# Electronic Supplementary Material (ESI) for RSC Advances.
# 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 1045303'
_audit_update_record             
;
2015-04-27 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H64 Cr2 Cu3 Mo12 N12 O64'
_chemical_formula_weight         3014.79

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                   10.6780(6)
_cell_length_b                   13.4480(8)
_cell_length_c                   14.0150(8)
_cell_angle_alpha                105.5870(10)
_cell_angle_beta                 102.5660(10)
_cell_angle_gamma                93.5890(11)
_cell_volume                     1876.32(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      25.00

_exptl_crystal_description       LATH
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1455
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5052
_exptl_absorpt_correction_T_max  0.5998
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10737
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6592
_reflns_number_gt                5292
_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)+(0.0483P)²+14.4772P] 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         6592
_refine_ls_number_parameters     508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Cr Cr 0.25290(10) 0.13204(8) 0.43914(8) 0.0106(2) Uani 1 1 d . . .
Mo1 Mo 0.28664(5) -0.11533(4) 0.35465(4) 0.01350(15) Uani 1 1 d . . .
Cu1 Cu 0.03394(9) 0.46670(8) 0.68971(7) 0.0267(2) Uani 1 1 d . . .
O1 O 0.0897(5) 0.3007(4) 0.7064(4) 0.0259(12) Uani 1 1 d . . .
C1 C -0.1840(7) 0.3497(6) 0.5127(5) 0.0207(16) Uani 1 1 d . . .
H1A H -0.1259 0.3406 0.4712 0.025 Uiso 1 1 calc R . .
N1 N -0.1437(6) 0.4045(5) 0.6109(5) 0.0204(13) Uani 1 1 d . . .
O1W O 0.1863(7) 0.5566(6) 0.7809(5) 0.0525(18) Uiso 1 1 d . . .
Mo2 Mo 0.23168(5) -0.02314(5) 0.58684(4) 0.01362(15) Uani 1 1 d . . .
O2 O 0.1068(5) 0.4426(4) 0.5727(4) 0.0241(12) Uani 1 1 d . . .
C2 C -0.3596(7) 0.3782(6) 0.6261(6) 0.0254(17) Uani 1 1 d . . .
H2A H -0.4191 0.3912 0.6662 0.030 Uiso 1 1 calc R . .
N2 N -0.3998(6) 0.3215(5) 0.5279(5) 0.0233(14) Uani 1 1 d . . .
Cu2 Cu -0.5000 1.0000 1.0000 0.0236(3) Uani 1 2 d S . .
O2W O -0.0110(7) 0.7586(6) 1.1283(5) 0.0525(18) Uiso 1 1 d . . .
Mo3 Mo 0.20772(6) 0.22756(5) 0.67158(4) 0.01557(15) Uani 1 1 d . . .
N3 N -0.3248(6) 1.0443(5) 1.0883(4) 0.0200(13) Uani 1 1 d . . .
O3 O -0.0478(5) 0.4978(4) 0.8025(4) 0.0295(13) Uani 1 1 d . . .
C3 C -0.2302(7) 0.4177(5) 0.6685(5) 0.0191(15) Uani 1 1 d . . .
O3W O -0.5964(7) 0.7467(6) 1.1095(6) 0.065(2) Uiso 1 1 d . . .
Mo4 Mo 0.23216(6) 0.38358(5) 0.52539(5) 0.01579(15) Uani 1 1 d . . .
O4 O -0.4450(5) 0.8606(4) 0.9846(4) 0.0238(12) Uani 1 1 d . . .
N4 N -0.0786(6) 1.0817(5) 1.2108(5) 0.0269(15) Uani 1 1 d . . .
C4 C -0.1692(7) 0.4721(6) 0.7792(6) 0.0222(16) Uani 1 1 d . . .
O4W O 0.1837(8) 0.6772(6) 0.9607(6) 0.069(2) Uiso 1 1 d . . .
Mo5 Mo 0.29621(6) 0.03994(5) 0.20050(4) 0.01596(15) Uani 1 1 d . . .
N5 N -0.2724(6) 0.7772(5) 1.0221(5) 0.0219(14) Uani 1 1 d . . .
H5C H -0.1903 0.7819 1.0465 0.026 Uiso 1 1 calc R . .
C5 C -0.1778(7) 0.5483(6) 0.9546(5) 0.0260(17) Uani 1 1 d . . .
H5A H -0.1158 0.6061 0.9584 0.031 Uiso 1 1 calc R . .
H5B H -0.1317 0.5020 0.9877 0.031 Uiso 1 1 calc R . .
O5W O -0.5049(8) 0.4333(6) 0.8245(6) 0.065(2) Uiso 1 1 d . . .
O5 O 0.4173(5) -0.0146(4) 0.1510(4) 0.0260(12) Uani 1 1 d . . .
Mo6 Mo 0.26315(6) 0.28707(5) 0.29099(5) 0.01760(16) Uani 1 1 d . . .
O6 O 0.1556(4) -0.0035(3) 0.4252(3) 0.0144(10) Uani 1 1 d . . .
N6 N -0.2376(6) 0.4921(5) 0.8469(5) 0.0229(14) Uani 1 1 d . . .
H6C H -0.3195 0.4720 0.8283 0.028 Uiso 1 1 calc R . .
C6 C -0.2792(8) 0.5887(6) 1.0091(5) 0.0251(17) Uani 1 1 d . . .
H6A H -0.2389 0.6161 1.0816 0.030 Uiso 1 1 calc R . .
H6B H -0.3438 0.5309 1.0003 0.030 Uiso 1 1 calc R . .
O6W O -0.3938(8) 1.3518(7) 1.2561(7) 0.077(2) Uiso 1 1 d . . .
O7 O 0.3289(4) 0.1276(4) 0.5796(3) 0.0149(10) Uani 1 1 d . . .
C7 C -0.3474(7) 0.6736(6) 0.9733(6) 0.0261(17) Uani 1 1 d . . .
H7A H -0.3610 0.6578 0.8998 0.031 Uiso 1 1 calc R . .
H7B H -0.4315 0.6742 0.9889 0.031 Uiso 1 1 calc R . .
O8 O 0.1330(4) 0.2171(3) 0.5040(3) 0.0140(10) Uani 1 1 d . . .
C8 C -0.3268(7) 0.8617(6) 1.0294(5) 0.0181(15) Uani 1 1 d . . .
O9 O 0.1738(4) 0.1336(4) 0.3006(3) 0.0140(10) Uani 1 1 d . . .
C9 C -0.2546(6) 0.9655(6) 1.0933(5) 0.0187(15) Uani 1 1 d . . .
C10 C -0.1324(7) 0.9846(6) 1.1546(5) 0.0243(17) Uani 1 1 d . . .
H10A H -0.0851 0.9292 1.1578 0.029 Uiso 1 1 calc R . .
O10 O 0.1242(4) 0.0857(4) 0.6287(4) 0.0172(10) Uani 1 1 d . . .
O11 O 0.3301(5) -0.0174(4) 0.7005(4) 0.0245(12) Uani 1 1 d . . .
C11 C -0.2731(7) 1.1395(6) 1.1435(6) 0.0281(18) Uani 1 1 d . . .
H46A H -0.3203 1.1948 1.1406 0.034 Uiso 1 1 calc R . .
O12 O 0.1161(5) -0.1282(4) 0.5612(4) 0.0238(12) Uani 1 1 d . . .
C12 C -0.1485(8) 1.1579(7) 1.2061(6) 0.0325(19) Uani 1 1 d . . .
H54A H -0.1141 1.2255 1.2453 0.039 Uiso 1 1 calc R . .
O13 O 0.3477(4) -0.0803(4) 0.5023(3) 0.0165(10) Uani 1 1 d . . .
C13 C -0.3123(7) 0.3062(6) 0.4725(6) 0.0231(17) Uani 1 1 d . . .
H15A H -0.3380 0.2652 0.4048 0.028 Uiso 1 1 calc R . .
O14 O 0.1725(5) -0.2181(4) 0.3296(4) 0.0239(12) Uani 1 1 d . . .
O15 O 0.4211(5) -0.1696(4) 0.3264(4) 0.0229(11) Uani 1 1 d . . .
O16 O 0.2163(4) -0.0754(4) 0.2335(3) 0.0173(10) Uani 1 1 d . . .
O17 O 0.3788(4) 0.0503(3) 0.3770(3) 0.0143(10) Uani 1 1 d . . .
O18 O 0.1794(5) 0.0389(4) 0.0955(4) 0.0252(12) Uani 1 1 d . . .
O19 O 0.3727(5) 0.1828(4) 0.2472(4) 0.0191(11) Uani 1 1 d . . .
O20 O 0.3452(4) 0.2670(4) 0.4494(3) 0.0142(10) Uani 1 1 d . . .
O21 O 0.1568(5) 0.3508(4) 0.3838(4) 0.0214(11) Uani 1 1 d . . .
O22 O 0.3737(5) 0.3916(4) 0.3094(4) 0.0292(13) Uani 1 1 d . . .
O23 O 0.3495(5) 0.4829(4) 0.5445(4) 0.0251(12) Uani 1 1 d . . .
O25 O 0.3073(4) 0.3379(4) 0.6409(4) 0.0180(10) Uani 1 1 d . . .
O26 O 0.3131(5) 0.2307(4) 0.7827(4) 0.0280(13) Uani 1 1 d . . .
O28 O 0.1542(5) 0.2779(4) 0.1800(4) 0.0295(13) 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
Cr O9 1.948(5) . ?
Cr O20 1.965(5) . ?
Cr O8 1.976(4) . ?
Cr O7 1.978(5) . ?
Cr O6 1.981(5) . ?
Cr O17 1.988(4) . ?
Mo1 O14 1.691(5) . ?
Mo1 O15 1.725(5) . ?
Mo1 O16 1.928(5) . ?
Mo1 O13 1.945(5) . ?
Mo1 O17 2.289(4) . ?
Mo1 O6 2.295(4) . ?
Cu1 O2 1.923(5) . ?
Cu1 O3 1.931(5) . ?
Cu1 O1W 1.939(7) . ?
Cu1 N1 1.977(6) . ?
Cu1 O1 2.404(6) . ?
O1 Mo3 1.721(5) . ?
C1 N1 1.335(9) . ?
C1 C13 1.387(10) . ?
N1 C3 1.344(9) . ?
Mo2 O11 1.686(5) . ?
Mo2 O12 1.722(5) . ?
Mo2 O13 1.948(4) . ?
Mo2 O10 1.961(5) . ?
Mo2 O7 2.256(5) . ?
Mo2 O6 2.326(5) . ?
O2 Mo4 1.761(5) . ?
C2 N2 1.341(10) . ?
C2 C3 1.388(10) . ?
N2 C13 1.332(10) . ?
Cu2 N3 1.961(6) 2_477 ?
Cu2 N3 1.961(6) . ?
Cu2 O4 1.970(5) 2_477 ?
Cu2 O4 1.970(5) . ?
Mo3 O26 1.699(5) . ?
Mo3 O10 1.932(5) . ?
Mo3 O25 1.966(5) . ?
Mo3 O7 2.271(4) . ?
Mo3 O8 2.273(5) . ?
N3 C11 1.317(10) . ?
N3 C9 1.343(9) . ?
O3 C4 1.267(9) . ?
C3 C4 1.502(10) . ?
Mo4 O23 1.696(5) . ?
Mo4 O21 1.890(5) . ?
Mo4 O25 1.916(5) . ?
Mo4 O20 2.225(5) . ?
Mo4 O8 2.330(5) . ?
O4 C8 1.279(8) . ?
N4 C12 1.312(11) . ?
N4 C10 1.347(10) . ?
C4 N6 1.302(9) . ?
Mo5 O18 1.706(5) . ?
Mo5 O5 1.711(5) . ?
Mo5 O19 1.919(5) . ?
Mo5 O16 1.935(5) . ?
Mo5 O9 2.306(4) . ?
Mo5 O17 2.402(5) . ?
N5 C8 1.298(9) . ?
N5 C7 1.469(9) . ?
C5 N6 1.471(9) . ?
C5 C6 1.504(10) . ?
Mo6 O28 1.696(5) . ?
Mo6 O22 1.704(5) . ?
Mo6 O19 1.941(5) . ?
Mo6 O21 1.970(5) . ?
Mo6 O9 2.269(4) . ?
Mo6 O20 2.296(5) . ?
C6 C7 1.530(11) . ?
C8 C9 1.497(10) . ?
C9 C10 1.363(10) . ?
C11 C12 1.391(11) . ?

