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

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 Cu2 Mo5 N4 O21 P2,2H2O'
_chemical_formula_sum            'C32 H30 Cu2 Mo5 N4 O23 P2'
_chemical_formula_weight         1507.34

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           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2
_symmetry_space_group_name_Hall  'F 2 -2d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'

_cell_length_a                   18.8251(9)
_cell_length_b                   42.656(2)
_cell_length_c                   10.6435(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8546.8(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7841
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      28.23

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5854
_exptl_absorpt_coefficient_mu    2.564
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7946
_exptl_absorpt_correction_T_max  0.8697
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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            10597
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3492
_reflns_number_gt                3381
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2005)'
_computing_cell_refinement       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997a)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0256P)²+5.5908P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         3492
_refine_ls_number_parameters     314
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0442
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.0000 0.0000 -0.07129(4) 0.01492(10) Uani 1 2 d S . .
Mo2 Mo 0.116645(17) 0.038701(8) 0.11148(3) 0.01643(8) Uani 1 1 d . . .
Mo3 Mo 0.085760(16) 0.020218(7) 0.41674(3) 0.01459(8) Uani 1 1 d . . .
Cu1 Cu -0.16657(3) 0.006770(11) -0.29705(5) 0.02215(12) Uani 1 1 d . . .
P1 P 0.05688(5) -0.03513(2) 0.20479(9) 0.0144(2) Uani 1 1 d . . .
O1 O 0.15022(14) 0.03155(6) 0.2870(2) 0.0182(6) Uani 1 1 d . . .
O2 O 0.14282(14) 0.00538(6) 0.5309(3) 0.0210(6) Uani 1 1 d . . .
O3 O 0.09854(13) -0.02585(6) 0.3193(2) 0.0185(6) Uani 1 1 d . . .
O4 O 0.04664(14) 0.03730(6) -0.0180(2) 0.0178(6) Uani 1 1 d . . .
O5 O 0.0000 0.0000 0.4634(4) 0.0179(8) Uani 1 2 d S . .
O6 O -0.06289(14) 0.01453(6) -0.1727(3) 0.0220(6) Uani 1 1 d . . .
O7 O 0.07247(13) -0.01328(6) 0.0938(3) 0.0160(6) Uani 1 1 d . . .
O8 O 0.06467(14) 0.05572(6) 0.4755(3) 0.0217(6) Uani 1 1 d . . .
O9 O 0.19186(15) 0.02375(7) 0.0424(3) 0.0270(7) Uani 1 1 d . . .
O10 O -0.02392(13) -0.03510(6) 0.2373(2) 0.0166(6) Uani 1 1 d . . .
O11 O 0.12856(15) 0.07790(7) 0.1055(3) 0.0281(6) Uani 1 1 d . . .
N1 N -0.16559(18) -0.03917(7) -0.2537(3) 0.0228(8) Uani 1 1 d . . .
N2 N -0.09833(17) -0.19771(7) -0.0903(3) 0.0212(7) Uani 1 1 d . . .
C1 C 0.0799(2) -0.07411(9) 0.1588(4) 0.0209(9) Uani 1 1 d . . .
C2 C 0.0634(3) -0.09866(10) 0.2380(5) 0.0464(14) Uani 1 1 d . . .
H2A H 0.0389 -0.0949 0.3124 0.056 Uiso 1 1 calc R . .
C3 C 0.0834(4) -0.12876(12) 0.2066(6) 0.0652(19) Uani 1 1 d . . .
H3A H 0.0730 -0.1452 0.2610 0.078 Uiso 1 1 calc R . .
C4 C 0.1174(4) -0.13463(12) 0.0989(6) 0.0570(17) Uani 1 1 d . . .
H4A H 0.1292 -0.1551 0.0774 0.068 Uiso 1 1 calc R . .
C5 C 0.1346(4) -0.11070(13) 0.0212(6) 0.065(2) Uani 1 1 d . . .
H5A H 0.1597 -0.1147 -0.0524 0.078 Uiso 1 1 calc R . .
C6 C 0.1152(3) -0.08013(12) 0.0508(5) 0.0473(15) Uani 1 1 d . . .
H6A H 0.1263 -0.0638 -0.0038 0.057 Uiso 1 1 calc R . .
C7 C -0.1017(2) -0.05313(9) -0.2605(4) 0.0222(9) Uani 1 1 d . . .
H7A H -0.0636 -0.0415 -0.2907 0.027 Uiso 1 1 calc R . .
C8 C -0.0895(2) -0.08340(10) -0.2257(4) 0.0245(9) Uani 1 1 d . . .
H8A H -0.0438 -0.0916 -0.2301 0.029 Uiso 1 1 calc R . .
C9 C -0.1450(2) -0.10208(9) -0.1838(4) 0.0237(9) Uani 1 1 d . . .
C10 C -0.2120(2) -0.08836(10) -0.1808(4) 0.0305(11) Uani 1 1 d . . .
H10A H -0.2512 -0.1001 -0.1559 0.037 Uiso 1 1 calc R . .
C11 C -0.2203(2) -0.05718(10) -0.2148(4) 0.0289(10) Uani 1 1 d . . .
H11A H -0.2654 -0.0483 -0.2107 0.035 Uiso 1 1 calc R . .
C12 C -0.1590(2) -0.18965(9) -0.1469(4) 0.0237(9) Uani 1 1 d . . .
H12A H -0.1905 -0.2055 -0.1691 0.028 Uiso 1 1 calc R . .
C13 C -0.1773(2) -0.15922(10) -0.1740(4) 0.0252(10) Uani 1 1 d . . .
H13A H -0.2210 -0.1548 -0.2108 0.030 Uiso 1 1 calc R . .
C16 C -0.0532(2) -0.17432(9) -0.0592(4) 0.0267(10) Uani 1 1 d . . .
H16A H -0.0112 -0.1793 -0.0179 0.032 Uiso 1 1 calc R . .
C14 C -0.1306(2) -0.13498(9) -0.1464(4) 0.0222(8) Uani 1 1 d . . .
C15 C -0.0674(2) -0.14336(9) -0.0867(4) 0.0277(10) Uani 1 1 d . . .
H15A H -0.0346 -0.1280 -0.0652 0.033 Uiso 1 1 calc R . .
O1W O -0.21987(15) 0.01794(7) -0.1471(3) 0.0248(6) Uani 1 1 d D . .
H1WA H -0.2630(9) 0.0220(10) -0.162(4) 0.030 Uiso 1 1 d D . .
H1WB H -0.211(2) 0.0029(7) -0.098(3) 0.030 Uiso 1 1 d 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 O6 1.718(3) 2 ?
Mo1 O6 1.718(3) . ?
