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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_1
_database_code_depnum_ccdc_archive 'CCDC 1056231'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT342_shelx_1             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0469 Ang

RESPONSE: The quality of this crystal was poor.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H36 Cu N10 O44 Si W12'
_chemical_formula_weight         3562.54

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.098(2)
_cell_length_b                   12.728(3)
_cell_length_c                   13.176(3)
_cell_angle_alpha                110.47(3)
_cell_angle_beta                 97.61(3)
_cell_angle_gamma                111.72(3)
_cell_volume                     1544.8(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5721
_cell_measurement_theta_min      3.4220
_cell_measurement_theta_max      28.8590

_exptl_crystal_description       block
_exptl_crystal_colour            dark_green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.829
_exptl_crystal_F_000             1581
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    22.702
_shelx_estimated_absorpt_T_min   0.064
_shelx_estimated_absorpt_T_max   0.189
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.049
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;  
R(int) was 0.0382 before and 0.0319 after correction. The Ratio of minimum to 
maximum transmission is 0.28.
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9737
_diffrn_reflns_number            12854
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.073
_diffrn_reflns_theta_max         29.049
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7017
_reflns_number_gt                6022
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0083P)²+139.3043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7017
_refine_ls_number_parameters     472
_refine_ls_number_restraints     420
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1468
_refine_ls_wR_factor_gt          0.1401
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.046
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.25654(9) 0.90758(10) 0.44721(8) 0.0414(2) Uani 1 1 d . . . . .
W2 W -0.04573(10) 0.69870(8) 0.46547(8) 0.0441(3) Uani 1 1 d . . . . .
W3 W 0.30057(8) 1.20759(8) 0.47915(7) 0.03089(19) Uani 1 1 d . . . . .
W4 W -0.05058(10) 0.77163(9) 0.23143(7) 0.0409(2) Uani 1 1 d . . . . .
W5 W 0.00895(9) 0.92893(8) 0.73610(7) 0.0332(2) Uani 1 1 d . . . . .
W6 W -0.30987(8) 0.86107(8) 0.28348(6) 0.02951(19) Uani 1 1 d . . . . .
Si1 Si 0.0000 1.0000 0.5000 0.0222(14) Uani 1 2 d S . P . .
O1 O 0.035(3) 0.878(3) 0.429(3) 0.048(5) Uani 0.5 1 d . U P . .
O2 O -0.067(3) 0.896(3) 0.546(3) 0.047(5) Uani 0.5 1 d . U P . .
O3 O 0.158(3) 1.052(3) 0.530(3) 0.048(5) Uani 0.5 1 d . U P . .
O4 O -0.073(3) 0.946(3) 0.367(3) 0.044(4) Uani 0.5 1 d . U P . .
O5 O -0.232(2) 0.7589(17) 0.2155(17) 0.065(4) Uani 1 1 d . U . . .
O6 O -0.4532(19) 0.7941(17) 0.1796(16) 0.064(5) Uani 1 1 d . U . . .
O7 O 0.0107(19) 0.7888(18) 0.6268(16) 0.065(4) Uani 1 1 d . U . . .
O8 O -0.0761(16) 0.6638(15) 0.1004(14) 0.045(4) Uani 1 1 d . U . . .
O9 O -0.324(2) 0.9942(16) 0.3931(15) 0.054(4) Uani 1 1 d . U . . .
O10 O -0.0741(17) 0.5541(15) 0.4496(14) 0.048(4) Uani 1 1 d . U . . .
O11 O -0.357(2) 0.7668(17) 0.3676(16) 0.059(4) Uani 1 1 d . U . . .
O12 O 0.0132(18) 0.898(2) 0.8505(15) 0.060(5) Uani 1 1 d . U . . .
O13 O 0.221(2) 1.3136(19) 0.5332(15) 0.071(5) Uani 1 1 d . U . . .
O14 O 0.316(2) 1.0569(17) 0.4287(15) 0.060(4) Uani 1 1 d . U . . .
O15 O 0.3794(17) 0.8658(15) 0.4221(14) 0.047(4) Uani 1 1 d . U . . .
O16 O 0.4454(18) 1.3059(17) 0.4710(14) 0.060(5) Uani 1 1 d . U . . .
O17 O 0.003(2) 1.0834(17) 0.7979(18) 0.069(5) Uani 1 1 d . U . . .
O18 O -0.195(2) 0.9831(16) 0.2416(17) 0.063(4) Uani 1 1 d . U . . .
O19 O -0.186(2) 0.8521(19) 0.6694(18) 0.075(5) Uani 1 1 d . U . . .
O20 O -0.090(2) 0.673(2) 0.3133(17) 0.074(4) Uani 1 1 d . U . . .
O21 O 0.141(2) 0.773(2) 0.4747(16) 0.075(4) Uani 1 1 d . U . . .
O22 O 0.134(2) 0.830(2) 0.2994(17) 0.077(4) Uani 1 1 d . U . . .
Cu1 Cu 0.0000 0.5000 0.0000 0.0344(8) Uani 1 2 d S . P . .
O24 O -0.2012(19) 0.3110(18) 0.1533(16) 0.063(5) Uani 1 1 d . U . . .
O23 O -0.1508(15) 0.3852(15) 0.0272(13) 0.044(4) Uani 1 1 d . U . . .
N1 N 0.1049(17) 0.5179(15) 0.1414(14) 0.033(4) Uani 1 1 d . . . . .
C1 C 0.239(2) 0.588(2) 0.196(2) 0.044(6) Uani 1 1 d . . . . .
H1A H 0.2924 0.6353 0.1647 0.053 Uiso 1 1 calc R U . . .
C2 C 0.299(3) 0.592(2) 0.293(2) 0.052(6) Uani 1 1 d . . . . .
H2A H 0.3913 0.6440 0.3287 0.062 Uiso 1 1 calc R U . . .
C3 C 0.222(3) 0.519(3) 0.339(2) 0.058(7) Uani 1 1 d . . . . .
H3A H 0.2644 0.5184 0.4046 0.069 Uiso 1 1 calc R U . . .
C4 C 0.081(3) 0.445(2) 0.289(2) 0.049(6) Uani 1 1 d . . . . .
H4A H 0.0262 0.3973 0.3199 0.058 Uiso 1 1 calc R U . . .
C5 C 0.030(2) 0.4512(19) 0.1898(18) 0.033(4) Uani 1 1 d . . . . .
C6 C -0.116(2) 0.376(2) 0.1187(18) 0.038(5) Uani 1 1 d . . . . .
N3 N 0.370(3) 0.329(2) 0.2263(18) 0.065(7) Uani 1 1 d . . . . .
N2 N 0.180(3) 0.231(3) 0.064(3) 0.093(10) Uani 1 1 d . . . . .
H2B H 0.1466 0.2115 -0.0062 0.112 Uiso 1 1 calc R U . . .
H2C H 0.1278 0.1997 0.0998 0.112 Uiso 1 1 calc R U . . .
C7 C 0.388(3) 0.353(3) 0.057(2) 0.067(9) Uani 1 1 d . . . . .
H7A H 0.3470 0.3390 -0.0156 0.081 Uiso 1 1 calc R U . . .
C8 C 0.526(4) 0.422(4) 0.101(4) 0.113(17) Uani 1 1 d . . . . .
H8A H 0.5782 0.4466 0.0560 0.135 Uiso 1 1 calc R U . . .
C9 C 0.587(4) 0.454(3) 0.210(3) 0.094(14) Uani 1 1 d . . . . .
H9A H 0.6793 0.5078 0.2436 0.113 Uiso 1 1 calc R U . . .
C10 C 0.509(4) 0.406(3) 0.274(2) 0.088(12) Uani 1 1 d . . . . .
H10A H 0.5513 0.4254 0.3489 0.105 Uiso 1 1 calc R U . . .
C11 C 0.305(3) 0.304(3) 0.116(2) 0.058(7) Uani 1 1 d . . . . .
N5 N 0.541(2) 0.1491(19) 0.1216(18) 0.051(5) Uani 1 1 d . . . . .
H5A H 0.6077 0.2040 0.1134 0.061 Uiso 1 1 calc R U . . .
N4 N 0.684(3) 0.201(3) 0.293(3) 0.101(11) Uani 1 1 d . . . . .
H4B H 0.7463 0.2589 0.2839 0.121 Uiso 1 1 calc R U . . .
H4C H 0.7006 0.1891 0.3527 0.121 Uiso 1 1 calc R U . . .
C16 C 0.451(3) 0.042(3) 0.228(3) 0.064(8) Uani 1 1 d . . . . .
H16A H 0.4663 0.0286 0.2928 0.076 Uiso 1 1 calc R U . . .
C15 C 0.330(3) -0.017(3) 0.156(3) 0.088(12) Uani 1 1 d . . . . .
H15A H 0.2585 -0.0731 0.1690 0.106 Uiso 1 1 calc R U . . .
C14 C 0.308(3) 0.005(3) 0.056(3) 0.079(10) Uani 1 1 d . . . . .
H14A H 0.2221 -0.0355 0.0032 0.095 Uiso 1 1 calc R U . . .
C13 C 0.417(3) 0.086(2) 0.043(2) 0.056(7) Uani 1 1 d . . . . .
H13A H 0.4069 0.0992 -0.0221 0.068 Uiso 1 1 calc R U . . .
C12 C 0.558(3) 0.126(3) 0.211(2) 0.050(6) 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
W1 O15 1.668(16) . ?
W1 O14 1.883(18) . ?
W1 O22 1.889(19) . ?
W1 O9 1.897(18) 2_576 ?
W1 O21 1.910(19) . ?
W1 O1 2.31(4) . ?
W1 O3 2.48(4) . ?
W2 O10 1.678(16) . ?
W2 O20 1.877(18) . ?
W2 O13 1.90(2) 2_576 ?
W2 O21 1.90(2) . ?
W2 O7 1.907(19) . ?
W2 O1 2.36(3) . ?
W2 O2 2.48(3) . ?
W3 O16 1.677(16) . ?
W3 O13 1.86(2) . ?
W3 O14 1.878(18) . ?
W3 O19 1.899(19) 2_576 ?
W3 O11 1.905(18) 2_576 ?
W3 O2 2.35(3) 2_576 ?
W3 O3 2.40(3) . ?
W4 O8 1.694(16) . ?
W4 O22 1.87(2) . ?
W4 O20 1.901(18) . ?
W4 O17 1.91(2) 2_576 ?
W4 O5 1.93(2) . ?
W4 O1 2.33(3) . ?
W4 O4 2.44(3) . ?
W5 O12 1.687(16) . ?
W5 O7 1.869(19) . ?
W5 O18 1.875(19) 2_576 ?
W5 O17 1.878(19) . ?
W5 O19 1.94(2) . ?
W5 O2 2.36(3) . ?
W5 O4 2.41(3) 2_576 ?
W6 O6 1.654(16) . ?
W6 O5 1.86(2) . ?
W6 O9 1.880(17) . ?
W6 O11 1.887(17) . ?
W6 O18 1.912(17) . ?
W6 O4 2.36(3) . ?
W6 O3 2.39(3) 2_576 ?
Si1 O3 1.57(3) 2_576 ?