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 Cr O20 83.84(19) . . ?
O9 Cr O8 95.66(19) . . ?
O20 Cr O8 84.43(19) . . ?
O9 Cr O7 178.33(19) . . ?
O20 Cr O7 97.71(19) . . ?
O8 Cr O7 83.89(19) . . ?
O9 Cr O6 94.47(19) . . ?
O20 Cr O6 178.2(2) . . ?
O8 Cr O6 95.08(19) . . ?
O7 Cr O6 83.97(19) . . ?
O9 Cr O17 85.39(19) . . ?
O20 Cr O17 93.95(19) . . ?
O8 Cr O17 177.95(19) . . ?
O7 Cr O17 95.11(19) . . ?
O6 Cr O17 86.58(18) . . ?
O14 Mo1 O15 104.8(2) . . ?
O14 Mo1 O16 96.0(2) . . ?
O15 Mo1 O16 102.0(2) . . ?
O14 Mo1 O13 101.7(2) . . ?
O15 Mo1 O13 96.4(2) . . ?
O16 Mo1 O13 150.2(2) . . ?
O14 Mo1 O17 160.3(2) . . ?
O15 Mo1 O17 93.0(2) . . ?
O16 Mo1 O17 71.78(18) . . ?
O13 Mo1 O17 84.16(18) . . ?
O14 Mo1 O6 90.9(2) . . ?
O15 Mo1 O6 162.5(2) . . ?
O16 Mo1 O6 83.69(18) . . ?
O13 Mo1 O6 72.38(17) . . ?
O17 Mo1 O6 72.83(16) . . ?
O2 Cu1 O3 175.5(2) . . ?
O2 Cu1 O1W 93.7(3) . . ?
O3 Cu1 O1W 87.6(3) . . ?
O2 Cu1 N1 95.2(2) . . ?
O3 Cu1 N1 82.7(2) . . ?
O1W Cu1 N1 165.7(3) . . ?
O2 Cu1 O1 88.4(2) . . ?
O3 Cu1 O1 95.7(2) . . ?
O1W Cu1 O1 100.0(3) . . ?
N1 Cu1 O1 91.5(2) . . ?
Mo3 O1 Cu1 132.8(3) . . ?
N1 C1 C13 120.0(7) . . ?
C1 N1 C3 118.6(6) . . ?
C1 N1 Cu1 128.5(5) . . ?
C3 N1 Cu1 112.8(5) . . ?
O11 Mo2 O12 105.1(3) . . ?
O11 Mo2 O13 97.1(2) . . ?
O12 Mo2 O13 102.3(2) . . ?
O11 Mo2 O10 100.9(2) . . ?
O12 Mo2 O10 97.1(2) . . ?
O13 Mo2 O10 149.1(2) . . ?
O11 Mo2 O7 93.8(2) . . ?
O12 Mo2 O7 160.0(2) . . ?
O13 Mo2 O7 81.38(18) . . ?
O10 Mo2 O7 72.52(17) . . ?
O11 Mo2 O6 161.6(2) . . ?
O12 Mo2 O6 91.6(2) . . ?
O13 Mo2 O6 71.61(18) . . ?
O10 Mo2 O6 84.06(18) . . ?
O7 Mo2 O6 70.61(16) . . ?
Mo4 O2 Cu1 141.1(3) . . ?
N2 C2 C3 120.7(7) . . ?
C13 N2 C2 117.9(6) . . ?
N3 Cu2 N3 179.998(1) 2_477 . ?
N3 Cu2 O4 82.6(2) 2_477 2_477 ?
N3 Cu2 O4 97.4(2) . 2_477 ?
N3 Cu2 O4 97.4(2) 2_477 . ?
N3 Cu2 O4 82.6(2) . . ?
O4 Cu2 O4 179.999(2) 2_477 . ?
O26 Mo3 O1 105.7(3) . . ?
O26 Mo3 O10 101.1(2) . . ?
O1 Mo3 O10 104.0(2) . . ?
O26 Mo3 O25 96.7(2) . . ?
O1 Mo3 O25 95.9(2) . . ?
O10 Mo3 O25 148.46(19) . . ?
O26 Mo3 O7 90.9(2) . . ?
O1 Mo3 O7 163.4(2) . . ?
O10 Mo3 O7 72.68(17) . . ?
O25 Mo3 O7 81.22(18) . . ?
O26 Mo3 O8 159.5(2) . . ?
O1 Mo3 O8 92.4(2) . . ?
O10 Mo3 O8 83.45(18) . . ?
O25 Mo3 O8 71.38(17) . . ?
O7 Mo3 O8 71.14(16) . . ?
C11 N3 C9 118.7(6) . . ?
C11 N3 Cu2 127.4(5) . . ?
C9 N3 Cu2 113.9(5) . . ?
C4 O3 Cu1 115.5(5) . . ?
N1 C3 C2 120.7(7) . . ?
N1 C3 C4 112.8(6) . . ?
C2 C3 C4 126.4(7) . . ?
O23 Mo4 O2 105.3(2) . . ?
O23 Mo4 O21 102.5(2) . . ?
O2 Mo4 O21 99.5(2) . . ?
O23 Mo4 O25 97.5(2) . . ?
O2 Mo4 O25 97.8(2) . . ?
O21 Mo4 O25 149.0(2) . . ?
O23 Mo4 O20 92.0(2) . . ?
O2 Mo4 O20 162.6(2) . . ?
O21 Mo4 O20 73.95(19) . . ?
O25 Mo4 O20 81.94(18) . . ?
O23 Mo4 O8 160.3(2) . . ?
O2 Mo4 O8 92.3(2) . . ?
O21 Mo4 O8 82.79(19) . . ?
O25 Mo4 O8 70.90(18) . . ?
O20 Mo4 O8 71.06(16) . . ?
C8 O4 Cu2 113.9(5) . . ?
C12 N4 C10 117.8(7) . . ?
O3 C4 N6 122.1(7) . . ?
O3 C4 C3 116.1(6) . . ?
N6 C4 C3 121.8(6) . . ?
O18 Mo5 O5 104.0(2) . . ?
O18 Mo5 O19 101.6(2) . . ?
O5 Mo5 O19 98.7(2) . . ?
O18 Mo5 O16 98.3(2) . . ?
O5 Mo5 O16 101.4(2) . . ?
O19 Mo5 O16 147.2(2) . . ?
O18 Mo5 O9 88.4(2) . . ?
O5 Mo5 O9 166.1(2) . . ?
O19 Mo5 O9 72.19(17) . . ?
O16 Mo5 O9 82.63(18) . . ?
O18 Mo5 O17 155.0(2) . . ?
O5 Mo5 O17 99.8(2) . . ?
O19 Mo5 O17 82.18(18) . . ?
O16 Mo5 O17 69.13(17) . . ?
O9 Mo5 O17 69.05(16) . . ?
C8 N5 C7 121.7(6) . . ?
N6 C5 C6 110.5(6) . . ?
O28 Mo6 O22 105.6(3) . . ?
O28 Mo6 O19 102.1(2) . . ?
O22 Mo6 O19 95.7(2) . . ?
O28 Mo6 O21 97.0(2) . . ?
O22 Mo6 O21 100.0(2) . . ?
O19 Mo6 O21 150.9(2) . . ?
O28 Mo6 O9 92.2(2) . . ?
O22 Mo6 O9 160.6(2) . . ?
O19 Mo6 O9 72.67(17) . . ?
O21 Mo6 O9 85.03(19) . . ?
O28 Mo6 O20 158.8(2) . . ?
O22 Mo6 O20 93.9(2) . . ?
O19 Mo6 O20 83.78(19) . . ?
O21 Mo6 O20 70.93(18) . . ?
O9 Mo6 O20 69.87(16) . . ?
Cr O6 Mo1 100.32(18) . . ?
Cr O6 Mo2 101.43(18) . . ?
Mo1 O6 Mo2 92.95(17) . . ?
C4 N6 C5 121.5(6) . . ?
C5 C6 C7 114.9(6) . . ?
Cr O7 Mo2 103.99(19) . . ?
Cr O7 Mo3 102.5(2) . . ?
Mo2 O7 Mo3 93.85(16) . . ?
N5 C7 C6 112.0(6) . . ?
Cr O8 Mo3 102.5(2) . . ?
Cr O8 Mo4 100.22(18) . . ?
Mo3 O8 Mo4 92.98(16) . . ?
O4 C8 N5 122.2(7) . . ?
O4 C8 C9 116.5(6) . . ?
N5 C8 C9 121.3(6) . . ?
Cr O9 Mo6 103.91(19) . . ?
Cr O9 Mo5 105.1(2) . . ?
Mo6 O9 Mo5 92.13(16) . . ?
N3 C9 C10 120.2(7) . . ?
N3 C9 C8 112.9(6) . . ?
C10 C9 C8 126.9(7) . . ?
N4 C10 C9 121.4(8) . . ?
Mo3 O10 Mo2 116.2(2) . . ?
N3 C11 C12 120.6(8) . . ?
N4 C12 C11 121.2(8) . . ?
Mo1 O13 Mo2 118.8(2) . . ?
N2 C13 C1 121.9(7) . . ?
Mo1 O16 Mo5 123.1(2) . . ?
Cr O17 Mo1 100.27(18) . . ?
Cr O17 Mo5 100.44(19) . . ?
Mo1 O17 Mo5 92.72(16) . . ?
Mo5 O19 Mo6 117.2(2) . . ?
Cr O20 Mo4 104.27(19) . . ?
Cr O20 Mo6 102.37(19) . . ?
Mo4 O20 Mo6 93.36(17) . . ?
Mo4 O21 Mo6 116.9(2) . . ?
Mo4 O25 Mo3 118.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         5.502
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.181



####################################################################### 
# 
# 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_liu
_database_code_depnum_ccdc_archive 'CCDC 1045304'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H16 Cu Mo4 N6 O16'
_chemical_formula_weight         959.62

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   'P2(1)/n  '