Mo1 O4 1.903(2) 2 ?
Mo1 O4 1.903(2) . ?
Mo1 O7 2.296(3) . ?
Mo1 O7 2.296(3) 2 ?
Mo1 Mo2 3.3662(4) . ?
Mo1 Mo2 3.3662(4) 2 ?
Mo2 O11 1.688(3) . ?
Mo2 O9 1.718(3) . ?
Mo2 O4 1.908(3) . ?
Mo2 O1 1.996(3) . ?
Mo2 O10 2.206(3) 2 ?
Mo2 O7 2.376(2) . ?
Mo2 Mo3 3.3936(5) . ?
Mo3 O8 1.686(2) . ?
Mo3 O2 1.741(3) . ?
Mo3 O5 1.8964(10) . ?
Mo3 O1 1.900(3) . ?
Mo3 O3 2.235(3) . ?
Mo3 O10 2.325(3) 2 ?
Cu1 O1W 1.944(3) . ?
Cu1 O2 1.955(3) 2_554 ?
Cu1 N1 2.013(3) . ?
Cu1 N2 2.015(3) 11_454 ?
Cu1 O6 2.381(3) . ?
Cu1 H1WB 2.28(4) . ?
P1 O3 1.502(3) . ?
P1 O7 1.533(3) . ?
P1 O10 1.560(3) . ?
P1 C1 1.787(4) . ?
O2 Cu1 1.955(3) 2_556 ?
O5 Mo3 1.8964(10) 2 ?
O10 Mo2 2.206(3) 2 ?
O10 Mo3 2.325(3) 2 ?
N1 C7 1.344(5) . ?
N1 C11 1.350(5) . ?
N2 C12 1.336(5) . ?
N2 C16 1.351(5) . ?
N2 Cu1 2.015(3) 15_445 ?
C1 C6 1.352(6) . ?
C1 C2 1.380(6) . ?
C2 C3 1.379(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.337(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.353(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.390(7) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.363(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.386(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.391(6) . ?
C9 C14 1.484(5) . ?
C10 C11 1.387(6) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 C13 1.374(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.388(6) . ?
C13 H13A 0.9300 . ?
C16 C15 1.379(5) . ?
C16 H16A 0.9300 . ?
C14 C15 1.395(6) . ?
C15 H15A 0.9300 . ?
O1W H1WA 0.845(10) . ?
O1W H1WB 0.842(10) . ?

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 Mo1 O6 102.14(19) 2 . ?
O6 Mo1 O4 101.73(12) 2 2 ?
O6 Mo1 O4 99.84(12) . 2 ?
O6 Mo1 O4 99.84(12) 2 . ?
O6 Mo1 O4 101.73(12) . . ?
O4 Mo1 O4 145.36(16) 2 . ?
O6 Mo1 O7 89.00(11) 2 . ?
O6 Mo1 O7 168.40(12) . . ?
O4 Mo1 O7 80.79(10) 2 . ?
O4 Mo1 O7 72.80(10) . . ?
O6 Mo1 O7 168.40(12) 2 2 ?
O6 Mo1 O7 89.00(11) . 2 ?
O4 Mo1 O7 72.80(10) 2 2 ?
O4 Mo1 O7 80.79(10) . 2 ?
O7 Mo1 O7 80.09(13) . 2 ?
O6 Mo1 Mo2 95.20(9) 2 . ?
O6 Mo1 Mo2 129.47(9) . . ?
O4 Mo1 Mo2 122.60(8) 2 . ?
O4 Mo1 Mo2 28.01(8) . . ?
O7 Mo1 Mo2 44.84(6) . . ?
O7 Mo1 Mo2 79.88(6) 2 . ?
O6 Mo1 Mo2 129.47(9) 2 2 ?
O6 Mo1 Mo2 95.20(9) . 2 ?
O4 Mo1 Mo2 28.01(8) 2 2 ?
O4 Mo1 Mo2 122.60(8) . 2 ?
O7 Mo1 Mo2 79.88(6) . 2 ?
O7 Mo1 Mo2 44.84(6) 2 2 ?
Mo2 Mo1 Mo2 109.394(17) . 2 ?
O11 Mo2 O9 104.01(14) . . ?
O11 Mo2 O4 95.49(13) . . ?
O9 Mo2 O4 104.39(13) . . ?
O11 Mo2 O1 98.31(13) . . ?
O9 Mo2 O1 94.75(13) . . ?
O4 Mo2 O1 152.90(11) . . ?
O11 Mo2 O10 101.36(12) . 2 ?
O9 Mo2 O10 152.39(12) . 2 ?
O4 Mo2 O10 83.68(10) . 2 ?
O1 Mo2 O10 70.82(11) . 2 ?
O11 Mo2 O7 165.46(12) . . ?
O9 Mo2 O7 84.73(11) . . ?
O4 Mo2 O7 70.84(9) . . ?
O1 Mo2 O7 92.42(10) . . ?
O10 Mo2 O7 72.90(9) 2 . ?
O11 Mo2 Mo1 123.41(10) . . ?
O9 Mo2 Mo1 96.22(9) . . ?
O4 Mo2 Mo1 27.94(7) . . ?
O1 Mo2 Mo1 132.27(8) . . ?
O10 Mo2 Mo1 78.49(7) 2 . ?
O7 Mo2 Mo1 42.97(6) . . ?
O11 Mo2 Mo3 106.79(11) . . ?
O9 Mo2 Mo3 117.68(10) . . ?
O4 Mo2 Mo3 124.48(8) . . ?
O1 Mo2 Mo3 28.65(8) . . ?
O10 Mo2 Mo3 42.85(7) 2 . ?
O7 Mo2 Mo3 78.40(7) . . ?
Mo1 Mo2 Mo3 109.123(12) . . ?
O8 Mo3 O2 102.30(13) . . ?
O8 Mo3 O5 96.37(10) . . ?
O2 Mo3 O5 100.22(13) . . ?
O8 Mo3 O1 101.03(12) . . ?
O2 Mo3 O1 101.86(12) . . ?
O5 Mo3 O1 148.13(14) . . ?
O8 Mo3 O3 170.86(12) . . ?
O2 Mo3 O3 86.45(11) . . ?
O5 Mo3 O3 79.24(9) . . ?
O1 Mo3 O3 79.49(11) . . ?
O8 Mo3 O10 86.64(11) . 2 ?
O2 Mo3 O10 168.97(11) . 2 ?
O5 Mo3 O10 85.00(12) . 2 ?
O1 Mo3 O10 69.73(10) . 2 ?
O3 Mo3 O10 84.99(9) . 2 ?
O8 Mo3 Mo2 100.76(9) . . ?
