# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_k
_database_code_depnum_ccdc_archive 'CCDC 1006424'
_audit_update_record             
;
2014-06-03 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H29 Cu3 N8 O40 Si W12'
_chemical_formula_weight         3602.46

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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 '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                   10.882(2)
_cell_length_b                   11.587(2)
_cell_length_c                   13.273(3)
_cell_angle_alpha                113.30(3)
_cell_angle_beta                 96.32(3)
_cell_angle_gamma                95.46(3)
_cell_volume                     1510.0(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1591
_exptl_absorpt_coefficient_mu    23.901
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0453
_exptl_absorpt_correction_T_max  0.0771
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14690
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6788
_reflns_number_gt                4660
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0523P)²+59.2044P] 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         6788
_refine_ls_number_parameters     473
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1758
_refine_ls_wR_factor_gt          0.1515
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W -1.77017(7) 0.76784(9) 0.39947(8) 0.0339(2) Uani 1 1 d . . .
W2 W -1.21067(7) 0.92003(8) 0.41455(8) 0.0288(2) Uani 1 1 d . . .
W3 W -1.74448(7) 1.01494(8) 0.30891(7) 0.0263(2) Uani 1 1 d . . .
W4 W -1.45494(9) 0.93546(8) 0.22535(7) 0.0343(2) Uani 1 1 d . . .
W5 W -1.52683(10) 0.75198(10) 0.59084(9) 0.0419(3) Uani 1 1 d . . .
W6 W -1.47998(10) 0.68838(9) 0.31748(8) 0.0441(3) Uani 1 1 d . . .
Si1 Si -1.5000 1.0000 0.5000 0.0245(16) Uani 1 2 d S . .
O1 O -1.562(2) 0.846(2) 0.463(2) 0.019(5) Uani 0.50 1 d PU . .
O2 O -1.638(2) 0.981(2) 0.463(2) 0.026(6) Uani 0.50 1 d PU . .
O3 O -1.424(2) 0.921(2) 0.398(2) 0.023(5) Uani 0.50 1 d PU . .
O4 O -1.541(2) 1.035(2) 0.395(2) 0.015(5) Uani 0.50 1 d P . .
O20 O -1.688(2) 0.734(3) 0.5176(16) 0.102(10) Uani 1 1 d . . .
O21 O -1.289(3) 0.939(3) 0.289(2) 0.096(8) Uani 1 1 d U . .
O22 O -1.075(2) 0.883(2) 0.3710(18) 0.073(7) Uani 1 1 d . . .
O5 O -1.8937(16) 0.6576(14) 0.3506(14) 0.045(4) Uani 1 1 d . . .
O6 O -1.863(2) 1.017(2) 0.2161(16) 0.075(7) Uani 1 1 d . . .
O7 O -1.7918(18) 0.8556(14) 0.3053(14) 0.044(4) Uani 1 1 d . . .
O8 O -1.4303(16) 1.1128(16) 0.287(2) 0.074(7) Uani 1 1 d . . .
O9 O -1.4366(14) 0.901(2) 0.0913(14) 0.055(5) Uani 1 1 d . . .
O10 O -1.305(3) 0.757(3) 0.360(2) 0.095(8) Uani 1 1 d U . .
O11 O -1.485(2) 0.766(2) 0.215(2) 0.088(7) Uani 1 1 d U . .
O12 O -1.627(2) 0.9398(15) 0.217(2) 0.089(9) Uani 1 1 d . . .
O13 O -1.472(2) 0.666(2) 0.450(2) 0.083(7) Uani 1 1 d U . .
O14 O -1.4737(13) 0.5408(13) 0.2274(13) 0.032(3) Uani 1 1 d . . .
O15 O -1.5396(16) 0.6348(17) 0.6344(18) 0.052(5) Uani 1 1 d . . .
O16 O -1.189(2) 0.9168(15) 0.5595(15) 0.055(5) Uani 1 1 d . . .
O17 O -1.8240(17) 0.9028(16) 0.5146(13) 0.046(4) Uani 1 1 d . . .
O18 O -1.6373(19) 1.175(2) 0.3558(18) 0.064(5) Uani 1 1 d U . .
O19 O -1.662(3) 0.677(3) 0.310(3) 0.114(9) Uani 1 1 d U . .
Cu1 Cu 0.4846(2) 0.2744(4) 0.1304(3) 0.0566(10) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 0.0000 0.079(2) Uani 1 2 d S . .
N1 N 0.6553(16) 0.2691(17) 0.1288(15) 0.032(4) Uani 1 1 d U . .
N3 N 0.6764(19) 0.500(3) 0.010(2) 0.058(7) Uani 1 1 d . . .
C1 C 0.701(2) 0.165(2) 0.064(2) 0.038(5) Uani 1 1 d . . .
H1A H 0.6448 0.0925 0.0193 0.045 Uiso 1 1 calc R . .
C2 C 0.827(2) 0.162(2) 0.062(2) 0.041(6) Uani 1 1 d . . .
H2A H 0.8538 0.0890 0.0137 0.049 Uiso 1 1 calc R . .
C3 C 0.9138(18) 0.2651(18) 0.1297(17) 0.024(4) Uani 1 1 d U . .
C9 C 0.8682(17) 0.3715(19) 0.1963(17) 0.026(4) Uani 1 1 d . . .
H9A H 0.9238 0.4437 0.2436 0.031 Uiso 1 1 calc R . .
C10 C 0.7419(18) 0.372(2) 0.194(2) 0.036(5) Uani 1 1 d . . .
H10A H 0.7144 0.4465 0.2385 0.043 Uiso 1 1 calc R . .
C11 C 0.720(2) 0.398(2) -0.062(2) 0.042(5) Uani 1 1 d U . .
H11A H 0.6634 0.3273 -0.1109 0.050 Uiso 1 1 calc R . .
C12 C 0.848(2) 0.398(2) -0.062(2) 0.047(7) Uani 1 1 d . . .
H12A H 0.8755 0.3257 -0.1106 0.057 Uiso 1 1 calc R . .
C13 C 0.9304(17) 0.497(2) 0.0025(18) 0.028(4) Uani 1 1 d . . .
C14 C 0.887(3) 0.607(3) 0.079(3) 0.053(8) Uani 1 1 d . . .
H14A H 0.9407 0.6799 0.1282 0.064 Uiso 1 1 calc R . .
C15 C 0.760(2) 0.596(2) 0.073(2) 0.044(6) Uani 1 1 d . . .
H15A H 0.7302 0.6661 0.1212 0.053 Uiso 1 1 calc R . .
C4 C 1.0470(17) 0.264(2) 0.1285(19) 0.032(5) Uani 1 1 d . . .
C8 C 1.1394(17) 0.3480(19) 0.219(2) 0.034(5) Uani 1 1 d . . .
H8A H 1.1137 0.4046 0.2824 0.041 Uiso 1 1 calc R . .
C5 C 1.0955(18) 0.180(2) 0.0399(19) 0.031(5) Uani 1 1 d . . .
H5A H 1.0414 0.1181 -0.0203 0.037 Uiso 1 1 calc R . .
C6 C 1.2248(19) 0.189(3) 0.040(2) 0.043(6) Uani 1 1 d . . .
H6A H 1.2534 0.1391 -0.0242 0.052 Uiso 1 1 calc R . .
C7 C 1.265(2) 0.348(3) 0.216(2) 0.057(8) Uani 1 1 d . . .
H7A H 1.3220 0.4076 0.2757 0.068 Uiso 1 1 calc R . .
N2 N 1.3077(15) 0.2627(18) 0.1274(18) 0.037(5) Uani 1 1 d . . .
N5 N -0.983(4) 0.572(5) 0.533(5) 0.105(18) Uani 0.50 1 d PGU . .
C17 C -0.996(5) 0.712(5) 0.577(5) 0.090(18) Uani 0.50 1 d PGU . .
C18 C -1.133(5) 0.721(4) 0.549(5) 0.23(3) Uani 0.50 1 d PGU . .
N4 N -1.204(4) 0.587(4) 0.488(3) 0.052(12) Uani 0.50 1 d PG . .
C20 C -1.111(4) 0.495(3) 0.478(4) 0.055(13) Uani 0.50 1 d PGU . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O5 1.639(15) . ?
W1 O19 1.86(3) . ?
W1 O17 1.899(16) . ?
W1 O7 1.906(16) . ?
W1 O20 1.914(19) . ?
W1 O1 2.29(2) . ?
W1 O2 2.51(3) . ?
W2 O22 1.672(18) . ?
W2 O17 1.868(17) 2_276 ?
W2 O10 1.88(3) . ?
W2 O21 1.89(3) . ?
W2 O16 1.928(18) . ?
W2 O3 2.31(3) . ?
W2 O2 2.48(2) 2_276 ?
W3 O6 1.689(18) . ?
W3 O7 1.850(15) . ?
W3 O16 1.867(17) 2_276 ?
W3 O12 1.897(18) . ?
W3 O18 1.92(2) . ?
W3 O4 2.32(2) . ?
W3 O2 2.42(3) . ?
W4 O9 1.700(16) . ?
W4 O8 1.865(17) . ?
W4 O12 1.87(2) . ?
W4 O21 1.89(3) . ?
W4 O11 1.91(3) . ?
W4 O3 2.35(3) . ?
W4 O4 2.43(2) . ?
W5 O15 1.673(16) . ?
W5 O18 1.84(2) 2_276 ?
W5 O20 1.86(2) . ?
W5 O8 1.894(17) 2_276 ?
W5 O13 1.93(2) . ?
W5 O1 2.36(2) . ?
W5 O4 2.44(2) 2_276 ?
W6 O14 1.667(13) . ?
W6 O13 1.87(3) . ?
W6 O11 1.90(3) . ?
W6 O10 1.92(3) . ?
W6 O19 1.96(3) . ?
W6 O1 2.40(2) . ?
W6 O3 2.46(3) . ?
Si1 O2 1.49(3) . ?
Si1 O2 1.49(3) 2_276 ?
Si1 O4 1.63(3) . ?
Si1 O4 1.63(3) 2_276 ?
Si1 O3 1.66(2) 2_276 ?
Si1 O3 1.66(2) . ?
Si1 O1 1.70(2) . ?
Si1 O1 1.70(2) 2_276 ?
O1 O2 1.84(4) . ?
O2 O4 1.68(4) . ?
O2 O3 1.76(4) 2_276 ?
O2 W2 2.48(2) 2_276 ?
O3 O2 1.76(4) 2_276 ?
O4 W5 2.44(2) 2_276 ?
O8 W5 1.894(17) 2_276 ?
O16 W3 1.867(16) 2_276 ?
O17 W2 1.868(17) 2_276 ?
O18 W5 1.84(2) 2_276 ?
Cu1 N1 1.866(17) . ?
Cu1 N2 1.912(16) 1_455 ?
Cu2 N3 1.910(19) 2_665 ?
Cu2 N3 1.910(19) . ?
N1 C1 1.35(3) . ?
N1 C10 1.36(3) . ?
N3 C15 1.29(4) . ?
N3 C11 1.35(3) . ?
C1 C2 1.38(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.37(3) . ?
C2 H2A 0.9300 . ?
C3 C9 1.38(3) . ?
C3 C4 1.45(3) . ?
C9 C10 1.37(3) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.40(3) . ?
C11 H11A 0.9300 . ?
C12 C13 1.31(3) . ?
C12 H12A 0.9300 . ?
C13 C14 1.45(3) . ?
C13 C13 1.52(4) 2_765 ?
C14 C15 1.36(3) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C4 C5 1.39(3) . ?
C4 C8 1.42(3) . ?
C8 C7 1.37(3) . ?
C8 H8A 0.9300 . ?
C5 C6 1.40(3) . ?
C5 H5A 0.9300 . ?
C6 N2 1.31(3) . ?
C6 H6A 0.9300 . ?
C7 N2 1.37(3) . ?
C7 H7A 0.9300 . ?
N2 Cu1 1.912(16) 1_655 ?
N5 C20 1.33(11) 2_366 ?
N5 C20 1.52(3) . ?
N5 C17 1.52(3) . ?
N5 N5 1.54(10) 2_366 ?
C17 C18 1.52(3) . ?
C18 N4 1.52(3) . ?
N4 C20 1.52(3) . ?
C20 N5 1.33(7) 2_366 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 W1 O19 97.9(12) . . ?
O5 W1 O17 103.3(8) . . ?
O19 W1 O17 158.6(12) . . ?
O5 W1 O7 101.9(9) . . ?
O19 W1 O7 88.5(11) . . ?
O17 W1 O7 89.6(7) . . ?
O5 W1 O20 102.3(12) . . ?
O19 W1 O20 88.1(11) . . ?
O17 W1 O20 85.0(8) . . ?
O7 W1 O20 155.8(12) . . ?
O5 W1 O1 155.3(9) . . ?
O19 W1 O1 65.1(12) . . ?
O17 W1 O1 94.0(8) . . ?
O7 W1 O1 95.7(9) . . ?
O20 W1 O1 61.4(11) . . ?
O5 W1 O2 159.9(9) . . ?
O19 W1 O2 95.4(11) . . ?
O17 W1 O2 64.9(8) . . ?
O7 W1 O2 63.4(8) . . ?
O20 W1 O2 93.1(12) . . ?
O1 W1 O2 44.8(9) . . ?
O22 W2 O17 101.7(10) . 2_276 ?
O22 W2 O10 100.6(12) . . ?
O17 W2 O10 157.7(10) 2_276 . ?
O22 W2 O21 98.5(11) . . ?
O17 W2 O21 87.6(10) 2_276 . ?
O10 W2 O21 88.5(12) . . ?
O22 W2 O16 102.9(10) . . ?
O17 W2 O16 88.0(7) 2_276 . ?
O10 W2 O16 87.6(10) . . ?
O21 W2 O16 158.5(10) . . ?
O22 W2 O3 156.4(11) . . ?
O17 W2 O3 92.4(9) 2_276 . ?
O10 W2 O3 66.5(10) . . ?
O21 W2 O3 62.9(10) . . ?
O16 W2 O3 96.3(9) . . ?
O22 W2 O2 160.6(11) . 2_276 ?
O17 W2 O2 65.7(8) 2_276 2_276 ?
O10 W2 O2 92.9(10) . 2_276 ?
O21 W2 O2 95.7(10) . 2_276 ?
O16 W2 O2 63.5(9) . 2_276 ?
O3 W2 O2 42.8(9) . 2_276 ?
O6 W3 O7 99.5(11) . . ?
O6 W3 O16 100.8(10) . 2_276 ?
O7 W3 O16 87.9(7) . 2_276 ?
O6 W3 O12 102.3(12) . . ?
O7 W3 O12 86.4(7) . . ?