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

_cell_length_a                   10.6557(4)
_cell_length_b                   13.8735(6)
_cell_length_c                   17.0837(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.7230(10)
_cell_angle_gamma                90.00
_cell_volume                     2489.24(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1844
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5320
_exptl_absorpt_correction_T_max  0.6550
_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            12264
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4388
_reflns_number_gt                3996
_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)+(0.0238P)²+3.1286P] 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         4388
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0503
_refine_ls_wR_factor_gt          0.0491
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_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 -0.37114(4) 0.85355(3) 0.22530(2) 0.03027(10) Uani 1 1 d . . .
Mo1 Mo -0.16609(2) 1.018992(19) 0.487769(14) 0.02106(7) Uani 1 1 d . . .
O1W O 0.0813(5) 0.9402(4) 0.1134(3) 0.147(2) Uani 1 1 d . . .
N1 N -0.3360(2) 0.92116(19) 0.12996(14) 0.0277(6) Uani 1 1 d . . .
O1 O -0.2468(2) 0.76146(16) 0.19647(12) 0.0304(5) Uani 1 1 d . . .
Mo2 Mo -0.05009(2) 0.982887(19) 0.329392(14) 0.02461(7) Uani 1 1 d . . .
N2 N -0.2634(3) 0.9969(2) -0.00519(17) 0.0438(7) Uani 1 1 d . . .
O2 O -0.1953(2) 0.93234(17) 0.29574(12) 0.0370(5) Uani 1 1 d . . .
Mo3 Mo -0.05814(3) 1.22459(2) 0.596775(16) 0.03103(8) Uani 1 1 d . . .
N3 N -0.0962(3) 0.7459(2) 0.11989(17) 0.0399(7) Uani 1 1 d . . .
H3A H -0.0659 0.7669 0.0795 0.048 Uiso 1 1 calc R . .
O3 O -0.0048(2) 0.45058(17) 0.25360(13) 0.0371(5) Uani 1 1 d . . .
O4 O -0.0157(2) 1.04904(18) 0.25234(13) 0.0418(6) Uani 1 1 d . . .
Mo4 Mo 0.06139(2) 1.182943(19) 0.435615(14) 0.02525(7) Uani 1 1 d . . .
N4 N 0.1374(3) 0.4870(2) 0.17470(17) 0.0394(7) Uani 1 1 d . . .
H4A H 0.1753 0.4684 0.1367 0.047 Uiso 1 1 calc R . .
N5 N -0.0796(2) 0.29108(19) 0.18082(14) 0.0282(6) Uani 1 1 d . . .
O5 O -0.11470(18) 1.08216(14) 0.39694(11) 0.0242(4) Uani 1 1 d . . .
N6 N 0.0060(3) 0.2304(2) 0.04440(19) 0.0486(8) Uani 1 1 d . . .
O6 O -0.3071(2) 0.96848(17) 0.44886(13) 0.0374(5) Uani 1 1 d . . .
O7 O -0.20906(19) 1.12467(16) 0.53305(13) 0.0324(5) Uani 1 1 d . . .
O8 O -0.0608(2) 1.12230(16) 0.67303(12) 0.0329(5) Uani 1 1 d . . .
O9 O -0.1709(3) 1.30195(19) 0.61863(15) 0.0542(7) Uani 1 1 d . . .
C10 C -0.3874(3) 1.0028(2) 0.09839(19) 0.0368(8) Uani 1 1 d . . .
H10A H -0.4484 1.0347 0.1217 0.044 Uiso 1 1 calc R . .
O10 O 0.0825(2) 1.27603(18) 0.63616(14) 0.0469(6) Uani 1 1 d . . .
O11 O 0.03830(17) 1.08283(14) 0.54266(10) 0.0218(4) Uani 1 1 d . . .
O12 O -0.0537(2) 1.25363(15) 0.48688(12) 0.0316(5) Uani 1 1 d . . .
C12 C -0.0757(3) 0.1800(3) 0.0777(2) 0.0473(9) Uani 1 1 d . . .
H12A H -0.1041 0.1214 0.0549 0.057 Uiso 1 1 calc R . .
O13 O 0.2029(2) 1.22746(18) 0.48143(14) 0.0406(6) Uani 1 1 d . . .
O14 O 0.0361(2) 1.23643(18) 0.34444(13) 0.0405(6) Uani 1 1 d . . .
O15 O 0.12364(18) 1.05224(15) 0.41165(11) 0.0251(4) Uani 1 1 d . . .
C22 C -0.2466(3) 0.8782(2) 0.09584(17) 0.0275(7) Uani 1 1 d . . .
C23 C -0.2124(3) 0.9165(3) 0.0280(2) 0.0375(8) Uani 1 1 d . . .
H23A H -0.1513 0.8848 0.0047 0.045 Uiso 1 1 calc R . .
C26 C 0.0079(3) 0.3419(2) 0.15007(19) 0.0322(7) Uani 1 1 d . . .
C27 C 0.1752(3) 0.5800(3) 0.2135(2) 0.0415(8) Uani 1 1 d . . .
H27A H 0.2666 0.5879 0.2178 0.050 Uiso 1 1 calc R . .
H27B H 0.1552 0.5794 0.2668 0.050 Uiso 1 1 calc R . .
C30 C -0.1951(3) 0.7896(2) 0.14034(18) 0.0292(7) Uani 1 1 d . . .
C31 C 0.1090(3) 0.6647(3) 0.1684(2) 0.0470(9) Uani 1 1 d . . .
H31A H 0.1284 0.6648 0.1149 0.056 Uiso 1 1 calc R . .
H31B H 0.1418 0.7240 0.1941 0.056 Uiso 1 1 calc R . .
C32 C -0.0352(3) 0.6620(3) 0.1639(2) 0.0425(8) Uani 1 1 d . . .
H32A H -0.0687 0.6031 0.1377 0.051 Uiso 1 1 calc R . .
H32B H -0.0552 0.6618 0.2172 0.051 Uiso 1 1 calc R . .
C35 C 0.0470(3) 0.3119(3) 0.0813(2) 0.0473(10) Uani 1 1 d . . .
H35A H 0.1043 0.3501 0.0597 0.057 Uiso 1 1 calc R . .
C36 C 0.0489(3) 0.4312(2) 0.19516(19) 0.0321(7) Uani 1 1 d . . .
C37 C -0.1218(3) 0.2098(3) 0.1454(2) 0.0368(8) Uani 1 1 d . . .
H37A H -0.1818 0.1728 0.1655 0.044 Uiso 1 1 calc R . .
C40 C -0.3500(4) 1.0401(3) 0.0310(2) 0.0426(8) Uani 1 1 d . . .
H40A H -0.3864 1.0975 0.0100 0.051 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 O1 1.962(2) . ?
Cu1 O3 1.963(2) 2_455 ?
Cu1 N1 1.969(2) . ?
Cu1 N5 1.971(3) 2_455 ?
Cu1 O2 2.322(2) . ?
Mo1 O6 1.689(2) . ?
Mo1 O7 1.754(2) . ?
Mo1 O5 1.9398(19) . ?
Mo1 O15 1.9675(19) 3_576 ?
Mo1 O11 2.0878(19) 3_576 ?
Mo1 O11 2.3911(18) . ?
Mo1 Mo2 3.1983(3) . ?
Mo1 Mo4 3.2114(4) 3_576 ?
N1 C10 1.332(4) . ?
N1 C22 1.338(4) . ?
O1 C30 1.246(4) . ?
Mo2 O4 1.695(2) . ?
Mo2 O2 1.708(2) . ?
Mo2 O8 1.882(2) 3_576 ?
Mo2 O5 1.9926(19) . ?
Mo2 O15 2.334(2) . ?
Mo2 O11 2.3521(18) 3_576 ?
N2 C23 1.326(5) . ?
N2 C40 1.336(5) . ?
Mo3 O10 1.693(2) . ?
Mo3 O9 1.699(2) . ?
Mo3 O12 1.929(2) . ?
Mo3 O8 1.930(2) . ?
Mo3 O7 2.259(2) . ?
Mo3 O11 2.4698(19) . ?
N3 C30 1.314(4) . ?
N3 C32 1.476(4) . ?
O3 C36 1.260(4) . ?
O3 Cu1 1.963(2) 2_445 ?
Mo4 O13 1.694(2) . ?
Mo4 O14 1.705(2) . ?
Mo4 O12 1.896(2) . ?
Mo4 O15 1.997(2) . ?
Mo4 O11 2.3422(18) . ?
Mo4 O5 2.3438(19) . ?
Mo4 Mo1 3.2115(4) 3_576 ?
N4 C36 1.313(4) . ?
N4 C27 1.475(4) . ?
N5 C37 1.322(4) . ?
N5 C26 1.344(4) . ?
N5 Cu1 1.971(3) 2_445 ?
N6 C12 1.319(5) . ?
N6 C35 1.332(5) . ?
O8 Mo2 1.882(2) 3_576 ?
C10 C40 1.381(5) . ?
O11 Mo1 2.0878(19) 3_576 ?
O11 Mo2 2.3520(18) 3_576 ?
C12 C37 1.393(5) . ?
O15 Mo1 1.9676(19) 3_576 ?
C22 C23 1.379(4) . ?
C22 C30 1.499(4) . ?
C26 C35 1.375(5) . ?
C26 C36 1.485(5) . ?
C27 C31 1.513(5) . ?
C31 C32 1.525(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O3 175.64(9) . 2_455 ?
O1 Cu1 N1 82.63(10) . . ?
O3 Cu1 N1 93.06(10) 2_455 . ?
O1 Cu1 N5 101.66(10) . 2_455 ?
O3 Cu1 N5 82.63(10) 2_455 2_455 ?
N1 Cu1 N5 175.21(10) . 2_455 ?
O1 Cu1 O2 85.22(9) . . ?
O3 Cu1 O2 95.26(9) 2_455 . ?
N1 Cu1 O2 87.41(9) . . ?
N5 Cu1 O2 95.04(9) 2_455 . ?
O6 Mo1 O7 103.85(11) . . ?
O6 Mo1 O5 103.01(10) . . ?
O7 Mo1 O5 96.04(9) . . ?
O6 Mo1 O15 101.15(10) . 3_576 ?
O7 Mo1 O15 94.20(9) . 3_576 ?
O5 Mo1 O15 150.60(8) . 3_576 ?
O6 Mo1 O11 101.27(10) . 3_576 ?
O7 Mo1 O11 154.83(9) . 3_576 ?
O5 Mo1 O11 79.77(8) . 3_576 ?
O15 Mo1 O11 79.29(8) 3_576 3_576 ?
O6 Mo1 O11 177.16(10) . . ?
O7 Mo1 O11 78.80(8) . . ?
O5 Mo1 O11 77.58(7) . . ?
O15 Mo1 O11 77.51(7) 3_576 . ?
O11 Mo1 O11 76.06(8) 3_576 . ?
O6 Mo1 Mo2 92.71(8) . . ?
O7 Mo1 Mo2 132.14(7) . . ?
O5 Mo1 Mo2 36.13(6) . . ?
O15 Mo1 Mo2 126.55(6) 3_576 . ?
O11 Mo1 Mo2 47.30(5) 3_576 . ?
O11 Mo1 Mo2 86.17(4) . . ?
O6 Mo1 Mo4 91.33(8) . 3_576 ?
O7 Mo1 Mo4 130.39(7) . 3_576 ?
O5 Mo1 Mo4 126.48(6) . 3_576 ?
O15 Mo1 Mo4 36.21(6) 3_576 3_576 ?
O11 Mo1 Mo4 46.76(5) 3_576 3_576 ?
O11 Mo1 Mo4 86.13(5) . 3_576 ?
Mo2 Mo1 Mo4 92.917(9) . 3_576 ?
C10 N1 C22 118.5(3) . . ?
C10 N1 Cu1 128.1(2) . . ?
C22 N1 Cu1 113.4(2) . . ?
C30 O1 Cu1 113.2(2) . . ?
O4 Mo2 O2 105.28(11) . . ?
O4 Mo2 O8 100.60(11) . 3_576 ?
O2 Mo2 O8 102.16(11) . 3_576 ?
O4 Mo2 O5 102.51(10) . . ?
O2 Mo2 O5 95.55(10) . . ?
O8 Mo2 O5 145.90(8) 3_576 . ?
O4 Mo2 O15 89.47(10) . . ?
O2 Mo2 O15 162.43(9) . . ?
O8 Mo2 O15 84.03(8) 3_576 . ?
O5 Mo2 O15 71.52(7) . . ?
O4 Mo2 O11 161.27(10) . 3_576 ?
O2 Mo2 O11 93.26(9) . 3_576 ?
O8 Mo2 O11 77.57(8) 3_576 3_576 ?
O5 Mo2 O11 72.49(7) . 3_576 ?
O15 Mo2 O11 71.81(7) . 3_576 ?
O4 Mo2 Mo1 137.51(9) . . ?
O2 Mo2 Mo1 83.77(7) . . ?
O8 Mo2 Mo1 118.27(6) 3_576 . ?
O5 Mo2 Mo1 35.03(6) . . ?
O15 Mo2 Mo1 78.85(5) . . ?
O11 Mo2 Mo1 40.72(5) 3_576 . ?
C23 N2 C40 116.4(3) . . ?
Mo2 O2 Cu1 166.84(13) . . ?
O10 Mo3 O9 104.92(14) . . ?
O10 Mo3 O12 97.65(10) . . ?
O9 Mo3 O12 102.52(11) . . ?
O10 Mo3 O8 98.88(11) . . ?
O9 Mo3 O8 103.00(11) . . ?
O12 Mo3 O8 144.72(9) . . ?
O10 Mo3 O7 163.85(11) . . ?
O9 Mo3 O7 91.23(11) . . ?
O12 Mo3 O7 77.98(9) . . ?
O8 Mo3 O7 77.51(9) . . ?
O10 Mo3 O11 95.06(10) . . ?
O9 Mo3 O11 160.02(11) . . ?
O12 Mo3 O11 73.84(8) . . ?
O8 Mo3 O11 73.82(7) . . ?
O7 Mo3 O11 68.79(7) . . ?
C30 N3 C32 122.2(3) . . ?
C36 O3 Cu1 114.1(2) . 2_445 ?
O13 Mo4 O14 104.74(11) . . ?
O13 Mo4 O12 101.11(11) . . ?
O14 Mo4 O12 100.50(11) . . ?
O13 Mo4 O15 97.19(10) . . ?
O14 Mo4 O15 102.39(10) . . ?
O12 Mo4 O15 145.85(9) . . ?
O13 Mo4 O11 93.33(9) . . ?
O14 Mo4 O11 161.82(9) . . ?
O12 Mo4 O11 77.57(8) . . ?
O15 Mo4 O11 72.78(7) . . ?
O13 Mo4 O5 162.86(10) . . ?
O14 Mo4 O5 90.38(9) . . ?
O12 Mo4 O5 83.66(8) . . ?
O15 Mo4 O5 71.24(7) . . ?
O11 Mo4 O5 71.44(6) . . ?
O13 Mo4 Mo1 84.77(8) . 3_576 ?
O14 Mo4 Mo1 137.93(9) . 3_576 ?
O12 Mo4 Mo1 118.05(6) . 3_576 ?
O15 Mo4 Mo1 35.59(5) . 3_576 ?
O11 Mo4 Mo1 40.49(5) . 3_576 ?
O5 Mo4 Mo1 78.52(5) . 3_576 ?
C36 N4 C27 123.4(3) . . ?
C37 N5 C26 118.2(3) . . ?
C37 N5 Cu1 129.1(2) . 2_445 ?
C26 N5 Cu1 112.6(2) . 2_445 ?
Mo1 O5 Mo2 108.83(9) . . ?
Mo1 O5 Mo4 111.39(8) . . ?
Mo2 O5 Mo4 103.72(8) . . ?
C12 N6 C35 115.7(3) . . ?
Mo1 O7 Mo3 120.52(10) . . ?
Mo2 O8 Mo3 118.33(10) 3_576 . ?
N1 C10 C40 120.0(3) . . ?
Mo1 O11 Mo4 92.75(7) 3_576 . ?
Mo1 O11 Mo2 91.97(7) 3_576 3_576 ?
Mo4 O11 Mo2 163.60(9) . 3_576 ?
Mo1 O11 Mo1 103.94(8) 3_576 . ?
Mo4 O11 Mo1 97.02(6) . . ?
Mo2 O11 Mo1 97.07(7) 3_576 . ?
Mo1 O11 Mo3 164.18(9) 3_576 . ?
Mo4 O11 Mo3 85.71(6) . . ?
Mo2 O11 Mo3 85.47(6) 3_576 . ?
Mo1 O11 Mo3 91.87(6) . . ?
Mo4 O12 Mo3 117.77(11) . . ?
N6 C12 C37 123.5(3) . . ?
Mo1 O15 Mo4 108.20(9) 3_576 . ?
Mo1 O15 Mo2 111.14(9) 3_576 . ?
Mo4 O15 Mo2 103.92(8) . . ?
N1 C22 C23 120.2(3) . . ?
N1 C22 C30 111.8(3) . . ?
C23 C22 C30 128.1(3) . . ?
N2 C23 C22 122.5(3) . . ?
N5 C26 C35 120.3(3) . . ?
N5 C26 C36 113.4(3) . . ?
C35 C26 C36 126.2(3) . . ?
N4 C27 C31 112.4(3) . . ?
O1 C30 N3 122.6(3) . . ?
O1 C30 C22 118.4(3) . . ?
N3 C30 C22 119.0(3) . . ?
C27 C31 C32 112.7(3) . . ?
N3 C32 C31 111.0(3) . . ?
N6 C35 C26 122.6(3) . . ?
O3 C36 N4 121.8(3) . . ?
O3 C36 C26 117.1(3) . . ?
N4 C36 C26 121.0(3) . . ?
N5 C37 C12 119.6(3) . . ?
N2 C40 C10 122.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_liu
_database_code_depnum_ccdc_archive 'CCDC 1045305'
_audit_update_record             
;
2015-05-20 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H37 Cu2 Mo12 N12 O48 P'
_chemical_formula_weight         2595.01

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           Triclinic
_symmetry_space_group_name_H-M   'P-1  '

