(11) . ?
C5 N9 1.289(12) . ?
C5 N11 1.352(12) . ?
Mo6 O24 1.692(7) . ?
Mo6 O10 1.705(7) . ?
Mo6 O15 1.916(7) . ?
Mo6 O16 1.971(7) . ?
Mo6 O22 2.289(6) . ?
Mo6 O21 2.297(6) . ?
C6 N10 1.302(12) . ?
C6 N11 1.329(12) . ?
N7 N8 1.423(11) . ?
C7 N13 1.296(13) . ?
C7 N15 1.335(12) . ?
C8 N14 1.318(12) . ?
C8 N15 1.358(13) . ?
N9 N10 1.380(10) . ?
N10 Cu2 2.028(8) 2_755 ?
N11 N12 1.424(11) . ?
N13 N14 1.373(10) . ?
N14 Cu2 2.286(8) 2_755 ?
N15 N16 1.408(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O1 105.2(4) . . ?
O2 Mo1 O16 99.6(3) . . ?
O1 Mo1 O16 103.5(3) . . ?
O2 Mo1 O11 97.5(3) . . ?
O1 Mo1 O11 90.4(3) . . ?
O16 Mo1 O11 154.2(3) . . ?
O2 Mo1 O17 96.7(3) . . ?
O1 Mo1 O17 153.1(3) . . ?
O16 Mo1 O17 87.8(3) . . ?
O11 Mo1 O17 71.1(3) . . ?
O2 Mo1 O22 166.3(3) . . ?
O1 Mo1 O22 88.1(3) . . ?
O16 Mo1 O22 73.4(3) . . ?
O11 Mo1 O22 85.6(3) . . ?
O17 Mo1 O22 71.6(2) . . ?
O25 Cu1 O25 180.0 2_656 . ?
O25 Cu1 N1 92.4(3) 2_656 . ?
O25 Cu1 N1 87.6(3) . . ?
O25 Cu1 N1 87.6(3) 2_656 2_656 ?
O25 Cu1 N1 92.4(3) . 2_656 ?
N1 Cu1 N1 180.0 . 2_656 ?
O25 Cu1 O1 87.9(3) 2_656 . ?
O25 Cu1 O1 92.1(3) . . ?
N1 Cu1 O1 85.4(3) . . ?
N1 Cu1 O1 94.6(3) 2_656 . ?
O25 Cu1 O1 92.1(3) 2_656 2_656 ?
O25 Cu1 O1 87.9(3) . 2_656 ?
N1 Cu1 O1 94.6(3) . 2_656 ?
N1 Cu1 O1 85.4(3) 2_656 2_656 ?
O1 Cu1 O1 180.0 . 2_656 ?
O17 Cr1 O22 84.0(3) . . ?
O17 Cr1 O18 83.6(3) . . ?
O22 Cr1 O18 98.0(3) . . ?
O17 Cr1 O20 177.6(3) . . ?
O22 Cr1 O20 93.8(3) . . ?
O18 Cr1 O20 95.9(3) . . ?
O17 Cr1 O19 99.1(3) . . ?
O22 Cr1 O19 176.5(3) . . ?
O18 Cr1 O19 84.2(3) . . ?
O20 Cr1 O19 83.2(3) . . ?
O17 Cr1 O21 97.1(3) . . ?
O22 Cr1 O21 82.1(3) . . ?
O18 Cr1 O21 179.3(3) . . ?
O20 Cr1 O21 83.4(3) . . ?
O19 Cr1 O21 95.7(3) . . ?
Mo1 O1 Cu1 147.7(5) . . ?
C1 N1 N2 106.0(8) . . ?
C1 N1 Cu1 129.8(6) . . ?
N2 N1 Cu1 120.7(6) . . ?
N1 C1 N3 110.3(8) . . ?
O23 Mo2 O3 106.2(4) . . ?
O23 Mo2 O12 98.7(3) . . ?
O3 Mo2 O12 102.4(3) . . ?
O23 Mo2 O11 97.6(3) . . ?
O3 Mo2 O11 91.8(3) . . ?
O12 Mo2 O11 154.4(3) . . ?
O23 Mo2 O17 90.0(3) . . ?
O3 Mo2 O17 158.1(3) . . ?
O12 Mo2 O17 89.3(3) . . ?
O11 Mo2 O17 71.1(3) . . ?
O23 Mo2 O18 161.3(3) . . ?
O3 Mo2 O18 92.4(3) . . ?
O12 Mo2 O18 75.7(3) . . ?
O11 Mo2 O18 82.6(3) . . ?
O17 Mo2 O18 72.4(2) . . ?
O23 Mo2 Mo3 132.4(3) . . ?
O3 Mo2 Mo3 90.5(3) . . ?
O12 Mo2 Mo3 33.7(2) . . ?
O11 Mo2 Mo3 126.7(2) . . ?
O17 Mo2 Mo3 89.12(18) . . ?
O18 Mo2 Mo3 44.06(17) . . ?
O25 Cu2 N5 165.7(3) . . ?
O25 Cu2 N10 88.0(3) . 2_755 ?
N5 Cu2 N10 93.1(3) . 2_755 ?
O25 Cu2 N2 86.4(3) . . ?
N5 Cu2 N2 92.1(3) . . ?
N10 Cu2 N2 174.3(3) 2_755 . ?
O25 Cu2 N14 103.9(3) . 2_755 ?
N5 Cu2 N14 90.4(3) . 2_755 ?
N10 Cu2 N14 90.4(3) 2_755 2_755 ?
N2 Cu2 N14 91.7(3) . 2_755 ?
C2 N2 N1 108.3(8) . . ?
C2 N2 Cu2 131.2(7) . . ?
N1 N2 Cu2 118.6(6) . . ?
N2 C2 N3 109.5(8) . . ?
O5 Mo3 O4 105.5(4) . . ?
O5 Mo3 O13 100.3(3) . . ?
O4 Mo3 O13 97.9(3) . . ?
O5 Mo3 O12 95.8(3) . . ?
O4 Mo3 O12 99.4(3) . . ?
O13 Mo3 O12 152.1(3) . . ?
O5 Mo3 O19 91.3(3) . . ?
O4 Mo3 O19 162.4(3) . . ?
O13 Mo3 O19 73.7(3) . . ?
O12 Mo3 O19 83.5(3) . . ?
O5 Mo3 O18 161.6(3) . . ?
O4 Mo3 O18 91.3(3) . . ?
O13 Mo3 O18 84.3(3) . . ?
O12 Mo3 O18 73.7(3) . . ?
O19 Mo3 O18 72.7(2) . . ?
O5 Mo3 Mo2 127.7(3) . . ?
O4 Mo3 Mo2 88.3(3) . . ?
O13 Mo3 Mo2 128.0(2) . . ?
O12 Mo3 Mo2 31.90(19) . . ?
O19 Mo3 Mo2 85.23(17) . . ?
O18 Mo3 Mo2 43.80(17) . . ?
N13 Cu3 N13 180.0 2_755 . ?
N13 Cu3 N9 88.4(3) 2_755 . ?
N13 Cu3 N9 91.6(3) . . ?