O16 W3 O12 156.9(12) 2_276 . ?
O6 W3 O18 105.5(11) . . ?
O7 W3 O18 155.0(9) . . ?
O16 W3 O18 88.4(8) 2_276 . ?
O12 W3 O18 87.4(8) . . ?
O6 W3 O4 159.1(11) . . ?
O7 W3 O4 94.0(8) . . ?
O16 W3 O4 95.5(9) 2_276 . ?
O12 W3 O4 62.7(10) . . ?
O18 W3 O4 61.8(8) . . ?
O6 W3 O2 159.3(11) . . ?
O7 W3 O2 65.9(9) . . ?
O16 W3 O2 65.6(9) 2_276 . ?
O12 W3 O2 91.8(11) . . ?
O18 W3 O2 90.1(9) . . ?
O4 W3 O2 41.5(9) . . ?
O9 W4 O8 102.0(10) . . ?
O9 W4 O12 101.1(10) . . ?
O8 W4 O12 88.0(7) . . ?
O9 W4 O21 100.5(10) . . ?
O8 W4 O21 89.7(11) . . ?
O12 W4 O21 158.3(12) . . ?
O9 W4 O11 98.3(11) . . ?
O8 W4 O11 159.7(11) . . ?
O12 W4 O11 89.0(10) . . ?
O21 W4 O11 85.8(12) . . ?
O9 W4 O3 156.2(9) . . ?
O8 W4 O3 94.3(10) . . ?
O12 W4 O3 96.6(11) . . ?
O21 W4 O3 62.0(10) . . ?
O11 W4 O3 66.1(10) . . ?
O9 W4 O4 156.2(9) . . ?
O8 W4 O4 64.7(8) . . ?
O12 W4 O4 60.6(10) . . ?
O21 W4 O4 99.1(10) . . ?
O11 W4 O4 96.5(9) . . ?
O3 W4 O4 47.5(8) . . ?
O15 W5 O18 102.6(9) . 2_276 ?
O15 W5 O20 101.8(12) . . ?
O18 W5 O20 155.6(12) 2_276 . ?
O15 W5 O8 101.0(10) . 2_276 ?
O18 W5 O8 87.5(8) 2_276 2_276 ?
O20 W5 O8 87.3(9) . 2_276 ?
O15 W5 O13 100.5(10) . . ?
O18 W5 O13 86.2(10) 2_276 . ?
O20 W5 O13 90.0(9) . . ?
O8 W5 O13 158.5(10) 2_276 . ?
O15 W5 O1 155.4(10) . . ?
O18 W5 O1 96.5(9) 2_276 . ?
O20 W5 O1 60.4(11) . . ?
O8 W5 O1 95.3(10) 2_276 . ?
O13 W5 O1 65.1(9) . . ?
O15 W5 O4 156.1(9) . 2_276 ?
O18 W5 O4 60.1(9) 2_276 2_276 ?
O20 W5 O4 96.3(11) . 2_276 ?
O8 W5 O4 64.2(8) 2_276 2_276 ?
O13 W5 O4 94.9(9) . 2_276 ?
O1 W5 O4 48.5(8) . 2_276 ?
O14 W6 O13 100.5(9) . . ?
O14 W6 O11 97.5(9) . . ?
O13 W6 O11 161.9(11) . . ?
O14 W6 O10 100.7(9) . . ?
O13 W6 O10 88.0(11) . . ?
O11 W6 O10 87.1(12) . . ?
O14 W6 O19 98.9(10) . . ?
O13 W6 O19 88.3(12) . . ?
O11 W6 O19 90.5(12) . . ?
O10 W6 O19 160.4(12) . . ?
O14 W6 O1 154.4(7) . . ?
O13 W6 O1 65.0(9) . . ?
O11 W6 O1 98.7(10) . . ?
O10 W6 O1 99.8(10) . . ?
O19 W6 O1 61.3(11) . . ?
O14 W6 O3 154.2(8) . . ?
O13 W6 O3 98.5(10) . . ?
O11 W6 O3 63.8(10) . . ?
O10 W6 O3 62.7(10) . . ?
O19 W6 O3 98.9(11) . . ?
O1 W6 O3 51.2(8) . . ?
O2 Si1 O2 180.000(4) . 2_276 ?
O2 Si1 O4 65.1(13) . . ?
O2 Si1 O4 114.9(13) 2_276 . ?
O2 Si1 O4 114.9(13) . 2_276 ?
O2 Si1 O4 65.1(13) 2_276 2_276 ?
O4 Si1 O4 180.000(7) . 2_276 ?
O2 Si1 O3 67.4(14) . 2_276 ?
O2 Si1 O3 112.6(14) 2_276 2_276 ?
O4 Si1 O3 108.3(12) . 2_276 ?
O4 Si1 O3 71.7(12) 2_276 2_276 ?
O2 Si1 O3 112.6(14) . . ?
O2 Si1 O3 67.4(14) 2_276 . ?
O4 Si1 O3 71.7(12) . . ?
O4 Si1 O3 108.3(12) 2_276 . ?
O3 Si1 O3 180.000(7) 2_276 . ?
O2 Si1 O1 69.8(13) . . ?
O2 Si1 O1 110.2(13) 2_276 . ?
O4 Si1 O1 107.3(12) . . ?
O4 Si1 O1 72.7(12) 2_276 . ?
O3 Si1 O1 102.7(12) 2_276 . ?
O3 Si1 O1 77.3(12) . . ?
O2 Si1 O1 110.2(13) . 2_276 ?
O2 Si1 O1 69.8(13) 2_276 2_276 ?
O4 Si1 O1 72.7(12) . 2_276 ?
O4 Si1 O1 107.3(12) 2_276 2_276 ?
O3 Si1 O1 77.3(12) 2_276 2_276 ?
O3 Si1 O1 102.7(12) . 2_276 ?
O1 Si1 O1 180.000(6) . 2_276 ?
Si1 O1 O2 49.8(11) . . ?
Si1 O1 W1 123.6(12) . . ?
O2 O1 W1 73.9(12) . . ?
Si1 O1 W5 119.5(13) . . ?
O2 O1 W5 134.9(15) . . ?
W1 O1 W5 98.7(9) . . ?
Si1 O1 W6 116.4(11) . . ?
O2 O1 W6 129.9(15) . . ?
W1 O1 W6 97.9(9) . . ?
W5 O1 W6 94.9(8) . . ?
Si1 O2 O4 61.3(13) . . ?
Si1 O2 O3 60.9(13) . 2_276 ?
O4 O2 O3 101.7(18) . 2_276 ?
Si1 O2 O1 60.4(12) . . ?
O4 O2 O1 99.2(16) . . ?
O3 O2 O1 93.9(17) 2_276 . ?
Si1 O2 W3 127.3(15) . . ?
O4 O2 W3 66.0(12) . . ?
O3 O2 W3 134.7(16) 2_276 . ?
O1 O2 W3 130.2(15) . . ?
Si1 O2 W2 124.1(15) . 2_276 ?
O4 O2 W2 132.7(16) . 2_276 ?
O3 O2 W2 63.3(11) 2_276 2_276 ?
O1 O2 W2 125.1(15) . 2_276 ?
W3 O2 W2 92.5(9) . 2_276 ?
Si1 O2 W1 121.8(14) . . ?
O4 O2 W1 129.7(16) . . ?
O3 O2 W1 124.1(16) 2_276 . ?
O1 O2 W1 61.4(11) . . ?
W3 O2 W1 91.0(9) . . ?
W2 O2 W1 89.8(8) 2_276 . ?
Si1 O3 O2 51.7(11) . 2_276 ?
Si1 O3 W2 125.6(14) . . ?
O2 O3 W2 73.9(12) 2_276 . ?
Si1 O3 W4 121.7(13) . . ?
O2 O3 W4 138.8(16) 2_276 . ?
W2 O3 W4 98.1(9) . . ?
Si1 O3 W6 115.1(13) . . ?
O2 O3 W6 126.2(16) 2_276 . ?
W2 O3 W6 95.0(9) . . ?
W4 O3 W6 94.4(9) . . ?
Si1 O4 O2 53.7(12) . . ?
Si1 O4 W3 126.2(12) . . ?
O2 O4 W3 72.5(12) . . ?
Si1 O4 W4 119.1(11) . . ?
O2 O4 W4 134.1(15) . . ?
W3 O4 W4 96.3(9) . . ?
Si1 O4 W5 119.2(11) . 2_276 ?
O2 O4 W5 132.2(14) . 2_276 ?
W3 O4 W5 96.2(8) . 2_276 ?
W4 O4 W5 92.5(8) . 2_276 ?
W5 O20 W1 138.8(17) . . ?
W2 O21 W4 136.8(15) . . ?
W3 O7 W1 138.8(10) . . ?
W4 O8 W5 138.5(11) . 2_276 ?
W2 O10 W6 135.6(15) . . ?
W6 O11 W4 135.7(15) . . ?
W4 O12 W3 139.8(15) . . ?
W6 O13 W5 134.9(13) . . ?
W3 O16 W2 138.0(12) 2_276 . ?
W2 O17 W1 138.6(9) 2_276 . ?
W5 O18 W3 141.2(12) 2_276 . ?
W1 O19 W6 135.6(18) . . ?
N1 Cu1 N2 174.6(8) . 1_455 ?
N3 Cu2 N3 180.0(17) 2_665 . ?
C1 N1 C10 115.8(17) . . ?
C1 N1 Cu1 123.1(15) . . ?
C10 N1 Cu1 121.1(13) . . ?
C15 N3 C11 116(2) . . ?
C15 N3 Cu2 125(2) . . ?
C11 N3 Cu2 119(2) . . ?
N1 C1 C2 123(2) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C3 C2 C1 120(2) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C9 116.8(18) . . ?
C2 C3 C4 121.6(18) . . ?
C9 C3 C4 121.5(19) . . ?
C10 C9 C3 121(2) . . ?
C10 C9 H9A 119.6 . . ?
C3 C9 H9A 119.6 . . ?
N1 C10 C9 122.7(19) . . ?
N1 C10 H10A 118.6 . . ?
C9 C10 H10A 118.6 . . ?
N3 C11 C12 121(2) . . ?
N3 C11 H11A 119.6 . . ?
C12 C11 H11A 119.6 . . ?
C13 C12 C11 122(2) . . ?
C13 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
C12 C13 C14 119(2) . . ?
C12 C13 C13 123(2) . 2_765 ?
C14 C13 C13 118(2) . 2_765 ?
C15 C14 C13 114(3) . . ?
C15 C14 H14A 122.9 . . ?
C13 C14 H14A 122.9 . . ?
N3 C15 C14 129(3) . . ?
N3 C15 H15A 115.7 . . ?
C14 C15 H15A 115.7 . . ?
C5 C4 C8 114.2(17) . . ?
C5 C4 C3 123(2) . . ?
C8 C4 C3 122.7(19) . . ?
C7 C8 C4 122(2) . . ?
C7 C8 H8A 118.9 . . ?
C4 C8 H8A 118.9 . . ?
C4 C5 C6 121(2) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
N2 C6 C5 123(2) . . ?
N2 C6 H6A 118.3 . . ?
C5 C6 H6A 118.3 . . ?
N2 C7 C8 121(3) . . ?
N2 C7 H7A 119.3 . . ?
C8 C7 H7A 119.3 . . ?
C6 N2 C7 117.6(19) . . ?
C6 N2 Cu1 124.1(16) . 1_655 ?
C7 N2 Cu1 117.8(17) . 1_655 ?
C20 N5 C20 115(7) 2_366 . ?
C20 N5 C17 136(7) 2_366 . ?
C20 N5 C17 108.0 . . ?
C20 N5 N5 64(5) 2_366 2_366 ?
C20 N5 N5 51(4) . 2_366 ?
C17 N5 N5 159(4) . 2_366 ?
N5 C17 C18 108.0 . . ?
N4 C18 C17 108.0 . . ?
C20 N4 C18 108.0 . . ?
N5 C20 N4 171(5) 2_366 . ?
N5 C20 N5 65(5) 2_366 . ?
N4 C20 N5 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         3.552
_refine_diff_density_min         -4.156
_refine_diff_density_rms         0.468
####################################################################### 
# 
# 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_k
_database_code_depnum_ccdc_archive 'CCDC 1006425'
_audit_update_record             
;
2014-06-03 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H31 Cu3 Mo12 N8 O40.50 P'
_chemical_formula_weight         2584.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   23.402(2)
_cell_length_b                   21.760(2)
_cell_length_c                   26.461(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.239(2)
_cell_angle_gamma                90.00
_cell_volume                     12086(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9816
_exptl_absorpt_coefficient_mu    3.564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2969
_exptl_absorpt_correction_T_max  0.5359
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39475
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         28.37
_reflns_number_total             14849
_reflns_number_gt                9989
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0675P)²+128.8078P] 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         14849
_refine_ls_number_parameters     896
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1555
_refine_ls_wR_factor_gt          0.1388
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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 -0.38265(3) -0.12861(3) 0.06260(3) 0.02215(15) Uani 1 1 d . . .
Mo2 Mo -0.60365(3) -0.37287(3) -0.05749(3) 0.02300(15) Uani 1 1 d . . .
Mo3 Mo -0.37006(3) -0.22431(3) -0.03554(3) 0.02716(17) Uani 1 1 d . . .
Mo4 Mo -0.65382(3) -0.21232(3) -0.09435(3) 0.02609(16) Uani 1 1 d . . .
Mo5 Mo -0.53720(3) -0.20419(3) -0.13908(3) 0.02355(15) Uani 1 1 d . . .
Mo6 Mo -0.54475(3) -0.09642(3) -0.04690(3) 0.02287(16) Uani 1 1 d . . .
Mo7 Mo -0.61787(4) -0.26861(3) 0.04641(3) 0.02876(17) Uani 1 1 d . . .
Mo8 Mo -0.45218(3) -0.40322(3) 0.04442(3) 0.02635(17) Uani 1 1 d . . .
Mo9 Mo -0.47675(3) -0.35853(3) -0.08848(3) 0.02397(16) Uani 1 1 d . . .
Mo10 Mo -0.51869(4) -0.14369(3) 0.09545(3) 0.02588(16) Uani 1 1 d . . .
Mo11 Mo -0.33657(3) -0.27793(3) 0.09611(3) 0.02851(17) Uani 1 1 d . . .
Mo12 Mo -0.46275(4) -0.28859(3) 0.14307(3) 0.02717(17) Uani 1 1 d . . .
Cu1 Cu -0.14716(6) 0.20048(4) 0.16891(5) 0.0393(3) Uani 1 1 d . . .
Cu2 Cu -0.24673(7) -0.28953(5) 0.25236(5) 0.0532(4) Uani 1 1 d . . .