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

_cell_length_a                   11.4981(11)
_cell_length_b                   11.7035(11)
_cell_length_c                   13.2243(13)
_cell_angle_alpha                64.013(2)
_cell_angle_beta                 89.207(2)
_cell_angle_gamma                83.681(2)
_cell_volume                     1588.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.71
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1238
_exptl_absorpt_coefficient_mu    3.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4904
_exptl_absorpt_correction_T_max  0.5781
_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            9069
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5589
_reflns_number_gt                4450
_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)+(0.0833P)²+8.1353P] 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         5589
_refine_ls_number_parameters     478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1501
_refine_ls_wR_factor_gt          0.1420
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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
P P 0.0000 0.0000 0.5000 0.0234(6) Uani 1 2 d S . .
Cu1 Cu -0.5000 0.5000 -0.5000 0.0430(4) Uani 1 2 d S . .
Mo1 Mo -0.13011(7) -0.01418(7) 0.26431(6) 0.0335(2) Uani 1 1 d . . .
O1 O -0.4534(7) 0.5006(6) -0.3592(6) 0.0516(18) Uani 1 1 d . . .
C1 C -0.4972(8) 0.2888(9) -0.2930(8) 0.045(2) Uani 1 1 d . . .
N1 N 0.1226(14) 0.0948(8) 0.0250(8) 0.081(4) Uani 1 1 d . . .
O1W O -0.3022(8) 0.4796(9) -0.5569(10) 0.094(3) Uani 1 1 d . . .
O2W O -0.3939(10) 0.1427(12) 0.0275(9) 0.119(4) Uani 1 1 d . . .
Mo2 Mo 0.01877(7) -0.27089(6) 0.76388(6) 0.0312(2) Uani 1 1 d . . .
C2 C -0.5411(8) 0.2292(9) -0.4291(9) 0.045(2) Uani 1 1 d . . .
H2A H -0.5526 0.2481 -0.5045 0.054 Uiso 1 1 calc R . .
N2 N -0.5390(8) 0.0781(8) -0.2414(9) 0.058(2) Uani 1 1 d . . .
Cu2 Cu 0.0000 0.0000 0.0000 0.0969(11) Uani 1 2 d S . .
O2 O -0.0898(10) 0.1690(7) -0.0668(6) 0.085(3) Uani 1 1 d . . .
Mo3 Mo -0.27438(6) 0.17541(7) 0.38645(6) 0.0322(2) Uani 1 1 d . . .
O3 O 0.0545(7) -0.2876(8) 0.4503(9) 0.093(4) Uani 1 1 d . . .
N3 N -0.4869(6) 0.6806(7) -0.5974(7) 0.0388(18) Uani 1 1 d . . .
N4 N -0.0809(10) 0.3761(8) -0.1082(9) 0.066(3) Uani 1 1 d . . .
Mo4 Mo 0.15564(8) -0.16398(8) 0.36224(8) 0.0428(2) Uani 1 1 d . . .
O4 O -0.0720(9) 0.0744(9) 0.4001(8) 0.022(2) Uani 0.50 1 d P . .
N5 N -0.4453(10) 0.3838(10) -0.1709(8) 0.069(3) Uani 1 1 d . . .
Mo5 Mo -0.08745(8) -0.28678(8) 0.52155(8) 0.0457(2) Uani 1 1 d . . .
O5 O -0.1366(7) -0.2143(10) 0.7520(9) 0.091(4) Uani 1 1 d . . .
C5 C -0.4646(9) 0.3997(10) -0.2736(9) 0.049(2) Uani 1 1 d . . .
Mo6 Mo -0.26002(7) -0.11341(9) 0.63715(7) 0.0426(2) Uani 1 1 d . . .
O6 O -0.2271(7) -0.2229(10) 0.5756(8) 0.086(3) Uani 1 1 d . . .
C6 C -0.2844(13) 0.4453(13) -0.0898(11) 0.077(4) Uani 1 1 d . . .
H6A H -0.2629 0.5123 -0.0718 0.092 Uiso 1 1 calc R . .
H6B H -0.2848 0.3682 -0.0197 0.092 Uiso 1 1 calc R . .
N6 N 0.2787(12) 0.2598(11) 0.0182(9) 0.084(4) Uani 1 1 d . . .
O7 O -0.3193(10) 0.0185(7) 0.5036(6) 0.081(3) Uani 1 1 d . . .
C7 C 0.1703(15) 0.2994(11) -0.0236(10) 0.075(4) Uani 1 1 d . . .
H7A H 0.1471 0.3871 -0.0563 0.090 Uiso 1 1 calc R . .
C8 C -0.1964(12) 0.4222(11) -0.1611(9) 0.066(4) Uani 1 1 d . . .
H8A H -0.2214 0.3602 -0.1839 0.080 Uiso 1 1 calc R . .
H8B H -0.1922 0.5013 -0.2286 0.080 Uiso 1 1 calc R . .
O9 O 0.2301(10) -0.0178(7) 0.3153(6) 0.085(3) Uani 1 1 d . . .
C9 C -0.5124(10) 0.1686(11) -0.2122(10) 0.057(3) Uani 1 1 d . . .
H9A H -0.5041 0.1498 -0.1365 0.068 Uiso 1 1 calc R . .
O10 O 0.0303(7) -0.4044(6) 0.8860(6) 0.057(2) Uani 1 1 d . . .
C10 C -0.0342(14) 0.2567(10) -0.0676(8) 0.065(4) Uani 1 1 d . . .
O11 O -0.1825(7) -0.0136(8) 0.1476(6) 0.060(2) Uani 1 1 d . . .
C11 C -0.4063(14) 0.4839(14) -0.1436(12) 0.083(4) Uani 1 1 d . . .
H11A H -0.4604 0.4989 -0.0926 0.099 Uiso 1 1 calc R . .
H11B H -0.4074 0.5632 -0.2119 0.099 Uiso 1 1 calc R . .
O12 O -0.3778(6) -0.1611(7) 0.7081(6) 0.0540(18) Uani 1 1 d . . .
C12 C 0.0884(15) 0.2208(9) -0.0226(9) 0.070(4) Uani 1 1 d . . .
O13 O 0.2490(10) -0.2279(7) 0.5036(6) 0.084(3) Uani 1 1 d . . .
O14 O -0.0621(6) 0.1533(6) 0.1939(6) 0.0467(17) Uani 1 1 d . . .
C14 C 0.3069(17) 0.1365(14) 0.0644(10) 0.092(5) Uani 1 1 d . . .
H14A H 0.3818 0.1042 0.0966 0.110 Uiso 1 1 calc R . .
O15 O -0.2503(6) 0.0747(7) 0.3021(6) 0.0524(18) Uani 1 1 d . . .
C15 C 0.231(2) 0.0505(13) 0.0681(11) 0.109(8) Uani 1 1 d . . .
H15A H 0.2560 -0.0368 0.1002 0.131 Uiso 1 1 calc R . .
O16 O -0.1546(7) -0.1679(8) 0.3710(8) 0.093(4) Uani 1 1 d . . .
O17 O -0.4051(6) 0.2548(8) 0.3336(10) 0.084(3) Uani 1 1 d . . .
O18 O -0.1738(6) 0.2826(7) 0.2904(7) 0.0536(19) Uani 1 1 d . . .
O20 O 0.0323(7) -0.0758(8) 0.2606(10) 0.111(5) Uani 1 1 d . . .
O21 O 0.2314(6) -0.2435(7) 0.3011(6) 0.0489(17) Uani 1 1 d . . .
O22 O -0.0126(8) -0.0786(9) 0.4292(8) 0.022(2) Uani 0.50 1 d P . .
O23 O 0.1238(9) -0.0442(10) 0.4799(8) 0.023(2) Uani 0.50 1 d P . .
C23 C -0.5537(9) 0.1087(10) -0.3483(10) 0.050(3) Uani 1 1 d . . .
H23A H -0.5731 0.0473 -0.3700 0.060 Uiso 1 1 calc R . .
O24 O 0.0543(9) 0.1205(9) 0.4166(9) 0.024(2) Uani 0.50 1 d P . .
O25 O -0.1346(8) -0.4346(9) 0.5320(8) 0.077(2) Uani 1 1 d . . .
O27 O -0.0167(7) -0.3490(10) 0.6650(8) 0.082(3) 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
P O4 1.433(10) 2_556 ?
P O4 1.433(10) . ?
P O23 1.520(10) 2_556 ?
P O23 1.520(10) . ?
P O24 1.552(10) 2_556 ?
P O24 1.552(10) . ?
P O22 1.592(9) 2_556 ?
P O22 1.592(9) . ?
Cu1 O1 1.947(7) 2_464 ?
Cu1 O1 1.948(7) . ?
Cu1 N3 1.957(7) 2_464 ?
Cu1 N3 1.957(7) . ?
Cu1 O1W 2.405(11) . ?
Cu1 O1W 2.405(11) 2_464 ?
Mo1 O11 1.661(6) . ?
Mo1 O16 1.784(7) . ?
Mo1 O15 1.834(7) . ?
Mo1 O20 1.934(8) . ?
Mo1 O14 2.009(6) . ?
Mo1 O22 2.359(10) . ?
O1 C5 1.245(12) . ?
C1 N3 1.342(12) 2_464 ?
C1 C9 1.372(14) . ?
C1 C5 1.513(14) . ?
N1 C15 1.33(2) . ?
N1 C12 1.339(14) . ?
N1 Cu2 2.002(13) . ?
Mo2 O10 1.678(6) . ?
Mo2 O14 1.813(6) 2_556 ?
Mo2 O5 1.820(8) . ?
Mo2 O18 1.926(7) 2_556 ?
Mo2 O27 1.965(7) . ?
Mo2 O24 2.355(10) 2_556 ?
Mo2 O4 2.504(10) 2_556 ?
C2 N3 1.320(12) 2_464 ?
C2 C23 1.368(14) . ?
N2 C23 1.306(14) . ?
N2 C9 1.341(14) . ?
Cu2 O2 1.950(9) . ?
Cu2 O2 1.950(9) 2 ?
Cu2 N1 2.002(13) 2 ?
O2 C10 1.264(13) . ?
Mo3 O17 1.662(7) . ?
Mo3 O18 1.846(7) . ?
Mo3 O13 1.847(7) 2_556 ?
Mo3 O7 1.932(7) . ?
Mo3 O15 1.944(6) . ?
Mo3 O23 2.367(10) 2_556 ?
Mo3 O4 2.462(10) . ?
O3 Mo5 1.874(8) . ?
O3 Mo4 1.913(8) . ?
N3 C2 1.320(12) 2_464 ?
N3 C1 1.342(12) 2_464 ?
N4 C10 1.309(15) . ?
N4 C8 1.443(16) . ?
Mo4 O21 1.655(6) . ?
Mo4 O20 1.844(9) . ?
Mo4 O9 1.850(7) . ?
Mo4 O13 1.965(9) . ?
Mo4 O22 2.413(10) . ?
Mo4 O23 2.511(10) . ?
O4 O23 1.589(14) 2_556 ?
O4 O24 1.653(14) . ?
O4 O22 1.720(14) . ?
O4 Mo2 2.504(10) 2_556 ?
N5 C5 1.305(13) . ?
N5 C11 1.482(15) . ?
Mo5 O25 1.816(9) . ?
Mo5 O27 1.868(8) . ?
Mo5 O6 1.954(8) . ?
Mo5 O16 1.968(9) . ?
Mo5 O22 2.448(10) . ?
Mo5 O24 2.484(10) 2_556 ?
O5 Mo6 1.958(8) . ?
Mo6 O12 1.642(7) . ?
Mo6 O6 1.802(7) . ?
Mo6 O7 1.838(8) . ?
Mo6 O9 1.959(7) 2_556 ?
Mo6 O24 2.464(11) 2_556 ?
Mo6 O23 2.514(10) 2_556 ?
C6 C8 1.457(18) . ?
C6 C11 1.510(19) . ?
N6 C14 1.301(17) . ?
N6 C7 1.320(18) . ?
C7 C12 1.383(19) . ?
O9 Mo6 1.959(7) 2_556 ?
C10 C12 1.48(2) . ?
O13 Mo3 1.847(7) 2_556 ?
O14 Mo2 1.813(6) 2_556 ?
C14 C15 1.38(3) . ?
O18 Mo2 1.926(7) 2_556 ?
O23 O4 1.589(14) 2_556 ?
O23 Mo3 2.367(10) 2_556 ?
O23 Mo6 2.514(10) 2_556 ?
O24 Mo2 2.355(10) 2_556 ?
O24 Mo6 2.464(11) 2_556 ?
O24 Mo5 2.484(10) 2_556 ?

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
O4 P O4 179.999(2) 2_556 . ?
O4 P O23 115.0(5) 2_556 2_556 ?
O4 P O23 65.0(5) . 2_556 ?
O4 P O23 65.0(5) 2_556 . ?
O4 P O23 115.0(5) . . ?
O23 P O23 180.000(2) 2_556 . ?
O4 P O24 67.1(5) 2_556 2_556 ?
O4 P O24 112.9(5) . 2_556 ?
O23 P O24 72.8(5) 2_556 2_556 ?
O23 P O24 107.2(5) . 2_556 ?
O4 P O24 112.9(5) 2_556 . ?
O4 P O24 67.1(5) . . ?
O23 P O24 107.2(5) 2_556 . ?
O23 P O24 72.8(5) . . ?
O24 P O24 179.999(2) 2_556 . ?
O4 P O22 69.1(5) 2_556 2_556 ?
O4 P O22 110.9(5) . 2_556 ?
O23 P O22 73.6(5) 2_556 2_556 ?
O23 P O22 106.4(5) . 2_556 ?
O24 P O22 103.6(5) 2_556 2_556 ?
O24 P O22 76.4(5) . 2_556 ?
O4 P O22 110.9(5) 2_556 . ?
O4 P O22 69.1(5) . . ?
O23 P O22 106.4(5) 2_556 . ?
O23 P O22 73.6(5) . . ?
O24 P O22 76.4(5) 2_556 . ?
O24 P O22 103.6(5) . . ?
O22 P O22 179.999(1) 2_556 . ?
O1 Cu1 O1 180.0(4) 2_464 . ?
O1 Cu1 N3 97.0(3) 2_464 2_464 ?
O1 Cu1 N3 83.0(3) . 2_464 ?
O1 Cu1 N3 83.0(3) 2_464 . ?
O1 Cu1 N3 97.0(3) . . ?
N3 Cu1 N3 180.000(1) 2_464 . ?
O1 Cu1 O1W 85.8(3) 2_464 . ?
O1 Cu1 O1W 94.2(3) . . ?
N3 Cu1 O1W 98.9(3) 2_464 . ?
N3 Cu1 O1W 81.1(3) . . ?
O1 Cu1 O1W 94.2(3) 2_464 2_464 ?
O1 Cu1 O1W 85.8(3) . 2_464 ?
N3 Cu1 O1W 81.1(3) 2_464 2_464 ?
N3 Cu1 O1W 98.9(3) . 2_464 ?
O1W Cu1 O1W 180.0 . 2_464 ?
O11 Mo1 O16 103.4(5) . . ?
O11 Mo1 O15 102.9(4) . . ?
O16 Mo1 O15 95.5(4) . . ?
O11 Mo1 O20 100.0(5) . . ?
O16 Mo1 O20 90.3(3) . . ?
O15 Mo1 O20 154.4(5) . . ?
O11 Mo1 O14 98.4(3) . . ?
O16 Mo1 O14 157.4(4) . . ?
O15 Mo1 O14 85.1(3) . . ?
O20 Mo1 O14 80.2(3) . . ?
O11 Mo1 O22 159.2(4) . . ?
O16 Mo1 O22 67.0(4) . . ?
O15 Mo1 O22 96.6(3) . . ?
O20 Mo1 O22 62.9(5) . . ?
O14 Mo1 O22 90.5(3) . . ?
C5 O1 Cu1 114.5(6) . . ?
N3 C1 C9 120.5(9) 2_464 . ?
N3 C1 C5 112.6(8) 2_464 . ?
C9 C1 C5 126.9(10) . . ?
C15 N1 C12 120.1(14) . . ?
C15 N1 Cu2 128.7(10) . . ?
C12 N1 Cu2 110.7(11) . . ?
O10 Mo2 O14 102.2(3) . 2_556 ?
O10 Mo2 O5 102.7(5) . . ?
O14 Mo2 O5 94.3(3) 2_556 . ?
O10 Mo2 O18 100.4(4) . 2_556 ?
O14 Mo2 O18 88.3(3) 2_556 2_556 ?
O5 Mo2 O18 155.6(4) . 2_556 ?
O10 Mo2 O27 97.7(4) . . ?
O14 Mo2 O27 159.2(4) 2_556 . ?
O5 Mo2 O27 86.9(3) . . ?
O18 Mo2 O27 82.4(3) 2_556 . ?
O10 Mo2 O24 159.0(4) . 2_556 ?
O14 Mo2 O24 95.2(3) 2_556 2_556 ?
O5 Mo2 O24 64.0(4) . 2_556 ?
O18 Mo2 O24 91.6(4) 2_556 2_556 ?
O27 Mo2 O24 66.6(4) . 2_556 ?
O10 Mo2 O4 160.6(4) . 2_556 ?
O14 Mo2 O4 67.7(3) 2_556 2_556 ?
O5 Mo2 O4 94.7(5) . 2_556 ?
O18 Mo2 O4 63.9(3) 2_556 2_556 ?
O27 Mo2 O4 91.5(4) . 2_556 ?
O24 Mo2 O4 39.6(3) 2_556 2_556 ?
N3 C2 C23 121.6(10) 2_464 . ?
C23 N2 C9 118.2(9) . . ?
O2 Cu2 O2 179.999(1) . 2 ?
O2 Cu2 N1 83.2(4) . . ?
O2 Cu2 N1 96.8(4) 2 . ?
O2 Cu2 N1 96.8(4) . 2 ?
O2 Cu2 N1 83.2(4) 2 2 ?
N1 Cu2 N1 179.999(1) . 2 ?
C10 O2 Cu2 113.6(10) . . ?
O17 Mo3 O18 102.4(4) . . ?
O17 Mo3 O13 101.0(5) . 2_556 ?
O18 Mo3 O13 92.4(3) . 2_556 ?
O17 Mo3 O7 100.7(5) . . ?
O18 Mo3 O7 156.4(4) . . ?
O13 Mo3 O7 88.0(3) 2_556 . ?
O17 Mo3 O15 100.4(4) . . ?
O18 Mo3 O15 87.3(3) . . ?
O13 Mo3 O15 158.2(4) 2_556 . ?
O7 Mo3 O15 83.7(3) . . ?
O17 Mo3 O23 160.0(5) . 2_556 ?
O18 Mo3 O23 94.0(4) . 2_556 ?
O13 Mo3 O23 66.6(4) 2_556 2_556 ?
O7 Mo3 O23 64.6(4) . 2_556 ?
O15 Mo3 O23 91.7(3) . 2_556 ?
O17 Mo3 O4 161.4(5) . . ?
O18 Mo3 O4 65.7(3) . . ?
O13 Mo3 O4 94.1(4) 2_556 . ?
O7 Mo3 O4 90.7(4) . . ?
O15 Mo3 O4 66.0(3) . . ?
O23 Mo3 O4 38.4(3) 2_556 . ?
Mo5 O3 Mo4 136.6(5) . . ?
C2 N3 C1 117.6(8) 2_464 2_464 ?
C2 N3 Cu1 129.5(7) 2_464 . ?
C1 N3 Cu1 112.7(6) 2_464 . ?
C10 N4 C8 124.4(10) . . ?
O21 Mo4 O20 102.9(5) . . ?
O21 Mo4 O9 102.0(4) . . ?
O20 Mo4 O9 91.3(4) . . ?
O21 Mo4 O3 100.2(4) . . ?
O20 Mo4 O3 89.0(4) . . ?
O9 Mo4 O3 157.1(5) . . ?
O21 Mo4 O13 99.7(4) . . ?
O20 Mo4 O13 157.2(5) . . ?
O9 Mo4 O13 86.4(3) . . ?
O3 Mo4 O13 84.6(4) . . ?
O21 Mo4 O22 158.6(3) . . ?
O20 Mo4 O22 62.7(4) . . ?
O9 Mo4 O22 94.5(4) . . ?
O3 Mo4 O22 65.4(4) . . ?
O13 Mo4 O22 94.8(4) . . ?
O21 Mo4 O23 156.7(3) . . ?
O20 Mo4 O23 96.6(5) . . ?
O9 Mo4 O23 64.6(4) . . ?
O3 Mo4 O23 92.5(4) . . ?
O13 Mo4 O23 62.0(4) . . ?
O22 Mo4 O23 44.4(3) . . ?
P O4 O23 60.2(5) . 2_556 ?
P O4 O24 59.9(5) . . ?
O23 O4 O24 99.4(7) 2_556 . ?
P O4 O22 59.8(5) . . ?
O23 O4 O22 97.7(7) 2_556 . ?
O24 O4 O22 94.1(7) . . ?
P O4 Mo3 127.7(6) . . ?
O23 O4 Mo3 67.6(5) 2_556 . ?
O24 O4 Mo3 131.0(6) . . ?
O22 O4 Mo3 133.3(6) . . ?
P O4 Mo2 125.1(6) . 2_556 ?
O23 O4 Mo2 135.3(6) 2_556 2_556 ?
O24 O4 Mo2 65.3(5) . 2_556 ?
O22 O4 Mo2 124.0(6) . 2_556 ?
Mo3 O4 Mo2 90.6(3) . 2_556 ?
C5 N5 C11 123.5(10) . . ?
O25 Mo5 O27 98.9(4) . . ?
O25 Mo5 O3 99.9(5) . . ?
O27 Mo5 O3 94.2(4) . . ?
O25 Mo5 O6 99.2(4) . . ?
O27 Mo5 O6 89.1(3) . . ?
O3 Mo5 O6 159.9(4) . . ?
O25 Mo5 O16 99.6(4) . . ?
O27 Mo5 O16 161.2(4) . . ?
O3 Mo5 O16 86.1(4) . . ?
O6 Mo5 O16 84.5(4) . . ?
O25 Mo5 O22 156.4(4) . . ?
O27 Mo5 O22 100.3(4) . . ?
O3 Mo5 O22 65.1(4) . . ?
O6 Mo5 O22 94.8(4) . . ?
O16 Mo5 O22 62.8(4) . . ?
O25 Mo5 O24 157.1(4) . 2_556 ?
O27 Mo5 O24 65.0(4) . 2_556 ?
O3 Mo5 O24 97.6(4) . 2_556 ?
O6 Mo5 O24 66.0(4) . 2_556 ?
O16 Mo5 O24 96.4(4) . 2_556 ?
O22 Mo5 O24 46.4(3) . 2_556 ?
Mo2 O5 Mo6 140.2(6) . . ?
O1 C5 N5 124.0(10) . . ?
O1 C5 C1 116.5(9) . . ?
N5 C5 C1 119.5(10) . . ?
O12 Mo6 O6 103.7(4) . . ?
O12 Mo6 O7 103.3(4) . . ?
O6 Mo6 O7 93.5(4) . . ?
O12 Mo6 O5 101.0(4) . . ?
O6 Mo6 O5 88.0(3) . . ?
O7 Mo6 O5 154.6(5) . . ?
O12 Mo6 O9 99.2(4) . 2_556 ?
O6 Mo6 O9 156.4(5) . 2_556 ?
O7 Mo6 O9 86.9(3) . 2_556 ?
O5 Mo6 O9 81.9(4) . 2_556 ?
O12 Mo6 O24 158.8(4) . 2_556 ?
O6 Mo6 O24 68.3(4) . 2_556 ?
O7 Mo6 O24 96.9(4) . 2_556 ?
O5 Mo6 O24 60.1(4) . 2_556 ?
O9 Mo6 O24 88.2(4) 2_556 2_556 ?
O12 Mo6 O23 156.6(4) . 2_556 ?
O6 Mo6 O23 95.9(4) . 2_556 ?
O7 Mo6 O23 62.4(4) . 2_556 ?
O5 Mo6 O23 92.2(4) . 2_556 ?
O9 Mo6 O23 63.4(3) 2_556 2_556 ?
O24 Mo6 O23 42.9(3) 2_556 2_556 ?
Mo6 O6 Mo5 136.1(5) . . ?
C8 C6 C11 113.3(11) . . ?
C14 N6 C7 115.3(15) . . ?
Mo6 O7 Mo3 139.5(6) . . ?
N6 C7 C12 125.1(12) . . ?
N4 C8 C6 114.2(10) . . ?
Mo4 O9 Mo6 140.5(5) . 2_556 ?
N2 C9 C1 120.7(11) . . ?
O2 C10 N4 122.2(13) . . ?
O2 C10 C12 117.6(11) . . ?
N4 C10 C12 120.2(10) . . ?
N5 C11 C6 111.5(11) . . ?
N1 C12 C7 116.8(14) . . ?
N1 C12 C10 114.4(12) . . ?
C7 C12 C10 128.8(10) . . ?
Mo3 O13 Mo4 137.5(5) 2_556 . ?
Mo2 O14 Mo1 138.1(4) 2_556 . ?
N6 C14 C15 123.6(17) . . ?
Mo1 O15 Mo3 139.2(4) . . ?
N1 C15 C14 119.0(12) . . ?
Mo1 O16 Mo5 136.9(6) . . ?
Mo3 O18 Mo2 138.6(4) . 2_556 ?
Mo4 O20 Mo1 137.6(7) . . ?
P O22 O4 51.1(4) . . ?
P O22 Mo1 127.0(5) . . ?
O4 O22 Mo1 76.0(5) . . ?
P O22 Mo4 121.9(5) . . ?
O4 O22 Mo4 133.2(6) . . ?
Mo1 O22 Mo4 95.1(3) . . ?
P O22 Mo5 118.6(5) . . ?
O4 O22 Mo5 132.9(6) . . ?
Mo1 O22 Mo5 93.1(3) . . ?
Mo4 O22 Mo5 92.8(3) . . ?
P O23 O4 54.8(5) . 2_556 ?
P O23 Mo3 128.9(6) . 2_556 ?
O4 O23 Mo3 74.1(5) 2_556 2_556 ?
P O23 Mo4 119.9(5) . . ?
O4 O23 Mo4 135.1(6) 2_556 . ?
Mo3 O23 Mo4 93.5(4) 2_556 . ?
P O23 Mo6 121.3(5) . 2_556 ?
O4 O23 Mo6 131.6(6) 2_556 2_556 ?
Mo3 O23 Mo6 92.9(3) 2_556 2_556 ?
Mo4 O23 Mo6 91.1(3) . 2_556 ?
N2 C23 C2 121.3(10) . . ?
P O24 O4 53.0(5) . . ?
P O24 Mo2 128.0(5) . 2_556 ?
O4 O24 Mo2 75.0(5) . 2_556 ?
P O24 Mo6 122.7(5) . 2_556 ?
O4 O24 Mo6 141.4(7) . 2_556 ?
Mo2 O24 Mo6 95.0(4) 2_556 2_556 ?
P O24 Mo5 118.5(6) . 2_556 ?
O4 O24 Mo5 127.7(6) . 2_556 ?
Mo2 O24 Mo5 93.7(3) 2_556 2_556 ?
Mo6 O24 Mo5 89.5(3) 2_556 2_556 ?
Mo5 O27 Mo2 134.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.547
_refine_diff_density_min         -1.893
_refine_diff_density_rms         0.184