Si1 O3 1.57(3) . ?
Si1 O4 1.60(3) 2_576 ?
Si1 O4 1.60(3) . ?
Si1 O2 1.62(3) . ?
Si1 O2 1.62(3) 2_576 ?
Si1 O1 1.72(4) 2_576 ?
Si1 O1 1.72(4) . ?
O2 O3 1.78(4) 2_576 ?
O2 W3 2.35(3) 2_576 ?
O3 O4 1.75(5) 2_576 ?
O3 O2 1.78(4) 2_576 ?
O3 W6 2.39(3) 2_576 ?
O4 O3 1.75(5) 2_576 ?
O4 W5 2.41(3) 2_576 ?
O9 W1 1.897(18) 2_576 ?
O11 W3 1.905(18) 2_576 ?
O13 W2 1.90(2) 2_576 ?
O17 W4 1.91(2) 2_576 ?
O18 W5 1.875(19) 2_576 ?
O19 W3 1.899(19) 2_576 ?
Cu1 O23 1.944(15) . ?
Cu1 O23 1.945(15) 2_565 ?
Cu1 N1 1.952(16) 2_565 ?
Cu1 N1 1.952(16) . ?
O24 C6 1.26(3) . ?
O23 C6 1.28(2) . ?
N1 C5 1.35(3) . ?
N1 C1 1.35(3) . ?
C1 C2 1.32(3) . ?
C2 C3 1.39(4) . ?
C3 C4 1.40(4) . ?
C4 C5 1.40(3) . ?
C5 C6 1.50(3) . ?
N3 C10 1.39(4) . ?
N3 C11 1.41(3) . ?
N2 C11 1.27(4) . ?
C7 C8 1.37(4) . ?
C7 C11 1.38(4) . ?
C8 C9 1.35(5) . ?
C9 C10 1.41(5) . ?
N5 C12 1.31(3) . ?
N5 C13 1.35(3) . ?
N4 C12 1.39(4) . ?
C16 C15 1.30(4) . ?
C16 C12 1.38(3) . ?
C15 C14 1.45(5) . ?
C14 C13 1.35(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
O15 W1 O14 101.3(9) . . ?
O15 W1 O22 101.5(10) . . ?
O14 W1 O22 86.3(8) . . ?
O15 W1 O9 101.4(8) . 2_576 ?
O14 W1 O9 88.8(7) . 2_576 ?
O22 W1 O9 157.0(10) . 2_576 ?
O15 W1 O21 100.6(10) . . ?
O14 W1 O21 158.1(10) . . ?
O22 W1 O21 88.5(8) . . ?
O9 W1 O21 87.7(8) 2_576 . ?
O15 W1 O1 155.8(11) . . ?
O14 W1 O1 95.2(10) . . ?
O22 W1 O1 61.8(11) . . ?
O9 W1 O1 96.4(10) 2_576 . ?
O21 W1 O1 63.8(10) . . ?
O15 W1 O3 156.5(10) . . ?
O14 W1 O3 62.9(10) . . ?
O22 W1 O3 94.9(11) . . ?
O9 W1 O3 63.0(9) 2_576 . ?
O21 W1 O3 96.5(11) . . ?
O1 W1 O3 47.6(12) . . ?
O10 W2 O20 101.0(9) . . ?
O10 W2 O13 99.1(9) . 2_576 ?
O20 W2 O13 88.8(9) . 2_576 ?
O10 W2 O21 102.3(9) . . ?
O20 W2 O21 88.6(8) . . ?
O13 W2 O21 158.6(10) 2_576 . ?
O10 W2 O7 101.4(8) . . ?
O20 W2 O7 157.6(9) . . ?
O13 W2 O7 87.5(8) 2_576 . ?
O21 W2 O7 86.9(9) . . ?
O10 W2 O1 156.5(11) . . ?
O20 W2 O1 62.7(10) . . ?
O13 W2 O1 97.4(11) 2_576 . ?
O21 W2 O1 62.8(11) . . ?
O7 W2 O1 95.9(11) . . ?
O10 W2 O2 153.9(10) . . ?
O20 W2 O2 96.7(10) . . ?
O13 W2 O2 62.1(10) 2_576 . ?
O21 W2 O2 97.2(11) . . ?
O7 W2 O2 62.2(9) . . ?
O1 W2 O2 49.5(12) . . ?
O16 W3 O13 101.5(10) . . ?
O16 W3 O14 101.6(10) . . ?
O13 W3 O14 156.9(10) . . ?
O16 W3 O19 99.2(10) . 2_576 ?
O13 W3 O19 88.6(8) . 2_576 ?
O14 W3 O19 87.8(8) . 2_576 ?
O16 W3 O11 100.4(8) . 2_576 ?
O13 W3 O11 85.7(8) . 2_576 ?
O14 W3 O11 90.0(8) . 2_576 ?
O19 W3 O11 160.2(10) 2_576 2_576 ?
O16 W3 O2 158.7(10) . 2_576 ?
O13 W3 O2 65.4(11) . 2_576 ?
O14 W3 O2 92.6(10) . 2_576 ?
O19 W3 O2 65.1(11) 2_576 2_576 ?
O11 W3 O2 95.4(10) 2_576 2_576 ?
O16 W3 O3 157.2(10) . . ?
O13 W3 O3 93.3(12) . . ?
O14 W3 O3 64.7(11) . . ?
O19 W3 O3 98.3(11) 2_576 . ?
O11 W3 O3 63.2(9) 2_576 . ?
O2 W3 O3 44.1(10) 2_576 . ?
O8 W4 O22 101.7(9) . . ?
O8 W4 O20 101.9(9) . . ?
O22 W4 O20 88.5(8) . . ?
O8 W4 O17 99.2(8) . 2_576 ?
O22 W4 O17 88.1(9) . 2_576 ?
O20 W4 O17 158.9(9) . 2_576 ?
O8 W4 O5 99.7(8) . . ?
O22 W4 O5 158.6(10) . . ?
O20 W4 O5 88.0(9) . . ?
O17 W4 O5 87.7(8) 2_576 . ?
O8 W4 O1 156.2(10) . . ?
O22 W4 O1 61.5(11) . . ?
O20 W4 O1 63.1(10) . . ?
O17 W4 O1 97.2(10) 2_576 . ?
O5 W4 O1 98.2(11) . . ?
O8 W4 O4 155.2(9) . . ?
O22 W4 O4 96.3(11) . . ?
O20 W4 O4 95.3(10) . . ?
O17 W4 O4 64.4(9) 2_576 . ?
O5 W4 O4 63.0(10) . . ?
O1 W4 O4 48.6(11) . . ?
O12 W5 O7 102.5(10) . . ?
O12 W5 O18 100.6(9) . 2_576 ?
O7 W5 O18 88.1(8) . 2_576 ?
O12 W5 O17 99.4(10) . . ?
O7 W5 O17 158.1(9) . . ?
O18 W5 O17 88.6(8) 2_576 . ?
O12 W5 O19 98.9(10) . . ?
O7 W5 O19 88.6(8) . . ?
O18 W5 O19 160.4(10) 2_576 . ?
O17 W5 O19 87.3(9) . . ?
O12 W5 O2 158.2(11) . . ?
O7 W5 O2 65.2(10) . . ?
O18 W5 O2 97.0(11) 2_576 . ?
O17 W5 O2 93.8(11) . . ?
O19 W5 O2 64.2(11) . . ?
O12 W5 O4 156.6(11) . 2_576 ?
O7 W5 O4 93.9(10) . 2_576 ?
O18 W5 O4 63.0(10) 2_576 2_576 ?
O17 W5 O4 65.5(10) . 2_576 ?
O19 W5 O4 98.1(11) . 2_576 ?
O2 W5 O4 45.2(11) . 2_576 ?
O6 W6 O5 98.5(10) . . ?
O6 W6 O9 103.1(10) . . ?
O5 W6 O9 158.4(9) . . ?
O6 W6 O11 101.8(9) . . ?
O5 W6 O11 87.0(8) . . ?
O9 W6 O11 90.3(8) . . ?
O6 W6 O18 100.6(9) . . ?
O5 W6 O18 87.8(8) . . ?
O9 W6 O18 86.6(7) . . ?
O11 W6 O18 157.5(9) . . ?
O6 W6 O4 156.8(11) . . ?
O5 W6 O4 65.6(10) . . ?
O9 W6 O4 93.2(10) . . ?
O11 W6 O4 94.3(9) . . ?
O18 W6 O4 63.6(9) . . ?
O6 W6 O3 160.0(12) . 2_576 ?
O5 W6 O3 94.5(11) . 2_576 ?
O9 W6 O3 65.2(10) . 2_576 ?
O11 W6 O3 63.6(10) . 2_576 ?
O18 W6 O3 95.0(10) . 2_576 ?
O4 W6 O3 43.1(11) . 2_576 ?
O3 Si1 O3 180.0 2_576 . ?
O3 Si1 O4 113.0(17) 2_576 2_576 ?
O3 Si1 O4 67.0(17) . 2_576 ?
O3 Si1 O4 67.0(17) 2_576 . ?
O3 Si1 O4 113.0(17) . . ?
O4 Si1 O4 180(3) 2_576 . ?
O3 Si1 O2 67.9(16) 2_576 . ?
O3 Si1 O2 112.1(16) . . ?
O4 Si1 O2 69.4(16) 2_576 . ?
O4 Si1 O2 110.6(16) . . ?
O3 Si1 O2 112.1(16) 2_576 2_576 ?
O3 Si1 O2 67.9(16) . 2_576 ?
O4 Si1 O2 110.6(16) 2_576 2_576 ?
O4 Si1 O2 69.4(16) . 2_576 ?
O2 Si1 O2 180.0 . 2_576 ?
O3 Si1 O1 72.1(17) 2_576 2_576 ?
O3 Si1 O1 107.9(17) . 2_576 ?
O4 Si1 O1 72.6(15) 2_576 2_576 ?
O4 Si1 O1 107.4(15) . 2_576 ?
O2 Si1 O1 105.4(16) . 2_576 ?
O2 Si1 O1 74.6(16) 2_576 2_576 ?
O3 Si1 O1 107.9(17) 2_576 . ?
O3 Si1 O1 72.1(17) . . ?
O4 Si1 O1 107.4(15) 2_576 . ?
O4 Si1 O1 72.6(15) . . ?
O2 Si1 O1 74.6(16) . . ?
O2 Si1 O1 105.4(16) 2_576 . ?
O1 Si1 O1 179.998(12) 2_576 . ?
Si1 O1 W1 121.0(17) . . ?
Si1 O1 W4 119.3(15) . . ?
W1 O1 W4 98.1(14) . . ?
Si1 O1 W2 118.6(17) . . ?
W1 O1 W2 97.9(12) . . ?
W4 O1 W2 96.9(12) . . ?
Si1 O2 O3 54.5(14) . 2_576 ?
Si1 O2 W3 124.1(16) . 2_576 ?
O3 O2 W3 69.5(16) 2_576 2_576 ?
Si1 O2 W5 123.6(18) . . ?
O3 O2 W5 138(2) 2_576 . ?
W3 O2 W5 96.9(12) 2_576 . ?
Si1 O2 W2 117.3(18) . . ?
O3 O2 W2 126(2) 2_576 . ?
W3 O2 W2 93.7(11) 2_576 . ?
W5 O2 W2 93.8(10) . . ?
Si1 O3 O4 57.4(16) . 2_576 ?
Si1 O3 O2 57.5(15) . 2_576 ?
O4 O3 O2 97(2) 2_576 2_576 ?
Si1 O3 W6 125.0(19) . 2_576 ?
O4 O3 W6 67.6(15) 2_576 2_576 ?
O2 O3 W6 136(2) 2_576 2_576 ?
Si1 O3 W3 123.9(15) . . ?
O4 O3 W3 135(2) 2_576 . ?
O2 O3 W3 66.3(14) 2_576 . ?
W6 O3 W3 94.9(12) 2_576 . ?
Si1 O3 W1 119.3(17) . . ?
O4 O3 W1 127.8(18) 2_576 . ?
O2 O3 W1 126(2) 2_576 . ?
W6 O3 W1 92.9(11) 2_576 . ?
W3 O3 W1 92.5(12) . . ?
Si1 O4 O3 55.7(15) . 2_576 ?
Si1 O4 W6 124.9(18) . . ?
O3 O4 W6 69.3(15) 2_576 . ?
Si1 O4 W5 121.9(17) . 2_576 ?
O3 O4 W5 134.8(19) 2_576 2_576 ?
W6 O4 W5 95.3(10) . 2_576 ?
Si1 O4 W4 119.5(15) . . ?
O3 O4 W4 129.1(18) 2_576 . ?
W6 O4 W4 94.5(12) . . ?
W5 O4 W4 93.1(11) 2_576 . ?
W6 O5 W4 136.7(11) . . ?
W5 O7 W2 138.5(11) . . ?
W6 O9 W1 138.3(10) . 2_576 ?
W6 O11 W3 137.0(11) . 2_576 ?
W3 O13 W2 138.6(11) . 2_576 ?
W3 O14 W1 139.3(12) . . ?
W5 O17 W4 136.7(12) . 2_576 ?
W5 O18 W6 137.6(12) 2_576 . ?
W3 O19 W5 133.4(14) 2_576 . ?
W2 O20 W4 137.2(12) . . ?
W2 O21 W1 135.4(13) . . ?
W4 O22 W1 138.3(13) . . ?
O23 Cu1 O23 180.0 . 2_565 ?
O23 Cu1 N1 96.6(7) . 2_565 ?
O23 Cu1 N1 83.4(7) 2_565 2_565 ?
O23 Cu1 N1 83.4(7) . . ?
O23 Cu1 N1 96.6(7) 2_565 . ?
N1 Cu1 N1 180.0 2_565 . ?
C6 O23 Cu1 113.1(14) . . ?
C5 N1 C1 116.8(19) . . ?
C5 N1 Cu1 114.1(14) . . ?
C1 N1 Cu1 129.1(16) . . ?
C2 C1 N1 123(2) . . ?
C1 C2 C3 119(2) . . ?
C2 C3 C4 121(2) . . ?
C5 C4 C3 114(2) . . ?
N1 C5 C4 125(2) . . ?
N1 C5 C6 111.2(17) . . ?
C4 C5 C6 123(2) . . ?
O24 C6 O23 122(2) . . ?
O24 C6 C5 120(2) . . ?
O23 C6 C5 118.2(18) . . ?
C10 N3 C11 120(3) . . ?
C8 C7 C11 124(3) . . ?
C9 C8 C7 119(4) . . ?
C8 C9 C10 120(3) . . ?
N3 C10 C9 120(2) . . ?
N2 C11 C7 120(3) . . ?
N2 C11 N3 123(3) . . ?
C7 C11 N3 117(3) . . ?
C12 N5 C13 119(2) . . ?
C15 C16 C12 121(3) . . ?
C16 C15 C14 119(3) . . ?
C13 C14 C15 117(3) . . ?
C14 C13 N5 122(3) . . ?
N5 C12 C16 122(2) . . ?
N5 C12 N4 116(3) . . ?
C16 C12 N4 121(3) . . ?