O2 Mo3 Mo2 130.31(9) . . ?
O5 Mo3 Mo2 120.14(11) . . ?
O1 Mo3 Mo2 30.24(8) . . ?
O3 Mo3 Mo2 75.01(7) . . ?
O10 Mo3 Mo2 40.17(6) 2 . ?
O1W Cu1 O2 162.14(12) . 2_554 ?
O1W Cu1 N1 93.16(13) . . ?
O2 Cu1 N1 87.39(13) 2_554 . ?
O1W Cu1 N2 91.32(13) . 11_454 ?
O2 Cu1 N2 90.56(13) 2_554 11_454 ?
N1 Cu1 N2 171.47(14) . 11_454 ?
O1W Cu1 O6 86.15(11) . . ?
O2 Cu1 O6 111.71(11) 2_554 . ?
N1 Cu1 O6 90.03(12) . . ?
N2 Cu1 O6 83.03(12) 11_454 . ?
O1W Cu1 H1WB 21.1(7) . . ?
O2 Cu1 H1WB 158.9(10) 2_554 . ?
N1 Cu1 H1WB 73.8(8) . . ?
N2 Cu1 H1WB 109.4(8) 11_454 . ?
O6 Cu1 H1WB 78.3(11) . . ?
O3 P1 O7 111.38(15) . . ?
O3 P1 O10 109.21(15) . . ?
O7 P1 O10 110.93(14) . . ?
O3 P1 C1 109.90(17) . . ?
O7 P1 C1 107.96(18) . . ?
O10 P1 C1 107.37(16) . . ?
Mo3 O1 Mo2 121.11(14) . . ?
Mo3 O2 Cu1 153.03(17) . 2_556 ?
P1 O3 Mo3 123.50(15) . . ?
Mo1 O4 Mo2 124.05(13) . . ?
Mo3 O5 Mo3 149.7(2) 2 . ?
Mo1 O6 Cu1 149.75(15) . . ?
P1 O7 Mo1 128.75(14) . . ?
P1 O7 Mo2 125.01(15) . . ?
Mo1 O7 Mo2 92.19(9) . . ?
P1 O10 Mo2 129.57(16) . 2 ?
P1 O10 Mo3 132.12(15) . 2 ?
Mo2 O10 Mo3 96.98(10) 2 2 ?
C7 N1 C11 116.6(3) . . ?
C7 N1 Cu1 115.3(3) . . ?
C11 N1 Cu1 128.1(3) . . ?
C12 N2 C16 117.2(3) . . ?
C12 N2 Cu1 118.0(3) . 15_445 ?
C16 N2 Cu1 124.6(3) . 15_445 ?
C6 C1 C2 119.1(4) . . ?
C6 C1 P1 121.9(4) . . ?
C2 C1 P1 119.0(3) . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C4 C3 C2 120.9(6) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C5 119.8(5) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 C6 120.4(5) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C1 C6 C5 120.0(5) . . ?
C1 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
N1 C7 C8 123.8(4) . . ?
N1 C7 H7A 118.1 . . ?
C8 C7 H7A 118.1 . . ?
C7 C8 C9 120.4(4) . . ?
C7 C8 H8A 119.8 . . ?
C9 C8 H8A 119.8 . . ?
C8 C9 C10 116.6(4) . . ?
C8 C9 C14 119.5(4) . . ?
C10 C9 C14 123.9(4) . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
N1 C11 C10 122.6(4) . . ?
N1 C11 H11A 118.7 . . ?
C10 C11 H11A 118.7 . . ?
N2 C12 C13 123.5(4) . . ?
N2 C12 H12A 118.2 . . ?
C13 C12 H12A 118.2 . . ?
C12 C13 C14 120.0(4) . . ?
C12 C13 H13A 120.0 . . ?
C14 C13 H13A 120.0 . . ?
N2 C16 C15 122.3(4) . . ?
N2 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C13 C14 C15 116.4(4) . . ?
C13 C14 C9 122.1(4) . . ?
C15 C14 C9 121.3(4) . . ?
C16 C15 C14 120.4(4) . . ?
C16 C15 H15A 119.8 . . ?
C14 C15 H15A 119.8 . . ?
Cu1 O1W H1WA 113(3) . . ?
Cu1 O1W H1WB 103(3) . . ?
H1WA O1W H1WB 117(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Mo1 Mo2 O11 103.38(16) 2 . . . ?
O6 Mo1 Mo2 O11 -7.01(17) . . . . ?
O4 Mo1 Mo2 O11 -149.13(15) 2 . . . ?
O4 Mo1 Mo2 O11 2.2(2) . . . . ?
O7 Mo1 Mo2 O11 -173.30(15) . . . . ?
O7 Mo1 Mo2 O11 -87.22(14) 2 . . . ?
Mo2 Mo1 Mo2 O11 -121.49(12) 2 . . . ?
O6 Mo1 Mo2 O9 -7.95(14) 2 . . . ?
O6 Mo1 Mo2 O9 -118.34(16) . . . . ?
O4 Mo1 Mo2 O9 99.54(14) 2 . . . ?
O4 Mo1 Mo2 O9 -109.2(2) . . . . ?
O7 Mo1 Mo2 O9 75.37(14) . . . . ?
O7 Mo1 Mo2 O9 161.45(12) 2 . . . ?
Mo2 Mo1 Mo2 O9 127.18(10) 2 . . . ?
O6 Mo1 Mo2 O4 101.21(19) 2 . . . ?
O6 Mo1 Mo2 O4 -9.2(2) . . . . ?
O4 Mo1 Mo2 O4 -151.31(16) 2 . . . ?
O7 Mo1 Mo2 O4 -175.48(19) . . . . ?
O7 Mo1 Mo2 O4 -89.39(18) 2 . . . ?
Mo2 Mo1 Mo2 O4 -123.66(17) 2 . . . ?
O6 Mo1 Mo2 O1 -110.16(14) 2 . . . ?
O6 Mo1 Mo2 O1 139.45(16) . . . . ?
O4 Mo1 Mo2 O1 -2.67(14) 2 . . . ?
O4 Mo1 Mo2 O1 148.6(2) . . . . ?
O7 Mo1 Mo2 O1 -26.84(14) . . . . ?
O7 Mo1 Mo2 O1 59.24(12) 2 . . . ?
Mo2 Mo1 Mo2 O1 24.97(11) 2 . . . ?
O6 Mo1 Mo2 O10 -160.51(12) 2 . . 2 ?
O6 Mo1 Mo2 O10 89.10(14) . . . 2 ?
O4 Mo1 Mo2 O10 -53.02(11) 2 . . 2 ?
O4 Mo1 Mo2 O10 98.29(18) . . . 2 ?