####################################################################### 
# 
# 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 1045306'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H36 Cu2 Mo12 N12 O48 Si'
_chemical_formula_weight         2591.12

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'
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                   11.3935(6)
_cell_length_b                   11.8235(6)
_cell_length_c                   13.0713(6)
_cell_angle_alpha                63.6790(10)
_cell_angle_beta                 88.7650(10)
_cell_angle_gamma                82.9660(10)
_cell_volume                     1565.35(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1236
_exptl_absorpt_coefficient_mu    3.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4450
_exptl_absorpt_correction_T_max  0.5342
_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            7989
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5485
_reflns_number_gt                5025
_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)+(0.0769P)²+28.5898P] 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         5485
_refine_ls_number_parameters     478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1699
_refine_ls_wR_factor_gt          0.1602
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.51533(8) 0.23286(8) 0.26736(7) 0.0311(2) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 -0.5000 0.0907(12) Uani 1 2 d S . .
Si1 Si 0.5000 0.5000 0.0000 0.0294(8) Uani 1 2 d S . .
N1 N 0.3746(16) 0.4028(10) -0.5164(10) 0.077(5) Uani 1 1 d . . .
C1 C 0.265(2) 0.4477(16) -0.5628(14) 0.097(8) Uani 1 1 d . . .
H1A H 0.2400 0.5347 -0.5998 0.117 Uiso 1 1 calc R . .
O1 O 0.5933(12) 0.3305(8) -0.4325(8) 0.080(4) Uani 1 1 d . . .
O1W O 0.7947(10) 0.0208(13) 0.0545(14) 0.101(4) Uani 1 1 d . . .
Mo2 Mo 0.36702(8) 0.49131(8) -0.23554(7) 0.0335(2) Uani 1 1 d . . .
Cu2 Cu 1.0000 0.0000 0.0000 0.0445(5) Uani 1 2 d S . .
N2 N 0.2192(15) 0.2373(13) -0.5027(12) 0.086(4) Uani 1 1 d . . .
C2 C 0.1898(19) 0.3623(17) -0.5541(13) 0.087(6) Uani 1 1 d . . .
H2A H 0.1137 0.3938 -0.5862 0.104 Uiso 1 1 calc R . .
O2 O 0.9554(7) -0.0054(8) -0.1409(7) 0.0477(19) Uani 1 1 d . . .
O2W O 0.912(2) 0.316(3) -0.5520(19) 0.31(2) Uani 1 1 d . . .
Mo3 Mo 0.77509(9) 0.31605(8) 0.11531(8) 0.0389(3) Uani 1 1 d . . .
C3 C 0.3276(16) 0.1949(13) -0.4579(14) 0.073(4) Uani 1 1 d . . .
H3A H 0.3506 0.1076 -0.4197 0.087 Uiso 1 1 calc R . .
O3 O 0.3135(12) 0.4927(13) -0.3527(9) 0.093(4) Uani 1 1 d . . .
N3 N 0.5800(11) 0.1231(9) -0.3767(10) 0.062(3) Uani 1 1 d . . .
H6A H 0.5366 0.0677 -0.3748 0.075 Uiso 1 1 calc R . .
C4 C 0.4079(16) 0.2769(12) -0.4664(11) 0.064(4) Uani 1 1 d . . .
Mo4 Mo 0.42062(9) 0.20957(9) 0.02246(11) 0.0488(3) Uani 1 1 d . . .
O4 O 0.5332(10) 0.4271(10) -0.2445(13) 0.132(7) Uani 1 1 d . . .
N4 N 0.9526(11) 0.1022(12) -0.3317(9) 0.063(3) Uani 1 1 d . . .
H9A H 0.9677 0.1705 -0.3894 0.075 Uiso 1 1 calc R . .
N5 N 1.0162(8) 0.1787(9) -0.1048(8) 0.042(2) Uani 1 1 d . . .
Mo5 Mo 0.65965(13) 0.34642(10) -0.14577(10) 0.0607(4) Uani 1 1 d . . .
O5 O 0.7365(7) 0.2665(8) -0.2063(7) 0.0455(19) Uani 1 1 d . . .
C5 C 0.5334(16) 0.2426(11) -0.4231(10) 0.059(4) Uani 1 1 d . . .
C6 C 0.7012(14) 0.0769(13) -0.3274(11) 0.060(4) Uani 1 1 d . . .
H6B H 0.6997 0.0022 -0.2548 0.071 Uiso 1 1 calc R . .
H6C H 0.7313 0.1419 -0.3129 0.071 Uiso 1 1 calc R . .
Mo6 Mo 0.76317(11) 0.61101(12) -0.13370(10) 0.0563(4) Uani 1 1 d . . .
N6 N 1.0443(11) 0.4162(11) -0.2736(12) 0.068(3) Uani 1 1 d . . .
O6 O 0.7366(19) 0.4827(11) -0.1899(8) 0.143(8) Uani 1 1 d . . .
O7 O 0.8816(7) 0.6598(9) -0.2073(7) 0.053(2) Uani 1 1 d . . .
C7 C 0.7826(15) 0.0443(14) -0.4036(12) 0.069(4) Uani 1 1 d . . .
H7A H 0.7809 0.1175 -0.4777 0.083 Uiso 1 1 calc R . .
H7B H 0.7556 -0.0245 -0.4143 0.083 Uiso 1 1 calc R . .
C8 C 0.9094(16) 0.0043(16) -0.3536(13) 0.079(5) Uani 1 1 d . . .
H8A H 0.9123 -0.0734 -0.2829 0.095 Uiso 1 1 calc R . .
H8B H 0.9606 -0.0131 -0.4066 0.095 Uiso 1 1 calc R . .
O8 O 0.6430(8) 0.7134(16) -0.2565(13) 0.111(6) Uani 1 1 d . . .
C9 C 0.9699(11) 0.0931(12) -0.2296(10) 0.047(3) Uani 1 1 d . . .
O9 O 0.8262(19) 0.4761(11) -0.0032(8) 0.148(8) Uani 1 1 d . . .
C10 C 1.0038(10) 0.2033(11) -0.2148(10) 0.047(3) Uani 1 1 d . . .
O10 O 0.9057(8) 0.2384(9) 0.1673(12) 0.081(4) Uani 1 1 d . . .
C11 C 1.0186(12) 0.3215(12) -0.2989(12) 0.058(3) Uani 1 1 d . . .
H11A H 1.0109 0.3376 -0.3750 0.070 Uiso 1 1 calc R . .
O11 O 0.7545(7) 0.4201(8) 0.1989(8) 0.050(2) Uani 1 1 d . . .
O12 O 0.6761(7) 0.2126(8) 0.2135(8) 0.051(2) Uani 1 1 d . . .
C12 C 1.0568(11) 0.3891(12) -0.1661(14) 0.059(4) Uani 1 1 d . . .
H12A H 1.0761 0.4514 -0.1466 0.071 Uiso 1 1 calc R . .
O13 O 0.5624(7) 0.3433(8) 0.3123(8) 0.049(2) Uani 1 1 d . . .
C13 C 1.0422(10) 0.2702(12) -0.0802(12) 0.051(3) Uani 1 1 d . . .
H13A H 1.0506 0.2544 -0.0042 0.061 Uiso 1 1 calc R . .
O14 O 0.5258(13) 0.0980(8) 0.3875(8) 0.087(4) Uani 1 1 d . . .
O15 O 0.4824(8) 0.1560(17) 0.1634(13) 0.118(6) Uani 1 1 d . . .
O16 O 0.3711(9) 0.0818(7) 0.0272(7) 0.056(2) Uani 1 1 d . . .
O17 O 0.7274(8) 0.7215(16) -0.0754(12) 0.107(5) Uani 1 1 d . . .
O18 O 0.3434(10) 0.3364(10) -0.1279(12) 0.121(6) Uani 1 1 d . . .
O19 O 0.4784(10) 0.4229(11) -0.0765(10) 0.023(2) Uani 0.50 1 d P . .
O20 O 0.5569(10) 0.2150(10) -0.0504(13) 0.124(7) Uani 1 1 d . . .
O21 O 0.4495(10) 0.3674(11) 0.0877(10) 0.022(2) Uani 0.50 1 d P . .
O22 O 0.5683(10) 0.4220(10) 0.1094(10) 0.019(2) Uani 0.50 1 d P . .
O23 O 0.7504(19) 0.2703(12) 0.0011(9) 0.145(8) Uani 1 1 d . . .
O24 O 0.6425(11) 0.4503(11) -0.0228(10) 0.025(3) Uani 0.50 1 d P . .