N13 Cu3 N9 91.6(3) 2_755 2_755 ?
N13 Cu3 N9 88.4(3) . 2_755 ?
N9 Cu3 N9 180.0 . 2_755 ?
N13 Cu3 N6 91.1(3) 2_755 . ?
N13 Cu3 N6 88.9(3) . . ?
N9 Cu3 N6 92.2(3) . . ?
N9 Cu3 N6 87.8(3) 2_755 . ?
N13 Cu3 N6 88.9(3) 2_755 2_755 ?
N13 Cu3 N6 91.1(3) . 2_755 ?
N9 Cu3 N6 87.8(3) . 2_755 ?
N9 Cu3 N6 92.2(3) 2_755 2_755 ?
N6 Cu3 N6 180.0 . 2_755 ?
C1 N3 C2 105.8(8) . . ?
C1 N3 N4 123.1(8) . . ?
C2 N3 N4 131.1(8) . . ?
N5 C3 N7 109.5(9) . . ?
O6 Mo4 O7 105.9(4) . . ?
O6 Mo4 O14 99.1(3) . . ?
O7 Mo4 O14 101.2(3) . . ?
O6 Mo4 O13 100.3(3) . . ?
O7 Mo4 O13 96.8(3) . . ?
O14 Mo4 O13 148.7(3) . . ?
O6 Mo4 O20 161.8(3) . . ?
O7 Mo4 O20 91.7(3) . . ?
O14 Mo4 O20 72.6(2) . . ?
O13 Mo4 O20 81.5(3) . . ?
O6 Mo4 O19 93.0(3) . . ?
O7 Mo4 O19 159.5(3) . . ?
O14 Mo4 O19 83.1(3) . . ?
O13 Mo4 O19 71.6(3) . . ?
O20 Mo4 O19 70.2(2) . . ?
N6 C4 N7 110.7(9) . . ?
O9 Mo5 O8 104.7(4) . . ?
O9 Mo5 O14 97.8(3) . . ?
O8 Mo5 O14 100.5(3) . . ?
O9 Mo5 O15 100.1(3) . . ?
O8 Mo5 O15 97.4(3) . . ?
O14 Mo5 O15 150.5(3) . . ?
O9 Mo5 O20 163.3(3) . . ?
O8 Mo5 O20 90.6(3) . . ?
O14 Mo5 O20 72.5(2) . . ?
O15 Mo5 O20 84.1(3) . . ?
O9 Mo5 O21 95.3(3) . . ?
O8 Mo5 O21 158.8(3) . . ?
O14 Mo5 O21 83.5(3) . . ?
O15 Mo5 O21 71.7(3) . . ?
O20 Mo5 O21 70.6(2) . . ?
C3 N5 N6 108.9(8) . . ?
C3 N5 Cu2 128.1(7) . . ?
N6 N5 Cu2 122.9(6) . . ?
N9 C5 N11 109.0(8) . . ?
O24 Mo6 O10 105.0(4) . . ?
O24 Mo6 O15 102.4(3) . . ?
O10 Mo6 O15 97.9(3) . . ?
O24 Mo6 O16 96.7(3) . . ?
O10 Mo6 O16 100.1(3) . . ?
O15 Mo6 O16 149.3(3) . . ?
O24 Mo6 O22 158.8(3) . . ?
O10 Mo6 O22 94.7(3) . . ?
O15 Mo6 O22 82.1(3) . . ?
O16 Mo6 O22 71.9(2) . . ?
O24 Mo6 O21 92.4(3) . . ?
O10 Mo6 O21 161.7(3) . . ?
O15 Mo6 O21 72.3(3) . . ?
O16 Mo6 O21 83.2(3) . . ?
O22 Mo6 O21 69.0(2) . . ?
N10 C6 N11 109.9(9) . . ?
C4 N6 N5 105.0(9) . . ?
C4 N6 Cu3 132.0(7) . . ?
N5 N6 Cu3 122.9(6) . . ?
C4 N7 C3 105.9(9) . . ?
C4 N7 N8 126.6(10) . . ?
C3 N7 N8 127.4(10) . . ?
N13 C7 N15 109.5(9) . . ?
N14 C8 N15 109.2(9) . . ?
C5 N9 N10 107.9(7) . . ?
C5 N9 Cu3 126.7(6) . . ?
N10 N9 Cu3 125.4(6) . . ?
C6 N10 N9 106.6(7) . . ?
C6 N10 Cu2 124.3(6) . 2_755 ?
N9 N10 Cu2 126.3(6) . 2_755 ?
C6 N11 C5 106.6(8) . . ?
C6 N11 N12 128.3(8) . . ?
C5 N11 N12 125.1(8) . . ?
Mo1 O11 Mo2 112.4(3) . . ?
Mo2 O12 Mo3 114.4(3) . . ?
C7 N13 N14 108.6(8) . . ?
C7 N13 Cu3 129.8(7) . . ?
N14 N13 Cu3 121.5(6) . . ?
Mo3 O13 Mo4 116.0(3) . . ?
C8 N14 N13 106.2(8) . . ?
C8 N14 Cu2 126.3(7) . 2_755 ?
N13 N14 Cu2 126.9(6) . 2_755 ?
Mo4 O14 Mo5 116.5(3) . . ?
Mo6 O15 Mo5 118.7(3) . . ?
C7 N15 C8 106.4(9) . . ?
C7 N15 N16 126.0(9) . . ?
C8 N15 N16 127.3(9) . . ?
Mo1 O16 Mo6 117.4(3) . . ?
Cr1 O17 Mo2 102.5(3) . . ?
Cr1 O17 Mo1 103.4(3) . . ?
Mo2 O17 Mo1 101.9(3) . . ?
Cr1 O18 Mo2 101.1(3) . . ?
Cr1 O18 Mo3 101.8(3) . . ?
Mo2 O18 Mo3 92.1(2) . . ?
Cr1 O19 Mo3 101.3(3) . . ?
Cr1 O19 Mo4 102.5(3) . . ?
Mo3 O19 Mo4 93.8(2) . . ?
Cr1 O20 Mo4 104.1(3) . . ?
Cr1 O20 Mo5 103.7(3) . . ?
Mo4 O20 Mo5 92.4(2) . . ?
Cr1 O21 Mo6 103.8(3) . . ?
Cr1 O21 Mo5 102.3(3) . . ?
Mo6 O21 Mo5 92.6(2) . . ?
Cr1 O22 Mo1 101.0(3) . . ?
Cr1 O22 Mo6 105.1(3) . . ?
Mo1 O22 Mo6 93.1(2) . . ?
Cu2 O25 Cu1 121.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        26.66
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         2.806
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.221
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1022776'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H32 Cu3 Mo8 N12 O37'
_chemical_formula_weight         1822.58

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   10.0148(7)
_cell_length_b                   19.0431(14)
_cell_length_c                   21.5320(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.7570(10)
_cell_angle_gamma                90.00
_cell_volume                     4005.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.44
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3484
_exptl_absorpt_coefficient_mu    4.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_T_max  0.6845
_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  '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            20030
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7038
_reflns_number_gt                6228
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
 During the refinement, the restraint command 'EADP' was used to refine the non-H atoms 'O1W, O5W' with ADP problems, 
 and command 'SIMU' was used to restraint all the O atoms with similar thermal parameters. 