O7 Mo1 Mo2 O10 -77.19(11) . . . 2 ?
O7 Mo1 Mo2 O10 8.89(10) 2 . . 2 ?
Mo2 Mo1 Mo2 O10 -25.38(7) 2 . . 2 ?
O6 Mo1 Mo2 O7 -83.32(13) 2 . . . ?
O6 Mo1 Mo2 O7 166.29(16) . . . . ?
O4 Mo1 Mo2 O7 24.17(13) 2 . . . ?
O4 Mo1 Mo2 O7 175.48(19) . . . . ?
O7 Mo1 Mo2 O7 86.08(14) 2 . . . ?
Mo2 Mo1 Mo2 O7 51.82(9) 2 . . . ?
O6 Mo1 Mo2 Mo3 -130.11(10) 2 . . . ?
O6 Mo1 Mo2 Mo3 119.50(12) . . . . ?
O4 Mo1 Mo2 Mo3 -22.62(9) 2 . . . ?
O4 Mo1 Mo2 Mo3 128.69(17) . . . . ?
O7 Mo1 Mo2 Mo3 -46.79(9) . . . . ?
O7 Mo1 Mo2 Mo3 39.29(7) 2 . . . ?
Mo2 Mo1 Mo2 Mo3 5.025(7) 2 . . . ?
O11 Mo2 Mo3 O8 17.21(14) . . . . ?
O9 Mo2 Mo3 O8 133.56(14) . . . . ?
O4 Mo2 Mo3 O8 -91.97(13) . . . . ?
O1 Mo2 Mo3 O8 93.47(19) . . . . ?
O10 Mo2 Mo3 O8 -71.49(13) 2 . . . ?
O7 Mo2 Mo3 O8 -148.78(11) . . . . ?
Mo1 Mo2 Mo3 O8 -118.30(9) . . . . ?
O11 Mo2 Mo3 O2 -99.25(16) . . . . ?
O9 Mo2 Mo3 O2 17.10(16) . . . . ?
O4 Mo2 Mo3 O2 151.57(15) . . . . ?
O1 Mo2 Mo3 O2 -22.99(19) . . . . ?
O10 Mo2 Mo3 O2 172.05(16) 2 . . . ?
O7 Mo2 Mo3 O2 94.76(14) . . . . ?
Mo1 Mo2 Mo3 O2 125.24(12) . . . . ?
O11 Mo2 Mo3 O5 121.15(10) . . . . ?
O9 Mo2 Mo3 O5 -122.50(11) . . . . ?
O4 Mo2 Mo3 O5 11.98(10) . . . . ?
O1 Mo2 Mo3 O5 -162.59(16) . . . . ?
O10 Mo2 Mo3 O5 32.46(10) 2 . . . ?
O7 Mo2 Mo3 O5 -44.83(7) . . . . ?
Mo1 Mo2 Mo3 O5 -14.36(3) . . . . ?
O11 Mo2 Mo3 O1 -76.26(19) . . . . ?
O9 Mo2 Mo3 O1 40.1(2) . . . . ?
O4 Mo2 Mo3 O1 174.56(19) . . . . ?
O10 Mo2 Mo3 O1 -165.0(2) 2 . . . ?
O7 Mo2 Mo3 O1 117.75(17) . . . . ?
Mo1 Mo2 Mo3 O1 148.23(16) . . . . ?
O11 Mo2 Mo3 O3 -171.11(12) . . . . ?
O9 Mo2 Mo3 O3 -54.76(12) . . . . ?
O4 Mo2 Mo3 O3 79.71(11) . . . . ?
O1 Mo2 Mo3 O3 -94.85(18) . . . . ?
O10 Mo2 Mo3 O3 100.19(12) 2 . . . ?
O7 Mo2 Mo3 O3 22.90(9) . . . . ?
Mo1 Mo2 Mo3 O3 53.38(7) . . . . ?
O11 Mo2 Mo3 O10 88.69(14) . . . 2 ?
O9 Mo2 Mo3 O10 -154.96(15) . . . 2 ?
O4 Mo2 Mo3 O10 -20.48(14) . . . 2 ?
O1 Mo2 Mo3 O10 165.0(2) . . . 2 ?
O7 Mo2 Mo3 O10 -77.29(11) . . . 2 ?
Mo1 Mo2 Mo3 O10 -46.82(10) . . . 2 ?
O8 Mo3 O1 Mo2 -92.49(17) . . . . ?
O2 Mo3 O1 Mo2 162.28(15) . . . . ?
O5 Mo3 O1 Mo2 29.4(3) . . . . ?
O3 Mo3 O1 Mo2 78.21(15) . . . . ?
O10 Mo3 O1 Mo2 -10.28(13) 2 . . . ?
O11 Mo2 O1 Mo3 109.97(17) . . . . ?
O9 Mo2 O1 Mo3 -145.09(17) . . . . ?
O4 Mo2 O1 Mo3 -9.9(3) . . . . ?
O10 Mo2 O1 Mo3 10.77(14) 2 . . . ?
O7 Mo2 O1 Mo3 -60.19(16) . . . . ?
Mo1 Mo2 O1 Mo3 -42.2(2) . . . . ?
O8 Mo3 O2 Cu1 56.4(4) . . . 2_556 ?
O5 Mo3 O2 Cu1 -42.5(4) . . . 2_556 ?
O1 Mo3 O2 Cu1 160.6(3) . . . 2_556 ?
O3 Mo3 O2 Cu1 -120.9(4) . . . 2_556 ?
O10 Mo3 O2 Cu1 -160.0(4) 2 . . 2_556 ?
Mo2 Mo3 O2 Cu1 172.2(3) . . . 2_556 ?
O7 P1 O3 Mo3 62.6(2) . . . . ?
O10 P1 O3 Mo3 -60.3(2) . . . . ?
C1 P1 O3 Mo3 -177.82(18) . . . . ?
O8 Mo3 O3 P1 10.3(8) . . . . ?
O2 Mo3 O3 P1 173.4(2) . . . . ?
O5 Mo3 O3 P1 72.30(19) . . . . ?
O1 Mo3 O3 P1 -83.83(19) . . . . ?
O10 Mo3 O3 P1 -13.55(18) 2 . . . ?
Mo2 Mo3 O3 P1 -53.15(16) . . . . ?
O6 Mo1 O4 Mo2 -82.52(18) 2 . . . ?
O6 Mo1 O4 Mo2 172.77(16) . . . . ?
O4 Mo1 O4 Mo2 45.36(13) 2 . . . ?
O7 Mo1 O4 Mo2 3.34(14) . . . . ?
O7 Mo1 O4 Mo2 85.74(16) 2 . . . ?