_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 O14 1.662(9) . ?
Mo1 O13 1.790(7) . ?
Mo1 O8 1.824(9) 2_665 ?
Mo1 O12 1.973(8) . ?
Mo1 O15 2.004(9) . ?
Mo1 O21 2.254(12) . ?
Mo1 O22 2.410(11) . ?
Cu1 O1 1.969(11) 2_664 ?
Cu1 O1 1.969(11) . ?
Cu1 N1 2.011(16) 2_664 ?
Cu1 N1 2.011(16) . ?
Si1 O22 1.484(11) 2_665 ?
Si1 O22 1.484(11) . ?
Si1 O21 1.643(12) . ?
Si1 O21 1.643(12) 2_665 ?
Si1 O19 1.663(12) 2_665 ?
Si1 O19 1.663(12) . ?
Si1 O24 1.724(12) . ?
Si1 O24 1.724(12) 2_665 ?
N1 C4 1.340(17) . ?
N1 C1 1.34(3) . ?
C1 C2 1.36(3) . ?
O1 C5 1.272(16) . ?
Mo2 O3 1.654(9) . ?
Mo2 O18 1.796(9) . ?
Mo2 O11 1.818(8) 2_665 ?
Mo2 O4 1.972(9) . ?
Mo2 O13 2.022(8) 2_665 ?
Mo2 O19 2.227(12) . ?
Mo2 O22 2.460(11) 2_665 ?
Cu2 O2 1.950(8) . ?
Cu2 O2 1.950(8) 2_755 ?
Cu2 N5 1.973(9) . ?
Cu2 N5 1.973(9) 2_755 ?
N2 C3 1.32(2) . ?
N2 C2 1.33(2) . ?
O2 C9 1.253(14) . ?
Mo3 O10 1.635(9) . ?
Mo3 O12 1.817(8) . ?
Mo3 O23 1.836(10) . ?
Mo3 O11 1.968(8) . ?
Mo3 O9 1.988(10) . ?
Mo3 O24 2.247(12) . ?
Mo3 O22 2.515(11) . ?
C3 C4 1.38(2) . ?
N3 C5 1.310(17) . ?
N3 C6 1.470(19) . ?
C4 C5 1.49(2) . ?
Mo4 O16 1.652(7) . ?
Mo4 O15 1.789(13) . ?
Mo4 O20 1.796(10) . ?
Mo4 O18 2.006(13) . ?
Mo4 O17 2.025(9) 2_665 ?
Mo4 O21 2.427(11) . ?
Mo4 O19 2.438(11) . ?
O4 Mo5 1.818(14) . ?
N4 C9 1.308(16) . ?
N4 C8 1.45(2) . ?
N5 C13 1.324(16) . ?
N5 C10 1.342(15) . ?
Mo5 O5 1.648(7) . ?
Mo5 O6 1.788(11) . ?
Mo5 O23 1.973(14) . ?
Mo5 O20 2.001(10) . ?
Mo5 O24 2.410(12) . ?
Mo5 O19 2.468(12) . ?
C6 C7 1.49(2) . ?
Mo6 O7 1.650(8) . ?
Mo6 O17 1.787(10) . ?
Mo6 O9 1.825(14) . ?
Mo6 O8 1.970(13) . ?
Mo6 O6 2.011(10) . ?
Mo6 O24 2.390(12) . ?
Mo6 O21 2.494(12) 2_665 ?
N6 C12 1.30(2) . ?
N6 C11 1.36(2) . ?
C7 C8 1.53(2) . ?
O8 Mo1 1.824(9) 2_665 ?
C9 C10 1.495(18) . ?
C10 C11 1.370(17) . ?
O11 Mo2 1.818(8) 2_665 ?
C12 C13 1.384(18) . ?
O13 Mo2 2.021(8) 2_665 ?
O17 Mo4 2.025(9) 2_665 ?
O19 O22 1.704(15) 2_665 ?
O21 O22 1.650(15) . ?
O21 Mo6 2.494(12) 2_665 ?
O22 O19 1.704(15) 2_665 ?
O22 O24 1.819(16) . ?
O22 Mo2 2.460(11) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 Mo1 O13 103.0(5) . . ?
O14 Mo1 O8 101.6(7) . 2_665 ?
O13 Mo1 O8 97.2(4) . 2_665 ?
O14 Mo1 O12 98.3(5) . . ?
O13 Mo1 O12 88.7(3) . . ?
O8 Mo1 O12 157.3(6) 2_665 . ?
O14 Mo1 O15 96.2(7) . . ?
O13 Mo1 O15 159.1(6) . . ?
O8 Mo1 O15 87.0(4) 2_665 . ?
O12 Mo1 O15 80.2(4) . . ?
O14 Mo1 O21 155.4(6) . . ?
O13 Mo1 O21 100.0(4) . . ?
O8 Mo1 O21 66.8(6) 2_665 . ?
O12 Mo1 O21 90.7(4) . . ?
O15 Mo1 O21 62.8(6) . . ?
O14 Mo1 O22 161.0(6) . . ?
O13 Mo1 O22 67.6(4) . . ?
O8 Mo1 O22 96.1(6) 2_665 . ?
O12 Mo1 O22 66.0(4) . . ?
O15 Mo1 O22 91.6(6) . . ?
O21 Mo1 O22 41.3(4) . . ?
O1 Cu1 O1 179.998(1) 2_664 . ?
O1 Cu1 N1 82.7(5) 2_664 2_664 ?
O1 Cu1 N1 97.3(5) . 2_664 ?
O1 Cu1 N1 97.3(5) 2_664 . ?
O1 Cu1 N1 82.7(5) . . ?
N1 Cu1 N1 180.0(5) 2_664 . ?
O22 Si1 O22 179.999(2) 2_665 . ?
O22 Si1 O21 116.6(6) 2_665 . ?
O22 Si1 O21 63.4(6) . . ?
O22 Si1 O21 63.4(6) 2_665 2_665 ?
O22 Si1 O21 116.6(6) . 2_665 ?
O21 Si1 O21 179.999(2) . 2_665 ?
O22 Si1 O19 114.7(6) 2_665 2_665 ?
O22 Si1 O19 65.3(6) . 2_665 ?
O21 Si1 O19 106.5(6) . 2_665 ?
O21 Si1 O19 73.5(6) 2_665 2_665 ?
O22 Si1 O19 65.3(6) 2_665 . ?
O22 Si1 O19 114.7(6) . . ?
O21 Si1 O19 73.5(6) . . ?
O21 Si1 O19 106.5(6) 2_665 . ?
O19 Si1 O19 179.999(1) 2_665 . ?
O22 Si1 O24 111.4(6) 2_665 . ?
O22 Si1 O24 68.6(6) . . ?
O21 Si1 O24 103.7(6) . . ?
O21 Si1 O24 76.3(6) 2_665 . ?
O19 Si1 O24 102.5(6) 2_665 . ?
O19 Si1 O24 77.5(6) . . ?
O22 Si1 O24 68.6(6) 2_665 2_665 ?
O22 Si1 O24 111.4(6) . 2_665 ?
O21 Si1 O24 76.2(6) . 2_665 ?
O21 Si1 O24 103.7(6) 2_665 2_665 ?
O19 Si1 O24 77.5(6) 2_665 2_665 ?
O19 Si1 O24 102.5(6) . 2_665 ?
O24 Si1 O24 180.000(1) . 2_665 ?
C4 N1 C1 119.2(17) . . ?
C4 N1 Cu1 112.2(14) . . ?
C1 N1 Cu1 128.4(12) . . ?
N1 C1 C2 118.3(14) . . ?
C5 O1 Cu1 112.9(11) . . ?
O3 Mo2 O18 102.4(7) . . ?
O3 Mo2 O11 101.9(6) . 2_665 ?
O18 Mo2 O11 96.6(4) . 2_665 ?
O3 Mo2 O4 98.4(7) . . ?
O18 Mo2 O4 90.1(4) . . ?
O11 Mo2 O4 156.7(6) 2_665 . ?
O3 Mo2 O13 97.1(4) . 2_665 ?
O18 Mo2 O13 159.0(6) . 2_665 ?
O11 Mo2 O13 86.7(3) 2_665 2_665 ?
O4 Mo2 O13 79.5(4) . 2_665 ?
O3 Mo2 O19 158.0(6) . . ?
O18 Mo2 O19 65.8(7) . . ?
O11 Mo2 O19 98.0(4) 2_665 . ?
O4 Mo2 O19 64.5(6) . . ?
O13 Mo2 O19 93.2(4) 2_665 . ?
O3 Mo2 O22 157.7(5) . 2_665 ?
O18 Mo2 O22 98.4(7) . 2_665 ?
O11 Mo2 O22 67.6(4) 2_665 2_665 ?
O4 Mo2 O22 89.4(6) . 2_665 ?
O13 Mo2 O22 63.7(4) 2_665 2_665 ?
O19 Mo2 O22 42.3(4) . 2_665 ?
O2 Cu2 O2 180.0 . 2_755 ?
O2 Cu2 N5 82.8(4) . . ?
O2 Cu2 N5 97.2(4) 2_755 . ?
O2 Cu2 N5 97.2(4) . 2_755 ?
O2 Cu2 N5 82.8(4) 2_755 2_755 ?
N5 Cu2 N5 179.998(1) . 2_755 ?
C3 N2 C2 116.9(18) . . ?
N2 C2 C1 124(2) . . ?
C9 O2 Cu2 113.9(8) . . ?
O10 Mo3 O12 102.6(5) . . ?
O10 Mo3 O23 101.7(8) . . ?
O12 Mo3 O23 95.0(5) . . ?
O10 Mo3 O11 99.4(5) . . ?
O12 Mo3 O11 88.4(3) . . ?
O23 Mo3 O11 157.3(7) . . ?
O10 Mo3 O9 98.6(7) . . ?
O12 Mo3 O9 157.6(7) . . ?
O23 Mo3 O9 87.9(4) . . ?
O11 Mo3 O9 80.8(4) . . ?
O10 Mo3 O24 155.3(6) . . ?
O12 Mo3 O24 99.3(4) . . ?
O23 Mo3 O24 64.9(7) . . ?
O11 Mo3 O24 92.4(4) . . ?
O9 Mo3 O24 61.9(7) . . ?
O10 Mo3 O22 159.1(5) . . ?
O12 Mo3 O22 65.5(4) . . ?
O23 Mo3 O22 96.5(7) . . ?
O11 Mo3 O22 64.5(3) . . ?
O9 Mo3 O22 92.1(7) . . ?
O24 Mo3 O22 44.5(4) . . ?
N2 C3 C4 121.6(14) . . ?
C5 N3 C6 124.7(12) . . ?
N1 C4 C3 119.9(17) . . ?
N1 C4 C5 112.8(14) . . ?
C3 C4 C5 127.3(12) . . ?
O16 Mo4 O15 103.4(6) . . ?
O16 Mo4 O20 103.0(6) . . ?
O15 Mo4 O20 98.1(6) . . ?
O16 Mo4 O18 97.8(6) . . ?
O15 Mo4 O18 156.1(7) . . ?
O20 Mo4 O18 87.7(5) . . ?
O16 Mo4 O17 97.4(5) . 2_665 ?
O15 Mo4 O17 87.0(5) . 2_665 ?
O20 Mo4 O17 157.0(6) . 2_665 ?
O18 Mo4 O17 79.3(5) . 2_665 ?
O16 Mo4 O21 156.3(4) . . ?
O15 Mo4 O21 61.6(6) . . ?
O20 Mo4 O21 97.5(6) . . ?
O18 Mo4 O21 94.7(6) . . ?
O17 Mo4 O21 65.2(4) 2_665 . ?
O16 Mo4 O19 153.5(4) . . ?
O15 Mo4 O19 102.2(6) . . ?
O20 Mo4 O19 66.6(5) . . ?
O18 Mo4 O19 58.8(5) . . ?
O17 Mo4 O19 90.5(6) 2_665 . ?
O21 Mo4 O19 48.0(4) . . ?
Mo5 O4 Mo2 136.7(9) . . ?
C9 N4 C8 124.1(13) . . ?
C13 N5 C10 118.8(11) . . ?
C13 N5 Cu2 128.8(9) . . ?
C10 N5 Cu2 112.3(8) . . ?
O5 Mo5 O6 101.3(7) . . ?
O5 Mo5 O4 102.9(6) . . ?
O6 Mo5 O4 95.9(7) . . ?
O5 Mo5 O23 97.9(6) . . ?
O6 Mo5 O23 88.7(5) . . ?
O4 Mo5 O23 157.3(7) . . ?
O5 Mo5 O20 98.9(5) . . ?
O6 Mo5 O20 158.2(7) . . ?
O4 Mo5 O20 87.7(5) . . ?
O23 Mo5 O20 80.2(6) . . ?
O5 Mo5 O24 152.4(4) . . ?
O6 Mo5 O24 64.7(5) . . ?
O4 Mo5 O24 102.2(6) . . ?
O23 Mo5 O24 59.8(5) . . ?
O20 Mo5 O24 93.4(6) . . ?
O5 Mo5 O19 155.0(4) . . ?
O6 Mo5 O19 99.5(7) . . ?
O4 Mo5 O19 61.2(5) . . ?
O23 Mo5 O19 96.2(6) . . ?
O20 Mo5 O19 63.5(4) . . ?
O24 Mo5 O19 51.5(4) . . ?
O1 C5 N3 121.4(16) . . ?
O1 C5 C4 119.0(13) . . ?
N3 C5 C4 119.6(12) . . ?
N3 C6 C7 112.5(11) . . ?
O7 Mo6 O17 103.2(6) . . ?
O7 Mo6 O9 102.5(7) . . ?
O17 Mo6 O9 97.7(6) . . ?
O7 Mo6 O8 97.9(5) . . ?
O17 Mo6 O8 88.3(5) . . ?
O9 Mo6 O8 156.7(7) . . ?
O7 Mo6 O6 97.0(6) . . ?
O17 Mo6 O6 157.9(7) . . ?
O9 Mo6 O6 86.5(5) . . ?
O8 Mo6 O6 80.1(6) . . ?
O7 Mo6 O24 152.7(4) . . ?
O17 Mo6 O24 100.5(6) . . ?
O9 Mo6 O24 60.8(6) . . ?
O8 Mo6 O24 96.0(5) . . ?
O6 Mo6 O24 62.5(5) . . ?
O7 Mo6 O21 154.6(4) . 2_665 ?
O17 Mo6 O21 66.6(4) . 2_665 ?
O9 Mo6 O21 101.9(7) . 2_665 ?
O8 Mo6 O21 59.9(5) . 2_665 ?
O6 Mo6 O21 91.2(7) . 2_665 ?
O24 Mo6 O21 50.4(4) . 2_665 ?
C12 N6 C11 117.4(11) . . ?
Mo5 O6 Mo6 137.6(8) . . ?
C6 C7 C8 111.4(12) . . ?
N4 C8 C7 111.6(12) . . ?
Mo1 O8 Mo6 137.1(8) 2_665 . ?
O2 C9 N4 122.1(12) . . ?
O2 C9 C10 117.3(10) . . ?
N4 C9 C10 120.5(11) . . ?
Mo6 O9 Mo3 137.3(11) . . ?
N5 C10 C11 119.7(13) . . ?
N5 C10 C9 112.9(10) . . ?
C11 C10 C9 127.3(12) . . ?
N6 C11 C10 121.5(14) . . ?
Mo2 O11 Mo3 137.3(5) 2_665 . ?
Mo3 O12 Mo1 136.6(5) . . ?
N6 C12 C13 121.8(14) . . ?
Mo1 O13 Mo2 135.5(5) . 2_665 ?
N5 C13 C12 120.8(13) . . ?
Mo4 O15 Mo1 137.4(10) . . ?
Mo6 O17 Mo4 136.2(6) . 2_665 ?
Mo2 O18 Mo4 136.4(10) . . ?
Si1 O19 O22 52.3(5) . 2_665 ?
Si1 O19 Mo2 128.2(6) . . ?
O22 O19 Mo2 76.2(6) 2_665 . ?
Si1 O19 Mo4 118.3(6) . . ?
O22 O19 Mo4 142.4(7) 2_665 . ?
Mo2 O19 Mo4 98.3(4) . . ?
Si1 O19 Mo5 115.2(6) . . ?
O22 O19 Mo5 125.1(7) 2_665 . ?
Mo2 O19 Mo5 97.1(4) . . ?
Mo4 O19 Mo5 92.4(4) . . ?
Mo4 O20 Mo5 137.5(7) . . ?
Si1 O21 O22 53.6(5) . . ?
Si1 O21 Mo1 127.8(6) . . ?
O22 O21 Mo1 74.5(6) . . ?
Si1 O21 Mo4 119.7(6) . . ?
O22 O21 Mo4 133.0(7) . . ?
Mo1 O21 Mo4 98.0(4) . . ?
Si1 O21 Mo6 115.7(6) . 2_665 ?
O22 O21 Mo6 134.6(7) . 2_665 ?
Mo1 O21 Mo6 96.0(4) . 2_665 ?
Mo4 O21 Mo6 91.9(4) . 2_665 ?
Si1 O22 O21 63.0(6) . . ?
Si1 O22 O19 62.4(6) . 2_665 ?
O21 O22 O19 104.3(8) . 2_665 ?
Si1 O22 O24 62.0(6) . . ?
O21 O22 O24 99.5(8) . . ?
O19 O22 O24 97.1(8) 2_665 . ?
Si1 O22 Mo1 127.0(6) . . ?
O21 O22 Mo1 64.3(5) . . ?
O19 O22 Mo1 128.8(7) 2_665 . ?
O24 O22 Mo1 133.2(6) . . ?
Si1 O22 Mo2 123.7(6) . 2_665 ?
O21 O22 Mo2 137.9(7) . 2_665 ?
O19 O22 Mo2 61.5(5) 2_665 2_665 ?
O24 O22 Mo2 120.7(6) . 2_665 ?
Mo1 O22 Mo2 92.8(4) . 2_665 ?
Si1 O22 Mo3 121.7(6) . . ?
O21 O22 Mo3 123.1(7) . . ?
O19 O22 Mo3 128.9(7) 2_665 . ?
O24 O22 Mo3 59.9(5) . . ?
Mo1 O22 Mo3 91.3(4) . . ?
Mo2 O22 Mo3 90.3(4) 2_665 . ?
Mo3 O23 Mo5 136.3(10) . . ?
Si1 O24 O22 49.4(5) . . ?
Si1 O24 Mo3 124.9(6) . . ?
O22 O24 Mo3 75.6(5) . . ?
Si1 O24 Mo6 117.4(6) . . ?
O22 O24 Mo6 130.2(7) . . ?
Mo3 O24 Mo6 99.9(5) . . ?
Si1 O24 Mo5 115.4(6) . . ?
O22 O24 Mo5 134.6(7) . . ?
Mo3 O24 Mo5 98.7(4) . . ?
Mo6 O24 Mo5 95.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.596
_refine_diff_density_min         -2.670
_refine_diff_density_rms         0.301
####################################################################### 
# 
# 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_liu3
_database_code_depnum_ccdc_archive 'CCDC 1045307'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H44 Cu2 Mo12 N12 O46 Si'
_chemical_formula_weight         2639.24