_refine_diff_density_max         2.703
_refine_diff_density_min         -2.671
_refine_diff_density_rms         0.358

####################################################################### 
# 
# 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_shelx_2
_database_code_depnum_ccdc_archive 'CCDC 1056232'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H36 Cu Ge N10 O44 W12'
_chemical_formula_weight         3606.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.110(2)
_cell_length_b                   12.786(3)
_cell_length_c                   13.191(3)
_cell_angle_alpha                110.394(3)
_cell_angle_beta                 97.412(3)
_cell_angle_gamma                111.891(2)
_cell_volume                     1555.8(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5357
_cell_measurement_theta_min      3.4100
_cell_measurement_theta_max      28.0990

_exptl_crystal_description       block
_exptl_crystal_colour            dark_green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.850
_exptl_crystal_F_000             1598
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    22.996
_shelx_estimated_absorpt_T_min   0.055
_shelx_estimated_absorpt_T_max   0.097
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_T_max  0.093
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
R(int) was 0.0456 before and 0.0430 after correction. The Ratio of minimum to 
maximum transmission is 0.4086.   
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 15.9737
_diffrn_reflns_number            13888
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.064
_diffrn_reflns_theta_max         29.091
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7152
_reflns_number_gt                5491
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0251P)²+27.8761P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7152
_refine_ls_number_parameters     436
_refine_ls_number_restraints     462
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1238
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.073
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.80211(6) 0.70692(5) 0.47908(5) 0.03574(15) Uani 1 1 d . . . . .
W2 W 1.24274(7) 0.59341(7) 0.55260(6) 0.0493(2) Uani 1 1 d . . . . .
W3 W 1.54643(7) 0.80120(6) 0.53354(6) 0.0534(2) Uani 1 1 d . . . . .
W4 W 1.18956(6) 0.36198(5) 0.28348(5) 0.03341(15) Uani 1 1 d . . . . .
W5 W 1.49227(7) 0.57086(5) 0.26362(5) 0.03733(16) Uani 1 1 d . . . . .
W6 W 1.55087(7) 0.72905(6) 0.76817(5) 0.0480(2) Uani 1 1 d . . . . .
Ge1 Ge 1.5000 0.5000 0.5000 0.0235(4) Uani 1 2 d S . P . .
O1 O 1.420(2) 0.4461(18) 0.3624(17) 0.039(3) Uani 0.5 1 d . U P . .
O2 O 1.331(2) 0.445(2) 0.4674(18) 0.044(4) Uani 0.5 1 d . U P . .
O3 O 1.426(2) 0.3914(19) 0.5521(16) 0.038(4) Uani 0.5 1 d . U P . .
O4 O 1.464(2) 0.630(2) 0.5773(18) 0.046(4) Uani 0.5 1 d . U P . .
O5 O 1.8609(16) 0.7299(12) 0.6315(11) 0.071(3) Uani 1 1 d . U . . .
O6 O 1.4898(13) 0.6040(14) 0.1526(11) 0.070(4) Uani 1 1 d . U . . .
O7 O 1.0464(13) 0.2975(11) 0.1789(11) 0.073(4) Uani 1 1 d . U . . .
O8 O 1.6837(15) 0.6458(13) 0.3313(12) 0.082(3) Uani 1 1 d . U . . .
O9 O 1.2686(13) 0.2588(11) 0.2144(12) 0.067(3) Uani 1 1 d . U . . .
O10 O 1.7211(15) 0.8109(14) 0.5336(12) 0.085(4) Uani 1 1 d . U . . .
O11 O 1.5778(13) 0.8339(11) 0.8959(10) 0.056(3) Uani 1 1 d . U . . .
O12 O 1.4878(14) 0.7110(13) 0.3729(12) 0.078(3) Uani 1 1 d . U . . .
O13 O 1.9466(13) 0.8047(12) 0.4701(9) 0.074(4) Uani 1 1 d . U . . .
O14 O 1.8185(16) 0.5560(12) 0.4286(10) 0.069(3) Uani 1 1 d . U . . .
O15 O 1.1721(14) 0.4953(11) 0.3914(11) 0.064(3) Uani 1 1 d . U . . .
O16 O 1.4998(14) 0.4168(11) 0.2057(13) 0.073(3) Uani 1 1 d . U . . .
O17 O 1.5765(12) 0.9437(10) 0.5499(10) 0.054(3) Uani 1 1 d . U . . .
O18 O 1.3569(15) 0.7277(14) 0.5262(12) 0.093(4) Uani 1 1 d . U . . .
O19 O 1.3037(15) 0.4836(12) 0.2405(12) 0.075(3) Uani 1 1 d . U . . .
O20 O 1.5922(15) 0.8312(15) 0.6888(12) 0.095(4) Uani 1 1 d . U . . .
O21 O 1.3661(15) 0.6721(14) 0.7008(12) 0.091(4) Uani 1 1 d . U . . .
O22 O 1.1209(14) 0.6357(11) 0.5763(10) 0.061(3) Uani 1 1 d . U . . .
Cu1 Cu 1.5000 1.0000 1.0000 0.0407(6) Uani 1 2 d S . P . .
O23 O 1.7031(13) 1.1887(12) 0.8467(11) 0.066(4) Uani 1 1 d . U . . .
O24 O 1.6521(11) 1.1159(10) 0.9724(9) 0.051(3) Uani 1 1 d . U . . .
N1 N 1.3963(8) 0.9823(8) 0.8604(6) 0.033(3) Uani 1 1 d G . . . .
C1 C 1.2576(8) 0.9107(8) 0.8059(8) 0.049(4) Uani 1 1 d G . . . .
H1A H 1.2030 0.8624 0.8362 0.059 Uiso 1 1 calc R U . . .
C2 C 1.2005(8) 0.9114(9) 0.7061(8) 0.053(4) Uani 1 1 d G . . . .
H2A H 1.1077 0.8636 0.6697 0.064 Uiso 1 1 calc R U . . .
C3 C 1.2820(11) 0.9837(10) 0.6608(7) 0.058(5) Uani 1 1 d G . . . .
H3A H 1.2438 0.9842 0.5941 0.070 Uiso 1 1 calc R U . . .
C4 C 1.4207(11) 1.0553(9) 0.7153(8) 0.049(4) Uani 1 1 d G . . . .
H4A H 1.4752 1.1036 0.6850 0.058 Uiso 1 1 calc R U . . .
C5 C 1.4778(7) 1.0546(8) 0.8151(7) 0.040(4) Uani 1 1 d G . . . .
C6 C 1.6203(17) 1.1260(15) 0.8830(13) 0.047(4) Uani 1 1 d . . . . .
N5 N 1.183(2) 0.696(2) 0.2885(18) 0.110(8) Uani 1 1 d . . . . .
H5A H 1.1999 0.6899 0.3510 0.132 Uiso 1 1 calc R U . . .
H5B H 1.2456 0.7480 0.2740 0.132 Uiso 1 1 calc R U . . .
N2 N 0.318(2) 0.271(2) 0.9380(18) 0.103(7) Uani 1 1 d . . . . .
H2B H 0.3691 0.3108 0.9068 0.124 Uiso 1 1 calc R U . . .
H2C H 0.3512 0.2825 1.0058 0.124 Uiso 1 1 calc R U . . .
C7 C 0.1120(14) 0.1435(13) 0.9432(9) 0.068(6) Uani 1 1 d G . . . .
H7A H 0.1527 0.1593 1.0165 0.082 Uiso 1 1 calc R U . . .
C8 C -0.0274(13) 0.0703(13) 0.8943(14) 0.118(11) Uani 1 1 d G . . . .
H8A H -0.0801 0.0372 0.9350 0.141 Uiso 1 1 calc R U . . .
C9 C -0.0881(11) 0.0467(13) 0.7846(14) 0.090(8) Uani 1 1 d G . . . .
H9A H -0.1814 -0.0022 0.7519 0.108 Uiso 1 1 calc R U . . .
C10 C -0.0094(16) 0.0963(13) 0.7238(9) 0.096(9) Uani 1 1 d G . . . .
H10A H -0.0501 0.0805 0.6504 0.115 Uiso 1 1 calc R U . . .
N3 N 0.1300(15) 0.1694(12) 0.7726(9) 0.074(5) Uani 1 1 d G . . . .
C11 C 0.1908(11) 0.1930(11) 0.8823(10) 0.059(5) Uani 1 1 d G . . . .
C12 C 1.0583(10) 0.6249(12) 0.2134(9) 0.068(6) Uani 1 1 d G . . . .
C13 C 0.9504(14) 0.5386(13) 0.2290(11) 0.067(6) Uani 1 1 d G . . . .
H13A H 0.9635 0.5239 0.2928 0.080 Uiso 1 1 calc R U . . .
C14 C 0.8231(11) 0.4742(12) 0.1491(14) 0.085(7) Uani 1 1 d G . . . .
H14A H 0.7509 0.4165 0.1595 0.103 Uiso 1 1 calc R U . . .
C15 C 0.8036(11) 0.4962(12) 0.0537(11) 0.091(8) Uani 1 1 d G . . . .
H15A H 0.7184 0.4531 0.0002 0.109 Uiso 1 1 calc R U . . .
C16 C 0.9115(15) 0.5825(13) 0.0381(8) 0.064(5) Uani 1 1 d G . . . .
H16A H 0.8985 0.5972 -0.0258 0.077 Uiso 1 1 calc R U . . .
N4 N 1.0388(12) 0.6469(10) 0.1180(10) 0.062(4) Uani 1 1 d G . . . .
H4B H 1.1056 0.7003 0.1083 0.075 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O13 1.677(11) . ?
W1 O10 1.867(14) . ?
W1 O14 1.897(12) . ?
W1 O8 1.911(13) . ?
W1 O5 1.914(12) . ?
W1 O3 2.28(2) 2_866 ?
W1 O2 2.36(2) 2_866 ?
W2 O22 1.662(12) . ?
W2 O14 1.892(12) 2_866 ?
W2 O18 1.894(13) . ?
W2 O21 1.903(12) . ?
W2 O15 1.920(13) . ?
W2 O4 2.28(2) . ?
W2 O2 2.45(2) . ?
W3 O17 1.653(10) . ?
W3 O10 1.898(15) . ?
W3 O12 1.904(14) . ?
W3 O20 1.907(14) . ?
W3 O18 1.933(16) . ?
W3 O4 2.341(19) . ?
W3 O3 2.48(2) 2_866 ?
W4 O7 1.666(11) . ?
W4 O5 1.882(13) 2_866 ?
W4 O9 1.891(12) . ?
W4 O15 1.897(13) . ?
W4 O19 1.917(13) . ?
W4 O1 2.30(2) . ?
W4 O2 2.34(2) . ?
W5 O6 1.661(11) . ?
W5 O16 1.887(12) . ?
W5 O12 1.890(13) . ?
W5 O19 1.893(14) . ?
W5 O8 1.906(14) . ?
W5 O3 2.291(18) 2_866 ?
W5 O1 2.378(18) . ?
W6 O11 1.650(12) . ?
W6 O21 1.870(15) . ?
W6 O16 1.905(13) 2_866 ?
W6 O20 1.909(14) . ?
W6 O9 1.930(13) 2_866 ?
W6 O4 2.26(2) . ?
W6 O1 2.47(2) 2_866 ?
Ge1 O2 1.67(2) 2_866 ?
Ge1 O2 1.67(2) . ?
Ge1 O1 1.68(2) 2_866 ?
Ge1 O1 1.68(2) . ?
Ge1 O3 1.741(18) . ?
Ge1 O3 1.741(18) 2_866 ?
Ge1 O4 1.84(2) . ?
Ge1 O4 1.84(2) 2_866 ?
O1 O2 1.80(3) . ?
O1 W6 2.47(2) 2_866 ?
O2 W1 2.355(19) 2_866 ?
O3 W1 2.28(2) 2_866 ?
O3 W5 2.291(18) 2_866 ?
O3 W3 2.48(2) 2_866 ?
O5 W4 1.882(12) 2_866 ?
O9 W6 1.930(13) 2_866 ?
O11 Cu1 2.605(12) . ?
O14 W2 1.892(12) 2_866 ?
O16 W6 1.905(13) 2_866 ?
Cu1 N1 1.934(6) 2_877 ?
Cu1 N1 1.934(6) . ?
Cu1 O24 1.963(11) . ?
Cu1 O24 1.963(11) 2_877 ?
Cu1 O11 2.605(12) 2_877 ?
O23 C6 1.244(19) . ?
O24 C6 1.251(18) . ?
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 H3A 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4A 0.9300 . ?
C5 C6 1.459(18) . ?
N5 C12 1.34(2) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N2 C11 1.31(2) . ?
N2 H2B 0.8600 . ?
N2 H2C 0.8600 . ?
C7 C8 1.3900 . ?
C7 C11 1.3900 . ?
C7 H7A 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8A 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9A 0.9300 . ?
C10 N3 1.3900 . ?
C10 H10A 0.9300 . ?
N3 C11 1.3900 . ?
C12 C13 1.3900 . ?
C12 N4 1.3900 . ?
C13 C14 1.3900 . ?
C13 H13A 0.9300 . ?
C14 C15 1.3900 . ?
C14 H14A 0.9300 . ?
C15 C16 1.3900 . ?
C15 H15A 0.9300 . ?
C16 N4 1.3900 . ?
C16 H16A 0.9300 . ?
N4 H4B 0.8600 . ?