Cu3 Cu -0.13297(8) -0.29907(5) 0.18293(8) 0.0663(5) Uani 1 1 d . . .
P1 P -0.49653(8) -0.24871(7) 0.00200(7) 0.0111(3) Uani 1 1 d . . .
O1 O -0.5924(3) -0.1862(2) 0.0815(2) 0.0287(13) Uani 1 1 d . . .
O2 O -0.4666(3) -0.3628(3) 0.0991(2) 0.0280(13) Uani 1 1 d . . .
O3 O -0.5535(3) -0.3000(3) 0.1159(2) 0.0291(13) Uani 1 1 d . . .
O4 O -0.4462(2) -0.1961(2) -0.0925(2) 0.0268(12) Uani 1 1 d . . .
O5 O -0.5212(3) -0.0860(3) 0.1364(3) 0.0382(15) Uani 1 1 d . . .
O6 O -0.4367(3) -0.3167(3) 0.2080(2) 0.0413(17) Uani 1 1 d . . .
O7 O -0.4070(3) -0.3058(2) -0.0604(2) 0.0281(13) Uani 1 1 d . . .
O8 O -0.5594(3) -0.0215(3) -0.0579(3) 0.0388(16) Uani 1 1 d . . .
O9 O -0.4201(3) -0.4689(3) 0.0764(3) 0.0382(16) Uani 1 1 d . . .
O10 O -0.3160(3) -0.2656(2) 0.0346(2) 0.0283(13) Uani 1 1 d . . .
O11 O -0.5144(2) -0.2411(2) 0.0506(2) 0.0188(11) Uani 1 1 d . . .
O12 O -0.5441(3) -0.1901(3) -0.2035(2) 0.0351(14) Uani 1 1 d . . .
O13 O -0.4670(3) -0.3996(3) -0.1372(2) 0.0343(14) Uani 1 1 d . . .
O14 O -0.5033(2) -0.3155(2) -0.0162(2) 0.0201(11) Uani 1 1 d . . .
O15 O -0.6128(3) -0.3370(2) 0.0074(2) 0.0269(12) Uani 1 1 d . . .
O16 O -0.5503(3) -0.1093(3) 0.0249(2) 0.0263(12) Uani 1 1 d . . .
O17 O -0.4725(3) -0.2058(2) 0.1550(2) 0.0292(13) Uani 1 1 d . . .
O18 O -0.6508(3) -0.2246(2) -0.0236(2) 0.0288(13) Uani 1 1 d . . .
O19 O -0.3261(3) -0.1888(2) 0.1072(2) 0.0280(13) Uani 1 1 d . . .
O20 O -0.3203(3) -0.2171(3) -0.0649(2) 0.0294(13) Uani 1 1 d . . .
O21 O -0.3857(2) -0.2746(2) 0.1383(2) 0.0242(12) Uani 1 1 d . . .
O22 O -0.6826(3) -0.2821(3) 0.0559(3) 0.0315(13) Uani 1 1 d . . .
O23 O -0.4339(2) -0.1313(2) 0.0984(2) 0.0253(12) Uani 1 1 d . . .
O24 O -0.3533(3) -0.1490(2) 0.0039(2) 0.0269(12) Uani 1 1 d . . .
O25 O -0.4431(3) -0.4116(3) -0.0263(2) 0.0290(13) Uani 1 1 d . . .
O26 O -0.2653(3) -0.2983(2) 0.1457(2) 0.0296(13) Uani 1 1 d . . .
O27 O -0.5255(2) -0.2879(2) -0.1321(2) 0.0252(12) Uani 1 1 d . . .
O28 O -0.6319(2) -0.1292(2) -0.0809(2) 0.0250(12) Uani 1 1 d . . .
O29 O -0.6388(3) -0.3002(2) -0.0931(2) 0.0243(12) Uani 1 1 d . . .
O30 O -0.5382(2) -0.4236(2) 0.0030(2) 0.0248(12) Uani 1 1 d . . .
O31 O -0.4571(2) -0.0992(2) -0.0040(2) 0.0226(11) Uani 1 1 d . . .
O32 O -0.6639(2) -0.4224(2) -0.0828(2) 0.0266(12) Uani 1 1 d . . .
O33 O -0.5405(3) -0.1191(2) -0.1138(2) 0.0247(12) Uani 1 1 d . . .
O34 O -0.7314(2) -0.2074(2) -0.1368(2) 0.0265(12) Uani 1 1 d . . .
O35 O -0.6233(2) -0.2107(2) -0.1525(2) 0.0213(11) Uani 1 1 d . . .
O36 O -0.5620(3) -0.3892(2) -0.1018(2) 0.0241(12) Uani 1 1 d . . .
O37 O -0.4265(2) -0.2290(2) 0.0223(2) 0.0202(11) Uani 1 1 d . . .
O38 O -0.3756(3) -0.3512(2) 0.0677(2) 0.0275(13) Uani 1 1 d . . .
O39 O -0.3386(2) -0.0657(2) 0.0877(2) 0.0262(12) Uani 1 1 d . . .
O40 O -0.5391(2) -0.2086(2) -0.0472(2) 0.0178(10) Uani 1 1 d . . .
N1 N -0.1345(5) 0.6138(4) 0.1768(5) 0.061(3) Uani 1 1 d . . .
N2 N -0.1432(3) 0.2878(3) 0.1730(3) 0.0223(14) Uani 1 1 d . . .
N3 N -0.1436(4) 0.1132(3) 0.1687(3) 0.0311(17) Uani 1 1 d . . .
N4 N -0.1319(4) -0.2117(3) 0.1841(3) 0.0350(18) Uani 1 1 d . . .
N5 N -0.2479(4) -0.2018(3) 0.2535(3) 0.0330(18) Uani 1 1 d . . .
N6 N -0.2487(4) -0.3772(3) 0.2500(3) 0.0356(19) Uani 1 1 d . . .
N7 N -0.7839(7) 0.1042(7) 0.0079(5) 0.104(5) Uani 1 1 d . . .
H7B H -0.7582 0.1350 0.0164 0.124 Uiso 1 1 calc R . .
H7C H -0.8225 0.1096 0.0029 0.124 Uiso 1 1 calc R . .
N8 N -0.7078(6) 0.0335(8) 0.0091(5) 0.104(5) Uani 1 1 d . . .
C1 C -0.1870(5) 0.5825(4) 0.1536(4) 0.039(2) Uani 1 1 d . . .
H1A H -0.2252 0.6042 0.1383 0.047 Uiso 1 1 calc R . .
C2 C -0.1902(5) 0.5189(4) 0.1501(4) 0.035(2) Uani 1 1 d . . .
H2A H -0.2294 0.4996 0.1303 0.042 Uiso 1 1 calc R . .
C3 C -0.1363(4) 0.4847(3) 0.1754(4) 0.035(2) Uani 1 1 d . . .
C4 C -0.1378(4) 0.4170(3) 0.1756(4) 0.0249(17) Uani 1 1 d . . .
C5 C -0.1883(4) 0.3848(3) 0.1344(4) 0.0273(18) Uani 1 1 d . . .
H5A H -0.2214 0.4063 0.1063 0.033 Uiso 1 1 calc R . .
C6 C -0.1898(4) 0.3216(3) 0.1345(3) 0.0252(17) Uani 1 1 d . . .
H6A H -0.2247 0.3016 0.1068 0.030 Uiso 1 1 calc R . .
C7 C -0.0931(4) 0.3181(3) 0.2126(4) 0.0275(18) Uani 1 1 d . . .
H7A H -0.0598 0.2952 0.2392 0.033 Uiso 1 1 calc R . .
C8 C -0.0890(4) 0.3811(4) 0.2157(4) 0.0275(18) Uani 1 1 d . . .
H8A H -0.0539 0.3999 0.2443 0.033 Uiso 1 1 calc R . .
C9 C -0.0812(6) 0.5175(5) 0.1974(10) 0.164(12) Uani 1 1 d . . .
H9A H -0.0423 0.4972 0.2120 0.197 Uiso 1 1 calc R . .
C10 C -0.0826(7) 0.5809(6) 0.1981(11) 0.180(13) Uani 1 1 d . . .
H10A H -0.0439 0.6015 0.2149 0.216 Uiso 1 1 calc R . .
C11 C -0.1971(4) 0.0789(3) 0.1521(3) 0.0268(18) Uani 1 1 d . . .
H11A H -0.2360 0.0993 0.1387 0.032 Uiso 1 1 calc R . .
C12 C -0.1972(4) 0.0158(3) 0.1538(3) 0.0254(17) Uani 1 1 d . . .
H12A H -0.2354 -0.0058 0.1413 0.030 Uiso 1 1 calc R . .
C13 C -0.1388(4) -0.0157(3) 0.1748(3) 0.0200(15) Uani 1 1 d . . .
C14 C -0.1366(4) -0.0832(3) 0.1793(3) 0.0187(15) Uani 1 1 d . . .
C15 C -0.1829(4) -0.1186(3) 0.1385(3) 0.0246(17) Uani 1 1 d . . .
H15A H -0.2165 -0.1000 0.1083 0.030 Uiso 1 1 calc R . .
C16 C -0.1791(4) -0.1824(4) 0.1430(4) 0.034(2) Uani 1 1 d . . .
H16A H -0.2115 -0.2056 0.1158 0.040 Uiso 1 1 calc R . .
C17 C -0.0861(4) -0.1774(4) 0.2256(4) 0.0313(19) Uani 1 1 d . . .
H17A H -0.0538 -0.1971 0.2560 0.038 Uiso 1 1 calc R . .
C18 C -0.0872(4) -0.1138(3) 0.2231(3) 0.0235(16) Uani 1 1 d . . .
H18A H -0.0547 -0.0914 0.2510 0.028 Uiso 1 1 calc R . .
C19 C -0.0843(4) 0.0196(4) 0.1899(4) 0.033(2) Uani 1 1 d . . .
H19A H -0.0447 0.0008 0.2024 0.040 Uiso 1 1 calc R . .
C20 C -0.0893(5) 0.0828(4) 0.1863(4) 0.043(2) Uani 1 1 d . . .
H20A H -0.0520 0.1055 0.1970 0.052 Uiso 1 1 calc R . .
C21 C -0.1945(4) -0.1702(4) 0.2799(3) 0.0282(18) Uani 1 1 d . . .
H21A H -0.1564 -0.1916 0.2984 0.034 Uiso 1 1 calc R . .
C22 C -0.1931(4) -0.1064(3) 0.2810(3) 0.0220(16) Uani 1 1 d . . .
H22A H -0.1546 -0.0857 0.3002 0.026 Uiso 1 1 calc R . .
C23 C -0.2497(3) -0.0735(3) 0.2531(3) 0.0169(14) Uani 1 1 d . . .
C24 C -0.3051(4) -0.1078(3) 0.2259(3) 0.0246(17) Uani 1 1 d . . .
H24A H -0.3442 -0.0881 0.2072 0.030 Uiso 1 1 calc R . .
C25 C -0.3021(4) -0.1707(4) 0.2268(3) 0.0289(19) Uani 1 1 d . . .
H25A H -0.3396 -0.1927 0.2077 0.035 Uiso 1 1 calc R . .
C26 C -0.2993(5) -0.4084(4) 0.2122(4) 0.036(2) Uani 1 1 d . . .
H26A H -0.3342 -0.3863 0.1868 0.044 Uiso 1 1 calc R . .
C27 C -0.3015(4) -0.4708(3) 0.2096(3) 0.0283(19) Uani 1 1 d . . .
H27A H -0.3374 -0.4905 0.1828 0.034 Uiso 1 1 calc R . .
C28 C -0.2498(3) -0.5056(3) 0.2472(3) 0.0181(15) Uani 1 1 d . . .
C29 C -0.1974(4) -0.4722(3) 0.2865(3) 0.0264(18) Uani 1 1 d . . .
H29A H -0.1621 -0.4929 0.3129 0.032 Uiso 1 1 calc R . .
C30 C -0.1982(5) -0.4100(4) 0.2859(4) 0.037(2) Uani 1 1 d . . .
H30A H -0.1625 -0.3890 0.3114 0.044 Uiso 1 1 calc R . .
C31 C -0.7639(9) 0.0484(5) 0.0027(5) 0.071(5) Uani 1 1 d . . .
C32 C -0.8124(10) -0.0005(7) -0.0135(6) 0.096(6) Uani 1 1 d . . .
H32A H -0.8547 0.0065 -0.0212 0.115 Uiso 1 1 calc R . .
C33 C -0.7881(12) -0.0580(7) -0.0160(7) 0.110(8) Uani 1 1 d . . .
H33A H -0.8169 -0.0902 -0.0242 0.132 Uiso 1 1 calc R . .
C34 C -0.7227(17) -0.0762(15) -0.0074(9) 0.186(17) Uani 1 1 d . . .
H34A H -0.7087 -0.1154 -0.0104 0.223 Uiso 1 1 calc R . .
C35 C -0.6879(17) -0.0227(14) 0.0056(9) 0.22(2) Uani 1 1 d . . .
H35A H -0.6453 -0.0263 0.0129 0.267 Uiso 1 1 calc R . .
OW1 O -0.4563(13) -0.4806(12) 0.1726(11) 0.136(9) Uiso 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 O39 1.664(5) . ?
Mo1 O23 1.828(6) . ?
Mo1 O19 1.865(5) . ?
Mo1 O31 1.959(5) . ?
Mo1 O24 2.007(6) . ?
Mo1 O37 2.448(5) . ?
Mo2 O32 1.662(5) . ?
Mo2 O29 1.839(5) . ?
Mo2 O36 1.861(5) . ?
Mo2 O15 1.983(5) . ?
Mo2 O30 1.990(5) . ?
Mo2 O14 2.449(5) . ?
Mo3 O20 1.668(6) . ?
Mo3 O4 1.857(5) . ?
Mo3 O24 1.888(5) . ?
Mo3 O10 1.942(5) . ?
Mo3 O7 1.956(5) . ?
Mo3 O37 2.426(5) . ?
Mo4 O34 1.664(5) . ?
Mo4 O18 1.862(5) . ?
Mo4 O28 1.870(5) . ?
Mo4 O29 1.942(5) . ?
Mo4 O35 1.963(5) . ?
Mo4 O40 2.411(5) . ?
Mo5 O12 1.667(6) . ?
Mo5 O27 1.839(5) . ?
Mo5 O35 1.890(5) . ?
Mo5 O4 1.940(5) . ?
Mo5 O33 1.982(5) . ?
Mo5 O40 2.453(5) . ?
Mo6 O8 1.666(6) . ?
Mo6 O31 1.854(5) . ?
Mo6 O33 1.881(5) . ?
Mo6 O28 1.964(5) . ?
Mo6 O16 1.980(6) . ?