;

_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)+(0.0541P)²+39.2126P] 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         7038
_refine_ls_number_parameters     592
_refine_ls_number_restraints     672
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.077
_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 0.12901(6) 0.27337(3) -0.11981(3) 0.01325(14) Uani 1 1 d . . .
Cu1 Cu -0.25123(9) 0.21012(4) -0.10059(4) 0.01749(19) Uani 1 1 d . . .
N1 N -0.2640(6) 0.2931(3) -0.1546(3) 0.0182(12) Uani 1 1 d . . .
C1 C -0.2894(8) 0.3592(4) -0.1455(3) 0.0224(16) Uani 1 1 d . . .
H1 H -0.3123 0.3774 -0.1091 0.027 Uiso 1 1 calc R . .
O1 O -0.1645(5) 0.2626(3) -0.0218(2) 0.0178(10) Uani 1 1 d U . .
O1W O -0.3061(11) 0.4950(5) -0.0380(5) 0.100(2) Uani 1 1 d U . .
H1WA H -0.2703 0.5242 -0.0594 0.120 Uiso 1 1 d R . .
H1WB H -0.2464 0.4638 -0.0239 0.120 Uiso 1 1 d R . .
Mo2 Mo -0.03670(6) 0.31989(3) 0.01716(2) 0.01234(14) Uani 1 1 d . . .
Cu2 Cu -0.25534(10) 0.04756(5) -0.16927(4) 0.0246(2) Uani 1 1 d . . .
C2 C -0.2428(7) 0.3502(4) -0.2380(3) 0.0193(15) Uani 1 1 d . . .
H2 H -0.2262 0.3615 -0.2776 0.023 Uiso 1 1 calc R . .
N2 N -0.2363(6) 0.2876(3) -0.2137(3) 0.0175(12) Uani 1 1 d . . .
O2 O -0.0718(5) 0.3242(3) 0.0968(2) 0.0193(10) Uani 1 1 d U . .
O2W O 0.0085(11) 0.4371(5) -0.2657(5) 0.097(3) Uani 1 1 d U . .
H2WA H 0.0474 0.4110 -0.2350 0.116 Uiso 1 1 d R . .
H2WB H 0.0458 0.4291 -0.2969 0.116 Uiso 1 1 d R . .
Mo3 Mo 0.46576(6) 0.27117(3) -0.02397(3) 0.01466(14) Uani 1 1 d . . .
Cu3 Cu -0.22407(10) 0.19284(5) -0.25053(4) 0.0224(2) Uani 1 1 d . . .
N3 N -0.2775(6) 0.3965(3) -0.1966(3) 0.0226(13) Uani 1 1 d . . .
C3 C -0.3001(8) 0.0856(4) -0.3569(3) 0.0224(15) Uani 1 1 d . . .
H3 H -0.2978 0.1159 -0.3905 0.027 Uiso 1 1 calc R . .
O3 O -0.0859(5) 0.3999(3) -0.0171(2) 0.0251(11) Uani 1 1 d U . .
O3W O 0.0653(9) 0.4452(5) 0.2151(4) 0.076(2) Uani 1 1 d U . .
H3WA H 0.1406 0.4323 0.2067 0.091 Uiso 1 1 d R . .
H3WB H 0.0600 0.4268 0.2504 0.091 Uiso 1 1 d R . .
Mo4 Mo 0.50378(6) 0.20495(3) 0.11947(3) 0.01263(14) Uani 1 1 d . . .
N4 N -0.3022(9) 0.4693(4) -0.2046(4) 0.046(2) Uani 1 1 d . . .
H4A H -0.3634 0.4766 -0.2390 0.055 Uiso 1 1 d R . .
H4B H -0.3308 0.4860 -0.1726 0.055 Uiso 1 1 d R . .
C4 C -0.3309(8) -0.0071(4) -0.3040(3) 0.0253(16) Uani 1 1 d . . .
H4 H -0.3523 -0.0527 -0.2942 0.030 Uiso 1 1 calc R . .
O4 O 0.1075(5) 0.2430(2) 0.0789(2) 0.0153(9) Uani 1 1 d U . .
O4W O -0.0594(12) -0.0037(5) -0.4012(7) 0.127(5) Uani 1 1 d . . .
H4WA H -0.0911 0.0102 -0.3699 0.152 Uiso 1 1 d R . .
H4WB H 0.0206 0.0133 -0.3970 0.152 Uiso 1 1 d R . .
Mo5 Mo 0.28213(6) 0.33161(3) 0.11985(3) 0.01234(14) Uani 1 1 d . . .
N5 N -0.2653(6) 0.1018(3) -0.2964(3) 0.0215(13) Uani 1 1 d . . .
C5 C -0.2246(7) 0.1170(4) 0.0102(3) 0.0213(15) Uani 1 1 d . . .
H5 H -0.2323 0.1528 0.0386 0.026 Uiso 1 1 calc R . .
O5 O 0.0966(5) 0.2854(2) -0.0303(2) 0.0150(9) Uani 1 1 d U . .
O5W O -0.6494(11) 0.0887(5) -0.1262(6) 0.100(2) Uani 1 1 d U . .
H5WA H -0.6715 0.1316 -0.1242 0.120 Uiso 1 1 d R . .
H5WB H -0.6167 0.0837 -0.1592 0.120 Uiso 1 1 d R . .
Mo6 Mo 0.18674(5) 0.19258(3) 0.01704(2) 0.01046(13) Uani 1 1 d . . .
N6 N -0.2876(7) 0.0426(3) -0.2627(3) 0.0230(13) Uani 1 1 d . . .
C6 C -0.1970(10) 0.0155(4) -0.0287(4) 0.039(2) Uani 1 1 d . . .
H6 H -0.1811 -0.0323 -0.0320 0.047 Uiso 1 1 calc R . .
O6 O 0.1592(5) 0.3799(2) 0.0649(2) 0.0191(9) Uani 1 1 d U . .
O6W O 0.4604(10) 0.0512(5) -0.0240(5) 0.097(2) Uani 1 1 d U . .
H6WA H 0.5407 0.0635 -0.0263 0.117 Uiso 1 1 d R . .
H6WB H 0.4348 0.0781 0.0026 0.117 Uiso 1 1 d R . .
N7 N -0.3397(6) 0.0182(3) -0.3625(3) 0.0219(13) Uani 1 1 d . . .
Mo7 Mo 0.32891(6) 0.24134(3) 0.25559(3) 0.01414(14) Uani 1 1 d . . .
O7 O 0.4079(5) 0.3902(3) 0.1473(2) 0.0235(11) Uani 1 1 d U . .
O7W O -0.2983(5) 0.1524(2) -0.1799(2) 0.0170(10) Uani 1 1 d U . .
Mo8 Mo 0.00982(6) 0.24469(3) 0.16025(3) 0.01428(14) Uani 1 1 d . . .
N8 N -0.3879(8) -0.0214(4) -0.4186(3) 0.0333(16) Uani 1 1 d . . .