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
O13 W1 O10 102.2(8) . . ?
O13 W1 O14 101.2(7) . . ?
O10 W1 O14 156.5(7) . . ?
O13 W1 O8 100.4(7) . . ?
O10 W1 O8 87.9(6) . . ?
O14 W1 O8 88.2(5) . . ?
O13 W1 O5 100.3(6) . . ?
O10 W1 O5 87.0(6) . . ?
O14 W1 O5 88.6(5) . . ?
O8 W1 O5 159.3(7) . . ?
O13 W1 O3 156.1(6) . 2_866 ?
O10 W1 O3 64.3(7) . 2_866 ?
O14 W1 O3 93.7(7) . 2_866 ?
O8 W1 O3 61.2(7) . 2_866 ?
O5 W1 O3 98.6(7) . 2_866 ?
O13 W1 O2 155.6(7) . 2_866 ?
O10 W1 O2 93.7(8) . 2_866 ?
O14 W1 O2 64.1(7) . 2_866 ?
O8 W1 O2 98.6(7) . 2_866 ?
O5 W1 O2 61.8(7) . 2_866 ?
O3 W1 O2 48.3(7) 2_866 2_866 ?
O22 W2 O14 101.5(6) . 2_866 ?
O22 W2 O18 99.5(7) . . ?
O14 W2 O18 158.9(7) 2_866 . ?
O22 W2 O21 102.1(7) . . ?
O14 W2 O21 86.7(6) 2_866 . ?
O18 W2 O21 88.0(6) . . ?
O22 W2 O15 100.1(6) . . ?
O14 W2 O15 89.1(5) 2_866 . ?
O18 W2 O15 88.1(6) . . ?
O21 W2 O15 157.9(7) . . ?
O22 W2 O4 153.4(7) . . ?
O14 W2 O4 96.5(7) 2_866 . ?
O18 W2 O4 63.4(7) . . ?
O21 W2 O4 59.5(8) . . ?
O15 W2 O4 99.5(7) . . ?
O22 W2 O2 154.6(7) . . ?
O14 W2 O2 62.0(6) 2_866 . ?
O18 W2 O2 98.4(8) . . ?
O21 W2 O2 96.4(8) . . ?
O15 W2 O2 62.7(6) . . ?
O4 W2 O2 52.0(8) . . ?
O17 W3 O10 99.6(6) . . ?
O17 W3 O12 101.9(6) . . ?
O10 W3 O12 88.7(6) . . ?
O17 W3 O20 99.4(6) . . ?
O10 W3 O20 87.9(7) . . ?
O12 W3 O20 158.7(7) . . ?
O17 W3 O18 102.5(7) . . ?
O10 W3 O18 157.9(7) . . ?
O12 W3 O18 86.7(6) . . ?
O20 W3 O18 88.5(6) . . ?
O17 W3 O4 153.9(7) . . ?
O10 W3 O4 97.6(7) . . ?
O12 W3 O4 97.9(7) . . ?
O20 W3 O4 61.8(7) . . ?
O18 W3 O4 61.7(7) . . ?
O17 W3 O3 151.1(6) . 2_866 ?
O10 W3 O3 59.6(6) . 2_866 ?
O12 W3 O3 61.0(5) . 2_866 ?
O20 W3 O3 99.5(7) . 2_866 ?
O18 W3 O3 99.6(7) . 2_866 ?
O4 W3 O3 54.8(7) . 2_866 ?
O7 W4 O5 102.3(6) . 2_866 ?
O7 W4 O9 98.9(7) . . ?
O5 W4 O9 88.5(6) 2_866 . ?
O7 W4 O15 101.4(7) . . ?
O5 W4 O15 89.6(5) 2_866 . ?
O9 W4 O15 159.5(6) . . ?
O7 W4 O19 99.2(6) . . ?
O5 W4 O19 158.5(7) 2_866 . ?
O9 W4 O19 87.8(5) . . ?
O15 W4 O19 86.5(5) . . ?
O7 W4 O1 155.6(8) . . ?
O5 W4 O1 96.3(6) 2_866 . ?
O9 W4 O1 65.7(7) . . ?
O15 W4 O1 94.3(7) . . ?
O19 W4 O1 63.0(6) . . ?
O7 W4 O2 158.7(8) . . ?
O5 W4 O2 62.6(6) 2_866 . ?
O9 W4 O2 95.7(7) . . ?
O15 W4 O2 65.5(7) . . ?
O19 W4 O2 96.8(7) . . ?
O1 W4 O2 45.7(7) . . ?
O6 W5 O16 101.6(7) . . ?
O6 W5 O12 101.5(7) . . ?
O16 W5 O12 156.9(6) . . ?
O6 W5 O19 100.5(6) . . ?
O16 W5 O19 89.3(6) . . ?
O12 W5 O19 87.1(6) . . ?
O6 W5 O8 99.5(7) . . ?
O16 W5 O8 86.7(6) . . ?
O12 W5 O8 88.9(6) . . ?
O19 W5 O8 160.0(7) . . ?
O6 W5 O3 155.2(7) . 2_866 ?
O16 W5 O3 93.0(7) . 2_866 ?
O12 W5 O3 65.2(6) . 2_866 ?
O19 W5 O3 99.7(7) . 2_866 ?
O8 W5 O3 61.0(7) . 2_866 ?
O6 W5 O1 156.0(7) . . ?
O16 W5 O1 64.7(6) . . ?
O12 W5 O1 93.7(7) . . ?
O19 W5 O1 61.5(7) . . ?
O8 W5 O1 99.2(7) . . ?
O3 W5 O1 48.8(7) 2_866 . ?
O11 W6 O21 102.3(7) . . ?
O11 W6 O16 100.1(6) . 2_866 ?
O21 W6 O16 87.4(6) . 2_866 ?
O11 W6 O20 100.8(7) . . ?
O21 W6 O20 88.8(6) . . ?
O16 W6 O20 159.0(7) 2_866 . ?
O11 W6 O9 98.4(6) . 2_866 ?
O21 W6 O9 159.2(7) . 2_866 ?
O16 W6 O9 87.7(5) 2_866 2_866 ?
O20 W6 O9 88.6(6) . 2_866 ?
O11 W6 O4 154.9(7) . . ?
O21 W6 O4 60.2(8) . . ?
O16 W6 O4 97.0(7) 2_866 . ?
O20 W6 O4 63.4(7) . . ?
O9 W6 O4 100.4(7) 2_866 . ?
O11 W6 O1 152.3(6) . 2_866 ?
O21 W6 O1 98.5(7) . 2_866 ?
O16 W6 O1 62.6(6) 2_866 2_866 ?
O20 W6 O1 97.7(7) . 2_866 ?
O9 W6 O1 61.5(6) 2_866 2_866 ?
O4 W6 O1 52.8(7) . 2_866 ?
O2 Ge1 O2 180.0(17) 2_866 . ?
O2 Ge1 O1 65.1(10) 2_866 2_866 ?
O2 Ge1 O1 114.9(10) . 2_866 ?
O2 Ge1 O1 114.9(10) 2_866 . ?
O2 Ge1 O1 65.1(10) . . ?
O1 Ge1 O1 180.0(16) 2_866 . ?
O2 Ge1 O3 112.4(9) 2_866 . ?
O2 Ge1 O3 67.6(9) . . ?
O1 Ge1 O3 68.7(9) 2_866 . ?
O1 Ge1 O3 111.3(9) . . ?
O2 Ge1 O3 67.6(9) 2_866 2_866 ?
O2 Ge1 O3 112.4(9) . 2_866 ?
O1 Ge1 O3 111.3(9) 2_866 2_866 ?
O1 Ge1 O3 68.7(9) . 2_866 ?
O3 Ge1 O3 180.0 . 2_866 ?
O2 Ge1 O4 107.5(10) 2_866 . ?
O2 Ge1 O4 72.5(10) . . ?
O1 Ge1 O4 73.6(9) 2_866 . ?
O1 Ge1 O4 106.4(9) . . ?
O3 Ge1 O4 103.4(9) . . ?
O3 Ge1 O4 76.6(9) 2_866 . ?
O2 Ge1 O4 72.5(10) 2_866 2_866 ?
O2 Ge1 O4 107.5(10) . 2_866 ?
O1 Ge1 O4 106.4(9) 2_866 2_866 ?
O1 Ge1 O4 73.6(9) . 2_866 ?
O3 Ge1 O4 76.6(9) . 2_866 ?
O3 Ge1 O4 103.4(9) 2_866 2_866 ?
O4 Ge1 O4 180.0(12) . 2_866 ?
Ge1 O1 O2 57.3(9) . . ?
Ge1 O1 W4 125.6(11) . . ?
O2 O1 W4 68.4(10) . . ?
Ge1 O1 W5 120.4(10) . . ?
O2 O1 W5 136.6(12) . . ?
W4 O1 W5 98.5(7) . . ?
Ge1 O1 W6 115.3(8) . 2_866 ?
O2 O1 W6 127.4(11) . 2_866 ?
W4 O1 W6 96.3(8) . 2_866 ?
W5 O1 W6 94.1(7) . 2_866 ?
Ge1 O2 O1 57.6(10) . . ?
Ge1 O2 W4 123.6(11) . . ?
O1 O2 W4 65.9(9) . . ?
Ge1 O2 W1 121.6(10) . 2_866 ?
O1 O2 W1 135.7(13) . 2_866 ?
W4 O2 W1 97.8(8) . 2_866 ?
Ge1 O2 W2 117.2(11) . . ?
O1 O2 W2 126.0(11) . . ?
W4 O2 W2 95.3(7) . . ?
W1 O2 W2 95.0(8) 2_866 . ?
Ge1 O3 W1 122.4(8) . 2_866 ?
Ge1 O3 W5 122.0(10) . 2_866 ?
W1 O3 W5 101.5(8) 2_866 2_866 ?
Ge1 O3 W3 113.2(10) . 2_866 ?
W1 O3 W3 96.1(7) 2_866 2_866 ?
W5 O3 W3 95.8(6) 2_866 2_866 ?
Ge1 O4 W6 118.3(9) . . ?
Ge1 O4 W2 118.3(11) . . ?
W6 O4 W2 101.9(9) . . ?
Ge1 O4 W3 115.5(11) . . ?
W6 O4 W3 99.9(8) . . ?
W2 O4 W3 99.8(7) . . ?
W4 O5 W1 137.4(8) 2_866 . ?
W5 O8 W1 136.0(10) . . ?
W4 O9 W6 136.5(7) . 2_866 ?
W1 O10 W3 139.9(8) . . ?
W6 O11 Cu1 141.1(6) . . ?
W5 O12 W3 137.8(7) . . ?
W2 O14 W1 138.7(8) 2_866 . ?
W4 O15 W2 136.2(7) . . ?
W5 O16 W6 138.4(8) . 2_866 ?
W2 O18 W3 135.1(9) . . ?
W5 O19 W4 136.6(8) . . ?
W3 O20 W6 134.9(8) . . ?
W6 O21 W2 138.4(10) . . ?
N1 Cu1 N1 180.0 2_877 . ?
N1 Cu1 O24 96.6(4) 2_877 . ?
N1 Cu1 O24 83.4(4) . . ?
N1 Cu1 O24 83.4(4) 2_877 2_877 ?
N1 Cu1 O24 96.6(4) . 2_877 ?
O24 Cu1 O24 180.0 . 2_877 ?
N1 Cu1 O11 93.4(4) 2_877 2_877 ?
N1 Cu1 O11 86.6(4) . 2_877 ?
O24 Cu1 O11 95.1(4) . 2_877 ?
O24 Cu1 O11 84.9(4) 2_877 2_877 ?
N1 Cu1 O11 86.6(4) 2_877 . ?
N1 Cu1 O11 93.4(4) . . ?
O24 Cu1 O11 84.9(4) . . ?
O24 Cu1 O11 95.1(5) 2_877 . ?
O11 Cu1 O11 180.0 2_877 . ?
C6 O24 Cu1 114.1(10) . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Cu1 128.3(5) . . ?
C5 N1 Cu1 111.7(5) . . ?
C2 C1 N1 120.0 . . ?
C2 C1 H1A 120.0 . . ?
N1 C1 H1A 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 126.5(9) . . ?
N1 C5 C6 113.5(9) . . ?
O23 C6 O24 124.1(16) . . ?
O23 C6 C5 118.6(14) . . ?
O24 C6 C5 117.3(14) . . ?
C12 N5 H5A 120.0 . . ?
C12 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C11 N2 H2B 120.0 . . ?
C11 N2 H2C 120.0 . . ?
H2B N2 H2C 120.0 . . ?
C8 C7 C11 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C11 C7 H7A 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C9 C10 N3 120.0 . . ?
C9 C10 H10A 120.0 . . ?
N3 C10 H10A 120.0 . . ?
C11 N3 C10 120.0 . . ?
N2 C11 N3 123.4(13) . . ?
N2 C11 C7 116.2(13) . . ?
N3 C11 C7 120.0 . . ?
N5 C12 C13 124.3(12) . . ?
N5 C12 N4 115.6(12) . . ?
C13 C12 N4 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
N4 C16 C15 120.0 . . ?
N4 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 N4 C12 120.0 . . ?
C16 N4 H4B 120.0 . . ?
C12 N4 H4B 120.0 . . ?