Mo2 Mo1 O4 Mo2 68.73(17) 2 . . . ?
O11 Mo2 O4 Mo1 -178.18(17) . . . . ?
O9 Mo2 O4 Mo1 75.81(18) . . . . ?
O1 Mo2 O4 Mo1 -57.7(3) . . . . ?
O10 Mo2 O4 Mo1 -77.32(16) 2 . . . ?
O7 Mo2 O4 Mo1 -3.26(14) . . . . ?
Mo3 Mo2 O4 Mo1 -63.46(18) . . . . ?
O8 Mo3 O5 Mo3 114.64(10) . . . 2 ?
O2 Mo3 O5 Mo3 -141.60(9) . . . 2 ?
O1 Mo3 O5 Mo3 -8.33(16) . . . 2 ?
O3 Mo3 O5 Mo3 -57.24(7) . . . 2 ?
O10 Mo3 O5 Mo3 28.59(6) 2 . . 2 ?
Mo2 Mo3 O5 Mo3 8.257(15) . . . 2 ?
O6 Mo1 O6 Cu1 88.1(3) 2 . . . ?
O4 Mo1 O6 Cu1 -16.3(3) 2 . . . ?
O4 Mo1 O6 Cu1 -169.0(3) . . . . ?
O7 Mo1 O6 Cu1 -108.4(6) . . . . ?
O7 Mo1 O6 Cu1 -88.6(3) 2 . . . ?
Mo2 Mo1 O6 Cu1 -164.6(2) . . . . ?
Mo2 Mo1 O6 Cu1 -44.1(3) 2 . . . ?
O1W Cu1 O6 Mo1 88.4(3) . . . . ?
O2 Cu1 O6 Mo1 -91.9(3) 2_554 . . . ?
N1 Cu1 O6 Mo1 -4.7(3) . . . . ?
N2 Cu1 O6 Mo1 -179.7(3) 11_454 . . . ?
O3 P1 O7 Mo1 -151.47(17) . . . . ?
O10 P1 O7 Mo1 -29.6(2) . . . . ?
C1 P1 O7 Mo1 87.8(2) . . . . ?
O3 P1 O7 Mo2 -23.0(2) . . . . ?
O10 P1 O7 Mo2 98.88(18) . . . . ?
C1 P1 O7 Mo2 -143.74(18) . . . . ?
O6 Mo1 O7 P1 -121.5(2) 2 . . . ?
O6 Mo1 O7 P1 74.6(6) . . . . ?
O4 Mo1 O7 P1 -19.47(19) 2 . . . ?
O4 Mo1 O7 P1 137.9(2) . . . . ?
O7 Mo1 O7 P1 54.52(15) 2 . . . ?
Mo2 Mo1 O7 P1 140.1(2) . . . . ?
Mo2 Mo1 O7 P1 8.94(17) 2 . . . ?
O6 Mo1 O7 Mo2 98.40(11) 2 . . . ?
O6 Mo1 O7 Mo2 -65.5(6) . . . . ?
O4 Mo1 O7 Mo2 -159.55(11) 2 . . . ?
O4 Mo1 O7 Mo2 -2.22(9) . . . . ?
O7 Mo1 O7 Mo2 -85.56(9) 2 . . . ?
Mo2 Mo1 O7 Mo2 -131.14(7) 2 . . . ?
O11 Mo2 O7 P1 -119.5(5) . . . . ?
O9 Mo2 O7 P1 112.67(19) . . . . ?
O4 Mo2 O7 P1 -140.09(19) . . . . ?
O1 Mo2 O7 P1 18.13(18) . . . . ?
O10 Mo2 O7 P1 -50.96(17) 2 . . . ?
Mo1 Mo2 O7 P1 -142.3(2) . . . . ?
Mo3 Mo2 O7 P1 -7.00(15) . . . . ?
O11 Mo2 O7 Mo1 22.8(5) . . . . ?
O9 Mo2 O7 Mo1 -104.99(12) . . . . ?
O4 Mo2 O7 Mo1 2.24(10) . . . . ?
O1 Mo2 O7 Mo1 160.46(10) . . . . ?
O10 Mo2 O7 Mo1 91.38(10) 2 . . . ?
Mo3 Mo2 O7 Mo1 135.33(8) . . . . ?
O3 P1 O10 Mo2 169.00(17) . . . 2 ?
O7 P1 O10 Mo2 45.9(2) . . . 2 ?
C1 P1 O10 Mo2 -71.9(2) . . . 2 ?
O3 P1 O10 Mo3 5.3(2) . . . 2 ?
O7 P1 O10 Mo3 -117.8(2) . . . 2 ?
C1 P1 O10 Mo3 124.5(2) . . . 2 ?
O1W Cu1 N1 C7 -130.9(3) . . . . ?
O2 Cu1 N1 C7 67.0(3) 2_554 . . . ?
N2 Cu1 N1 C7 -9.2(12) 11_454 . . . ?
O6 Cu1 N1 C7 -44.8(3) . . . . ?
O1W Cu1 N1 C11 46.6(4) . . . . ?
O2 Cu1 N1 C11 -115.5(4) 2_554 . . . ?
N2 Cu1 N1 C11 168.2(9) 11_454 . . . ?
O6 Cu1 N1 C11 132.7(4) . . . . ?
O3 P1 C1 C6 -112.4(4) . . . . ?
O7 P1 C1 C6 9.3(4) . . . . ?
O10 P1 C1 C6 128.9(4) . . . . ?
O3 P1 C1 C2 65.4(4) . . . . ?
O7 P1 C1 C2 -172.9(4) . . . . ?
O10 P1 C1 C2 -53.3(4) . . . . ?
C6 C1 C2 C3 0.5(8) . . . . ?
P1 C1 C2 C3 -177.4(5) . . . . ?
C1 C2 C3 C4 -1.3(10) . . . . ?
C2 C3 C4 C5 2.1(11) . . . . ?
C3 C4 C5 C6 -2.1(11) . . . . ?
C2 C1 C6 C5 -0.5(8) . . . . ?
P1 C1 C6 C5 177.3(5) . . . . ?
C4 C5 C6 C1 1.3(10) . . . . ?
C11 N1 C7 C8 -2.9(6) . . . . ?
Cu1 N1 C7 C8 174.9(3) . . . . ?
N1 C7 C8 C9 2.0(7) . . . . ?
C7 C8 C9 C10 0.5(6) . . . . ?
C7 C8 C9 C14 180.0(4) . . . . ?
C8 C9 C10 C11 -2.0(6) . . . . ?
C14 C9 C10 C11 178.6(4) . . . . ?
C7 N1 C11 C10 1.3(6) . . . . ?