H8A H -0.3819 -0.0656 -0.4102 0.040 Uiso 1 1 d R . .
H8B H -0.4721 -0.0106 -0.4341 0.040 Uiso 1 1 d R . .
O8 O 0.4185(5) 0.1673(3) 0.2808(2) 0.0265(12) Uani 1 1 d U . .
O8W O -0.2034(9) -0.0550(3) -0.1587(3) 0.0580(19) Uani 1 1 d U . .
N9 N -0.2246(7) 0.0589(3) -0.0760(3) 0.0262(14) Uani 1 1 d . . .
O9 O -0.1046(5) 0.1811(3) 0.1309(2) 0.0250(11) Uani 1 1 d U . .
O9W O -0.0277(6) 0.0737(3) -0.1647(3) 0.0440(15) Uani 1 1 d U . .
N10 N -0.2411(6) 0.1240(3) -0.0512(3) 0.0181(12) Uani 1 1 d . . .
O10 O 0.1920(5) 0.3207(3) 0.1865(2) 0.0181(9) Uani 1 1 d U . .
O10W O -0.4815(9) 0.0147(5) -0.1751(4) 0.072(2) Uani 1 1 d U . .
N11 N -0.1948(7) 0.0497(3) 0.0257(3) 0.0264(14) Uani 1 1 d . . .
O11 O 0.3584(5) 0.2779(2) 0.0579(2) 0.0148(9) Uani 1 1 d U . .
N12 N -0.1726(10) 0.0218(4) 0.0878(3) 0.053(2) Uani 1 1 d . . .
H12A H -0.1287 -0.0179 0.0890 0.063 Uiso 1 1 d R . .
H12B H -0.1226 0.0490 0.1164 0.063 Uiso 1 1 d R . .
O12 O 0.6349(5) 0.2594(3) 0.1549(2) 0.0203(10) Uani 1 1 d U . .
O13 O 0.5348(5) 0.2363(3) -0.0831(2) 0.0236(10) Uani 1 1 d U . .
O14 O 0.5378(5) 0.1972(3) 0.0367(2) 0.0196(9) Uani 1 1 d U . .
O15 O 0.0636(5) 0.1334(2) -0.0129(2) 0.0188(10) Uani 1 1 d U . .
O16 O 0.3167(5) 0.3311(3) -0.0753(2) 0.0191(10) Uani 1 1 d U . .
O17 O 0.0546(5) 0.3500(3) -0.1487(2) 0.0265(11) Uani 1 1 d U . .
O18 O 0.3723(5) 0.2381(2) 0.1672(2) 0.0167(9) Uani 1 1 d U . .
O19 O 0.3068(5) 0.1416(2) 0.0703(2) 0.0188(9) Uani 1 1 d U . .
O20 O -0.0011(5) 0.2128(3) -0.1366(2) 0.0217(10) Uani 1 1 d U . .
O21 O 0.5668(5) 0.3411(3) 0.0028(3) 0.0276(12) Uani 1 1 d U . .
O22 O 0.2769(5) 0.2053(2) -0.0512(2) 0.0157(9) Uani 1 1 d U . .
O23 O 0.5492(5) 0.1242(3) 0.1523(2) 0.0258(11) Uani 1 1 d U . .
O24 O 0.2261(5) 0.2449(3) -0.1810(2) 0.0229(11) Uani 1 1 d U . .
O25 O 0.1486(5) 0.1912(3) 0.2056(2) 0.0177(9) Uani 1 1 d U . .
O26 O 0.4417(5) 0.3091(3) 0.2786(2) 0.0233(11) Uani 1 1 d U . .
O27 O -0.0599(5) 0.2144(3) -0.2812(2) 0.0215(10) 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 O17 1.693(5) . ?
Mo1 O20 1.718(5) . ?
Mo1 O24 1.881(5) . ?
Mo1 O5 2.038(4) . ?
Mo1 O16 2.206(5) . ?
Mo1 O22 2.256(5) . ?
Cu1 N10 1.945(6) . ?
Cu1 N1 1.951(6) . ?
Cu1 O1 1.996(5) . ?
Cu1 O7W 1.998(5) . ?
Cu1 O13 2.310(5) 1_455 ?
N1 C1 1.307(9) . ?
N1 N2 1.365(8) . ?
C1 N3 1.337(10) . ?
O1 Mo2 1.748(5) . ?
Mo2 O3 1.716(5) . ?
Mo2 O2 1.826(5) . ?
Mo2 O5 1.964(4) . ?
Mo2 O4 2.269(5) . ?
Mo2 O6 2.307(5) . ?
Cu2 N6 1.969(6) . ?
Cu2 N9 1.976(6) . ?
Cu2 O8W 2.020(7) . ?
Cu2 O7W 2.045(5) . ?
Cu2 O9W 2.314(6) . ?
Cu2 O10W 2.327(8) . ?
C2 N2 1.298(9) . ?
C2 N3 1.352(9) . ?
N2 Cu3 1.985(6) . ?
O2 Mo8 2.082(5) . ?
Mo3 O21 1.696(5) . ?
Mo3 O13 1.712(5) . ?
Mo3 O14 1.948(5) . ?
Mo3 O16 2.006(5) . ?
Mo3 O22 2.237(5) . ?
Mo3 O11 2.261(4) . ?
Cu3 O27 1.946(5) . ?
Cu3 O7W 1.989(5) . ?
Cu3 N5 1.993(6) . ?
Cu3 O12 2.387(5) 4_465 ?
N3 N4 1.413(9) . ?
C3 N5 1.308(9) . ?
C3 N7 1.342(10) . ?
Mo4 O23 1.711(5) . ?
Mo4 O12 1.714(5) . ?
Mo4 O14 1.893(5) . ?
Mo4 O18 1.947(5) . ?
Mo4 O11 2.226(4) . ?
Mo4 O19 2.355(5) . ?
C4 N6 1.304(10) . ?
C4 N7 1.333(9) . ?
O4 Mo6 1.947(4) . ?
O4 Mo8 2.187(4) . ?
O4 Mo5 2.451(5) . ?
Mo5 O7 1.689(5) . ?
Mo5 O6 1.765(5) . ?
Mo5 O10 1.867(4) . ?
Mo5 O11 1.965(5) . ?
Mo5 O18 2.149(5) . ?
N5 N6 1.386(8) . ?
C5 N10 1.302(9) . ?
C5 N11 1.342(10) . ?
O5 Mo6 2.138(5) . ?
Mo6 O15 1.690(5) . ?
Mo6 O19 1.758(5) . ?
Mo6 O22 1.902(4) . ?
Mo6 O11 2.387(5) . ?
C6 N9 1.292(10) . ?
C6 N11 1.336(10) . ?
N7 N8 1.415(8) . ?
Mo7 O8 1.695(5) . ?
Mo7 O26 1.714(5) . ?
Mo7 O24 1.902(5) 4_566 ?
Mo7 O18 2.044(5) . ?
Mo7 O25 2.115(5) . ?
Mo7 O10 2.340(5) . ?
Mo8 O9 1.691(5) . ?
Mo8 O27 1.752(5) 4_566 ?