Mo6 O40 2.445(5) . ?
Mo7 O22 1.666(6) . ?
Mo7 O15 1.845(5) . ?
Mo7 O3 1.914(6) . ?
Mo7 O18 1.918(5) . ?
Mo7 O1 1.986(5) . ?
Mo7 O11 2.449(5) . ?
Mo8 O9 1.661(6) . ?
Mo8 O2 1.848(6) . ?
Mo8 O30 1.870(5) . ?
Mo8 O38 1.974(5) . ?
Mo8 O25 1.984(6) . ?
Mo8 O14 2.438(5) . ?
Mo9 O13 1.664(6) . ?
Mo9 O7 1.860(5) . ?
Mo9 O25 1.875(6) . ?
Mo9 O27 1.958(5) . ?
Mo9 O36 1.981(5) . ?
Mo9 O14 2.444(5) . ?
Mo10 O5 1.677(6) . ?
Mo10 O16 1.837(6) . ?
Mo10 O1 1.846(5) . ?
Mo10 O23 1.971(5) . ?
Mo10 O17 1.993(6) . ?
Mo10 O11 2.453(5) . ?
Mo11 O26 1.663(5) . ?
Mo11 O38 1.825(5) . ?
Mo11 O10 1.910(6) . ?
Mo11 O21 1.924(6) . ?
Mo11 O19 1.961(5) . ?
Mo11 O37 2.396(5) . ?
Mo12 O6 1.664(6) . ?
Mo12 O17 1.860(6) . ?
Mo12 O21 1.888(5) . ?
Mo12 O3 1.935(6) . ?
Mo12 O2 1.968(5) . ?
Mo12 O11 2.428(5) . ?
Cu1 N3 1.902(7) . ?
Cu1 N2 1.902(6) . ?
Cu2 N6 1.909(7) . ?
Cu2 N5 1.910(7) . ?
Cu3 N4 1.902(7) . ?
Cu3 N1 1.902(8) 1_545 ?
P1 O40 1.517(5) . ?
P1 O14 1.518(5) . ?
P1 O11 1.527(5) . ?
P1 O37 1.543(5) . ?
N1 C1 1.298(13) . ?
N1 C10 1.303(16) . ?
N1 Cu3 1.902(8) 1_565 ?
N2 C6 1.336(10) . ?
N2 C7 1.350(10) . ?
N3 C20 1.321(12) . ?
N3 C11 1.352(11) . ?
N4 C16 1.321(12) . ?
N4 C17 1.367(11) . ?
N5 C21 1.323(11) . ?
N5 C25 1.331(11) . ?
N6 C26 1.346(11) . ?
N6 C30 1.348(11) . ?
N7 C31 1.332(16) . ?
N8 C31 1.289(19) . ?
N8 C35 1.33(3) . ?
C1 C2 1.385(11) . ?
C2 C3 1.359(12) . ?
C3 C9 1.359(15) . ?
C3 C4 1.476(10) . ?
C4 C5 1.391(11) . ?
C4 C8 1.403(11) . ?
C5 C6 1.376(10) . ?
C7 C8 1.375(11) . ?
C9 C10 1.378(16) . ?
C11 C12 1.376(10) . ?
C12 C13 1.406(10) . ?
C13 C19 1.387(11) . ?
C13 C14 1.473(9) . ?
C14 C15 1.378(10) . ?
C14 C18 1.392(10) . ?
C15 C16 1.393(11) . ?
C17 C18 1.385(10) . ?
C19 C20 1.381(11) . ?
C21 C22 1.389(10) . ?
C22 C23 1.396(10) . ?
C23 C24 1.390(10) . ?
C23 C28 1.478(10) 4_455 ?
C24 C25 1.369(10) . ?
C26 C27 1.361(10) . ?
C27 C28 1.400(10) . ?
C28 C29 1.409(10) . ?
C28 C23 1.478(10) 4_445 ?
C29 C30 1.353(11) . ?
C31 C32 1.47(2) . ?
C32 C33 1.39(2) . ?
C33 C34 1.50(4) . ?
C34 C35 1.37(4) . ?

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
O39 Mo1 O23 104.6(3) . . ?
O39 Mo1 O19 100.6(2) . . ?
O23 Mo1 O19 95.4(2) . . ?
O39 Mo1 O31 103.7(2) . . ?
O23 Mo1 O31 87.2(2) . . ?
O19 Mo1 O31 154.1(2) . . ?
O39 Mo1 O24 97.2(3) . . ?
O23 Mo1 O24 157.2(2) . . ?
O19 Mo1 O24 86.8(2) . . ?
O31 Mo1 O24 81.3(2) . . ?
O39 Mo1 O37 166.8(2) . . ?
O23 Mo1 O37 87.3(2) . . ?
O19 Mo1 O37 72.1(2) . . ?
O31 Mo1 O37 82.28(19) . . ?
O24 Mo1 O37 71.76(19) . . ?
O32 Mo2 O29 104.1(3) . . ?
O32 Mo2 O36 102.1(3) . . ?
O29 Mo2 O36 94.6(2) . . ?
O32 Mo2 O15 101.9(3) . . ?
O29 Mo2 O15 84.9(2) . . ?
O36 Mo2 O15 155.3(2) . . ?
O32 Mo2 O30 100.3(2) . . ?
O29 Mo2 O30 154.2(2) . . ?
O36 Mo2 O30 88.3(2) . . ?
O15 Mo2 O30 82.0(2) . . ?
O32 Mo2 O14 170.2(2) . . ?
O29 Mo2 O14 85.1(2) . . ?
O36 Mo2 O14 73.30(19) . . ?
O15 Mo2 O14 82.1(2) . . ?
O30 Mo2 O14 71.21(19) . . ?
O20 Mo3 O4 102.0(3) . . ?
O20 Mo3 O24 99.1(3) . . ?
O4 Mo3 O24 93.0(2) . . ?
O20 Mo3 O10 101.2(3) . . ?
O4 Mo3 O10 156.0(2) . . ?
O24 Mo3 O10 89.1(2) . . ?
O20 Mo3 O7 103.0(3) . . ?
O4 Mo3 O7 84.5(2) . . ?
O24 Mo3 O7 157.9(2) . . ?
O10 Mo3 O7 84.6(2) . . ?
O20 Mo3 O37 169.9(2) . . ?
O4 Mo3 O37 86.1(2) . . ?
O24 Mo3 O37 74.1(2) . . ?
O10 Mo3 O37 71.6(2) . . ?
O7 Mo3 O37 83.8(2) . . ?
O34 Mo4 O18 103.5(3) . . ?
O34 Mo4 O28 101.1(2) . . ?
O18 Mo4 O28 93.6(2) . . ?
O34 Mo4 O29 102.1(2) . . ?
O18 Mo4 O29 85.2(2) . . ?
O28 Mo4 O29 156.4(2) . . ?
O34 Mo4 O35 97.8(3) . . ?
O18 Mo4 O35 157.8(2) . . ?
O28 Mo4 O35 88.1(2) . . ?
O29 Mo4 O35 84.5(2) . . ?
O34 Mo4 O40 168.8(2) . . ?
O18 Mo4 O40 86.9(2) . . ?
O28 Mo4 O40 73.8(2) . . ?
O29 Mo4 O40 82.7(2) . . ?
O35 Mo4 O40 72.34(18) . . ?
O12 Mo5 O27 103.2(3) . . ?
O12 Mo5 O35 102.0(3) . . ?
O27 Mo5 O35 92.5(2) . . ?
O12 Mo5 O4 102.5(3) . . ?
O27 Mo5 O4 87.3(2) . . ?
O35 Mo5 O4 154.9(2) . . ?
O12 Mo5 O33 99.9(3) . . ?
O27 Mo5 O33 156.6(2) . . ?
O35 Mo5 O33 86.3(2) . . ?
O4 Mo5 O33 84.1(2) . . ?
O12 Mo5 O40 169.7(2) . . ?
O27 Mo5 O40 85.9(2) . . ?
O35 Mo5 O40 72.46(19) . . ?
O4 Mo5 O40 82.5(2) . . ?
O33 Mo5 O40 71.41(19) . . ?
O8 Mo6 O31 103.0(3) . . ?
O8 Mo6 O33 100.7(3) . . ?
O31 Mo6 O33 93.7(2) . . ?
O8 Mo6 O28 100.6(3) . . ?
O31 Mo6 O28 155.8(2) . . ?
O33 Mo6 O28 87.1(2) . . ?
O8 Mo6 O16 102.2(3) . . ?
O31 Mo6 O16 86.1(2) . . ?
O33 Mo6 O16 156.6(2) . . ?
O28 Mo6 O16 83.8(2) . . ?
O8 Mo6 O40 169.9(2) . . ?
O31 Mo6 O40 85.6(2) . . ?
O33 Mo6 O40 73.10(19) . . ?
O28 Mo6 O40 71.49(19) . . ?
O16 Mo6 O40 83.6(2) . . ?
O22 Mo7 O15 103.3(3) . . ?
O22 Mo7 O3 100.0(3) . . ?
O15 Mo7 O3 91.8(2) . . ?
O22 Mo7 O18 103.3(3) . . ?
O15 Mo7 O18 87.8(2) . . ?
O3 Mo7 O18 156.2(2) . . ?
O22 Mo7 O1 101.1(3) . . ?
O15 Mo7 O1 155.5(2) . . ?
O3 Mo7 O1 85.8(2) . . ?
O18 Mo7 O1 84.8(2) . . ?
O22 Mo7 O11 169.1(2) . . ?
O15 Mo7 O11 85.2(2) . . ?
O3 Mo7 O11 72.6(2) . . ?
O18 Mo7 O11 83.6(2) . . ?
O1 Mo7 O11 70.87(19) . . ?
O9 Mo8 O2 102.1(3) . . ?
O9 Mo8 O30 102.8(3) . . ?
O2 Mo8 O30 92.9(2) . . ?
O9 Mo8 O38 101.0(3) . . ?
O2 Mo8 O38 86.4(2) . . ?
O30 Mo8 O38 155.8(2) . . ?
O9 Mo8 O25 100.8(3) . . ?
O2 Mo8 O25 156.4(2) . . ?
O30 Mo8 O25 87.8(2) . . ?
O38 Mo8 O25 83.5(2) . . ?
O9 Mo8 O14 171.0(2) . . ?
O2 Mo8 O14 86.3(2) . . ?
O30 Mo8 O14 73.3(2) . . ?
O38 Mo8 O14 82.5(2) . . ?
O25 Mo8 O14 71.22(19) . . ?
O13 Mo9 O7 104.1(3) . . ?
O13 Mo9 O25 101.5(3) . . ?
O7 Mo9 O25 94.3(2) . . ?
O13 Mo9 O27 102.0(3) . . ?
O7 Mo9 O27 86.1(2) . . ?
O25 Mo9 O27 155.6(2) . . ?
O13 Mo9 O36 98.8(3) . . ?
O7 Mo9 O36 156.3(2) . . ?
O25 Mo9 O36 87.1(2) . . ?
O27 Mo9 O36 83.1(2) . . ?
O13 Mo9 O14 168.7(3) . . ?
O7 Mo9 O14 86.2(2) . . ?
O25 Mo9 O14 72.7(2) . . ?
O27 Mo9 O14 83.0(2) . . ?
O36 Mo9 O14 71.59(19) . . ?
O5 Mo10 O16 103.8(3) . . ?
O5 Mo10 O1 102.0(3) . . ?
O16 Mo10 O1 94.6(2) . . ?
O5 Mo10 O23 101.2(3) . . ?
O16 Mo10 O23 86.0(2) . . ?
O1 Mo10 O23 155.9(2) . . ?
O5 Mo10 O17 99.1(3) . . ?
O16 Mo10 O17 156.1(2) . . ?
O1 Mo10 O17 87.2(2) . . ?
O23 Mo10 O17 82.9(2) . . ?
O5 Mo10 O11 168.6(3) . . ?
O16 Mo10 O11 86.8(2) . . ?
O1 Mo10 O11 72.8(2) . . ?
O23 Mo10 O11 83.2(2) . . ?
O17 Mo10 O11 70.9(2) . . ?
O26 Mo11 O38 103.7(3) . . ?
O26 Mo11 O10 99.7(3) . . ?
O38 Mo11 O10 92.4(2) . . ?
O26 Mo11 O21 101.5(3) . . ?
O38 Mo11 O21 87.3(2) . . ?
O10 Mo11 O21 158.3(2) . . ?
O26 Mo11 O19 97.5(2) . . ?
O38 Mo11 O19 158.7(2) . . ?
O10 Mo11 O19 85.8(2) . . ?
O21 Mo11 O19 86.7(2) . . ?
O26 Mo11 O37 167.1(2) . . ?
O38 Mo11 O37 87.3(2) . . ?
O10 Mo11 O37 72.8(2) . . ?
O21 Mo11 O37 85.5(2) . . ?
O19 Mo11 O37 71.87(19) . . ?
O6 Mo12 O17 101.4(3) . . ?
O6 Mo12 O21 101.7(3) . . ?
O17 Mo12 O21 92.8(2) . . ?
O6 Mo12 O3 100.3(3) . . ?
O17 Mo12 O3 89.5(2) . . ?
O21 Mo12 O3 157.0(2) . . ?
O6 Mo12 O2 102.0(3) . . ?
O17 Mo12 O2 156.6(2) . . ?
O21 Mo12 O2 83.6(2) . . ?
O3 Mo12 O2 85.3(2) . . ?
O6 Mo12 O11 171.1(3) . . ?
O17 Mo12 O11 73.5(2) . . ?
O21 Mo12 O11 85.9(2) . . ?
O3 Mo12 O11 72.8(2) . . ?
O2 Mo12 O11 83.2(2) . . ?
N3 Cu1 N2 175.2(3) . . ?
N6 Cu2 N5 178.0(3) . . ?
N4 Cu3 N1 176.1(4) . 1_545 ?
O40 P1 O14 110.0(3) . . ?
O40 P1 O11 110.0(3) . . ?
O14 P1 O11 109.9(3) . . ?
O40 P1 O37 109.4(3) . . ?
O14 P1 O37 108.8(3) . . ?
O11 P1 O37 108.7(3) . . ?
Mo10 O1 Mo7 127.4(3) . . ?
Mo8 O2 Mo12 151.2(3) . . ?
Mo7 O3 Mo12 125.4(3) . . ?
Mo3 O4 Mo5 151.1(3) . . ?
Mo9 O7 Mo3 150.8(3) . . ?
Mo11 O10 Mo3 125.2(3) . . ?
P1 O11 Mo12 127.1(3) . . ?
P1 O11 Mo7 124.6(3) . . ?
Mo12 O11 Mo7 89.07(17) . . ?