_refine_diff_density_max         2.395
_refine_diff_density_min         -2.889
_refine_diff_density_rms         0.314

####################################################################### 
# 
# 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_shelx_3
_database_code_depnum_ccdc_archive 'CCDC 1056233'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT342_shelx_3             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0346 Ang

RESPONSE: The quality of this crystal was poor.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H36 Cu Mo12 N10 O44 Si'
_chemical_formula_weight         2507.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1938(13)
_cell_length_b                   12.7022(14)
_cell_length_c                   13.1616(15)
_cell_angle_alpha                110.302(2)
_cell_angle_beta                 98.157(2)
_cell_angle_gamma                111.880(2)
_cell_volume                     1547.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4167
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            dark_green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.691
_exptl_crystal_F_000             1197
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.811
_shelx_estimated_absorpt_T_min   0.457
_shelx_estimated_absorpt_T_max   0.552
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_T_max  0.561
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7773
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.736
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5412
_reflns_number_gt                4723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0604P)²+65.1497P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0054(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5412
_refine_ls_number_parameters     473
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0876
_refine_ls_wR_factor_ref         0.2250
_refine_ls_wR_factor_gt          0.2099
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.053
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo -0.31292(14) -0.14848(15) -0.21714(11) 0.0455(4) Uani 1 1 d . . . . .
Mo2 Mo -0.02094(18) 0.07165(14) -0.23619(11) 0.0510(5) Uani 1 1 d . . . . .
Mo3 Mo -0.29456(14) -0.20535(14) 0.02817(14) 0.0474(4) Uani 1 1 d . . . . .
Mo4 Mo -0.04652(18) -0.22433(16) -0.26983(11) 0.0574(5) Uani 1 1 d . . . . .
Mo5 Mo -0.25633(16) 0.09126(18) 0.04771(15) 0.0582(5) Uani 1 1 d . . . . .
Mo6 Mo 0.04909(19) 0.30467(15) 0.03994(16) 0.0605(5) Uani 1 1 d . . . . .
Cu1 Cu 0.0000 -0.5000 -0.5000 0.0430(7) Uani 1 2 d S . P . .
Si1 Si 0.0000 0.0000 0.0000 0.0320(12) Uani 1 2 d S . P . .
O1 O -0.0749(18) -0.0517(16) -0.1314(15) 0.027(4) Uani 0.5 1 d . . P . .
O2 O -0.1603(19) -0.0565(16) -0.0335(14) 0.030(4) Uani 0.5 1 d . . P . .
O3 O 0.0647(19) 0.1036(16) -0.0488(13) 0.028(4) Uani 0.5 1 d . . P . .
O4 O 0.0327(18) -0.1222(15) -0.0725(14) 0.025(4) Uani 0.5 1 d . . P . .
O5 O -0.4576(13) -0.2129(13) -0.3211(12) 0.075(4) Uani 1 1 d . . . . .
O6 O -0.2315(15) -0.2457(11) -0.2895(15) 0.080(5) Uani 1 1 d . . . . .
O7 O -0.3768(14) 0.1295(14) 0.0731(12) 0.067(4) Uani 1 1 d . . . . .
O8 O 0.0756(13) 0.4473(12) 0.0561(12) 0.061(3) Uani 1 1 d . . . . .
O9 O -0.0754(13) -0.3317(12) -0.3985(10) 0.059(3) Uani 1 1 d . . . . .
O10 O -0.0231(15) 0.1044(17) -0.3483(12) 0.081(5) Uani 1 1 d . . . . .
O11 O -0.0125(14) 0.2145(14) -0.1254(12) 0.085(5) Uani 1 1 d . . . . .
O12 O 0.0921(14) 0.329(2) 0.1913(15) 0.132(9) Uani 1 1 d . . . . .
O13 O -0.3161(18) -0.0596(13) 0.0703(10) 0.075(5) Uani 1 1 d . . . . .
O14 O 0.2199(16) 0.3175(16) 0.0365(13) 0.098(6) Uani 1 1 d . . . . .
O15 O -0.2019(16) -0.0209(12) -0.2620(16) 0.090(6) Uani 1 1 d . . . . .
O16 O -0.3286(19) -0.0113(13) -0.1103(11) 0.081(5) Uani 1 1 d . . . . .
O17 O -0.1799(16) -0.1499(15) 0.1724(14) 0.102(7) Uani 1 1 d . . . . .
O18 O -0.4370(14) -0.3045(14) 0.0334(11) 0.075(4) Uani 1 1 d . . . . .
O19 O 0.1362(15) -0.173(2) -0.2039(16) 0.133(10) Uani 1 1 d . . . . .
O20 O -0.3607(18) -0.2358(14) -0.1318(11) 0.075(5) Uani 1 1 d . . . . .
O21 O -0.0083(16) -0.0831(12) -0.2998(16) 0.084(5) Uani 1 1 d . . . . .
O22 O -0.1400(18) 0.2314(17) 0.0265(14) 0.094(5) Uani 1 1 d . U . . .
O23 O -0.1993(13) -0.6876(13) -0.3459(12) 0.070(4) Uani 1 1 d . . . . .
O24 O -0.1508(12) -0.6149(11) -0.4745(10) 0.053(3) Uani 1 1 d . . . . .
N1 N 0.1047(13) -0.4810(12) -0.3579(11) 0.041(3) Uani 1 1 d . . . . .
C6 C -0.1200(17) -0.6245(15) -0.3810(13) 0.044(4) Uani 1 1 d . . . . .
C15 C -0.542(2) -0.1500(17) -0.6252(14) 0.050(4) Uani 1 1 d . . . . .
H15A H -0.6141 -0.2086 -0.6158 0.060 Uiso 1 1 calc R U . . .
C14 C -0.421(3) -0.087(2) -0.5466(17) 0.066(6) Uani 1 1 d . . . . .
H14A H -0.4107 -0.1028 -0.4829 0.079 Uiso 1 1 calc R U . . .
N2 N 0.370(3) 0.3297(18) -0.2743(14) 0.086(6) Uani 1 1 d . . . . .
C5 C 0.0260(17) -0.5506(13) -0.3125(13) 0.041(4) Uani 1 1 d . . . . .
C13 C -0.312(3) -0.001(3) -0.555(2) 0.090(8) Uani 1 1 d . . . . .
H13A H -0.2296 0.0435 -0.4974 0.108 Uiso 1 1 calc R U . . .