Cu1 N1 C11 C10 -176.2(3) . . . . ?
C9 C10 C11 N1 1.1(7) . . . . ?
C16 N2 C12 C13 -0.2(6) . . . . ?
Cu1 N2 C12 C13 175.8(3) 15_445 . . . ?
N2 C12 C13 C14 2.3(7) . . . . ?
C12 N2 C16 C15 -1.6(7) . . . . ?
Cu1 N2 C16 C15 -177.3(3) 15_445 . . . ?
C12 C13 C14 C15 -2.5(6) . . . . ?
C12 C13 C14 C9 174.5(4) . . . . ?
C8 C9 C14 C13 -141.2(4) . . . . ?
C10 C9 C14 C13 38.2(7) . . . . ?
C8 C9 C14 C15 35.7(7) . . . . ?
C10 C9 C14 C15 -144.9(5) . . . . ?
N2 C16 C15 C14 1.2(7) . . . . ?
C13 C14 C15 C16 0.9(7) . . . . ?
C9 C14 C15 C16 -176.2(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O1 0.845(10) 1.769(13) 2.609(4) 173(5) 9_454
O1W H1WB O9 0.842(10) 1.916(16) 2.741(4) 166(5) 2

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 1012272'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Cu2 Mo5 N2 O21 P2,4H2O'
_chemical_formula_sum            'C22 H26 Cu2 Mo5 N2 O25 P2'
_chemical_formula_weight         1387.17

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
_symmetry_space_group_name_Hall  '-C 2yc'

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                   17.3158(12)
_cell_length_b                   9.8869(7)
_cell_length_c                   21.7619(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.9070(10)
_cell_angle_gamma                90.00
_cell_volume                     3631.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6642
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.12

_exptl_crystal_description       block
_exptl_crystal_colour            light-blue
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2680
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7757
_exptl_absorpt_correction_T_max  0.8473
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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            8868
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3198
_reflns_number_gt                2636
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2005)'
_computing_cell_refinement       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997a)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0298P)²+2.4800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3198
_refine_ls_number_parameters     269
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0614
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.059
_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 0.0000 0.32527(5) 0.2500 0.01729(13) Uani 1 2 d S . .
Mo2 Mo 0.13230(2) 0.13301(4) 0.347764(17) 0.01586(10) Uani 1 1 d . . .
Mo3 Mo 0.10212(2) -0.19770(4) 0.300798(18) 0.02082(11) Uani 1 1 d D . .
Cu1 Cu 0.19716(3) -0.17252(5) 0.17353(3) 0.02179(14) Uani 1 1 d . . .
P1 P 0.05959(6) 0.04583(11) 0.18123(5) 0.0153(2) Uani 1 1 d . . .
O1 O 0.07528(16) 0.1426(3) 0.23774(13) 0.0170(6) Uani 1 1 d . . .
O2 O 0.05551(17) 0.2724(3) 0.33405(13) 0.0196(7) Uani 1 1 d . . .
O3 O 0.06957(18) 0.4305(3) 0.23208(16) 0.0310(8) Uani 1 1 d . . .
O4 O 0.16641(16) -0.0448(3) 0.32611(13) 0.0199(7) Uani 1 1 d . . .
O5 O 0.21222(17) 0.2165(3) 0.32926(15) 0.0264(7) Uani 1 1 d . . .
O6 O 0.15507(18) 0.1266(3) 0.42677(14) 0.0287(8) Uani 1 1 d . . .
O7 O 0.02794(16) 0.0040(3) 0.33803(13) 0.0187(7) Uani 1 1 d . . .
O8 O 0.10795(16) -0.0835(3) 0.19837(13) 0.0197(7) Uani 1 1 d D . .
O9 O 0.0000 -0.2251(4) 0.2500 0.0206(9) Uani 1 2 d S . .
O10 O 0.16384(18) -0.2992(3) 0.27006(16) 0.0321(8) Uani 1 1 d . . .
O11 O 0.0987(2) -0.2748(3) 0.36923(15) 0.0374(9) Uani 1 1 d . . .
N1 N 0.1274(2) -0.2877(4) 0.10903(17) 0.0226(9) Uani 1 1 d . . .
C1 C 0.0911(2) 0.1295(4) 0.11862(19) 0.0190(9) Uani 1 1 d . . .
C2 C 0.1481(3) 0.2294(5) 0.1313(2) 0.0342(12) Uani 1 1 d . . .
H2A H 0.1676 0.2568 0.1728 0.041 Uiso 1 1 calc R . .
C3 C 0.1768(3) 0.2898(5) 0.0833(2) 0.0382(13) Uani 1 1 d . . .
H3A H 0.2153 0.3569 0.0926 0.046 Uiso 1 1 calc R . .
C4 C 0.1485(3) 0.2506(5) 0.0228(2) 0.0377(13) Uani 1 1 d . . .
H4A H 0.1676 0.2913 -0.0094 0.045 Uiso 1 1 calc R . .
C5 C 0.0924(4) 0.1521(7) 0.0088(3) 0.065(2) Uani 1 1 d . . .
H5A H 0.0731 0.1251 -0.0328 0.078 Uiso 1 1 calc R . .
C6 C 0.0644(3) 0.0926(6) 0.0573(2) 0.0521(17) Uani 1 1 d . . .
H6A H 0.0261 0.0252 0.0476 0.063 Uiso 1 1 calc R . .
C7 C 0.1331(3) -0.2944(6) 0.0494(2) 0.0503(17) Uani 1 1 d . . .
H7A H 0.1717 -0.2430 0.0366 0.060 Uiso 1 1 calc R . .
C8 C 0.0839(4) -0.3748(6) 0.0057(3) 0.0564(18) Uani 1 1 d . . .
H8A H 0.0891 -0.3748 -0.0359 0.068 Uiso 1 1 calc R . .
C9 C 0.0272(3) -0.4551(4) 0.0227(2) 0.0244(11) Uani 1 1 d . . .
C10 C 0.0244(3) -0.4507(5) 0.0849(2) 0.0300(12) Uani 1 1 d . . .
H10A H -0.0110 -0.5063 0.0995 0.036 Uiso 1 1 calc R . .
C11 C 0.0730(3) -0.3654(5) 0.1264(2) 0.0301(11) Uani 1 1 d . . .
H11A H 0.0676 -0.3617 0.1680 0.036 Uiso 1 1 calc R . .
O1W O 0.26461(19) -0.0599(4) 0.23820(18) 0.0368(9) Uani 1 1 d D . .
H1WA H 0.3144(7) -0.053(5) 0.244(3) 0.044 Uiso 1 1 d D . .
H1WB H 0.245(3) -0.035(5) 0.2684(17) 0.044 Uiso 1 1 d D . .