P1 O11 Mo10 125.8(3) . . ?
Mo12 O11 Mo10 89.38(16) . . ?
Mo7 O11 Mo10 88.95(16) . . ?
P1 O14 Mo8 126.1(3) . . ?
P1 O14 Mo9 126.0(3) . . ?
Mo8 O14 Mo9 89.69(16) . . ?
P1 O14 Mo2 125.1(3) . . ?
Mo8 O14 Mo2 89.42(17) . . ?
Mo9 O14 Mo2 88.90(16) . . ?
Mo7 O15 Mo2 149.3(3) . . ?
Mo10 O16 Mo6 149.9(3) . . ?
Mo12 O17 Mo10 125.9(3) . . ?
Mo4 O18 Mo7 149.6(3) . . ?
Mo1 O19 Mo11 126.4(3) . . ?
Mo12 O21 Mo11 150.0(3) . . ?
Mo1 O23 Mo10 149.7(3) . . ?
Mo3 O24 Mo1 124.1(3) . . ?
Mo9 O25 Mo8 126.3(3) . . ?
Mo5 O27 Mo9 149.2(3) . . ?
Mo4 O28 Mo6 125.5(3) . . ?
Mo2 O29 Mo4 153.2(3) . . ?
Mo8 O30 Mo2 125.9(3) . . ?
Mo6 O31 Mo1 149.8(3) . . ?
Mo6 O33 Mo5 126.1(3) . . ?
Mo5 O35 Mo4 125.6(3) . . ?
Mo2 O36 Mo9 126.2(3) . . ?
P1 O37 Mo11 125.1(3) . . ?
P1 O37 Mo3 125.6(3) . . ?
Mo11 O37 Mo3 90.35(17) . . ?
P1 O37 Mo1 125.2(3) . . ?
Mo11 O37 Mo1 89.65(16) . . ?
Mo3 O37 Mo1 89.82(17) . . ?
Mo11 O38 Mo8 148.2(3) . . ?
P1 O40 Mo4 125.7(3) . . ?
P1 O40 Mo6 126.0(3) . . ?
Mo4 O40 Mo6 89.16(16) . . ?
P1 O40 Mo5 125.5(3) . . ?
Mo4 O40 Mo5 89.56(16) . . ?
Mo6 O40 Mo5 89.36(16) . . ?
C1 N1 C10 114.9(9) . . ?
C1 N1 Cu3 122.8(7) . 1_565 ?
C10 N1 Cu3 122.2(9) . 1_565 ?
C6 N2 C7 117.3(6) . . ?
C6 N2 Cu1 120.2(5) . . ?
C7 N2 Cu1 122.4(5) . . ?
C20 N3 C11 116.6(7) . . ?
C20 N3 Cu1 122.3(6) . . ?
C11 N3 Cu1 121.1(6) . . ?
C16 N4 C17 118.1(7) . . ?
C16 N4 Cu3 117.9(6) . . ?
C17 N4 Cu3 124.0(6) . . ?
C21 N5 C25 118.2(7) . . ?
C21 N5 Cu2 120.7(6) . . ?
C25 N5 Cu2 121.1(6) . . ?
C26 N6 C30 117.8(7) . . ?
C26 N6 Cu2 121.9(6) . . ?
C30 N6 Cu2 120.3(6) . . ?
C31 N8 C35 126(2) . . ?
N1 C1 C2 124.6(9) . . ?
C3 C2 C1 120.2(9) . . ?
C9 C3 C2 114.9(9) . . ?
C9 C3 C4 122.9(9) . . ?
C2 C3 C4 122.0(8) . . ?
C5 C4 C8 116.0(7) . . ?
C5 C4 C3 120.9(8) . . ?
C8 C4 C3 123.1(7) . . ?
C6 C5 C4 121.0(7) . . ?
N2 C6 C5 122.6(7) . . ?
N2 C7 C8 123.2(7) . . ?
C7 C8 C4 119.8(7) . . ?
C3 C9 C10 120.4(12) . . ?
N1 C10 C9 124.6(12) . . ?
N3 C11 C12 123.8(7) . . ?
C11 C12 C13 118.9(7) . . ?
C19 C13 C12 117.1(7) . . ?
C19 C13 C14 122.2(7) . . ?
C12 C13 C14 120.7(7) . . ?
C15 C14 C18 117.5(7) . . ?
C15 C14 C13 120.5(7) . . ?
C18 C14 C13 122.0(7) . . ?
C14 C15 C16 119.5(8) . . ?
N4 C16 C15 123.3(8) . . ?
N4 C17 C18 121.1(8) . . ?
C17 C18 C14 120.5(8) . . ?
C20 C19 C13 119.5(8) . . ?
N3 C20 C19 124.2(9) . . ?
N5 C21 C22 122.5(8) . . ?
C21 C22 C23 119.6(7) . . ?
C24 C23 C22 116.7(7) . . ?
C24 C23 C28 122.1(7) . 4_455 ?
C22 C23 C28 121.3(6) . 4_455 ?
C25 C24 C23 119.9(8) . . ?
N5 C25 C24 123.2(8) . . ?
N6 C26 C27 122.8(8) . . ?
C26 C27 C28 120.1(8) . . ?
C27 C28 C29 116.2(7) . . ?
C27 C28 C23 122.2(6) . 4_445 ?
C29 C28 C23 121.5(6) . 4_445 ?
C30 C29 C28 120.3(8) . . ?
N6 C30 C29 122.7(8) . . ?
N8 C31 N7 126.9(17) . . ?
N8 C31 C32 117.7(14) . . ?
N7 C31 C32 115.3(17) . . ?
C33 C32 C31 112.7(18) . . ?
C32 C33 C34 130(2) . . ?
C35 C34 C33 105(3) . . ?
N8 C35 C34 128(4) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         2.668
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.214
####################################################################### 
# 
# 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_k
_database_code_depnum_ccdc_archive 'CCDC 1006426'
_audit_update_record             
;
2014-06-03 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H23 Cu2 Mo12 N6 O40 P'
_chemical_formula_weight         2356.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p2(1)/c

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

_cell_length_a                   10.8252(14)
_cell_length_b                   10.8613(14)
_cell_length_c                   23.243(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.379(5)
_cell_angle_gamma                90.00
_cell_volume                     2647.2(6)
_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       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2223
_exptl_absorpt_coefficient_mu    3.663
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4379
_exptl_absorpt_correction_T_max  0.6474
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16947
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         28.41
_reflns_number_total             6590
_reflns_number_gt                5396
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0610P)²+34.1219P] 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         6590
_refine_ls_number_parameters     427
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1454
_refine_ls_wR_factor_gt          0.1359
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.016
_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 0.95517(9) 0.31331(7) -0.04214(4) 0.0431(2) Uani 1 1 d . . .
Mo2 Mo 0.98293(8) -0.09313(9) 0.14352(3) 0.0459(2) Uani 1 1 d . . .
Mo3 Mo 0.70897(6) 0.03507(8) 0.04377(3) 0.03410(18) Uani 1 1 d . . .
Mo4 Mo 1.28283(6) -0.09341(8) 0.10660(3) 0.0381(2) Uani 1 1 d . . .
Mo5 Mo 0.97556(7) 0.22629(6) 0.10691(3) 0.02933(16) Uani 1 1 d . . .
Mo6 Mo 1.25398(6) 0.21281(6) 0.05116(3) 0.02479(15) Uani 1 1 d . . .
Cu1 Cu 0.99899(9) 0.09534(15) 0.27086(6) 0.0545(4) Uani 1 1 d . . .
P1 P 1.0000 0.0000 0.0000 0.0192(5) Uani 1 2 d S . .
O1 O 0.9860(10) -0.2431(12) 0.1083(5) 0.119(5) Uani 1 1 d . . .
O2 O 1.1373(8) 0.0232(8) 0.0190(4) 0.0169(17) Uani 0.50 1 d P . .
O3 O 0.9589(8) -0.1234(8) -0.0218(4) 0.0161(17) Uani 0.50 1 d P . .
O4 O 0.8116(9) -0.0650(8) 0.1091(4) 0.096(4) Uani 1 1 d . . .
O5 O 1.0007(9) 0.0862(9) 0.1536(4) 0.103(4) Uani 1 1 d . . .
O6 O 0.7968(9) 0.1683(9) 0.0789(4) 0.103(4) Uani 1 1 d . . .
O7 O 1.2049(10) -0.2519(11) 0.0774(5) 0.112(5) Uani 1 1 d . . .
O8 O 0.9324(8) 0.0388(8) 0.0505(4) 0.0157(17) Uani 0.50 1 d P . .
O9 O 1.3696(9) 0.3138(9) 0.0789(3) 0.082(3) Uani 1 1 d . . .
O10 O 0.9564(6) 0.3338(8) 0.1545(3) 0.062(2) Uani 1 1 d . . .
O11 O 0.5769(8) 0.0446(8) 0.0663(4) 0.062(2) Uani 1 1 d . . .
O12 O 1.1377(8) 0.3051(8) -0.0031(3) 0.061(2) Uani 1 1 d . . .
O13 O 1.4150(8) -0.1412(7) 0.1539(3) 0.058(2) Uani 1 1 d . . .
O14 O 1.3116(8) 0.1288(7) -0.0041(3) 0.0531(19) Uani 1 1 d . . .
O15 O 0.9397(8) 0.4584(7) -0.0624(3) 0.060(2) Uani 1 1 d . . .
O16 O 0.9248(6) 0.3153(7) 0.0321(3) 0.0512(18) Uani 1 1 d . . .
O17 O 1.3337(7) -0.1015(6) 0.0312(3) 0.0495(18) Uani 1 1 d . . .
O18 O 1.3066(8) 0.0738(7) 0.1051(3) 0.0527(19) Uani 1 1 d . . .
O19 O 1.1408(7) 0.2442(7) 0.1056(3) 0.053(2) Uani 1 1 d . . .
O20 O 0.9823(6) -0.1326(6) 0.2128(2) 0.0373(13) Uani 1 1 d . . .
O21 O 1.1671(9) -0.0837(11) 0.1520(5) 0.112(5) Uani 1 1 d . . .
O22 O 1.0626(8) -0.0970(8) 0.0527(4) 0.0160(17) Uani 0.50 1 d P . .
N1 N 0.8216(6) 0.0834(8) 0.2653(3) 0.0403(18) Uani 1 1 d . . .
N2 N 0.1771(6) 0.0982(8) 0.2771(3) 0.0382(17) Uani 1 1 d . . .
C1 C 0.7324(8) 0.1354(10) 0.2210(4) 0.044(2) Uani 1 1 d . . .
H1A H 0.7581 0.1734 0.1901 0.053 Uiso 1 1 calc R . .
C2 C 0.6045(7) 0.1340(9) 0.2200(4) 0.0371(19) Uani 1 1 d . . .
H2A H 0.5452 0.1686 0.1881 0.045 Uiso 1 1 calc R . .
C3 C 0.5644(6) 0.0810(7) 0.2665(3) 0.0260(14) Uani 1 1 d . . .
C4 C 0.4298(6) 0.0864(7) 0.2696(3) 0.0255(14) Uani 1 1 d . . .
C5 C 0.3563(7) 0.1899(8) 0.2514(4) 0.0360(18) Uani 1 1 d . . .
H5A H 0.3901 0.2571 0.2358 0.043 Uiso 1 1 calc R . .
C6 C 0.2313(7) 0.1923(9) 0.2565(4) 0.0368(19) Uani 1 1 d . . .
H6A H 0.1834 0.2632 0.2450 0.044 Uiso 1 1 calc R . .
C7 C 0.2473(8) -0.0019(10) 0.2934(5) 0.048(2) Uani 1 1 d . . .
H7A H 0.2099 -0.0692 0.3071 0.057 Uiso 1 1 calc R . .
C8 C 0.3738(8) -0.0113(9) 0.2909(4) 0.041(2) Uani 1 1 d . . .
H8A H 0.4199 -0.0827 0.3035 0.049 Uiso 1 1 calc R . .
C9 C 0.6571(7) 0.0232(8) 0.3110(3) 0.0323(17) Uani 1 1 d . . .
H9A H 0.6341 -0.0168 0.3422 0.039 Uiso 1 1 calc R . .
C10 C 0.7821(7) 0.0259(9) 0.3084(4) 0.0381(19) Uani 1 1 d . . .
H10A H 0.8423 -0.0140 0.3381 0.046 Uiso 1 1 calc R . .
C11 C 1.3549(15) 0.5628(13) -0.0188(7) 0.065(6) Uani 0.50 1 d PGU . .
N3 N 1.3101(12) 0.4672(16) -0.0583(8) 0.103(8) Uani 0.50 1 d PGDU . .
C12 C 1.3919(16) 0.3730(15) -0.0654(8) 0.105(10) Uani 0.50 1 d PGDU . .
C13 C 1.5185(15) 0.3744(15) -0.0331(9) 0.094(10) Uani 0.50 1 d PGU . .
C14 C 1.5634(13) 0.4699(17) 0.0063(9) 0.072(8) Uani 0.50 1 d PGU . .
C15 C 1.4815(16) 0.5641(13) 0.0135(7) 0.055(6) Uani 0.50 1 d PG . .
N4 N 1.359(2) 0.2686(17) -0.1034(10) 0.094(8) Uani 0.50 1 d PDU . .


_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 O15 1.641(7) . ?
Mo1 O16 1.836(6) . ?
Mo1 O7 1.848(9) 3_755 ?
Mo1 O1 1.960(8) 3_755 ?
Mo1 O12 1.961(8) . ?
Mo1 O22 2.365(9) 3_755 ?
Mo1 O3 2.578(9) 3_755 ?
Mo2 O20 1.667(5) . ?
Mo2 O1 1.827(10) . ?
Mo2 O4 1.854(9) . ?
Mo2 O21 1.957(9) . ?
Mo2 O5 1.966(9) . ?
Mo2 O22 2.472(8) . ?
Mo2 O8 2.538(9) . ?
Mo3 O11 1.642(6) . ?
Mo3 O6 1.811(8) . ?
Mo3 O17 1.835(6) 3_755 ?
Mo3 O4 1.970(7) . ?
Mo3 O14 1.991(7) 3_755 ?
Mo3 O8 2.385(8) . ?
Mo3 O2 2.551(8) 3_755 ?
Mo4 O13 1.656(7) . ?
Mo4 O21 1.830(7) . ?
Mo4 O18 1.836(8) . ?
Mo4 O7 1.962(8) . ?
Mo4 O17 1.966(6) . ?
Mo4 O22 2.402(9) . ?
Mo4 O2 2.577(9) . ?
Mo5 O10 1.658(6) . ?
Mo5 O19 1.807(7) . ?
Mo5 O5 1.849(7) . ?