C11 C 0.312(2) 0.304(2) -0.3841(17) 0.064(5) Uani 1 1 d . . . . .
C4 C 0.0816(19) -0.5567(16) -0.2128(15) 0.050(4) Uani 1 1 d . . . . .
H4A H 0.0282 -0.6086 -0.1848 0.060 Uiso 1 1 calc R U . . .
C1 C 0.2391(17) -0.4104(15) -0.3015(15) 0.050(4) Uani 1 1 d . . . . .
H1A H 0.2917 -0.3592 -0.3304 0.060 Uiso 1 1 calc R U . . .
C10 C 0.383(2) 0.348(2) -0.4470(15) 0.062(5) Uani 1 1 d . . . . .
H10A H 0.3383 0.3292 -0.5209 0.075 Uiso 1 1 calc R U . . .
N3 N 0.180(2) 0.226(2) -0.4323(18) 0.092(6) Uani 1 1 d . . . . .
H3B H 0.1413 0.2049 -0.5026 0.110 Uiso 1 1 calc R U . . .
H3C H 0.1328 0.1971 -0.3933 0.110 Uiso 1 1 calc R U . . .
C16 C -0.559(2) -0.130(2) -0.7138(18) 0.065(5) Uani 1 1 d . . . . .
N4 N -0.457(2) -0.041(2) -0.731(2) 0.097(7) Uani 1 1 d . . . . .
C3 C 0.221(2) -0.481(2) -0.1580(16) 0.062(5) Uani 1 1 d . . . . .
H3A H 0.2616 -0.4769 -0.0892 0.074 Uiso 1 1 calc R U . . .
C9 C 0.517(3) 0.419(2) -0.405(3) 0.104(9) Uani 1 1 d . . . . .
H9A H 0.5663 0.4432 -0.4513 0.125 Uiso 1 1 calc R U . . .
N5 N -0.690(2) -0.202(2) -0.795(2) 0.102(8) Uani 1 1 d . . . . .
H5A H -0.7536 -0.2562 -0.7829 0.122 Uiso 1 1 calc R U . . .
H5B H -0.7065 -0.1922 -0.8556 0.122 Uiso 1 1 calc R U . . .
C2 C 0.2992(18) -0.4103(17) -0.2082(17) 0.057(5) Uani 1 1 d . . . . .
H2A H 0.3928 -0.3641 -0.1754 0.069 Uiso 1 1 calc R U . . .
C12 C -0.329(3) 0.021(2) -0.657(3) 0.097(9) Uani 1 1 d . . . . .
H12A H -0.2561 0.0738 -0.6708 0.117 Uiso 1 1 calc R U . . .
C8 C 0.582(3) 0.456(2) -0.294(2) 0.087(7) Uani 1 1 d . . . . .
H8A H 0.6751 0.5086 -0.2632 0.104 Uiso 1 1 calc R U . . .
C7 C 0.511(3) 0.414(2) -0.2286(18) 0.093(9) Uani 1 1 d . . . . .
H7A H 0.5548 0.4417 -0.1522 0.111 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O5 1.665(11) . ?
Mo1 O20 1.837(13) . ?
Mo1 O6 1.880(13) . ?
Mo1 O16 1.908(12) . ?
Mo1 O15 1.972(13) . ?
Mo1 O2 2.346(17) . ?
Mo1 O1 2.372(18) . ?
Mo2 O10 1.665(11) . ?
Mo2 O15 1.832(14) . ?
Mo2 O11 1.851(13) . ?
Mo2 O21 1.919(13) . ?
Mo2 O17 1.992(15) 2 ?
Mo2 O3 2.348(15) . ?
Mo2 O1 2.398(17) . ?
Mo3 O18 1.652(12) . ?
Mo3 O13 1.858(12) . ?
Mo3 O17 1.858(15) . ?
Mo3 O14 1.923(14) 2 ?
Mo3 O20 1.977(12) . ?
Mo3 O3 2.334(19) 2 ?
Mo3 O2 2.406(19) . ?
Mo4 O9 1.657(11) . ?
Mo4 O19 1.862(16) . ?
Mo4 O21 1.878(14) . ?
Mo4 O12 1.918(15) 2 ?
Mo4 O6 1.951(15) . ?
Mo4 O4 2.316(16) . ?
Mo4 O1 2.478(17) . ?
Mo5 O7 1.633(13) . ?
Mo5 O16 1.880(14) . ?
Mo5 O22 1.914(16) . ?
Mo5 O13 1.925(13) . ?
Mo5 O19 1.952(15) 2 ?
Mo5 O4 2.339(18) 2 ?
Mo5 O2 2.501(19) . ?
Mo6 O8 1.653(12) . ?
Mo6 O14 1.866(16) . ?
Mo6 O12 1.868(15) . ?
Mo6 O22 1.921(17) . ?
Mo6 O11 1.944(14) . ?
Mo6 O4 2.369(16) 2 ?
Mo6 O3 2.498(17) . ?
Cu1 O24 1.938(12) 2_544 ?
Cu1 O24 1.938(12) . ?
Cu1 N1 1.945(13) . ?
Cu1 N1 1.945(13) 2_544 ?
Si1 O1 1.586(17) 2 ?
Si1 O1 1.586(17) . ?
Si1 O2 1.589(19) 2 ?
Si1 O2 1.589(19) . ?
Si1 O3 1.635(19) 2 ?
Si1 O3 1.635(19) . ?
Si1 O4 1.718(17) 2 ?
Si1 O4 1.718(17) . ?
O1 O2 1.71(3) . ?
O1 O3 1.80(2) . ?
O2 O3 1.81(2) 2 ?
O3 O2 1.81(2) 2 ?
O3 Mo3 2.334(19) 2 ?
O4 Mo5 2.339(18) 2 ?
O4 Mo6 2.369(16) 2 ?
O12 Mo4 1.918(15) 2 ?
O14 Mo3 1.923(14) 2 ?
O17 Mo2 1.992(15) 2 ?
O19 Mo5 1.951(15) 2 ?
O23 C6 1.22(2) . ?
O24 C6 1.289(19) . ?
N1 C1 1.35(2) . ?
N1 C5 1.36(2) . ?
C6 C5 1.49(2) . ?
C15 C16 1.28(3) . ?
C15 C14 1.33(3) . ?
C14 C13 1.35(3) . ?
N2 C11 1.37(3) . ?
N2 C7 1.42(3) . ?
C5 C4 1.41(2) . ?
C13 C12 1.47(4) . ?
C11 N3 1.33(3) . ?
C11 C10 1.35(3) . ?
C4 C3 1.40(3) . ?
C1 C2 1.31(3) . ?
C10 C9 1.34(3) . ?
C16 N4 1.39(3) . ?
C16 N5 1.42(3) . ?
N4 C12 1.36(3) . ?
C3 C2 1.41(3) . ?
C9 C8 1.36(3) . ?
C8 C7 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
O5 Mo1 O20 102.3(7) . . ?
O5 Mo1 O6 99.7(8) . . ?
O20 Mo1 O6 92.6(6) . . ?
O5 Mo1 O16 100.0(8) . . ?
O20 Mo1 O16 89.8(5) . . ?
O6 Mo1 O16 159.1(8) . . ?
O5 Mo1 O15 98.2(8) . . ?
O20 Mo1 O15 159.4(8) . . ?
O6 Mo1 O15 86.3(6) . . ?
O16 Mo1 O15 84.2(6) . . ?
O5 Mo1 O2 160.2(8) . . ?
O20 Mo1 O2 64.9(7) . . ?
O6 Mo1 O2 96.0(7) . . ?
O16 Mo1 O2 66.4(7) . . ?
O15 Mo1 O2 94.8(7) . . ?
O5 Mo1 O1 156.8(7) . . ?
O20 Mo1 O1 97.4(7) . . ?
O6 Mo1 O1 66.9(6) . . ?
O16 Mo1 O1 92.2(7) . . ?
O15 Mo1 O1 63.3(7) . . ?
O2 Mo1 O1 42.6(6) . . ?
O10 Mo2 O15 101.6(8) . . ?
O10 Mo2 O11 102.3(8) . . ?
O15 Mo2 O11 93.0(6) . . ?
O10 Mo2 O21 98.7(8) . . ?
O15 Mo2 O21 88.7(6) . . ?
O11 Mo2 O21 158.2(8) . . ?
O10 Mo2 O17 96.2(8) . 2 ?
O15 Mo2 O17 161.7(9) . 2 ?
O11 Mo2 O17 87.2(6) . 2 ?
O21 Mo2 O17 84.5(6) . 2 ?
O10 Mo2 O3 156.2(7) . . ?
O15 Mo2 O3 99.7(8) . . ?
O11 Mo2 O3 65.9(6) . . ?
O21 Mo2 O3 92.3(7) . . ?
O17 Mo2 O3 63.8(8) 2 . ?
O10 Mo2 O1 158.5(7) . . ?
O15 Mo2 O1 64.5(7) . . ?
O11 Mo2 O1 95.1(7) . . ?
O21 Mo2 O1 66.1(6) . . ?
O17 Mo2 O1 97.3(8) 2 . ?
O3 Mo2 O1 44.6(6) . . ?
O18 Mo3 O13 101.2(8) . . ?
O18 Mo3 O17 100.4(8) . . ?
O13 Mo3 O17 92.7(6) . . ?
O18 Mo3 O14 100.7(9) . 2 ?
O13 Mo3 O14 157.0(8) . 2 ?
O17 Mo3 O14 90.2(6) . 2 ?
O18 Mo3 O20 97.7(7) . . ?
O13 Mo3 O20 87.1(5) . . ?
O17 Mo3 O20 161.7(8) . . ?
O14 Mo3 O20 83.1(6) 2 . ?
O18 Mo3 O3 159.6(7) . 2 ?
O13 Mo3 O3 94.7(7) . 2 ?
O17 Mo3 O3 65.9(8) . 2 ?
O14 Mo3 O3 65.9(7) 2 2 ?