Mo8 O25 1.824(5) . ?
Mo8 O10 2.299(5) . ?
N9 N10 1.374(8) . ?
N11 N12 1.410(9) . ?
O12 Cu3 2.387(5) 4_666 ?
O13 Cu1 2.310(5) 1_655 ?
O24 Mo7 1.902(5) 4_565 ?
O27 Mo8 1.752(5) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O17 Mo1 O20 104.4(2) . . ?
O17 Mo1 O24 104.2(2) . . ?
O20 Mo1 O24 98.3(2) . . ?
O17 Mo1 O5 95.8(2) . . ?
O20 Mo1 O5 90.1(2) . . ?
O24 Mo1 O5 155.46(19) . . ?
O17 Mo1 O16 89.6(2) . . ?
O20 Mo1 O16 163.8(2) . . ?
O24 Mo1 O16 85.7(2) . . ?
O5 Mo1 O16 80.28(18) . . ?
O17 Mo1 O22 155.2(2) . . ?
O20 Mo1 O22 96.3(2) . . ?
O24 Mo1 O22 85.80(19) . . ?
O5 Mo1 O22 70.34(17) . . ?
O16 Mo1 O22 68.19(17) . . ?
N10 Cu1 N1 176.6(2) . . ?
N10 Cu1 O1 89.8(2) . . ?
N1 Cu1 O1 93.5(2) . . ?
N10 Cu1 O7W 88.7(2) . . ?
N1 Cu1 O7W 87.9(2) . . ?
O1 Cu1 O7W 168.2(2) . . ?
N10 Cu1 O13 91.8(2) . 1_455 ?
N1 Cu1 O13 88.9(2) . 1_455 ?
O1 Cu1 O13 89.92(19) . 1_455 ?
O7W Cu1 O13 101.87(19) . 1_455 ?
C1 N1 N2 107.6(6) . . ?
C1 N1 Cu1 132.8(5) . . ?
N2 N1 Cu1 119.5(4) . . ?
N1 C1 N3 109.3(6) . . ?
Mo2 O1 Cu1 148.8(3) . . ?
O3 Mo2 O1 103.7(2) . . ?
O3 Mo2 O2 105.5(2) . . ?
O1 Mo2 O2 101.9(2) . . ?
O3 Mo2 O5 103.7(2) . . ?
O1 Mo2 O5 93.0(2) . . ?
O2 Mo2 O5 142.8(2) . . ?
O3 Mo2 O4 155.4(2) . . ?
O1 Mo2 O4 100.5(2) . . ?
O2 Mo2 O4 73.05(18) . . ?
O5 Mo2 O4 70.80(17) . . ?
O3 Mo2 O6 83.5(2) . . ?
O1 Mo2 O6 169.5(2) . . ?
O2 Mo2 O6 83.12(19) . . ?
O5 Mo2 O6 77.80(18) . . ?
O4 Mo2 O6 71.95(17) . . ?
N6 Cu2 N9 176.5(3) . . ?
N6 Cu2 O8W 92.8(3) . . ?
N9 Cu2 O8W 90.7(3) . . ?
N6 Cu2 O7W 87.1(2) . . ?
N9 Cu2 O7W 89.4(2) . . ?
O8W Cu2 O7W 177.3(3) . . ?
N6 Cu2 O9W 89.5(3) . . ?
N9 Cu2 O9W 90.1(3) . . ?
O8W Cu2 O9W 88.6(3) . . ?
O7W Cu2 O9W 88.6(2) . . ?
N6 Cu2 O10W 89.7(3) . . ?
N9 Cu2 O10W 90.9(3) . . ?
O8W Cu2 O10W 88.3(3) . . ?
O7W Cu2 O10W 94.5(3) . . ?
O9W Cu2 O10W 176.8(3) . . ?
N2 C2 N3 109.4(6) . . ?
C2 N2 N1 107.5(6) . . ?
C2 N2 Cu3 132.6(5) . . ?
N1 N2 Cu3 119.1(4) . . ?
Mo2 O2 Mo8 117.0(2) . . ?
O21 Mo3 O13 104.4(3) . . ?
O21 Mo3 O14 103.6(2) . . ?
O13 Mo3 O14 93.9(2) . . ?
O21 Mo3 O16 93.2(2) . . ?
O13 Mo3 O16 100.6(2) . . ?
O14 Mo3 O16 154.3(2) . . ?
O21 Mo3 O22 159.5(2) . . ?
O13 Mo3 O22 92.6(2) . . ?
O14 Mo3 O22 86.38(19) . . ?
O16 Mo3 O22 72.04(18) . . ?
O21 Mo3 O11 92.4(2) . . ?
O13 Mo3 O11 160.3(2) . . ?
O14 Mo3 O11 71.83(18) . . ?
O16 Mo3 O11 88.46(18) . . ?
O22 Mo3 O11 73.50(16) . . ?
O27 Cu3 N2 94.3(2) . . ?
O27 Cu3 O7W 145.9(2) . . ?
N2 Cu3 O7W 88.9(2) . . ?
O27 Cu3 N5 96.5(2) . . ?
N2 Cu3 N5 164.6(2) . . ?
O7W Cu3 N5 88.3(2) . . ?
O27 Cu3 O12 90.84(19) . 4_465 ?
N2 Cu3 O12 85.2(2) . 4_465 ?
O7W Cu3 O12 123.30(18) . 4_465 ?
N5 Cu3 O12 83.7(2) . 4_465 ?
C1 N3 C2 106.2(6) . . ?
C1 N3 N4 125.2(6) . . ?
C2 N3 N4 128.6(7) . . ?
N5 C3 N7 108.9(6) . . ?
O23 Mo4 O12 104.6(2) . . ?
O23 Mo4 O14 103.5(2) . . ?
O12 Mo4 O14 100.7(2) . . ?
O23 Mo4 O18 102.8(2) . . ?
O12 Mo4 O18 96.3(2) . . ?
O14 Mo4 O18 143.7(2) . . ?
O23 Mo4 O11 152.4(2) . . ?
O12 Mo4 O11 102.9(2) . . ?
O14 Mo4 O11 73.59(18) . . ?
O18 Mo4 O11 71.49(18) . . ?
O23 Mo4 O19 81.1(2) . . ?
O12 Mo4 O19 173.3(2) . . ?
O14 Mo4 O19 81.02(19) . . ?
O18 Mo4 O19 78.84(18) . . ?
O11 Mo4 O19 71.26(17) . . ?
N6 C4 N7 109.0(7) . . ?
Mo6 O4 Mo8 151.3(2) . . ?
Mo6 O4 Mo2 102.73(19) . . ?
Mo8 O4 Mo2 96.92(18) . . ?
Mo6 O4 Mo5 102.66(19) . . ?
Mo8 O4 Mo5 96.39(17) . . ?
Mo2 O4 Mo5 94.45(17) . . ?
O7 Mo5 O6 104.2(2) . . ?
O7 Mo5 O10 104.7(2) . . ?
O6 Mo5 O10 100.9(2) . . ?
O7 Mo5 O11 102.1(2) . . ?
O6 Mo5 O11 97.7(2) . . ?