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'
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                   12.3112(7)
_cell_length_b                   12.7440(8)
_cell_length_c                   13.6911(9)
_cell_angle_alpha                110.9730(10)
_cell_angle_beta                 95.1360(10)
_cell_angle_gamma                117.4280(10)
_cell_volume                     1694.33(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3386
_exptl_absorpt_correction_T_max  0.4074
_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            9708
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5959
_reflns_number_gt                5466
_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)+(0.1022P)²+33.6855P] 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         5959
_refine_ls_number_parameters     496
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1980
_refine_ls_wR_factor_gt          0.1951
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.050
_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 -0.24366(9) -0.06625(10) 0.62724(9) 0.0344(3) Uani 1 1 d . . .
O1 O -0.8519(7) -0.4386(7) -0.5506(6) 0.0316(16) Uani 1 1 d . . .
N1 N -0.5644(9) -0.1217(10) 0.0686(7) 0.035(2) Uani 1 1 d . . .
C1 C -0.5126(12) -0.1956(13) 0.0544(10) 0.045(3) Uani 1 1 d . . .
Cu1 Cu -0.5000 0.0000 0.0000 0.0376(5) Uani 1 2 d S . .
O1W O -0.063(3) 0.170(3) 0.949(3) 0.220(12) Uani 1 1 d U . .
Mo2 Mo 0.05176(10) -0.25406(10) 0.35325(9) 0.0382(3) Uani 1 1 d . . .
N2 N -0.6750(9) -0.1743(10) -0.1678(8) 0.040(2) Uani 1 1 d . . .
Cu2 Cu -1.0000 -0.5000 -0.5000 0.0328(4) Uani 1 2 d S . .
C2 C -0.576(2) -0.392(2) -0.6499(17) 0.098(6) Uani 1 1 d U . .
H2A H -0.4980 -0.3547 -0.6635 0.118 Uiso 1 1 calc R . .
O2 O -0.3969(8) -0.0797(8) -0.0396(7) 0.0425(19) Uani 1 1 d . . .
Mo3 Mo -0.28047(9) -0.01340(10) 0.39294(9) 0.0368(3) Uani 1 1 d . . .
N3 N -0.6518(16) -0.3225(17) 0.1295(15) 0.083(5) Uani 1 1 d . . .
O3 O -0.0675(12) -0.1591(14) 0.4113(13) 0.030(3) Uani 0.50 1 d P . .
C3 C -0.5582(15) -0.2985(16) 0.0819(13) 0.058(4) Uani 1 1 d . . .
H3A H -0.5239 -0.3519 0.0674 0.070 Uiso 1 1 calc R . .
Mo4 Mo 0.02161(11) -0.08693(11) 0.71474(9) 0.0407(3) Uani 1 1 d . . .
N4 N -0.8755(8) -0.3641(8) -0.3565(7) 0.0306(19) Uani 1 1 d . . .
O4 O -0.0955(13) -0.0283(13) 0.3924(11) 0.027(3) Uani 0.50 1 d P . .
C4 C -0.6982(16) -0.2446(18) 0.1490(13) 0.066(4) Uani 1 1 d . . .
H4A H -0.7601 -0.2567 0.1853 0.079 Uiso 1 1 calc R . .
Mo5 Mo -0.21145(9) -0.32624(10) 0.45662(10) 0.0413(3) Uani 1 1 d . . .
O5 O -0.1085(12) 0.0293(14) 0.5288(12) 0.026(3) Uani 0.50 1 d P . .
C5 C -0.6562(13) -0.1448(14) 0.1161(11) 0.049(3) Uani 1 1 d . . .
H5A H -0.6929 -0.0936 0.1277 0.058 Uiso 1 1 calc R . .
N5 N -0.3427(13) -0.2156(14) -0.0130(10) 0.061(3) Uani 1 1 d . . .
H5B H -0.3565 -0.2709 0.0134 0.073 Uiso 1 1 calc R . .
Mo6 Mo -0.20952(10) -0.24802(11) 0.23393(9) 0.0456(3) Uani 1 1 d . . .
O6 O -0.0797(12) -0.0859(13) 0.5596(11) 0.026(3) Uani 0.50 1 d P . .
C6 C -0.8969(11) -0.3312(11) -0.2580(9) 0.036(2) Uani 1 1 d . . .
H6A H -0.9795 -0.3736 -0.2529 0.043 Uiso 1 1 calc R . .
N6 N -0.6426(8) -0.2852(9) -0.4967(8) 0.036(2) Uani 1 1 d . . .
H6B H -0.5738 -0.2258 -0.4422 0.043 Uiso 1 1 calc R . .
O7 O 0.1828(12) -0.1655(9) 0.4832(8) 0.076(4) Uani 1 1 d . . .
C7 C -0.7939(11) -0.2335(12) -0.1651(10) 0.040(3) Uani 1 1 d . . .
H7A H -0.8092 -0.2085 -0.0976 0.048 Uiso 1 1 calc R . .
O8 O 0.1617(13) -0.1142(9) 0.3142(9) 0.080(4) Uani 1 1 d . . .
C8 C -0.6549(11) -0.2046(11) -0.2646(9) 0.035(2) Uani 1 1 d . . .
H8A H -0.5720 -0.1605 -0.2686 0.042 Uiso 1 1 calc R . .
Si9 Si 0.0000 0.0000 0.5000 0.0263(8) Uani 1 2 d S . .
O9 O -0.0828(12) -0.2850(18) 0.2392(12) 0.103(6) Uani 1 1 d . . .
C9 C -0.7547(9) -0.3003(10) -0.3591(8) 0.026(2) Uani 1 1 d . . .
C10 C -0.7487(9) -0.3451(9) -0.4748(8) 0.027(2) Uani 1 1 d . . .
O10 O -0.1645(12) 0.0747(10) 0.3212(12) 0.090(5) Uani 1 1 d . . .
O11 O -0.1188(13) -0.1082(10) 0.2048(13) 0.092(5) Uani 1 1 d . . .
C11 C -0.632(3) -0.509(4) -0.667(3) 0.151(11) Uani 1 1 d U . .
H11A H -0.6890 -0.5334 -0.6283 0.181 Uiso 1 1 calc R . .
O12 O -0.3098(13) -0.1709(10) 0.2884(13) 0.091(5) Uani 1 1 d . . .
C12 C -0.4148(12) -0.1624(14) -0.0018(10) 0.042(3) Uani 1 1 d . . .
O13 O -0.3276(13) -0.0776(9) 0.4912(9) 0.086(4) Uani 1 1 d . . .
C13 C -0.258(3) -0.305(3) -0.150(3) 0.145(10) Uani 1 1 d U . .
H13A H -0.2641 -0.3650 -0.1202 0.174 Uiso 1 1 calc R . .
H13B H -0.1838 -0.2811 -0.1765 0.174 Uiso 1 1 calc R . .
C14 C -0.385(3) -0.378(3) -0.251(3) 0.142(10) Uani 1 1 d U . .
H14A H -0.4624 -0.4143 -0.2303 0.170 Uiso 1 1 calc R . .
H14B H -0.3843 -0.3199 -0.2813 0.170 Uiso 1 1 calc R . .
O15 O -0.2711(12) -0.3389(19) 0.3230(13) 0.111(6) Uani 1 1 d . . .
C15 C -0.6323(14) -0.3120(16) -0.6082(12) 0.060(4) Uani 1 1 d . . .
H15A H -0.7176 -0.3565 -0.6584 0.073 Uiso 1 1 calc R . .
H15B H -0.5807 -0.2278 -0.6094 0.073 Uiso 1 1 calc R . .
O16 O -0.0919(11) -0.2537(11) 0.6007(10) 0.087(4) Uani 1 1 d . . .
C16 C -0.2427(16) -0.1880(17) -0.0660(13) 0.064(4) Uani 1 1 d . . .
H16A H -0.2423 -0.1311 -0.0978 0.076 Uiso 1 1 calc R . .
H16B H -0.1599 -0.1402 -0.0108 0.076 Uiso 1 1 calc R . .
O17 O -0.1246(12) -0.0622(11) 0.7214(10) 0.089(5) Uani 1 1 d . . .
O18 O 0.0775(10) -0.3700(9) 0.2752(8) 0.052(2) Uani 1 1 d . . .
O19 O -0.3054(9) -0.4809(8) 0.4349(9) 0.053(2) Uani 1 1 d . . .
O20 O -0.2913(12) -0.2465(12) 0.5258(10) 0.089(5) Uani 1 1 d . . .
O21 O -0.0719(11) -0.3427(18) 0.4076(12) 0.098(5) Uani 1 1 d . . .
O22 O -0.3163(9) -0.3631(9) 0.1113(7) 0.052(2) Uani 1 1 d . . .
O23 O 0.0318(11) -0.1166(12) 0.8230(8) 0.063(3) Uani 1 1 d . . .
O24 O -0.4081(8) -0.0117(9) 0.3424(9) 0.057(3) Uani 1 1 d . . .
O25 O -0.3684(8) -0.1057(10) 0.6759(8) 0.057(3) 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 O25 1.664(8) . ?
Mo1 O8 1.830(10) 2_556 ?
Mo1 O17 1.832(10) . ?
Mo1 O13 1.970(10) . ?
Mo1 O20 1.970(10) . ?
Mo1 O6 2.372(13) . ?
Mo1 O5 2.404(13) . ?
O1 C10 1.263(12) . ?
O1 Cu2 1.928(7) . ?
N1 C5 1.323(16) . ?
N1 C1 1.331(16) . ?
N1 Cu1 1.990(10) . ?
C1 C3 1.37(2) . ?
C1 C12 1.466(18) . ?
Cu1 O2 1.963(8) 2_455 ?
Cu1 O2 1.963(8) . ?
Cu1 N1 1.990(10) 2_455 ?
Cu1 N2 2.430(9) . ?
Cu1 N2 2.430(9) 2_455 ?
Mo2 O18 1.670(9) . ?
Mo2 O21 1.835(11) . ?
Mo2 O7 1.848(10) . ?
Mo2 O9 1.958(11) . ?
Mo2 O8 1.971(10) . ?
Mo2 O3 2.326(13) . ?
Mo2 O5 2.438(14) 2_556 ?
N2 C7 1.314(15) . ?
N2 C8 1.321(15) . ?
Cu2 O1 1.928(7) 2_344 ?
Cu2 N4 1.946(9) . ?
Cu2 N4 1.946(9) 2_344 ?
C2 C11 1.23(4) . ?
C2 C15 1.47(2) . ?
O2 C12 1.274(15) . ?
Mo3 O24 1.672(8) . ?
Mo3 O13 1.819(10) . ?
Mo3 O12 1.841(10) . ?
Mo3 O10 1.957(10) . ?
Mo3 O7 1.965(9) 2_556 ?
Mo3 O4 2.372(13) . ?
Mo3 O5 2.398(13) . ?
N3 C4 1.32(2) . ?
N3 C3 1.34(2) . ?
O3 Si9 1.667(14) . ?
O3 Mo6 2.384(15) . ?
O3 Mo5 2.393(13) . ?
Mo4 O23 1.663(9) . ?
Mo4 O10 1.821(11) 2_556 ?
Mo4 O16 1.846(10) . ?
Mo4 O17 1.969(11) . ?
Mo4 O11 1.973(11) 2_556 ?
Mo4 O6 2.372(13) . ?
Mo4 O4 2.385(14) 2_556 ?
N4 C9 1.338(13) . ?
N4 C6 1.351(15) . ?
O4 Si9 1.612(13) . ?
O4 O5 1.80(2) . ?
O4 Mo4 2.385(14) 2_556 ?
O4 Mo6 2.450(14) . ?
C4 C5 1.39(2) . ?
Mo5 O19 1.653(8) . ?
Mo5 O20 1.814(11) . ?
Mo5 O15 1.831(11) . ?
Mo5 O16 1.958(11) . ?
Mo5 O21 1.971(10) . ?
Mo5 O6 2.434(14) . ?
O5 Si9 1.589(13) . ?
O5 Mo2 2.438(14) 2_556 ?
N5 C12 1.333(16) . ?
N5 C16 1.453(19) . ?
Mo6 O22 1.662(8) . ?
Mo6 O11 1.826(11) . ?
Mo6 O9 1.828(12) . ?
Mo6 O15 1.942(10) . ?
Mo6 O12 1.950(10) . ?
O6 Si9 1.619(13) . ?
C6 C7 1.378(16) . ?
N6 C10 1.301(14) . ?
N6 C15 1.471(17) . ?
O7 Mo3 1.965(9) 2_556 ?
O8 Mo1 1.830(10) 2_556 ?
C8 C9 1.370(14) . ?
Si9 O5 1.589(13) 2_556 ?
Si9 O4 1.612(13) 2_556 ?
Si9 O6 1.619(13) 2_556 ?
Si9 O3 1.667(14) 2_556 ?
C9 C10 1.501(15) . ?
O10 Mo4 1.821(11) 2_556 ?
O11 Mo4 1.973(11) 2_556 ?
C11 C14 1.59(4) 2_444 ?
C13 C16 1.43(3) . ?
C13 C14 1.60(4) . ?
C14 C11 1.59(4) 2_444 ?