O20 Mo3 O3 95.8(6) . 2 ?
O18 Mo3 O2 155.1(7) . . ?
O13 Mo3 O2 65.8(6) . . ?
O17 Mo3 O2 101.4(8) . . ?
O14 Mo3 O2 91.3(8) 2 . ?
O20 Mo3 O2 61.9(6) . . ?
O3 Mo3 O2 44.9(6) 2 . ?
O9 Mo4 O19 100.8(9) . . ?
O9 Mo4 O21 99.8(7) . . ?
O19 Mo4 O21 92.5(8) . . ?
O9 Mo4 O12 100.2(9) . 2 ?
O19 Mo4 O12 89.2(6) . 2 ?
O21 Mo4 O12 159.2(9) . 2 ?
O9 Mo4 O6 97.1(7) . . ?
O19 Mo4 O6 161.9(9) . . ?
O21 Mo4 O6 87.2(6) . . ?
O12 Mo4 O6 84.8(7) 2 . ?
O9 Mo4 O4 156.6(6) . . ?
O19 Mo4 O4 64.3(8) . . ?
O21 Mo4 O4 98.8(7) . . ?
O12 Mo4 O4 63.4(8) 2 . ?
O6 Mo4 O4 97.8(7) . . ?
O9 Mo4 O1 154.7(6) . . ?
O19 Mo4 O1 99.9(9) . . ?
O21 Mo4 O1 64.8(6) . . ?
O12 Mo4 O1 94.4(9) 2 . ?
O6 Mo4 O1 63.7(6) . . ?
O4 Mo4 O1 48.3(6) . . ?
O7 Mo5 O16 101.3(7) . . ?
O7 Mo5 O22 101.0(8) . . ?
O16 Mo5 O22 91.8(7) . . ?
O7 Mo5 O13 99.3(7) . . ?
O16 Mo5 O13 88.3(5) . . ?
O22 Mo5 O13 159.2(8) . . ?
O7 Mo5 O19 98.7(9) . 2 ?
O16 Mo5 O19 159.6(9) . 2 ?
O22 Mo5 O19 88.0(7) . 2 ?
O13 Mo5 O19 84.8(7) . 2 ?
O7 Mo5 O4 155.8(7) . 2 ?
O16 Mo5 O4 98.8(7) . 2 ?
O22 Mo5 O4 65.0(7) . 2 ?
O13 Mo5 O4 94.4(6) . 2 ?
O19 Mo5 O4 62.7(8) 2 2 ?
O7 Mo5 O2 155.3(7) . . ?
O16 Mo5 O2 63.3(6) . . ?
O22 Mo5 O2 98.7(7) . . ?
O13 Mo5 O2 62.9(6) . . ?
O19 Mo5 O2 96.5(9) 2 . ?
O4 Mo5 O2 48.4(6) 2 . ?
O8 Mo6 O14 99.3(7) . . ?
O8 Mo6 O12 101.5(9) . . ?
O14 Mo6 O12 90.2(8) . . ?
O8 Mo6 O22 100.3(7) . . ?
O14 Mo6 O22 160.1(8) . . ?
O12 Mo6 O22 89.6(7) . . ?
O8 Mo6 O11 100.5(7) . . ?
O14 Mo6 O11 87.7(6) . . ?
O12 Mo6 O11 157.9(9) . . ?
O22 Mo6 O11 85.0(7) . . ?
O8 Mo6 O4 156.7(6) . 2 ?
O14 Mo6 O4 98.1(8) . 2 ?
O12 Mo6 O4 62.9(8) . 2 ?
O22 Mo6 O4 64.3(7) . 2 ?
O11 Mo6 O4 95.7(7) . 2 ?
O8 Mo6 O3 153.5(7) . . ?
O14 Mo6 O3 62.9(7) . . ?
O12 Mo6 O3 98.1(9) . . ?
O22 Mo6 O3 97.4(7) . . ?
O11 Mo6 O3 61.6(6) . . ?
O4 Mo6 O3 49.8(6) 2 . ?
O24 Cu1 O24 180.0 2_544 . ?
O24 Cu1 N1 96.0(5) 2_544 . ?
O24 Cu1 N1 84.0(5) . . ?
O24 Cu1 N1 84.0(5) 2_544 2_544 ?
O24 Cu1 N1 96.0(5) . 2_544 ?
N1 Cu1 N1 180.0 . 2_544 ?
O1 Si1 O1 180.0 2 . ?
O1 Si1 O2 65.3(9) 2 2 ?
O1 Si1 O2 114.7(9) . 2 ?
O1 Si1 O2 114.6(9) 2 . ?
O1 Si1 O2 65.4(9) . . ?
O2 Si1 O2 180.0 2 . ?
O1 Si1 O3 68.0(8) 2 2 ?
O1 Si1 O3 112.0(8) . 2 ?
O2 Si1 O3 111.7(9) 2 2 ?
O2 Si1 O3 68.3(9) . 2 ?
O1 Si1 O3 112.0(8) 2 . ?
O1 Si1 O3 68.0(8) . . ?
O2 Si1 O3 68.3(9) 2 . ?
O2 Si1 O3 111.7(9) . . ?
O3 Si1 O3 180.0 2 . ?
O1 Si1 O4 73.0(8) 2 2 ?
O1 Si1 O4 107.0(8) . 2 ?
O2 Si1 O4 106.1(9) 2 2 ?
O2 Si1 O4 73.9(9) . 2 ?
O3 Si1 O4 104.5(8) 2 2 ?
O3 Si1 O4 75.5(8) . 2 ?
O1 Si1 O4 107.0(8) 2 . ?
O1 Si1 O4 73.0(8) . . ?
O2 Si1 O4 73.9(9) 2 . ?
O2 Si1 O4 106.1(9) . . ?
O3 Si1 O4 75.5(8) 2 . ?
O3 Si1 O4 104.5(8) . . ?
O4 Si1 O4 180.0 2 . ?
Si1 O1 O2 57.4(8) . . ?
Si1 O1 O3 57.3(8) . . ?
O2 O1 O3 98.8(12) . . ?
Si1 O1 Mo1 125.3(10) . . ?
O2 O1 Mo1 67.9(8) . . ?
O3 O1 Mo1 139.4(10) . . ?
Si1 O1 Mo2 123.5(9) . . ?
O2 O1 Mo2 135.0(11) . . ?
O3 O1 Mo2 66.2(7) . . ?
Mo1 O1 Mo2 95.5(6) . . ?
Si1 O1 Mo4 118.0(9) . . ?
O2 O1 Mo4 128.7(10) . . ?
O3 O1 Mo4 121.6(11) . . ?
Mo1 O1 Mo4 93.9(6) . . ?
Mo2 O1 Mo4 92.5(6) . . ?
Si1 O2 O1 57.2(9) . . ?
Si1 O2 O3 57.1(9) . 2 ?
O1 O2 O3 98.5(13) . 2 ?
Si1 O2 Mo1 126.7(10) . . ?
O1 O2 Mo1 69.5(8) . . ?
O3 O2 Mo1 136.8(10) 2 . ?
Si1 O2 Mo3 122.5(9) . . ?
O1 O2 Mo3 139.5(11) . . ?
O3 O2 Mo3 65.5(8) 2 . ?
Mo1 O2 Mo3 96.3(6) . . ?
Si1 O2 Mo5 117.5(9) . . ?
O1 O2 Mo5 125.0(11) . . ?
O3 O2 Mo5 124.8(10) 2 . ?
Mo1 O2 Mo5 93.1(6) . . ?
Mo3 O2 Mo5 92.3(7) . . ?
Si1 O3 O1 54.7(8) . . ?
Si1 O3 O2 54.7(8) . 2 ?
O1 O3 O2 95.5(11) . 2 ?
Si1 O3 Mo3 124.3(9) . 2 ?
O1 O3 Mo3 137.3(11) . 2 ?
O2 O3 Mo3 69.7(8) 2 2 ?
Si1 O3 Mo2 123.8(9) . . ?
O1 O3 Mo2 69.2(7) . . ?
O2 O3 Mo2 141.9(11) 2 . ?
Mo3 O3 Mo2 97.6(7) 2 . ?
Si1 O3 Mo6 115.9(9) . . ?
O1 O3 Mo6 126.6(11) . . ?
O2 O3 Mo6 121.7(9) 2 . ?
Mo3 O3 Mo6 93.7(6) 2 . ?
Mo2 O3 Mo6 94.0(6) . . ?
Si1 O4 Mo4 120.5(8) . . ?
Si1 O4 Mo5 120.1(8) . 2 ?
Mo4 O4 Mo5 98.2(6) . 2 ?
Si1 O4 Mo6 118.7(8) . 2 ?
Mo4 O4 Mo6 97.2(6) . 2 ?
Mo5 O4 Mo6 97.0(6) 2 2 ?
Mo1 O6 Mo4 135.4(8) . . ?
Mo2 O11 Mo6 138.4(8) . . ?
Mo6 O12 Mo4 136.2(12) . 2 ?
Mo3 O13 Mo5 138.8(8) . . ?
Mo6 O14 Mo3 137.2(9) . 2 ?
Mo2 O15 Mo1 136.4(11) . . ?
Mo5 O16 Mo1 136.7(9) . . ?
Mo3 O17 Mo2 132.4(12) . 2 ?
Mo4 O19 Mo5 134.7(13) . 2 ?
Mo1 O20 Mo3 136.3(10) . . ?
Mo4 O21 Mo2 136.3(8) . . ?
Mo5 O22 Mo6 133.7(10) . . ?
C6 O24 Cu1 114.5(10) . . ?
C1 N1 C5 118.4(14) . . ?
C1 N1 Cu1 129.5(12) . . ?
C5 N1 Cu1 112.1(10) . . ?
O23 C6 O24 125.7(16) . . ?
O23 C6 C5 119.0(15) . . ?
O24 C6 C5 115.3(14) . . ?
C16 C15 C14 120(2) . . ?
C15 C14 C13 123(2) . . ?
C11 N2 C7 114.7(19) . . ?
N1 C5 C4 121.9(15) . . ?
N1 C5 C6 114.1(14) . . ?
C4 C5 C6 123.8(15) . . ?
C14 C13 C12 118(2) . . ?
N3 C11 C10 119.0(19) . . ?
N3 C11 N2 118.0(19) . . ?
C10 C11 N2 123(2) . . ?
C3 C4 C5 116.8(16) . . ?
C2 C1 N1 123.6(18) . . ?
C9 C10 C11 121(2) . . ?
C15 C16 N4 123(2) . . ?
C15 C16 N5 117(2) . . ?
N4 C16 N5 120(2) . . ?
C12 N4 C16 120(2) . . ?
C4 C3 C2 119.5(16) . . ?
C10 C9 C8 120(3) . . ?
C1 C2 C3 119.6(17) . . ?
N4 C12 C13 116(2) . . ?
C9 C8 C7 120(2) . . ?
C8 C7 N2 121.7(19) . . ?