O10 Mo5 O11 142.2(2) . . ?
O7 Mo5 O18 100.3(2) . . ?
O6 Mo5 O18 155.1(2) . . ?
O10 Mo5 O18 76.49(19) . . ?
O11 Mo5 O18 72.88(18) . . ?
O7 Mo5 O4 177.4(2) . . ?
O6 Mo5 O4 77.35(19) . . ?
O10 Mo5 O4 76.81(18) . . ?
O11 Mo5 O4 75.56(17) . . ?
O18 Mo5 O4 78.00(17) . . ?
C3 N5 N6 106.9(6) . . ?
C3 N5 Cu3 132.7(5) . . ?
N6 N5 Cu3 119.2(4) . . ?
N10 C5 N11 108.8(6) . . ?
Mo2 O5 Mo1 142.9(2) . . ?
Mo2 O5 Mo6 107.0(2) . . ?
Mo1 O5 Mo6 102.66(19) . . ?
O15 Mo6 O19 102.5(2) . . ?
O15 Mo6 O22 102.8(2) . . ?
O19 Mo6 O22 101.6(2) . . ?
O15 Mo6 O4 102.5(2) . . ?
O19 Mo6 O4 98.6(2) . . ?
O22 Mo6 O4 143.1(2) . . ?
O15 Mo6 O5 100.0(2) . . ?
O19 Mo6 O5 157.3(2) . . ?
O22 Mo6 O5 75.47(18) . . ?
O4 Mo6 O5 74.06(18) . . ?
O15 Mo6 O11 178.8(2) . . ?
O19 Mo6 O11 78.61(19) . . ?
O22 Mo6 O11 76.78(18) . . ?
O4 Mo6 O11 77.42(18) . . ?
O5 Mo6 O11 78.85(17) . . ?
C4 N6 N5 107.5(6) . . ?
C4 N6 Cu2 133.3(5) . . ?
N5 N6 Cu2 119.1(4) . . ?
N9 C6 N11 109.8(7) . . ?
Mo5 O6 Mo2 116.0(2) . . ?
C4 N7 C3 107.6(6) . . ?
C4 N7 N8 123.6(6) . . ?
C3 N7 N8 128.7(6) . . ?
O8 Mo7 O26 105.4(3) . . ?
O8 Mo7 O24 102.5(2) . 4_566 ?
O26 Mo7 O24 96.6(2) . 4_566 ?
O8 Mo7 O18 93.9(2) . . ?
O26 Mo7 O18 91.7(2) . . ?
O24 Mo7 O18 158.9(2) 4_566 . ?
O8 Mo7 O25 96.8(2) . . ?
O26 Mo7 O25 157.1(2) . . ?
O24 Mo7 O25 83.76(19) 4_566 . ?
O18 Mo7 O25 81.12(18) . . ?
O8 Mo7 O10 159.3(2) . . ?
O26 Mo7 O10 87.4(2) . . ?
O24 Mo7 O10 91.96(19) 4_566 . ?
O18 Mo7 O10 69.03(17) . . ?
O25 Mo7 O10 69.73(17) . . ?
Cu3 O7W Cu1 112.5(2) . . ?
Cu3 O7W Cu2 111.0(2) . . ?
Cu1 O7W Cu2 115.9(2) . . ?
O9 Mo8 O27 104.1(2) . 4_566 ?
O9 Mo8 O25 100.0(2) . . ?
O27 Mo8 O25 104.0(2) 4_566 . ?
O9 Mo8 O2 98.0(2) . . ?
O27 Mo8 O2 89.3(2) 4_566 . ?
O25 Mo8 O2 154.2(2) . . ?
O9 Mo8 O4 94.3(2) . . ?
O27 Mo8 O4 154.5(2) 4_566 . ?
O25 Mo8 O4 89.86(19) . . ?
O2 Mo8 O4 70.43(17) . . ?
O9 Mo8 O10 167.9(2) . . ?
O27 Mo8 O10 88.0(2) 4_566 . ?
O25 Mo8 O10 75.55(19) . . ?
O2 Mo8 O10 83.04(19) . . ?
O4 Mo8 O10 74.63(17) . . ?
C6 N9 N10 107.1(6) . . ?
C6 N9 Cu2 133.6(6) . . ?
N10 N9 Cu2 119.2(4) . . ?
C5 N10 N9 107.6(6) . . ?
C5 N10 Cu1 128.4(5) . . ?
N9 N10 Cu1 123.1(4) . . ?
Mo5 O10 Mo8 111.9(2) . . ?
Mo5 O10 Mo7 104.2(2) . . ?
Mo8 O10 Mo7 94.11(18) . . ?
C6 N11 C5 106.7(6) . . ?
C6 N11 N12 128.0(7) . . ?
C5 N11 N12 125.2(7) . . ?
Mo5 O11 Mo4 102.77(19) . . ?
Mo5 O11 Mo3 151.8(2) . . ?
Mo4 O11 Mo3 93.91(17) . . ?
Mo5 O11 Mo6 104.36(19) . . ?
Mo4 O11 Mo6 96.77(17) . . ?
Mo3 O11 Mo6 95.88(16) . . ?
Mo4 O12 Cu3 149.4(3) . 4_666 ?
Mo3 O13 Cu1 138.3(3) . 1_655 ?
Mo4 O14 Mo3 117.2(2) . . ?
Mo3 O16 Mo1 114.5(2) . . ?
Mo4 O18 Mo7 144.0(3) . . ?
Mo4 O18 Mo5 106.3(2) . . ?
Mo7 O18 Mo5 105.3(2) . . ?
Mo6 O19 Mo4 113.3(2) . . ?
Mo6 O22 Mo3 112.8(2) . . ?
Mo6 O22 Mo1 102.9(2) . . ?
Mo3 O22 Mo1 104.15(19) . . ?
Mo1 O24 Mo7 155.4(3) . 4_565 ?
Mo8 O25 Mo7 118.9(2) . . ?
Mo8 O27 Cu3 147.0(3) 4_565 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.151
_refine_diff_density_min         -2.657
_refine_diff_density_rms         0.233
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1022777'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H17 Cu3 N12 O18 V5'
_chemical_formula_weight         990.64

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'
V V 0.3005 0.5294 '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'

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

_cell_length_a                   8.7273(9)
_cell_length_b                   12.8497(9)
_cell_length_c                   12.8591(10)
_cell_angle_alpha                86.1540(10)
_cell_angle_beta                 75.8790(10)
_cell_angle_gamma                75.8440(10)
_cell_volume                     1356.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.63
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             966
_exptl_absorpt_coefficient_mu    4.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5462
_exptl_absorpt_correction_T_max  0.6877
_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  '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            6986
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4762
_reflns_number_gt                3866
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0588P)²+0.2849P] 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         4762
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.003
_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
Cu1 Cu 0.53183(7) 0.11841(5) 0.66554(5) 0.01731(16) Uani 1 1 d . . .
V1 V 0.65598(10) -0.14284(7) 0.68504(6) 0.0185(2) Uani 1 1 d . . .
N1 N 0.4223(5) 0.1007(3) 0.8178(3) 0.0215(9) Uani 1 1 d . . .