O2W O 0.2562(3) -0.0313(4) 0.0998(3) 0.0848(16) 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 O3 1.702(3) . ?
Mo1 O3 1.702(3) 2 ?
Mo1 O2 1.938(3) 2 ?
Mo1 O2 1.938(3) . ?
Mo1 O1 2.278(3) 2 ?
Mo1 O1 2.278(3) . ?
Mo2 O6 1.677(3) . ?
Mo2 O5 1.735(3) . ?
Mo2 O2 1.892(3) . ?
Mo2 O4 1.946(3) . ?
Mo2 O7 2.183(3) . ?
Mo2 O1 2.379(3) . ?
Mo3 O11 1.685(3) . ?
Mo3 O10 1.708(3) . ?
Mo3 O9 1.8839(7) . ?
Mo3 O4 1.885(3) . ?
Cu1 O5 1.927(3) 4_545 ?
Cu1 O8 1.956(3) . ?
Cu1 O1W 1.962(3) . ?
Cu1 N1 1.992(4) . ?
P1 O8 1.528(3) . ?
P1 O1 1.534(3) . ?
P1 O7 1.536(3) 2 ?
P1 C1 1.781(4) . ?
O5 Cu1 1.927(3) 4 ?
O7 P1 1.536(3) 2 ?
O9 Mo3 1.8839(7) 2 ?
N1 C7 1.324(6) . ?
N1 C11 1.335(6) . ?
C1 C6 1.361(6) . ?
C1 C2 1.380(6) . ?
C2 C3 1.389(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.353(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.362(7) . ?
C4 H4A 0.9300 . ?
C5 C6 1.388(7) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.379(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.376(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.366(6) . ?
C9 C9 1.496(8) 5_545 ?
C10 C11 1.377(6) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
O1W H1WA 0.845(10) . ?
O1W H1WB 0.843(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
O3 Mo1 O3 104.6(2) . 2 ?
O3 Mo1 O2 100.13(14) . 2 ?
O3 Mo1 O2 98.86(14) 2 2 ?
O3 Mo1 O2 98.86(14) . . ?
O3 Mo1 O2 100.13(14) 2 . ?
O2 Mo1 O2 148.70(16) 2 . ?
O3 Mo1 O1 164.72(13) . 2 ?
O3 Mo1 O1 90.30(13) 2 2 ?
O2 Mo1 O1 73.77(11) 2 2 ?
O2 Mo1 O1 81.47(11) . 2 ?
O3 Mo1 O1 90.30(13) . . ?
O3 Mo1 O1 164.72(13) 2 . ?
O2 Mo1 O1 81.47(11) 2 . ?
O2 Mo1 O1 73.77(11) . . ?
O1 Mo1 O1 75.07(14) 2 . ?
O6 Mo2 O5 103.82(15) . . ?
O6 Mo2 O2 100.68(14) . . ?
O5 Mo2 O2 100.70(13) . . ?
O6 Mo2 O4 101.51(14) . . ?
O5 Mo2 O4 94.18(13) . . ?
O2 Mo2 O4 149.39(12) . . ?
O6 Mo2 O7 94.44(13) . . ?
O5 Mo2 O7 160.34(13) . . ?
O2 Mo2 O7 82.69(11) . . ?
O4 Mo2 O7 74.82(11) . . ?
O6 Mo2 O1 169.39(13) . . ?
O5 Mo2 O1 85.45(12) . . ?
O2 Mo2 O1 72.14(11) . . ?
O4 Mo2 O1 82.67(10) . . ?
O7 Mo2 O1 77.12(10) . . ?
O11 Mo3 O10 103.22(17) . . ?
O11 Mo3 O9 103.89(13) . . ?
O10 Mo3 O9 105.85(13) . . ?
O11 Mo3 O4 103.84(14) . . ?
O10 Mo3 O4 101.85(14) . . ?
O9 Mo3 O4 134.62(14) . . ?
O5 Cu1 O8 164.57(13) 4_545 . ?
O5 Cu1 O1W 89.26(13) 4_545 . ?
O8 Cu1 O1W 85.79(13) . . ?
O5 Cu1 N1 91.28(14) 4_545 . ?
O8 Cu1 N1 93.44(14) . . ?
O1W Cu1 N1 178.92(16) . . ?
O8 P1 O1 109.68(16) . . ?
O8 P1 O7 107.15(16) . 2 ?
O1 P1 O7 111.96(16) . 2 ?
O8 P1 C1 109.32(18) . . ?
O1 P1 C1 107.10(18) . . ?
O7 P1 C1 111.62(18) 2 . ?
P1 O1 Mo1 125.80(15) . . ?
P1 O1 Mo2 137.87(16) . . ?
Mo1 O1 Mo2 91.91(10) . . ?
Mo2 O2 Mo1 121.89(15) . . ?
Mo3 O4 Mo2 127.15(15) . . ?
Mo2 O5 Cu1 167.5(2) . 4 ?
P1 O7 Mo2 127.89(16) 2 . ?
P1 O8 Cu1 137.09(18) . . ?
Mo3 O9 Mo3 163.5(2) 2 . ?
C7 N1 C11 117.5(4) . . ?
C7 N1 Cu1 123.5(3) . . ?
C11 N1 Cu1 119.0(3) . . ?
C6 C1 C2 117.3(4) . . ?
C6 C1 P1 122.0(4) . . ?
C2 C1 P1 120.5(3) . . ?
C1 C2 C3 121.2(4) . . ?
C1 C2 H2A 119.4 . . ?
C3 C2 H2A 119.4 . . ?
C4 C3 C2 119.7(5) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
C1 C6 C5 122.2(5) . . ?
C1 C6 H6A 118.9 . . ?
C5 C6 H6A 118.9 . . ?
N1 C7 C8 122.3(5) . . ?
N1 C7 H7A 118.9 . . ?
C8 C7 H7A 118.9 . . ?
C9 C8 C7 121.1(5) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C10 C9 C8 115.7(4) . . ?
C10 C9 C9 121.2(5) . 5_545 ?
C8 C9 C9 123.1(6) . 5_545 ?
C9 C10 C11 121.2(5) . . ?
C9 C10 H10A 119.4 . . ?
C11 C10 H10A 119.4 . . ?
N1 C11 C10 122.2(5) . . ?
N1 C11 H11A 118.9 . . ?
C10 C11 H11A 118.9 . . ?
Cu1 O1W H1WA 126(4) . . ?
Cu1 O1W H1WB 116(4) . . ?
H1WA O1W H1WB 116(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 P1 O1 Mo1 -164.13(17) . . . . ?
O7 P1 O1 Mo1 -45.3(2) 2 . . . ?