Mo5 O16 1.945(6) . ?
Mo5 O6 1.985(8) . ?
Mo5 O8 2.404(9) . ?
Mo5 O3 2.522(9) 3_755 ?
Mo6 O9 1.669(7) . ?
Mo6 O14 1.809(6) . ?
Mo6 O12 1.842(7) . ?
Mo6 O18 1.954(6) . ?
Mo6 O19 1.997(6) . ?
Mo6 O2 2.434(9) . ?
Mo6 O3 2.436(9) 3_755 ?
Cu1 N1 1.897(6) . ?
Cu1 N2 1.897(6) 1_655 ?
P1 O3 1.463(8) 3_755 ?
P1 O3 1.463(8) . ?
P1 O2 1.463(8) . ?
P1 O2 1.463(8) 3_755 ?
P1 O8 1.586(8) 3_755 ?
P1 O8 1.586(8) . ?
P1 O22 1.630(8) 3_755 ?
P1 O22 1.630(8) . ?
O1 Mo1 1.960(8) 3_755 ?
O2 O3 1.519(12) 3_755 ?
O2 O8 1.740(12) 3_755 ?
O2 O22 1.812(12) . ?
O2 Mo3 2.551(8) 3_755 ?
O3 O2 1.519(12) 3_755 ?
O3 O8 1.750(12) 3_755 ?
O3 O22 1.838(12) . ?
O3 Mo6 2.436(9) 3_755 ?
O3 Mo5 2.522(9) 3_755 ?
O3 Mo1 2.578(9) 3_755 ?
O7 Mo1 1.848(9) 3_755 ?
O8 O2 1.740(12) 3_755 ?
O8 O3 1.750(12) 3_755 ?
O14 Mo3 1.991(7) 3_755 ?
O17 Mo3 1.835(6) 3_755 ?
O22 Mo1 2.365(9) 3_755 ?
N1 C10 1.337(12) . ?
N1 C1 1.349(12) . ?
N2 C6 1.325(12) . ?
N2 C7 1.327(13) . ?
N2 Cu1 1.897(6) 1_455 ?
C1 C2 1.379(10) . ?
C1 H1A 0.9300 . ?
C2 C3 1.387(11) . ?
C2 H2A 0.9300 . ?
C3 C9 1.398(10) . ?
C3 C4 1.477(9) . ?
C4 C8 1.374(11) . ?
C4 C5 1.382(11) . ?
C5 C6 1.387(10) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.388(11) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.369(10) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C14 0.93(3) 3_865 ?
C11 N3 1.3900 . ?
C11 C15 1.3900 . ?
C11 C13 1.73(3) 3_865 ?
N3 C12 1.3900 . ?
N3 C14 1.73(2) 3_865 ?
C12 C13 1.3900 . ?
C12 N4 1.427(5) . ?
C12 C15 1.73(2) 3_865 ?
C13 C15 0.81(3) 3_865 ?
C13 C14 1.3900 . ?
C13 C11 1.73(2) 3_865 ?
C14 C15 0.69(3) 3_865 ?
C14 C11 0.93(3) 3_865 ?
C14 C15 1.3900 . ?
C14 C14 1.48(3) 3_865 ?
C14 N3 1.73(2) 3_865 ?
C15 C14 0.69(2) 3_865 ?
C15 C13 0.81(2) 3_865 ?
C15 C15 1.62(3) 3_865 ?
C15 C12 1.73(2) 3_865 ?

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
O15 Mo1 O16 103.3(4) . . ?
O15 Mo1 O7 101.6(5) . 3_755 ?
O16 Mo1 O7 93.1(4) . 3_755 ?
O15 Mo1 O1 100.2(5) . 3_755 ?
O16 Mo1 O1 155.8(5) . 3_755 ?
O7 Mo1 O1 87.9(4) 3_755 3_755 ?
O15 Mo1 O12 101.3(4) . . ?
O16 Mo1 O12 87.8(3) . . ?
O7 Mo1 O12 156.2(5) 3_755 . ?
O1 Mo1 O12 81.9(4) 3_755 . ?
O15 Mo1 O22 157.5(3) . 3_755 ?
O16 Mo1 O22 94.6(3) . 3_755 ?
O7 Mo1 O22 63.4(5) 3_755 3_755 ?
O1 Mo1 O22 64.3(4) 3_755 3_755 ?
O12 Mo1 O22 92.8(3) . 3_755 ?
O15 Mo1 O3 158.5(3) . 3_755 ?
O16 Mo1 O3 65.8(3) . 3_755 ?
O7 Mo1 O3 97.6(5) 3_755 3_755 ?
O1 Mo1 O3 90.0(5) 3_755 3_755 ?
O12 Mo1 O3 61.2(3) . 3_755 ?
O22 Mo1 O3 43.4(3) 3_755 3_755 ?
O20 Mo2 O1 102.0(5) . . ?
O20 Mo2 O4 102.5(4) . . ?
O1 Mo2 O4 94.6(5) . . ?
O20 Mo2 O21 99.5(4) . . ?
O1 Mo2 O21 87.7(4) . . ?
O4 Mo2 O21 156.9(5) . . ?
O20 Mo2 O5 99.4(4) . . ?
O1 Mo2 O5 157.7(5) . . ?
O4 Mo2 O5 86.9(4) . . ?
O21 Mo2 O5 82.5(5) . . ?
O20 Mo2 O22 155.0(3) . . ?
O1 Mo2 O22 63.5(4) . . ?
O4 Mo2 O22 99.1(4) . . ?
O21 Mo2 O22 61.6(4) . . ?
O5 Mo2 O22 94.2(4) . . ?
O20 Mo2 O8 156.3(3) . . ?
O1 Mo2 O8 98.4(5) . . ?
O4 Mo2 O8 63.8(3) . . ?
O21 Mo2 O8 93.2(4) . . ?
O5 Mo2 O8 62.4(3) . . ?
O22 Mo2 O8 47.8(3) . . ?
O11 Mo3 O6 101.9(5) . . ?
O11 Mo3 O17 104.1(4) . 3_755 ?
O6 Mo3 O17 95.4(3) . 3_755 ?
O11 Mo3 O4 99.1(5) . . ?
O6 Mo3 O4 87.8(3) . . ?
O17 Mo3 O4 155.3(4) 3_755 . ?
O11 Mo3 O14 101.4(3) . 3_755 ?
O6 Mo3 O14 155.4(5) . 3_755 ?
O17 Mo3 O14 86.5(3) 3_755 3_755 ?
O4 Mo3 O14 80.8(3) . 3_755 ?
O11 Mo3 O8 157.9(4) . . ?
O6 Mo3 O8 63.1(5) . . ?
O17 Mo3 O8 93.9(3) 3_755 . ?
O4 Mo3 O8 65.8(4) . . ?
O14 Mo3 O8 92.3(3) 3_755 . ?
O11 Mo3 O2 160.2(3) . 3_755 ?
O6 Mo3 O2 96.5(5) . 3_755 ?
O17 Mo3 O2 66.5(3) 3_755 3_755 ?
O4 Mo3 O2 88.9(4) . 3_755 ?
O14 Mo3 O2 61.8(3) 3_755 3_755 ?
O8 Mo3 O2 41.1(3) . 3_755 ?
O13 Mo4 O21 103.7(5) . . ?
O13 Mo4 O18 102.8(4) . . ?
O21 Mo4 O18 94.2(4) . . ?
O13 Mo4 O7 100.4(5) . . ?
O21 Mo4 O7 87.3(3) . . ?
O18 Mo4 O7 155.7(5) . . ?
O13 Mo4 O17 101.0(4) . . ?
O21 Mo4 O17 154.2(4) . . ?
O18 Mo4 O17 87.4(3) . . ?
O7 Mo4 O17 81.1(3) . . ?
O13 Mo4 O22 157.3(4) . . ?
O21 Mo4 O22 64.5(4) . . ?
O18 Mo4 O22 97.6(3) . . ?
O7 Mo4 O22 61.3(5) . . ?
O17 Mo4 O22 89.7(3) . . ?
O13 Mo4 O2 159.5(4) . . ?
O21 Mo4 O2 93.2(5) . . ?
O18 Mo4 O2 63.9(3) . . ?
O7 Mo4 O2 91.8(5) . . ?
O17 Mo4 O2 64.5(3) . . ?
O22 Mo4 O2 42.5(3) . . ?
O10 Mo5 O19 103.0(3) . . ?
O10 Mo5 O5 102.3(5) . . ?
O19 Mo5 O5 95.5(4) . . ?
O10 Mo5 O16 101.1(4) . . ?
O19 Mo5 O16 89.6(3) . . ?
O5 Mo5 O16 154.3(4) . . ?
O10 Mo5 O6 99.7(5) . . ?
O19 Mo5 O6 156.5(5) . . ?
O5 Mo5 O6 85.5(3) . . ?
O16 Mo5 O6 80.1(3) . . ?
O10 Mo5 O8 157.2(3) . . ?
O19 Mo5 O8 98.1(3) . . ?
O5 Mo5 O8 66.7(4) . . ?
O16 Mo5 O8 87.7(3) . . ?
O6 Mo5 O8 60.7(4) . . ?
O10 Mo5 O3 160.4(4) . 3_755 ?
O19 Mo5 O3 64.0(3) . 3_755 ?
O5 Mo5 O3 93.8(5) . 3_755 ?
O16 Mo5 O3 65.9(3) . 3_755 ?
O6 Mo5 O3 92.5(4) . 3_755 ?
O8 Mo5 O3 41.5(3) . 3_755 ?
O9 Mo6 O14 104.4(4) . . ?
O9 Mo6 O12 103.0(5) . . ?
O14 Mo6 O12 94.9(3) . . ?
O9 Mo6 O18 100.9(4) . . ?
O14 Mo6 O18 88.2(3) . . ?
O12 Mo6 O18 154.2(4) . . ?
O9 Mo6 O19 99.4(4) . . ?
O14 Mo6 O19 155.5(4) . . ?
O12 Mo6 O19 85.3(3) . . ?
O18 Mo6 O19 81.5(3) . . ?
O9 Mo6 O2 163.1(5) . . ?
O14 Mo6 O2 66.4(3) . . ?
O12 Mo6 O2 92.1(4) . . ?
O18 Mo6 O2 65.8(3) . . ?
O19 Mo6 O2 89.2(3) . . ?
O9 Mo6 O3 159.5(4) . 3_755 ?
O14 Mo6 O3 94.0(3) . 3_755 ?
O12 Mo6 O3 65.6(3) . 3_755 ?
O18 Mo6 O3 88.6(3) . 3_755 ?
O19 Mo6 O3 63.8(3) . 3_755 ?
O2 Mo6 O3 36.3(3) . 3_755 ?
N1 Cu1 N2 177.0(4) . 1_655 ?
O3 P1 O3 180.0(7) 3_755 . ?
O3 P1 O2 62.5(5) 3_755 . ?
O3 P1 O2 117.5(5) . . ?
O3 P1 O2 117.5(5) 3_755 3_755 ?
O3 P1 O2 62.5(5) . 3_755 ?
O2 P1 O2 180.0(10) . 3_755 ?
O3 P1 O8 110.1(5) 3_755 3_755 ?
O3 P1 O8 69.9(5) . 3_755 ?
O2 P1 O8 69.4(5) . 3_755 ?
O2 P1 O8 110.6(5) 3_755 3_755 ?
O3 P1 O8 69.9(5) 3_755 . ?
O3 P1 O8 110.1(5) . . ?
O2 P1 O8 110.6(5) . . ?
O2 P1 O8 69.4(5) 3_755 . ?
O8 P1 O8 180.0(5) 3_755 . ?
O3 P1 O22 72.7(5) 3_755 3_755 ?
O3 P1 O22 107.3(5) . 3_755 ?
O2 P1 O22 108.5(5) . 3_755 ?
O2 P1 O22 71.5(5) 3_755 3_755 ?
O8 P1 O22 78.4(4) 3_755 3_755 ?
O8 P1 O22 101.6(4) . 3_755 ?
O3 P1 O22 107.3(5) 3_755 . ?
O3 P1 O22 72.7(5) . . ?
O2 P1 O22 71.5(5) . . ?
O2 P1 O22 108.5(5) 3_755 . ?
O8 P1 O22 101.6(4) 3_755 . ?
O8 P1 O22 78.4(4) . . ?
O22 P1 O22 180.0(6) 3_755 . ?
Mo2 O1 Mo1 138.1(6) . 3_755 ?
P1 O2 O3 58.7(5) . 3_755 ?
P1 O2 O8 58.6(4) . 3_755 ?
O3 O2 O8 100.0(6) 3_755 3_755 ?
P1 O2 O22 58.5(4) . . ?
O3 O2 O22 96.5(6) 3_755 . ?
O8 O2 O22 89.1(6) 3_755 . ?
P1 O2 Mo6 130.5(5) . . ?
O3 O2 Mo6 71.9(5) 3_755 . ?
O8 O2 Mo6 133.2(5) 3_755 . ?
O22 O2 Mo6 136.9(5) . . ?
P1 O2 Mo3 122.9(5) . 3_755 ?
O3 O2 Mo3 139.0(6) 3_755 3_755 ?
O8 O2 Mo3 64.3(4) 3_755 3_755 ?
O22 O2 Mo3 119.5(5) . 3_755 ?
Mo6 O2 Mo3 91.3(3) . 3_755 ?
P1 O2 Mo4 122.0(5) . . ?
O3 O2 Mo4 127.5(6) 3_755 . ?
O8 O2 Mo4 125.6(5) 3_755 . ?
O22 O2 Mo4 63.6(4) . . ?
Mo6 O2 Mo4 90.3(3) . . ?
Mo3 O2 Mo4 88.4(3) 3_755 . ?
P1 O3 O2 58.7(4) . 3_755 ?
P1 O3 O8 58.4(4) . 3_755 ?
O2 O3 O8 100.0(6) 3_755 3_755 ?
P1 O3 O22 57.9(4) . . ?
O2 O3 O22 96.4(6) 3_755 . ?
O8 O3 O22 88.0(5) 3_755 . ?
P1 O3 Mo6 130.3(5) . 3_755 ?
O2 O3 Mo6 71.8(5) 3_755 3_755 ?
O8 O3 Mo6 141.4(5) 3_755 3_755 ?
O22 O3 Mo6 129.8(5) . 3_755 ?
P1 O3 Mo5 123.9(5) . 3_755 ?
O2 O3 Mo5 132.9(6) 3_755 3_755 ?
O8 O3 Mo5 65.6(4) 3_755 3_755 ?
O22 O3 Mo5 125.7(5) . 3_755 ?
Mo6 O3 Mo5 92.0(3) 3_755 3_755 ?
P1 O3 Mo1 119.8(5) . 3_755 ?