O1 O 0.5513(4) -0.0309(3) 0.6357(3) 0.0237(8) Uani 1 1 d . . .
C1 C 0.3116(6) 0.0491(4) 0.8595(4) 0.0262(12) Uani 1 1 d . . .
H1 H 0.2696 0.0081 0.8217 0.031 Uiso 1 1 calc R . .
O1W O -0.0497(5) -0.2709(4) 1.0998(4) 0.0638(15) Uani 1 1 d . . .
H1WA H -0.0001 -0.3095 1.0450 0.077 Uiso 1 1 d R . .
H1WB H 0.0122 -0.2325 1.1096 0.077 Uiso 1 1 d R . .
Cu2 Cu 0.57058(8) 0.26819(5) 0.86421(5) 0.02113(16) Uani 1 1 d . . .
V2 V 0.38947(10) -0.27159(7) 0.87159(6) 0.0170(2) Uani 1 1 d . . .
N2 N 0.4514(5) 0.1517(3) 0.8988(3) 0.0223(9) Uani 1 1 d . . .
O2 O 0.7602(5) -0.1061(4) 0.7582(3) 0.0426(11) Uani 1 1 d . . .
C2 C 0.3551(6) 0.1290(4) 0.9879(4) 0.0248(12) Uani 1 1 d . . .
H2 H 0.3486 0.1536 1.0555 0.030 Uiso 1 1 calc R . .
O2W O 0.8437(5) 0.1637(3) 0.8298(3) 0.0401(10) Uani 1 1 d . . .
Cu3 Cu 0.69802(8) 0.33708(5) 0.60243(5) 0.02392(17) Uani 1 1 d . . .
V3 V 0.23766(10) -0.47383(7) 0.83755(7) 0.0213(2) Uani 1 1 d . . .
O3 O 0.5112(5) -0.2080(3) 0.7694(3) 0.0384(10) Uani 1 1 d . . .
N3 N 0.2669(5) 0.0643(3) 0.9662(3) 0.0243(10) Uani 1 1 d . . .
C3 C 0.7337(6) 0.0686(4) 0.4425(4) 0.0223(11) Uani 1 1 d . . .
H3 H 0.7142 0.0010 0.4397 0.027 Uiso 1 1 calc R . .
O4 O 0.2073(5) -0.1981(3) 0.8992(3) 0.0427(11) Uani 1 1 d . . .
N4 N 0.1365(6) 0.0329(4) 1.0369(4) 0.0453(14) Uani 1 1 d . . .
H4A H 0.1674 -0.0292 1.0706 0.054 Uiso 1 1 d R . .
H4B H 0.0851 0.0810 1.0888 0.054 Uiso 1 1 d R . .
C4 C 0.8239(6) 0.2127(4) 0.3993(4) 0.0256(12) Uani 1 1 d . . .
H4 H 0.8785 0.2622 0.3612 0.031 Uiso 1 1 calc R . .
V4 V 0.22821(10) -0.51733(7) 0.59967(7) 0.0186(2) Uani 1 1 d . . .
O5 O 0.4579(4) -0.2897(3) 0.9840(3) 0.0286(9) Uani 1 1 d . . .
C5 C 0.6962(6) 0.4610(4) 0.8819(4) 0.0267(12) Uani 1 1 d . . .
H5 H 0.6759 0.4584 0.9563 0.032 Uiso 1 1 calc R . .
N5 N 0.6719(5) 0.1351(3) 0.5235(3) 0.0209(9) Uani 1 1 d . . .
V5 V 0.15152(10) -0.75433(6) 0.56430(6) 0.0170(2) Uani 1 1 d . . .
O6 O 0.3914(4) -0.3996(3) 0.8271(3) 0.0299(9) Uani 1 1 d . . .
C6 C 0.7673(6) 0.5108(4) 0.7188(4) 0.0250(12) Uani 1 1 d . . .
H6 H 0.8056 0.5489 0.6580 0.030 Uiso 1 1 calc R . .
N6 N 0.7288(5) 0.2259(3) 0.4951(3) 0.0199(9) Uani 1 1 d . . .
O7 O 0.0966(5) -0.4292(4) 0.9441(3) 0.0383(10) Uani 1 1 d . . .
N7 N 0.8294(5) 0.1140(3) 0.3649(3) 0.0228(10) Uani 1 1 d . . .
O8 O 0.3097(5) -0.6030(3) 0.8556(4) 0.0411(11) Uani 1 1 d . . .
N8 N 0.9153(6) 0.0675(4) 0.2647(4) 0.0343(12) Uani 1 1 d . . .
H8A H 1.0207 0.0648 0.2534 0.041 Uiso 1 1 d R . .
H8B H 0.9004 0.0023 0.2665 0.041 Uiso 1 1 d R . .
N9 N 0.6670(5) 0.3939(3) 0.8235(3) 0.0201(9) Uani 1 1 d . . .
O9 O 0.1437(4) -0.4488(3) 0.7264(3) 0.0302(9) Uani 1 1 d . . .
N10 N 0.7116(5) 0.4243(3) 0.7189(3) 0.0196(9) Uani 1 1 d . . .
O10 O 0.1206(4) -0.6149(3) 0.5911(3) 0.0288(9) Uani 1 1 d . . .
N11 N 0.7603(5) 0.5353(3) 0.8195(3) 0.0224(10) Uani 1 1 d . . .
O11 O 0.7900(5) -0.2253(3) 0.5792(3) 0.0374(10) Uani 1 1 d . . .
N12 N 0.8003(5) 0.6259(4) 0.8521(4) 0.0349(12) Uani 1 1 d . . .
H12A H 0.7236 0.6613 0.9064 0.042 Uiso 1 1 d R . .
H12B H 0.8916 0.6103 0.8769 0.042 Uiso 1 1 d R . .
O12 O 0.2948(4) -0.8254(3) 0.6198(3) 0.0326(9) Uani 1 1 d . . .
O13 O 0.2032(4) -0.4253(3) 0.5041(3) 0.0229(8) Uani 1 1 d . . .
O14 O -0.0180(4) -0.7914(3) 0.6161(3) 0.0297(9) Uani 1 1 d . . .
O15 O 0.5613(4) 0.2568(2) 0.7097(2) 0.0165(7) Uani 1 1 d . . .
O16 O 0.4179(4) -0.5732(3) 0.5916(3) 0.0357(10) Uani 1 1 d . . .


_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
Cu1 O1 1.940(3) . ?
Cu1 N5 1.966(4) . ?
Cu1 N1 1.983(4) . ?
Cu1 O15 1.995(3) . ?
Cu1 O12 2.225(4) 1_565 ?
V1 O2 1.619(4) . ?
V1 O1 1.680(4) . ?
V1 O11 1.775(4) . ?
V1 O3 1.789(4) . ?
N1 C1 1.294(6) . ?
N1 N2 1.372(5) . ?
C1 N3 1.346(6) . ?
Cu2 O5 1.936(3) 2_657 ?
Cu2 N9 1.982(4) . ?
Cu2 N2 1.991(4) . ?
Cu2 O15 2.025(3) . ?