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
O25 Mo1 O8 102.6(6) . 2_556 ?
O25 Mo1 O17 103.9(6) . . ?
O8 Mo1 O17 94.2(5) 2_556 . ?
O25 Mo1 O13 97.3(6) . . ?
O8 Mo1 O13 88.2(4) 2_556 . ?
O17 Mo1 O13 157.5(7) . . ?
O25 Mo1 O20 98.6(6) . . ?
O8 Mo1 O20 157.5(7) 2_556 . ?
O17 Mo1 O20 87.9(4) . . ?
O13 Mo1 O20 81.6(5) . . ?
O25 Mo1 O6 157.8(5) . . ?
O8 Mo1 O6 97.0(6) 2_556 . ?
O17 Mo1 O6 64.2(6) . . ?
O13 Mo1 O6 93.4(6) . . ?
O20 Mo1 O6 63.8(5) . . ?
O25 Mo1 O5 155.5(5) . . ?
O8 Mo1 O5 65.4(5) 2_556 . ?
O17 Mo1 O5 98.5(6) . . ?
O13 Mo1 O5 62.3(5) . . ?
O20 Mo1 O5 92.1(6) . . ?
O6 Mo1 O5 45.1(4) . . ?
C10 O1 Cu2 113.9(7) . . ?
C5 N1 C1 118.2(11) . . ?
C5 N1 Cu1 128.8(9) . . ?
C1 N1 Cu1 112.8(8) . . ?
N1 C1 C3 121.2(13) . . ?
N1 C1 C12 112.6(11) . . ?
C3 C1 C12 125.9(13) . . ?
O2 Cu1 O2 179.998(1) 2_455 . ?
O2 Cu1 N1 82.8(4) 2_455 2_455 ?
O2 Cu1 N1 97.2(4) . 2_455 ?
O2 Cu1 N1 97.2(4) 2_455 . ?
O2 Cu1 N1 82.8(4) . . ?
N1 Cu1 N1 179.999(1) 2_455 . ?
O2 Cu1 N2 89.4(3) 2_455 . ?
O2 Cu1 N2 90.6(3) . . ?
N1 Cu1 N2 91.6(4) 2_455 . ?
N1 Cu1 N2 88.4(4) . . ?
O2 Cu1 N2 90.6(3) 2_455 2_455 ?
O2 Cu1 N2 89.4(3) . 2_455 ?
N1 Cu1 N2 88.4(4) 2_455 2_455 ?
N1 Cu1 N2 91.6(4) . 2_455 ?
N2 Cu1 N2 179.999(1) . 2_455 ?
O18 Mo2 O21 102.9(6) . . ?
O18 Mo2 O7 102.1(5) . . ?
O21 Mo2 O7 93.7(5) . . ?
O18 Mo2 O9 97.6(6) . . ?
O21 Mo2 O9 89.4(5) . . ?
O7 Mo2 O9 158.7(7) . . ?
O18 Mo2 O8 97.5(5) . . ?
O21 Mo2 O8 158.8(6) . . ?
O7 Mo2 O8 87.5(4) . . ?
O9 Mo2 O8 82.2(5) . . ?
O18 Mo2 O3 156.4(5) . . ?
O21 Mo2 O3 65.8(6) . . ?
O7 Mo2 O3 99.3(6) . . ?
O9 Mo2 O3 62.9(6) . . ?
O8 Mo2 O3 93.1(5) . . ?
O18 Mo2 O5 155.7(5) . 2_556 ?
O21 Mo2 O5 98.5(6) . 2_556 ?
O7 Mo2 O5 64.8(5) . 2_556 ?
O9 Mo2 O5 94.0(6) . 2_556 ?
O8 Mo2 O5 63.0(5) . 2_556 ?
O3 Mo2 O5 46.2(5) . 2_556 ?
C7 N2 C8 118.2(10) . . ?
C7 N2 Cu1 120.3(8) . . ?
C8 N2 Cu1 121.2(7) . . ?
O1 Cu2 O1 180.0(5) 2_344 . ?
O1 Cu2 N4 96.6(3) 2_344 . ?
O1 Cu2 N4 83.4(3) . . ?
O1 Cu2 N4 83.4(3) 2_344 2_344 ?
O1 Cu2 N4 96.6(3) . 2_344 ?
N4 Cu2 N4 180.0(4) . 2_344 ?
C11 C2 C15 121(3) . . ?
C12 O2 Cu1 112.0(7) . . ?
O24 Mo3 O13 103.0(6) . . ?
O24 Mo3 O12 102.1(6) . . ?
O13 Mo3 O12 93.9(5) . . ?
O24 Mo3 O10 98.9(6) . . ?
O13 Mo3 O10 157.3(7) . . ?
O12 Mo3 O10 87.4(4) . . ?
O24 Mo3 O7 98.9(5) . 2_556 ?
O13 Mo3 O7 88.0(4) . 2_556 ?
O12 Mo3 O7 157.8(6) . 2_556 ?
O10 Mo3 O7 82.6(5) . 2_556 ?
O24 Mo3 O4 156.8(5) . . ?
O13 Mo3 O4 97.3(6) . . ?
O12 Mo3 O4 65.2(6) . . ?
O10 Mo3 O4 62.7(5) . . ?
O7 Mo3 O4 92.7(5) 2_556 . ?
O24 Mo3 O5 158.0(5) . . ?
O13 Mo3 O5 64.2(5) . . ?
O12 Mo3 O5 96.8(6) . . ?
O10 Mo3 O5 93.1(6) . . ?
O7 Mo3 O5 64.3(5) 2_556 . ?
O4 Mo3 O5 44.3(5) . . ?
C4 N3 C3 118.1(14) . . ?
Si9 O3 Mo2 122.9(7) . . ?
Si9 O3 Mo6 120.3(6) . . ?
Mo2 O3 Mo6 96.8(6) . . ?
Si9 O3 Mo5 119.2(8) . . ?
Mo2 O3 Mo5 96.3(5) . . ?
Mo6 O3 Mo5 95.3(5) . . ?
N3 C3 C1 120.6(14) . . ?
O23 Mo4 O10 102.3(6) . 2_556 ?
O23 Mo4 O16 102.9(6) . . ?
O10 Mo4 O16 95.2(5) 2_556 . ?
O23 Mo4 O17 98.0(6) . . ?
O10 Mo4 O17 158.2(7) 2_556 . ?
O16 Mo4 O17 87.6(4) . . ?
O23 Mo4 O11 97.6(6) . 2_556 ?
O10 Mo4 O11 88.3(5) 2_556 2_556 ?
O16 Mo4 O11 157.9(6) . 2_556 ?
O17 Mo4 O11 81.4(5) . 2_556 ?
O23 Mo4 O6 157.0(5) . . ?
O10 Mo4 O6 98.9(6) 2_556 . ?
O16 Mo4 O6 66.1(5) . . ?
O17 Mo4 O6 62.5(5) . . ?
O11 Mo4 O6 91.7(6) 2_556 . ?
O23 Mo4 O4 156.0(5) . 2_556 ?
O10 Mo4 O4 64.0(6) 2_556 2_556 ?
O16 Mo4 O4 98.1(6) . 2_556 ?
O17 Mo4 O4 94.2(6) . 2_556 ?
O11 Mo4 O4 63.9(5) 2_556 2_556 ?
O6 Mo4 O4 45.4(4) . 2_556 ?
C9 N4 C6 118.2(9) . . ?
C9 N4 Cu2 113.8(7) . . ?
C6 N4 Cu2 128.0(7) . . ?
Si9 O4 O5 55.2(6) . . ?
Si9 O4 Mo3 123.7(8) . . ?
O5 O4 Mo3 68.6(6) . . ?
Si9 O4 Mo4 122.4(7) . 2_556 ?
O5 O4 Mo4 130.3(8) . 2_556 ?
Mo3 O4 Mo4 95.5(4) . 2_556 ?
Si9 O4 Mo6 119.4(7) . . ?
O5 O4 Mo6 132.4(8) . . ?
Mo3 O4 Mo6 94.5(5) . . ?
Mo4 O4 Mo6 94.1(5) 2_556 . ?
N3 C4 C5 121.1(14) . . ?
O19 Mo5 O20 102.5(6) . . ?
O19 Mo5 O15 100.6(7) . . ?
O20 Mo5 O15 94.9(6) . . ?
O19 Mo5 O16 99.8(5) . . ?
O20 Mo5 O16 88.3(5) . . ?
O15 Mo5 O16 158.1(7) . . ?
O19 Mo5 O21 97.9(6) . . ?
O20 Mo5 O21 158.4(7) . . ?
O15 Mo5 O21 88.1(5) . . ?
O16 Mo5 O21 81.4(5) . . ?
O19 Mo5 O3 153.8(5) . . ?
O20 Mo5 O3 99.7(6) . . ?
O15 Mo5 O3 63.6(6) . . ?
O16 Mo5 O3 94.6(6) . . ?
O21 Mo5 O3 62.6(5) . . ?
O19 Mo5 O6 157.6(5) . . ?
O20 Mo5 O6 64.3(5) . . ?
O15 Mo5 O6 98.6(7) . . ?
O16 Mo5 O6 63.4(5) . . ?
O21 Mo5 O6 94.2(6) . . ?
O3 Mo5 O6 47.9(5) . . ?
Si9 O5 O4 56.5(6) . . ?
Si9 O5 Mo3 123.4(8) . . ?
O4 O5 Mo3 67.1(6) . . ?
Si9 O5 Mo1 122.4(7) . . ?
O4 O5 Mo1 136.2(8) . . ?
Mo3 O5 Mo1 94.9(4) . . ?
Si9 O5 Mo2 120.4(7) . 2_556 ?
O4 O5 Mo2 125.6(8) . 2_556 ?
Mo3 O5 Mo2 94.2(5) . 2_556 ?
Mo1 O5 Mo2 94.0(5) . 2_556 ?
N1 C5 C4 120.7(14) . . ?
C12 N5 C16 125.5(13) . . ?
O22 Mo6 O11 101.3(6) . . ?
O22 Mo6 O9 103.6(6) . . ?
O11 Mo6 O9 93.9(6) . . ?
O22 Mo6 O15 100.6(6) . . ?
O11 Mo6 O15 157.2(7) . . ?
O9 Mo6 O15 86.9(4) . . ?
O22 Mo6 O12 97.5(6) . . ?
O11 Mo6 O12 87.9(5) . . ?
O9 Mo6 O12 157.9(7) . . ?
O15 Mo6 O12 83.1(5) . . ?
O22 Mo6 O3 157.7(5) . . ?
O11 Mo6 O3 97.7(6) . . ?
O9 Mo6 O3 63.2(6) . . ?
O15 Mo6 O3 62.5(6) . . ?
O12 Mo6 O3 94.8(6) . . ?
O22 Mo6 O4 154.1(4) . . ?
O11 Mo6 O4 64.2(5) . . ?
O9 Mo6 O4 99.0(6) . . ?
O15 Mo6 O4 93.2(7) . . ?
O12 Mo6 O4 62.2(5) . . ?
O3 Mo6 O4 47.4(4) . . ?
Si9 O6 Mo1 122.7(7) . . ?
Si9 O6 Mo4 122.7(7) . . ?
Mo1 O6 Mo4 96.3(5) . . ?
Si9 O6 Mo5 119.3(7) . . ?
Mo1 O6 Mo5 94.4(5) . . ?
Mo4 O6 Mo5 94.4(4) . . ?
N4 C6 C7 118.8(10) . . ?
C10 N6 C15 124.6(10) . . ?
Mo2 O7 Mo3 136.6(7) . 2_556 ?
N2 C7 C6 122.7(11) . . ?
Mo1 O8 Mo2 137.4(7) 2_556 . ?
N2 C8 C9 120.9(11) . . ?
O5 Si9 O5 179.999(4) 2_556 . ?
O5 Si9 O4 111.7(7) 2_556 . ?
O5 Si9 O4 68.3(7) . . ?
O5 Si9 O4 68.3(7) 2_556 2_556 ?
O5 Si9 O4 111.7(7) . 2_556 ?
O4 Si9 O4 180.0(11) . 2_556 ?
O5 Si9 O6 110.4(6) 2_556 . ?
O5 Si9 O6 69.6(6) . . ?
O4 Si9 O6 110.7(7) . . ?
O4 Si9 O6 69.3(7) 2_556 . ?
O5 Si9 O6 69.6(6) 2_556 2_556 ?
O5 Si9 O6 110.4(6) . 2_556 ?
O4 Si9 O6 69.3(7) . 2_556 ?
O4 Si9 O6 110.7(7) 2_556 2_556 ?
O6 Si9 O6 179.998(3) . 2_556 ?
O5 Si9 O3 109.8(7) 2_556 2_556 ?
O5 Si9 O3 70.2(7) . 2_556 ?
O4 Si9 O3 107.3(7) . 2_556 ?
O4 Si9 O3 72.7(7) 2_556 2_556 ?
O6 Si9 O3 106.8(7) . 2_556 ?
O6 Si9 O3 73.2(7) 2_556 2_556 ?
O5 Si9 O3 70.2(7) 2_556 . ?
O5 Si9 O3 109.8(7) . . ?
O4 Si9 O3 72.7(7) . . ?
O4 Si9 O3 107.3(7) 2_556 . ?
O6 Si9 O3 73.2(7) . . ?
O6 Si9 O3 106.8(7) 2_556 . ?
O3 Si9 O3 179.999(2) 2_556 . ?
Mo6 O9 Mo2 136.9(9) . . ?
N4 C9 C8 121.1(10) . . ?
N4 C9 C10 111.3(8) . . ?
C8 C9 C10 127.5(10) . . ?
O1 C10 N6 121.2(10) . . ?
O1 C10 C9 117.5(9) . . ?
N6 C10 C9 121.2(9) . . ?
Mo4 O10 Mo3 137.5(8) 2_556 . ?
Mo6 O11 Mo4 137.4(8) . 2_556 ?
C2 C11 C14 127(3) . 2_444 ?
Mo3 O12 Mo6 138.0(8) . . ?
O2 C12 N5 119.0(12) . . ?
O2 C12 C1 119.6(10) . . ?
N5 C12 C1 121.4(12) . . ?
Mo3 O13 Mo1 138.0(8) . . ?
C16 C13 C14 111(3) . . ?
C11 C14 C13 99(3) 2_444 . ?
Mo5 O15 Mo6 138.6(9) . . ?
C2 C15 N6 116.1(16) . . ?
Mo4 O16 Mo5 135.9(7) . . ?
C13 C16 N5 113.4(19) . . ?
Mo1 O17 Mo4 136.7(8) . . ?
Mo5 O20 Mo1 137.3(8) . . ?
Mo2 O21 Mo5 134.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.192