O2 O3 Mo1 134.6(6) 3_755 3_755 ?
O8 O3 Mo1 117.3(5) 3_755 3_755 ?
O22 O3 Mo1 62.1(4) . 3_755 ?
Mo6 O3 Mo1 91.3(3) 3_755 3_755 ?
Mo5 O3 Mo1 88.1(3) 3_755 3_755 ?
Mo2 O4 Mo3 137.4(5) . . ?
Mo5 O5 Mo2 138.5(5) . . ?
Mo3 O6 Mo5 139.6(8) . . ?
Mo1 O7 Mo4 138.2(8) 3_755 . ?
P1 O8 O2 51.9(4) . 3_755 ?
P1 O8 O3 51.7(4) . 3_755 ?
O2 O8 O3 91.6(5) 3_755 3_755 ?
P1 O8 Mo3 126.4(5) . . ?
O2 O8 Mo3 74.6(4) 3_755 . ?
O3 O8 Mo3 138.7(5) 3_755 . ?
P1 O8 Mo5 124.4(5) . . ?
O2 O8 Mo5 144.6(6) 3_755 . ?
O3 O8 Mo5 72.8(4) 3_755 . ?
Mo3 O8 Mo5 96.1(3) . . ?
P1 O8 Mo2 116.0(4) . . ?
O2 O8 Mo2 121.6(5) 3_755 . ?
O3 O8 Mo2 126.7(5) 3_755 . ?
Mo3 O8 Mo2 92.7(3) . . ?
Mo5 O8 Mo2 92.4(3) . . ?
Mo6 O12 Mo1 141.3(5) . . ?
Mo6 O14 Mo3 139.6(5) . 3_755 ?
Mo1 O16 Mo5 139.2(4) . . ?
Mo3 O17 Mo4 140.3(4) 3_755 . ?
Mo4 O18 Mo6 139.2(4) . . ?
Mo5 O19 Mo6 139.3(5) . . ?
Mo4 O21 Mo2 139.9(6) . . ?
P1 O22 O2 50.0(4) . . ?
P1 O22 O3 49.5(4) . . ?
O2 O22 O3 86.5(5) . . ?
P1 O22 Mo1 123.8(5) . 3_755 ?
O2 O22 Mo1 134.8(5) . 3_755 ?
O3 O22 Mo1 74.5(4) . 3_755 ?
P1 O22 Mo4 123.7(5) . . ?
O2 O22 Mo4 73.9(4) . . ?
O3 O22 Mo4 142.1(5) . . ?
Mo1 O22 Mo4 96.6(3) 3_755 . ?
P1 O22 Mo2 117.5(4) . . ?
O2 O22 Mo2 130.1(5) . . ?
O3 O22 Mo2 123.1(5) . . ?
Mo1 O22 Mo2 93.9(3) 3_755 . ?
Mo4 O22 Mo2 93.8(3) . . ?
C10 N1 C1 117.8(7) . . ?
C10 N1 Cu1 119.2(6) . . ?
C1 N1 Cu1 122.9(6) . . ?
C6 N2 C7 117.4(7) . . ?
C6 N2 Cu1 121.2(6) . 1_455 ?
C7 N2 Cu1 120.5(6) . 1_455 ?
N1 C1 C2 122.3(8) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C1 C2 C3 119.9(8) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C2 C3 C9 117.1(6) . . ?
C2 C3 C4 121.6(7) . . ?
C9 C3 C4 121.2(7) . . ?
C8 C4 C5 117.8(7) . . ?
C8 C4 C3 121.0(7) . . ?
C5 C4 C3 121.2(7) . . ?
C4 C5 C6 119.2(8) . . ?
C4 C5 H5A 120.4 . . ?
C6 C5 H5A 120.4 . . ?
N2 C6 C5 123.1(8) . . ?
N2 C6 H6A 118.5 . . ?
C5 C6 H6A 118.5 . . ?
N2 C7 C8 123.4(9) . . ?
N2 C7 H7A 118.3 . . ?
C8 C7 H7A 118.3 . . ?
C4 C8 C7 119.1(9) . . ?
C4 C8 H8A 120.5 . . ?
C7 C8 H8A 120.5 . . ?
C10 C9 C3 119.6(8) . . ?
C10 C9 H9A 120.2 . . ?
C3 C9 H9A 120.2 . . ?
N1 C10 C9 123.1(8) . . ?
N1 C10 H10A 118.4 . . ?
C9 C10 H10A 118.4 . . ?
C14 C11 N3 94.0(13) 3_865 . ?
C14 C11 C15 26.0(13) 3_865 . ?
N3 C11 C15 120.0 . . ?
C14 C11 C13 53.4(15) 3_865 3_865 ?
N3 C11 C13 147.5(12) . 3_865 ?
C15 C11 C13 27.5(12) . 3_865 ?
C11 N3 C12 120.0 . . ?
C11 N3 C14 32.5(9) . 3_865 ?
C12 N3 C14 87.5(9) . 3_865 ?
C13 C12 N3 120.0 . . ?
C13 C12 N4 113.7(9) . . ?
N3 C12 N4 126.3(9) . . ?
C13 C12 C15 27.5(9) . 3_865 ?
N3 C12 C15 92.5(9) . 3_865 ?
N4 C12 C15 141.1(13) . 3_865 ?
C15 C13 C12 100.1(17) 3_865 . ?
C15 C13 C14 20.0(17) 3_865 . ?
C12 C13 C14 120.0 . . ?
C15 C13 C11 52.5(15) 3_865 3_865 ?
C12 C13 C11 152.5(10) . 3_865 ?
C14 C13 C11 32.5(9) . 3_865 ?
C15 C14 C11 118(3) 3_865 3_865 ?
C15 C14 C13 24(2) 3_865 . ?
C11 C14 C13 94.0(14) 3_865 . ?
C15 C14 C15 96(2) 3_865 . ?
C11 C14 C15 145.9(14) 3_865 . ?
C13 C14 C15 120.0 . . ?
C15 C14 C14 69(2) 3_865 3_865 ?
C11 C14 C14 173(2) 3_865 3_865 ?
C13 C14 C14 92.5(8) . 3_865 ?
C15 C14 C14 27.5(8) . 3_865 ?
C15 C14 N3 171(4) 3_865 3_865 ?
C11 C14 N3 53.4(15) 3_865 3_865 ?
C13 C14 N3 147.5(18) . 3_865 ?
C15 C14 N3 92.5(18) . 3_865 ?
C14 C14 N3 120(2) 3_865 3_865 ?
C14 C15 C13 136(5) 3_865 3_865 ?
C14 C15 C14 84(2) 3_865 . ?
C13 C15 C14 140(3) 3_865 . ?
C14 C15 C11 36(2) 3_865 . ?
C13 C15 C11 100(3) 3_865 . ?
C14 C15 C11 120.0 . . ?
C14 C15 C15 59(2) 3_865 3_865 ?
C13 C15 C15 165(3) 3_865 3_865 ?
C14 C15 C15 25.0(8) . 3_865 ?
C11 C15 C15 95.0(8) . 3_865 ?
C14 C15 C12 171(4) 3_865 3_865 ?
C13 C15 C12 52.5(15) 3_865 3_865 ?
C14 C15 C12 87.5(18) . 3_865 ?
C11 C15 C12 152.5(18) . 3_865 ?
C15 C15 C12 112.4(19) 3_865 3_865 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.356
_refine_diff_density_min         -2.347
_refine_diff_density_rms         0.231
####################################################################### 
# 
# 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_k
_database_code_depnum_ccdc_archive 'CCDC 1006427'
_audit_update_record             
;
2014-06-03 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H44 Cu2 N10 O42 P W12'
_chemical_formula_weight         3869.14

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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/m

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

_cell_length_a                   22.726(4)
_cell_length_b                   15.455(3)
_cell_length_c                   12.036(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.17(3)
_cell_angle_gamma                90.00
_cell_volume                     3826.0(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3469
_exptl_absorpt_coefficient_mu    18.619
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0635
_exptl_absorpt_correction_T_max  0.1440
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18862
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4515
_reflns_number_gt                4152
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0000P)²+2170.1165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4515
_refine_ls_number_parameters     277
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.1017
_refine_ls_wR_factor_ref         0.2347
_refine_ls_wR_factor_gt          0.2294
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W -0.64646(6) -0.61431(7) 0.83420(11) 0.0324(4) Uani 1 1 d . . .
W2 W -0.52112(7) -0.61607(10) 0.73013(13) 0.0437(4) Uani 1 1 d . . .
W3 W -0.5000 -0.73045(9) 1.0000 0.0380(5) Uani 1 2 d S . .
W4 W -0.37596(8) -0.5000 0.89152(15) 0.0247(4) Uani 1 2 d S . .
Cu1 Cu -0.6952(3) -1.0000 0.8635(4) 0.0257(10) Uani 1 2 d S . .
P1 P -0.5000 -0.5000 1.0000 0.029(3) Uani 1 4 d S . .
OW1 O -0.5846(14) -1.0000 0.929(3) 0.033(6) Uani 1 2 d S . .
O1 O -0.575(2) -0.5000 0.962(4) 0.018(9) Uani 0.50 2 d SP . .
O2 O -0.488(2) -0.5000 0.883(4) 0.019(9) Uani 0.50 2 d SPU . .
O3 O -0.5258(15) -0.580(2) 0.930(3) 0.018(6) Uani 0.50 1 d PU . .
O4 O -0.671(3) -0.5000 0.781(4) 0.10(2) Uani 1 2 d S . .
O5 O -0.3154(13) -0.5000 0.842(3) 0.030(6) Uani 1 2 d S . .
O6 O -0.7152(10) -0.6702(15) 0.7559(19) 0.039(5) Uani 1 1 d . . .
O7 O -0.5000 -0.838(2) 1.0000 0.055(9) Uani 1 2 d S . .
O8 O -0.4308(11) -0.5854(15) 0.794(2) 0.041(5) Uani 1 1 d U . .
O9 O -0.653(2) -0.5852(15) 0.984(2) 0.087(13) Uani 1 1 d . . .
O10 O -0.5422(15) -0.5000 0.667(3) 0.053(9) Uani 1 2 d S . .
O11 O -0.6057(10) -0.619(2) 0.725(3) 0.070(9) Uani 1 1 d . . .
O12 O -0.5887(12) -0.703(2) 0.927(3) 0.065(8) Uani 1 1 d . . .
O13 O -0.4977(10) -0.707(2) 0.846(2) 0.062(8) Uani 1 1 d . . .
O14 O -0.5335(16) -0.673(2) 0.594(4) 0.098(13) Uani 1 1 d . . .
N3 N -0.499(4) 0.0000 0.202(6) 0.11(3) Uani 1 2 d S . .
N1 N -0.7154(8) -0.9096(9) 0.7300(13) 0.028(5) Uani 1 1 d G . .
C1 C -0.6653(6) -0.8738(12) 0.7079(15) 0.042(8) Uani 1 1 d G . .
H1A H -0.6226 -0.8911 0.7543 0.051 Uiso 1 1 calc R . .
C2 C -0.6790(7) -0.8119(12) 0.6164(16) 0.029(6) Uani 1 1 d G . .
H2A H -0.6455 -0.7879 0.6016 0.034 Uiso 1 1 calc R . .
C3 C -0.7428(8) -0.7859(10) 0.5470(13) 0.024(5) Uani 1 1 d G . .
C4 C -0.7929(6) -0.8218(12) 0.5691(15) 0.037(7) Uani 1 1 d G . .
H4A H -0.8356 -0.8044 0.5226 0.044 Uiso 1 1 calc R . .
C5 C -0.7792(7) -0.8836(11) 0.6606(16) 0.033(6) Uani 1 1 d G . .
H5A H -0.8127 -0.9076 0.6754 0.039 Uiso 1 1 calc R . .
C6 C -0.6770(10) -0.8263(9) 0.9974(14) 0.035(7) Uani 1 1 d G . .
H6A H -0.6806 -0.7993 0.9257 0.042 Uiso 1 1 calc R . .
C7 C -0.6665(11) -0.7772(7) 1.1009(18) 0.050(9) Uani 1 1 d G . .
H7A H -0.6631 -0.7173 1.0984 0.060 Uiso 1 1 calc R . .
C8 C -0.6611(10) -0.8175(11) 1.2080(14) 0.037(7) Uani 1 1 d G . .
H8A H -0.6541 -0.7847 1.2772 0.045 Uiso 1 1 calc R . .
C9 C -0.6663(9) -0.9070(11) 1.2116(12) 0.031(6) Uani 1 1 d G . .
C10 C -0.6768(9) -0.9561(7) 1.1081(14) 0.026(6) Uani 1 1 d G . .
C13 C -0.501(2) 0.074(3) 0.378(4) 0.064(12) Uani 1 1 d . . .
H13A H -0.5013 0.1268 0.4155 0.076 Uiso 1 1 calc R . .
C14 C -0.502(2) 0.0000 0.436(4) 0.043(12) Uani 1 2 d S . .
C12 C -0.500(3) 0.075(4) 0.263(4) 0.10(2) Uani 1 1 d . . .
H12A H -0.5003 0.1281 0.2262 0.117 Uiso 1 1 calc R . .
C11 C -0.6634(16) -0.959(2) 1.317(2) 0.047(9) Uani 1 1 d . . .
H11A H -0.6615 -0.9308 1.3862 0.056 Uiso 1 1 calc R . .
N2 N -0.6822(8) -0.9158(9) 1.0010(11) 0.022(4) Uani 1 1 d G . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O6 1.68(2) . ?
W1 O4 1.879(19) . ?
W1 O12 1.90(3) . ?
W1 O11 1.90(3) . ?
W1 O9 1.92(3) . ?
W1 O1 2.45(3) . ?
W1 O3 2.54(3) . ?
W2 O14 1.77(3) . ?
W2 O13 1.89(3) . ?
W2 O11 1.90(2) . ?
W2 O8 1.92(2) . ?
W2 O10 1.927(13) . ?
W2 O2 2.45(3) . ?
W2 O3 2.51(3) . ?
W3 O7 1.66(3) . ?
W3 O12 1.87(3) 2_457 ?
W3 O12 1.87(3) . ?
W3 O13 1.92(3) 2_457 ?
W3 O13 1.92(3) . ?
W3 O3 2.45(3) 2_457 ?
W3 O3 2.45(3) . ?
W4 O5 1.72(2) . ?
W4 O8 1.85(2) . ?
W4 O8 1.85(2) 6_545 ?
W4 O9 1.89(2) 5_447 ?
W4 O9 1.89(2) 2_457 ?
W4 O1 2.46(5) 5_447 ?
W4 O2 2.50(5) . ?
Cu1 N2 2.026(11) . ?