Cu2 O2W 2.383(4) . ?
V2 O4 1.606(4) . ?
V2 O5 1.676(3) . ?
V2 O3 1.767(4) . ?
V2 O6 1.773(3) . ?
N2 C2 1.308(6) . ?
C2 N3 1.346(6) . ?
Cu3 O13 1.897(3) 2_656 ?
Cu3 N10 1.972(4) . ?
Cu3 N6 1.979(4) . ?
Cu3 O15 2.000(3) . ?
V3 O7 1.630(4) . ?
V3 O8 1.647(4) . ?
V3 O9 1.789(4) . ?
V3 O6 1.802(3) . ?
N3 N4 1.398(6) . ?
C3 N5 1.313(6) . ?
C3 N7 1.337(6) . ?
C4 N6 1.302(6) . ?
C4 N7 1.357(6) . ?
V4 O16 1.616(4) . ?
V4 O13 1.663(3) . ?
V4 O10 1.765(3) . ?
V4 O9 1.806(3) . ?
O5 Cu2 1.936(3) 2_657 ?
C5 N9 1.289(6) . ?
C5 N11 1.344(7) . ?
N5 N6 1.370(5) . ?
V5 O14 1.637(3) . ?
V5 O12 1.642(4) . ?
V5 O10 1.789(3) . ?
V5 O11 1.810(4) 2_646 ?
C6 N10 1.318(6) . ?
C6 N11 1.336(7) . ?
N7 N8 1.411(5) . ?
N9 N10 1.365(6) . ?
N11 N12 1.410(6) . ?
O11 V5 1.810(4) 2_646 ?
O12 Cu1 2.225(4) 1_545 ?
O13 Cu3 1.897(3) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N5 90.43(16) . . ?
O1 Cu1 N1 91.70(15) . . ?
N5 Cu1 N1 170.66(17) . . ?
O1 Cu1 O15 165.73(14) . . ?
N5 Cu1 O15 89.27(14) . . ?
N1 Cu1 O15 86.43(14) . . ?
O1 Cu1 O12 93.77(14) . 1_565 ?
N5 Cu1 O12 97.11(16) . 1_565 ?
N1 Cu1 O12 91.82(16) . 1_565 ?
O15 Cu1 O12 100.42(14) . 1_565 ?
O2 V1 O1 107.4(2) . . ?
O2 V1 O11 109.5(2) . . ?
O1 V1 O11 110.49(18) . . ?
O2 V1 O3 108.6(2) . . ?
O1 V1 O3 107.45(18) . . ?
O11 V1 O3 113.19(19) . . ?
C1 N1 N2 108.1(4) . . ?
C1 N1 Cu1 130.1(4) . . ?
N2 N1 Cu1 121.7(3) . . ?
V1 O1 Cu1 129.6(2) . . ?
N1 C1 N3 109.2(4) . . ?
O5 Cu2 N9 92.86(16) 2_657 . ?
O5 Cu2 N2 89.65(16) 2_657 . ?
N9 Cu2 N2 173.26(17) . . ?
O5 Cu2 O15 170.71(15) 2_657 . ?
N9 Cu2 O15 89.07(14) . . ?
N2 Cu2 O15 87.48(14) . . ?
O5 Cu2 O2W 97.56(15) 2_657 . ?
N9 Cu2 O2W 85.91(16) . . ?
N2 Cu2 O2W 99.96(16) . . ?
O15 Cu2 O2W 91.64(14) . . ?
O4 V2 O5 108.4(2) . . ?
O4 V2 O3 108.9(2) . . ?
O5 V2 O3 112.09(19) . . ?
O4 V2 O6 110.4(2) . . ?
O5 V2 O6 107.71(19) . . ?
O3 V2 O6 109.36(18) . . ?
C2 N2 N1 106.9(4) . . ?
C2 N2 Cu2 130.7(3) . . ?
N1 N2 Cu2 119.9(3) . . ?
N2 C2 N3 109.3(4) . . ?
O13 Cu3 N10 91.89(16) 2_656 . ?
O13 Cu3 N6 91.20(16) 2_656 . ?
N10 Cu3 N6 166.44(17) . . ?
O13 Cu3 O15 171.09(14) 2_656 . ?
N10 Cu3 O15 89.78(15) . . ?
N6 Cu3 O15 89.20(14) . . ?
O7 V3 O8 107.8(2) . . ?
O7 V3 O9 106.87(19) . . ?
O8 V3 O9 111.9(2) . . ?
O7 V3 O6 106.13(18) . . ?
O8 V3 O6 111.41(19) . . ?
O9 V3 O6 112.29(18) . . ?
V2 O3 V1 168.9(3) . . ?
C1 N3 C2 106.4(4) . . ?
C1 N3 N4 126.0(4) . . ?
C2 N3 N4 126.9(4) . . ?
N5 C3 N7 108.9(4) . . ?
N6 C4 N7 108.0(4) . . ?
O16 V4 O13 111.95(19) . . ?
O16 V4 O10 110.40(19) . . ?
O13 V4 O10 109.19(17) . . ?
O16 V4 O9 108.88(19) . . ?
O13 V4 O9 106.84(18) . . ?
O10 V4 O9 109.50(18) . . ?
V2 O5 Cu2 151.6(2) . 2_657 ?
N9 C5 N11 110.1(5) . . ?
C3 N5 N6 107.2(4) . . ?
C3 N5 Cu1 130.9(4) . . ?
N6 N5 Cu1 121.8(3) . . ?
O14 V5 O12 108.95(19) . . ?
O14 V5 O10 108.72(18) . . ?
O12 V5 O10 109.84(18) . . ?
O14 V5 O11 110.30(19) . 2_646 ?
O12 V5 O11 109.80(19) . 2_646 ?
O10 V5 O11 109.21(18) . 2_646 ?
V2 O6 V3 133.9(2) . . ?
N10 C6 N11 109.6(5) . . ?
C4 N6 N5 108.5(4) . . ?
C4 N6 Cu3 129.5(3) . . ?
N5 N6 Cu3 120.9(3) . . ?
C3 N7 C4 107.4(4) . . ?
C3 N7 N8 125.4(4) . . ?
C4 N7 N8 127.1(4) . . ?
C5 N9 N10 107.8(4) . . ?
C5 N9 Cu2 130.7(4) . . ?
N10 N9 Cu2 121.4(3) . . ?
V3 O9 V4 123.7(2) . . ?
C6 N10 N9 106.7(4) . . ?
C6 N10 Cu3 132.5(4) . . ?
N9 N10 Cu3 120.7(3) . . ?
V4 O10 V5 141.6(2) . . ?
C6 N11 C5 105.8(4) . . ?
C6 N11 N12 126.2(5) . . ?
C5 N11 N12 127.9(4) . . ?
V1 O11 V5 145.2(2) . 2_646 ?
V5 O12 Cu1 160.9(2) . 1_545 ?
V4 O13 Cu3 146.7(2) . 2_656 ?
Cu1 O15 Cu3 118.38(15) . . ?
Cu1 O15 Cu2 116.98(15) . . ?
Cu3 O15 Cu2 115.68(14) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.125