C1 P1 O1 Mo1 77.3(2) . . . . ?
O8 P1 O1 Mo2 -15.0(3) . . . . ?
O7 P1 O1 Mo2 103.9(2) 2 . . . ?
C1 P1 O1 Mo2 -133.5(2) . . . . ?
O3 Mo1 O1 P1 -104.4(2) . . . . ?
O3 Mo1 O1 P1 88.2(5) 2 . . . ?
O2 Mo1 O1 P1 -4.2(2) 2 . . . ?
O2 Mo1 O1 P1 156.4(2) . . . . ?
O1 Mo1 O1 P1 71.13(18) 2 . . . ?
O3 Mo1 O1 Mo2 95.68(13) . . . . ?
O3 Mo1 O1 Mo2 -71.7(5) 2 . . . ?
O2 Mo1 O1 Mo2 -164.12(12) 2 . . . ?
O2 Mo1 O1 Mo2 -3.46(10) . . . . ?
O1 Mo1 O1 Mo2 -88.75(11) 2 . . . ?
O6 Mo2 O1 P1 -103.4(7) . . . . ?
O5 Mo2 O1 P1 105.4(3) . . . . ?
O2 Mo2 O1 P1 -151.8(3) . . . . ?
O4 Mo2 O1 P1 10.6(2) . . . . ?
O7 Mo2 O1 P1 -65.5(2) . . . . ?
O6 Mo2 O1 Mo1 52.0(7) . . . . ?
O5 Mo2 O1 Mo1 -99.20(12) . . . . ?
O2 Mo2 O1 Mo1 3.58(10) . . . . ?
O4 Mo2 O1 Mo1 165.98(12) . . . . ?
O7 Mo2 O1 Mo1 89.95(11) . . . . ?
O6 Mo2 O2 Mo1 -176.89(17) . . . . ?
O5 Mo2 O2 Mo1 76.67(19) . . . . ?
O4 Mo2 O2 Mo1 -41.0(3) . . . . ?
O7 Mo2 O2 Mo1 -83.72(17) . . . . ?
O1 Mo2 O2 Mo1 -4.96(14) . . . . ?
O3 Mo1 O2 Mo2 -82.58(19) . . . . ?
O3 Mo1 O2 Mo2 170.74(17) 2 . . . ?
O2 Mo1 O2 Mo2 44.22(14) 2 . . . ?
O1 Mo1 O2 Mo2 81.97(17) 2 . . . ?
O1 Mo1 O2 Mo2 5.13(15) . . . . ?
O11 Mo3 O4 Mo2 -88.4(2) . . . . ?
O10 Mo3 O4 Mo2 164.65(19) . . . . ?
O9 Mo3 O4 Mo2 37.8(3) . . . . ?
O6 Mo2 O4 Mo3 100.1(2) . . . . ?
O5 Mo2 O4 Mo3 -154.9(2) . . . . ?
O2 Mo2 O4 Mo3 -35.6(4) . . . . ?
O7 Mo2 O4 Mo3 8.58(17) . . . . ?
O1 Mo2 O4 Mo3 -70.00(18) . . . . ?
O6 Mo2 O5 Cu1 -28.1(9) . . . 4 ?
O2 Mo2 O5 Cu1 75.9(8) . . . 4 ?
O4 Mo2 O5 Cu1 -131.0(8) . . . 4 ?
O7 Mo2 O5 Cu1 174.2(6) . . . 4 ?
O1 Mo2 O5 Cu1 146.7(8) . . . 4 ?
O6 Mo2 O7 P1 107.3(2) . . . 2 ?
O5 Mo2 O7 P1 -94.3(4) . . . 2 ?
O2 Mo2 O7 P1 7.1(2) . . . 2 ?
O4 Mo2 O7 P1 -152.0(2) . . . 2 ?
O1 Mo2 O7 P1 -66.2(2) . . . 2 ?
O1 P1 O8 Cu1 -112.6(3) . . . . ?
O7 P1 O8 Cu1 125.7(2) 2 . . . ?
C1 P1 O8 Cu1 4.6(3) . . . . ?
O5 Cu1 O8 P1 158.3(4) 4_545 . . . ?
O1W Cu1 O8 P1 86.6(3) . . . . ?
N1 Cu1 O8 P1 -94.2(3) . . . . ?
O11 Mo3 O9 Mo3 120.44(13) . . . 2 ?
O10 Mo3 O9 Mo3 -131.20(12) . . . 2 ?
O4 Mo3 O9 Mo3 -5.74(13) . . . 2 ?
O5 Cu1 N1 C7 -68.1(4) 4_545 . . . ?
O8 Cu1 N1 C7 126.6(4) . . . . ?
O1W Cu1 N1 C7 172(8) . . . . ?
O5 Cu1 N1 C11 110.2(4) 4_545 . . . ?
O8 Cu1 N1 C11 -55.1(3) . . . . ?
O1W Cu1 N1 C11 -10(8) . . . . ?
O8 P1 C1 C6 81.9(5) . . . . ?
O1 P1 C1 C6 -159.4(4) . . . . ?
O7 P1 C1 C6 -36.5(5) 2 . . . ?
O8 P1 C1 C2 -93.8(4) . . . . ?
O1 P1 C1 C2 25.0(4) . . . . ?
O7 P1 C1 C2 147.8(4) 2 . . . ?
C6 C1 C2 C3 0.1(8) . . . . ?
P1 C1 C2 C3 176.0(4) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
C2 C3 C4 C5 -0.3(9) . . . . ?
C3 C4 C5 C6 0.2(10) . . . . ?
C2 C1 C6 C5 -0.3(9) . . . . ?
P1 C1 C6 C5 -176.0(5) . . . . ?
C4 C5 C6 C1 0.1(11) . . . . ?
C11 N1 C7 C8 1.8(9) . . . . ?
Cu1 N1 C7 C8 -179.8(5) . . . . ?
N1 C7 C8 C9 -1.6(10) . . . . ?
C7 C8 C9 C10 -1.0(9) . . . . ?
C7 C8 C9 C9 -179.5(6) . . . 5_545 ?
C8 C9 C10 C11 3.2(7) . . . . ?
C9 C9 C10 C11 -178.2(5) 5_545 . . . ?
C7 N1 C11 C10 0.5(7) . . . . ?
Cu1 N1 C11 C10 -177.9(4) . . . . ?
C9 C10 C11 N1 -3.1(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O3 0.845(10) 1.967(15) 2.800(4) 168(5) 4_545
O1W H1WB O4 0.843(11) 2.05(2) 2.833(5) 155(5) .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.105
_database_code_depnum_ccdc_archive 'CCDC 1012273'