Cu1 N2 2.026(19) 6_535 ?
Cu1 N1 2.029(11) 6_535 ?
Cu1 N1 2.029(11) . ?
Cu1 OW1 2.29(3) . ?
Cu1 O5 2.63(3) 3_445 ?
P1 O3 1.48(3) 5_447 ?
P1 O3 1.48(3) . ?
P1 O3 1.48(3) 6_545 ?
P1 O3 1.48(3) 2_457 ?
P1 O2 1.54(5) . ?
P1 O2 1.54(5) 5_447 ?
P1 O1 1.56(4) 5_447 ?
P1 O1 1.56(4) . ?
O1 O2 1.80(7) 5_447 ?
O1 O3 1.82(5) . ?
O1 O3 1.82(5) 6_545 ?
O1 W1 2.45(3) 6_545 ?
O1 W4 2.46(5) 5_447 ?
O2 O3 1.73(5) 6_545 ?
O2 O3 1.73(5) . ?
O2 O1 1.80(7) 5_447 ?
O2 W2 2.45(3) 6_545 ?
O3 O3 1.60(6) 2_457 ?
O4 W1 1.879(18) 6_545 ?
O5 Cu1 2.63(3) 3 ?
O9 W4 1.89(2) 5_447 ?
O10 W2 1.927(13) 6_545 ?
N3 C12 1.38(5) . ?
N3 C12 1.38(5) 6 ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C1 H1A 0.9300 . ?
C2 C3 1.3900 . ?
C2 H2A 0.9300 . ?
C3 C4 1.3900 . ?
C3 C3 1.52(2) 7_336 ?
C4 C5 1.3900 . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.3900 . ?
C6 N2 1.3900 . ?
C6 H6A 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7A 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8A 0.9300 . ?
C9 C10 1.3900 . ?
C9 C11 1.48(3) . ?
C10 C10 1.36(2) 6_535 ?
C10 N2 1.3900 . ?
C13 C14 1.35(4) . ?
C13 C12 1.39(6) . ?
C13 H13A 0.9300 . ?
C14 C13 1.35(4) 6 ?
C14 C14 1.50(8) 5_456 ?
C12 H12A 0.9300 . ?
C11 C11 1.25(7) 6_535 ?
C11 H11A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O4 103(2) . . ?
O6 W1 O12 101.8(12) . . ?
O4 W1 O12 155(2) . . ?
O6 W1 O11 101.7(12) . . ?
O4 W1 O11 87.8(18) . . ?
O12 W1 O11 87.6(12) . . ?
O6 W1 O9 103.0(14) . . ?
O4 W1 O9 88.3(13) . . ?
O12 W1 O9 85.8(13) . . ?
O11 W1 O9 155.3(15) . . ?
O6 W1 O1 159.1(12) . . ?
O4 W1 O1 63.7(18) . . ?
O12 W1 O1 92.4(13) . . ?
O11 W1 O1 94.1(15) . . ?
O9 W1 O1 62.4(15) . . ?
O6 W1 O3 158.2(10) . . ?
O4 W1 O3 94(2) . . ?
O12 W1 O3 62.5(11) . . ?
O11 W1 O3 64.6(11) . . ?
O9 W1 O3 91.4(14) . . ?
O1 W1 O3 42.6(12) . . ?
O14 W2 O13 101.4(17) . . ?
O14 W2 O11 101.4(15) . . ?
O13 W2 O11 88.4(11) . . ?
O14 W2 O8 102.4(13) . . ?
O13 W2 O8 88.3(10) . . ?
O11 W2 O8 156.1(13) . . ?
O14 W2 O10 100.5(18) . . ?
O13 W2 O10 158.1(15) . . ?
O11 W2 O10 86.0(14) . . ?
O8 W2 O10 88.4(12) . . ?
O14 W2 O2 159.2(17) . . ?
O13 W2 O2 95.2(13) . . ?
O11 W2 O2 91.5(15) . . ?
O8 W2 O2 65.4(13) . . ?
O10 W2 O2 63.9(13) . . ?
O14 W2 O3 159.8(15) . . ?
O13 W2 O3 64.7(13) . . ?
O11 W2 O3 65.3(12) . . ?
O8 W2 O3 92.0(10) . . ?
O10 W2 O3 93.8(14) . . ?
O2 W2 O3 40.9(12) . . ?
O7 W3 O12 103.1(10) . 2_457 ?
O7 W3 O12 103.1(11) . . ?
O12 W3 O12 154(2) 2_457 . ?
O7 W3 O13 100.9(10) . 2_457 ?
O12 W3 O13 88.1(10) 2_457 2_457 ?
O12 W3 O13 87.0(11) . 2_457 ?
O7 W3 O13 100.9(10) . . ?
O12 W3 O13 87.0(11) 2_457 . ?
O12 W3 O13 88.1(10) . . ?
O13 W3 O13 158(2) 2_457 . ?
O7 W3 O3 161.0(7) . 2_457 ?
O12 W3 O3 64.6(12) 2_457 2_457 ?
O12 W3 O3 90.0(13) . 2_457 ?
O13 W3 O3 65.6(12) 2_457 2_457 ?
O13 W3 O3 93.2(12) . 2_457 ?
O7 W3 O3 161.0(7) . . ?
O12 W3 O3 90.0(13) 2_457 . ?
O12 W3 O3 64.6(12) . . ?
O13 W3 O3 93.2(12) 2_457 . ?
O13 W3 O3 65.6(12) . . ?
O3 W3 O3 38.1(15) 2_457 . ?
O5 W4 O8 101.6(10) . . ?
O5 W4 O8 101.6(10) . 6_545 ?
O8 W4 O8 90.9(14) . 6_545 ?
O5 W4 O9 102.7(14) . 5_447 ?
O8 W4 O9 155.6(14) . 5_447 ?
O8 W4 O9 85.2(12) 6_545 5_447 ?
O5 W4 O9 102.7(14) . 2_457 ?
O8 W4 O9 85.2(12) . 2_457 ?
O8 W4 O9 155.6(14) 6_545 2_457 ?
O9 W4 O9 88.4(14) 5_447 2_457 ?
O5 W4 O1 158.0(15) . 5_447 ?
O8 W4 O1 93.7(10) . 5_447 ?
O8 W4 O1 93.7(10) 6_545 5_447 ?
O9 W4 O1 62.7(13) 5_447 5_447 ?
O9 W4 O1 62.7(13) 2_457 5_447 ?
O5 W4 O2 159.5(15) . . ?
O8 W4 O2 64.9(10) . . ?
O8 W4 O2 64.9(10) 6_545 . ?
O9 W4 O2 91.9(15) 5_447 . ?
O9 W4 O2 91.9(15) 2_457 . ?
O1 W4 O2 42.5(15) 5_447 . ?
N2 Cu1 N2 79.9(11) . 6_535 ?
N2 Cu1 N1 174.0(7) . 6_535 ?
N2 Cu1 N1 96.3(9) 6_535 6_535 ?
N2 Cu1 N1 96.3(7) . . ?
N2 Cu1 N1 174.0(12) 6_535 . ?
N1 Cu1 N1 87.0(10) 6_535 . ?
N2 Cu1 OW1 87.8(7) . . ?
N2 Cu1 OW1 87.8(13) 6_535 . ?
N1 Cu1 OW1 96.8(7) 6_535 . ?
N1 Cu1 OW1 96.8(7) . . ?
N2 Cu1 O5 82.3(7) . 3_445 ?
N2 Cu1 O5 82.3(13) 6_535 3_445 ?
N1 Cu1 O5 92.6(7) 6_535 3_445 ?
N1 Cu1 O5 92.6(7) . 3_445 ?
OW1 Cu1 O5 167.0(10) . 3_445 ?
O3 P1 O3 180.0(14) 5_447 . ?
O3 P1 O3 66(2) 5_447 6_545 ?
O3 P1 O3 114(2) . 6_545 ?
O3 P1 O3 114(2) 5_447 2_457 ?
O3 P1 O3 66(2) . 2_457 ?
O3 P1 O3 180.000(9) 6_545 2_457 ?
O3 P1 O2 110.0(15) 5_447 . ?
O3 P1 O2 70.0(15) . . ?
O3 P1 O2 70.0(15) 6_545 . ?
O3 P1 O2 110.0(15) 2_457 . ?
O3 P1 O2 70.0(15) 5_447 5_447 ?
O3 P1 O2 110.0(15) . 5_447 ?
O3 P1 O2 110.0(15) 6_545 5_447 ?
O3 P1 O2 70.0(15) 2_457 5_447 ?
O2 P1 O2 180(3) . 5_447 ?
O3 P1 O1 73.5(15) 5_447 5_447 ?
O3 P1 O1 106.5(15) . 5_447 ?
O3 P1 O1 106.5(15) 6_545 5_447 ?
O3 P1 O1 73.5(15) 2_457 5_447 ?
O2 P1 O1 71(2) . 5_447 ?
O2 P1 O1 109(2) 5_447 5_447 ?
O3 P1 O1 106.5(15) 5_447 . ?
O3 P1 O1 73.5(15) . . ?
O3 P1 O1 73.5(15) 6_545 . ?
O3 P1 O1 106.5(15) 2_457 . ?
O2 P1 O1 109(2) . . ?
O2 P1 O1 71(2) 5_447 . ?
O1 P1 O1 180.000(3) 5_447 . ?
P1 O1 O2 54(2) . 5_447 ?
P1 O1 O3 51.3(15) . . ?
O2 O1 O3 86(2) 5_447 . ?
P1 O1 O3 51.3(15) . 6_545 ?
O2 O1 O3 86(2) 5_447 6_545 ?
O3 O1 O3 86(3) . 6_545 ?
P1 O1 W1 122.3(15) . . ?
O2 O1 W1 132.2(11) 5_447 . ?
O3 O1 W1 71.1(13) . . ?
O3 O1 W1 131(3) 6_545 . ?
P1 O1 W1 122.3(15) . 6_545 ?
O2 O1 W1 132.2(11) 5_447 6_545 ?
O3 O1 W1 131(3) . 6_545 ?
O3 O1 W1 71.1(13) 6_545 6_545 ?
W1 O1 W1 92.1(15) . 6_545 ?
P1 O1 W4 124(3) . 5_447 ?
O2 O1 W4 70(2) 5_447 5_447 ?
O3 O1 W4 131.4(18) . 5_447 ?
O3 O1 W4 131.4(18) 6_545 5_447 ?
W1 O1 W4 93.7(13) . 5_447 ?
W1 O1 W4 93.7(13) 6_545 5_447 ?
P1 O2 O3 53.2(17) . 6_545 ?
P1 O2 O3 53.2(17) . . ?
O3 O2 O3 92(3) 6_545 . ?
P1 O2 O1 55(2) . 5_447 ?
O3 O2 O1 87(2) 6_545 5_447 ?
O3 O2 O1 87(2) . 5_447 ?
P1 O2 W2 124.6(14) . . ?
O3 O2 W2 137(3) 6_545 . ?
O3 O2 W2 71.4(13) . . ?
O1 O2 W2 129.3(12) 5_447 . ?
P1 O2 W2 124.6(14) . 6_545 ?
O3 O2 W2 71.4(13) 6_545 6_545 ?
O3 O2 W2 137(3) . 6_545 ?
O1 O2 W2 129.3(12) 5_447 6_545 ?
W2 O2 W2 94.2(16) . 6_545 ?
P1 O2 W4 122(2) . . ?
O3 O2 W4 128.5(18) 6_545 . ?
O3 O2 W4 128.5(18) . . ?
O1 O2 W4 67(2) 5_447 . ?
W2 O2 W4 90.8(13) . . ?
W2 O2 W4 90.8(13) 6_545 . ?
P1 O3 O3 57.2(12) . 2_457 ?
P1 O3 O2 56.8(17) . . ?
O3 O3 O2 96(2) 2_457 . ?
P1 O3 O1 55.3(16) . . ?
O3 O3 O1 91(2) 2_457 . ?
O2 O3 O1 91(2) . . ?
P1 O3 W3 128.2(17) . . ?
O3 O3 W3 71.0(7) 2_457 . ?
O2 O3 W3 135(2) . . ?
O1 O3 W3 131(2) . . ?
P1 O3 W2 124.5(18) . . ?
O3 O3 W2 135(3) 2_457 . ?
O2 O3 W2 67.7(17) . . ?
O1 O3 W2 129(2) . . ?
W3 O3 W2 91.3(11) . . ?
P1 O3 W1 121.5(17) . . ?
O3 O3 W1 130(3) 2_457 . ?
O2 O3 W1 126(2) . . ?
O1 O3 W1 66.2(15) . . ?
W3 O3 W1 90.8(11) . . ?
W2 O3 W1 90.0(10) . . ?
W1 O4 W1 140(3) 6_545 . ?
W4 O5 Cu1 156.4(16) . 3 ?
W4 O8 W2 138.3(13) . . ?
W4 O9 W1 140.3(18) 5_447 . ?
W2 O10 W2 137(2) 6_545 . ?
W2 O11 W1 139.5(17) . . ?
W3 O12 W1 141.2(17) . . ?
W2 O13 W3 137.7(19) . . ?
C12 N3 C12 115(5) . 6 ?
C1 N1 C5 120.0 . . ?
C1 N1 Cu1 119.9(9) . . ?
C5 N1 Cu1 120.1(9) . . ?
N1 C1 C2 120.0 . . ?
N1 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 C3 120(2) . 7_336 ?
C4 C3 C3 120(2) . 7_336 ?
C3 C4 C5 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 H5A 120.0 . . ?
N1 C5 H5A 120.0 . . ?
C7 C6 N2 120.0 . . ?
C7 C6 H6A 120.0 . . ?
N2 C6 H6A 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 C11 126.7(17) . . ?
C10 C9 C11 113.3(17) . . ?
C10 C10 N2 116.7 6_535 . ?
C10 C10 C9 123.1 6_535 . ?
N2 C10 C9 120.0 . . ?
C14 C13 C12 122(5) . . ?
C14 C13 H13A 118.9 . . ?
C12 C13 H13A 118.9 . . ?
C13 C14 C13 116(5) 6 . ?
C13 C14 C14 122(3) 6 5_456 ?
C13 C14 C14 122(3) . 5_456 ?
N3 C12 C13 122(5) . . ?
N3 C12 H12A 118.9 . . ?
C13 C12 H12A 118.9 . . ?
C11 C11 C9 123.2(14) 6_535 . ?
C11 C11 H11A 118.4 6_535 . ?
C9 C11 H11A 118.4 . . ?
C10 N2 C6 120.0 . . ?
C10 N2 Cu1 113.2(8) . . ?
C6 N2 Cu1 126.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         3.128
_refine_diff_density_min         -3.592
_refine_diff_density_rms         0.515