_refine_diff_density_max         1.734
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.336

####################################################################### 
# 
# 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_shelx_4
_database_code_depnum_ccdc_archive 'CCDC 1056234'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT430_shelx_4             
;
PROBLEM: Short Inter D...A Contact  Ow2..O26  .. 2.59 Ang.

RESPONSE: There should be a strong hydron bond between 
the two atoms.
;

# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H31 Cu2.50 Mo12 N7 O43.50 Si'
_chemical_formula_weight         2595.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.8585(7)
_cell_length_b                   21.4521(11)
_cell_length_c                   21.8852(12)
_cell_angle_alpha                90
_cell_angle_beta                 100.3010(10)
_cell_angle_gamma                90
_cell_volume                     6401.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7768
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.94

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_F_000             4938
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.202
_shelx_estimated_absorpt_T_min   0.418
_shelx_estimated_absorpt_T_max   0.645
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40823
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.340
_diffrn_reflns_theta_max         28.427
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15828
_reflns_number_gt                10485
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15828
_refine_ls_number_parameters     925
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.05479(5) 0.10918(3) 0.87662(3) 0.02977(16) Uani 1 1 d . . . . .
Mo2 Mo -0.16585(5) 0.28040(4) 0.88947(3) 0.03559(18) Uani 1 1 d . . . . .
Mo3 Mo 0.24019(5) 0.19907(4) 0.85033(3) 0.03417(17) Uani 1 1 d . . . . .
Mo4 Mo 0.19124(5) 0.35104(3) 0.77193(3) 0.03214(16) Uani 1 1 d . . . . .
Mo5 Mo -0.19968(5) 0.14990(3) 0.80497(4) 0.03494(17) Uani 1 1 d . . . . .
Mo6 Mo -0.24624(5) 0.28711(4) 0.73503(3) 0.03361(17) Uani 1 1 d . . . . .
Mo7 Mo 0.02873(6) 0.39052(3) 0.86155(3) 0.03687(18) Uani 1 1 d . . . . .
Mo8 Mo -0.02148(6) 0.10404(3) 0.70537(3) 0.03534(18) Uani 1 1 d . . . . .
Mo9 Mo 0.15202(5) 0.20445(4) 0.68064(3) 0.03789(19) Uani 1 1 d . . . . .
Mo10 Mo 0.09741(6) 0.24597(4) 0.94955(3) 0.03823(19) Uani 1 1 d . . . . .
Mo11 Mo -0.08620(6) 0.23523(4) 0.62702(3) 0.03979(19) Uani 1 1 d . . . . .
Mo12 Mo -0.03844(6) 0.38728(4) 0.70614(4) 0.0458(2) Uani 1 1 d . . . . .
Cu1 Cu -0.16864(7) -0.02105(5) 0.61452(5) 0.0336(2) Uani 1 1 d . . . . .
Cu2 Cu 0.30548(7) 0.03962(5) 0.92597(5) 0.0365(2) Uani 1 1 d . . . . .
Si1 Si 0.00018(13) 0.24473(8) 0.78825(8) 0.0190(4) Uani 1 1 d . . . . .
O1 O 0.0719(3) 0.2106(2) 0.8454(2) 0.0196(9) Uani 1 1 d . . . . .
O2 O 0.0077(3) 0.2089(2) 0.7240(2) 0.0234(10) Uani 1 1 d . . . . .
O3 O -0.1120(3) 0.2420(2) 0.8004(2) 0.0209(10) Uani 1 1 d . . . . .
O4 O 0.0333(3) 0.3172(2) 0.7840(2) 0.0235(10) Uani 1 1 d . . . . .
O5 O -0.0884(4) 0.3562(2) 0.8734(2) 0.0322(12) Uani 1 1 d . . . . .
O6 O -0.0459(4) 0.3200(2) 0.6516(2) 0.0337(12) Uani 1 1 d . . . . .
O7 O 0.0395(3) 0.0916(2) 0.7872(2) 0.0276(11) Uani 1 1 d . . . . .
O8 O -0.0469(4) 0.0302(2) 0.6789(3) 0.0364(13) Uani 1 1 d . . . . .
O9 O 0.2368(4) 0.2859(2) 0.8276(2) 0.0280(11) Uani 1 1 d . . . . .
O10 O -0.0902(4) 0.1480(2) 0.6312(2) 0.0315(12) Uani 1 1 d . . . . .
O11 O -0.0808(3) 0.1239(2) 0.8607(2) 0.0275(11) Uani 1 1 d . . . . .
O12 O -0.1896(4) 0.2474(2) 0.6691(2) 0.0303(12) Uani 1 1 d . . . . .
O13 O 0.0932(4) 0.3267(2) 0.9157(2) 0.0298(11) Uani 1 1 d . . . . .
O14 O -0.0498(4) 0.2526(2) 0.9339(2) 0.0304(12) Uani 1 1 d . . . . .
O15 O -0.1391(4) 0.1218(2) 0.7412(2) 0.0285(11) Uani 1 1 d . . . . .
O16 O 0.0713(3) 0.1554(2) 0.9508(2) 0.0274(11) Uani 1 1 d . . . . .
O17 O 0.1960(3) 0.1192(2) 0.8763(2) 0.0247(10) Uani 1 1 d . . . . .
O18 O 0.2213(4) 0.2287(2) 0.9329(2) 0.0302(12) Uani 1 1 d . . . . .
O19 O 0.2116(4) 0.1802(2) 0.7674(2) 0.0296(11) Uani 1 1 d . . . . .
O20 O 0.0954(4) 0.1189(2) 0.6772(2) 0.0300(12) Uani 1 1 d . . . . .
O21 O 0.2455(4) 0.1890(3) 0.6438(3) 0.0528(18) Uani 1 1 d . . . . .
O22 O -0.1363(5) 0.2476(3) 0.5521(3) 0.0495(17) Uani 1 1 d . . . . .
O23 O 0.1210(5) 0.2588(3) 1.0261(3) 0.0493(17) Uani 1 1 d . . . . .
O24 O 0.3625(4) 0.1882(3) 0.8677(3) 0.0409(14) Uani 1 1 d . . . . .
O25 O -0.3545(4) 0.3125(3) 0.6952(3) 0.0421(14) Uani 1 1 d . . . . .
O26 O -0.0265(4) 0.4306(2) 0.7856(3) 0.0376(13) Uani 1 1 d . . . . .
O27 O 0.0533(4) 0.2255(3) 0.6150(2) 0.0337(12) Uani 1 1 d . . . . .
O28 O 0.2961(4) 0.3849(3) 0.7602(3) 0.0404(14) Uani 1 1 d . . . . .
O29 O -0.2591(3) 0.3116(2) 0.8167(2) 0.0294(11) Uani 1 1 d . . . . .
O30 O 0.0435(5) 0.4524(3) 0.9105(3) 0.0443(15) Uani 1 1 d . . . . .
O31 O -0.2875(4) 0.2031(2) 0.7540(2) 0.0302(11) Uani 1 1 d . . . . .
O32 O -0.1625(4) 0.3542(2) 0.7258(2) 0.0315(12) Uani 1 1 d . . . . .
O33 O 0.0567(4) 0.0356(2) 0.9034(3) 0.0380(13) Uani 1 1 d . . . . .
O34 O -0.2749(4) 0.0906(3) 0.8159(3) 0.0426(15) Uani 1 1 d . . . . .
O35 O 0.0982(4) 0.3975(2) 0.7101(2) 0.0347(13) Uani 1 1 d . . . . .
O36 O -0.2241(4) 0.2024(2) 0.8764(2) 0.0315(12) Uani 1 1 d . . . . .
O37 O 0.1775(4) 0.2846(2) 0.7080(2) 0.0324(12) Uani 1 1 d . . . . .
O38 O -0.0810(5) 0.4460(3) 0.6580(3) 0.0541(18) Uani 1 1 d . . . . .
O39 O 0.1586(4) 0.4011(2) 0.8336(2) 0.0305(12) Uani 1 1 d . . . . .
O40 O -0.2243(4) 0.3090(3) 0.9445(3) 0.0471(16) Uani 1 1 d . . . . .
N6 N 0.3476(5) 0.0403(3) 0.8453(3) 0.0343(15) Uani 1 1 d . . . . .
N3 N 0.2346(5) -0.0428(3) 0.9286(3) 0.0309(14) Uani 1 1 d . . . . .
N4 N 0.2507(5) 0.0546(3) 1.0008(3) 0.0303(14) Uani 1 1 d . . . . .
N1 N -0.0924(5) -0.0931(3) 0.5935(4) 0.0455(19) Uani 1 1 d . . . . .
N5 N 0.4394(5) 0.0780(3) 0.9532(3) 0.0389(16) Uani 1 1 d . . . . .
N2 N -0.1480(5) 0.0079(4) 0.5316(3) 0.0460(19) Uani 1 1 d . . . . .
C15 C 0.1903(6) -0.0481(4) 0.9787(4) 0.0331(17) Uani 1 1 d . . . . .
C20 C 0.2547(6) 0.1091(4) 1.0310(4) 0.0379(19) Uani 1 1 d . . . . .
H20A H 0.2898 0.1419 1.0178 0.046 Uiso 1 1 calc R U . . .
C16 C 0.2003(5) 0.0066(4) 1.0203(3) 0.0311(17) Uani 1 1 d . . . . .
C26 C 0.4368(6) 0.0658(4) 0.8446(4) 0.0353(18) Uani 1 1 d . . . . .
C11 C 0.1375(7) -0.1015(4) 0.9883(4) 0.046(2) Uani 1 1 d . . . . .
H11A H 0.1086 -0.1050 1.0233 0.055 Uiso 1 1 calc R U . . .
C27 C 0.4704(7) 0.0743(5) 0.7908(4) 0.050(2) Uani 1 1 d . . . . .
H27A H 0.5329 0.0904 0.7915 0.060 Uiso 1 1 calc R U . . .
C30 C 0.2896(7) 0.0270(4) 0.7907(4) 0.044(2) Uani 1 1 d . . . . .
H30A H 0.2273 0.0111 0.7911 0.053 Uiso 1 1 calc R U . . .
C19 C 0.2092(6) 0.1183(4) 1.0804(4) 0.042(2) Uani 1 1 d . . . . .
H19A H 0.2096 0.1573 1.0989 0.051 Uiso 1 1 calc R U . . .
C17 C 0.1564(7) 0.0121(5) 1.0718(4) 0.046(2) Uani 1 1 d . . . . .
H17A H 0.1235 -0.0216 1.0852 0.055 Uiso 1 1 calc R U . . .
C29 C 0.3186(8) 0.0360(4) 0.7340(4) 0.050(2) Uani 1 1 d . . . . .
H29A H 0.2770 0.0269 0.6968 0.060 Uiso 1 1 calc R U . . .
C28 C 0.4123(8) 0.0591(5) 0.7350(4) 0.053(3) Uani 1 1 d . . . . .
H28A H 0.4358 0.0643 0.6981 0.064 Uiso 1 1 calc R U . . .
C14 C 0.2273(7) -0.0894(4) 0.8885(4) 0.045(2) Uani 1 1 d . . . . .
H14A H 0.2595 -0.0860 0.8548 0.054 Uiso 1 1 calc R U . . .
C25 C 0.4881(6) 0.0872(4) 0.9066(4) 0.0378(19) Uani 1 1 d . . . . .
C21 C 0.4768(6) 0.1002(5) 1.0089(4) 0.046(2) Uani 1 1 d . . . . .
H21A H 0.4446 0.0918 1.0418 0.056 Uiso 1 1 calc R U . . .
C5 C -0.0850(7) -0.0931(5) 0.5317(5) 0.057(3) Uani 1 1 d . . . . .
C22 C 0.5624(7) 0.1358(5) 1.0203(5) 0.060(3) Uani 1 1 d . . . . .
H22A H 0.5851 0.1521 1.0596 0.072 Uiso 1 1 calc R U . . .
C24 C 0.5759(6) 0.1198(5) 0.9153(5) 0.055(3) Uani 1 1 d . . . . .
H24A H 0.6100 0.1238 0.8826 0.065 Uiso 1 1 calc R U . . .
C1 C -0.0572(7) -0.1402(5) 0.6316(7) 0.070(3) Uani 1 1 d . . . . .
H1A H -0.0637 -0.1393 0.6731 0.084 Uiso 1 1 calc R U . . .
C10 C -0.1742(7) 0.0628(6) 0.5052(5) 0.057(3) Uani 1 1 d . . . . .
H10A H -0.1957 0.0938 0.5293 0.068 Uiso 1 1 calc R U . . .
C18 C 0.1618(7) 0.0679(5) 1.1029(4) 0.054(3) Uani 1 1 d . . . . .
H18A H 0.1343 0.0722 1.1384 0.065 Uiso 1 1 calc R U . . .
C13 C 0.1747(8) -0.1425(4) 0.8942(5) 0.055(3) Uani 1 1 d . . . . .
H13A H 0.1696 -0.1739 0.8645 0.066 Uiso 1 1 calc R U . . .
C6 C -0.1172(7) -0.0366(6) 0.4971(5) 0.059(3) Uani 1 1 d . . . . .
C23 C 0.6133(7) 0.1465(6) 0.9722(6) 0.067(3) Uani 1 1 d . . . . .
H23A H 0.6700 0.1705 0.9779 0.080 Uiso 1 1 calc R U . . .
C8 C -0.1414(10) 0.0301(10) 0.4093(6) 0.101(6) Uani 1 1 d . . . . .
H8A H -0.1407 0.0370 0.3674 0.121 Uiso 1 1 calc R U . . .
C12 C 0.1289(8) -0.1483(5) 0.9459(5) 0.058(3) Uani 1 1 d . . . . .
H12A H 0.0928 -0.1838 0.9512 0.070 Uiso 1 1 calc R U . . .
C7 C -0.1126(9) -0.0252(8) 0.4347(6) 0.080(4) Uani 1 1 d . . . . .
H7A H -0.0897 -0.0560 0.4110 0.095 Uiso 1 1 calc R U . . .
C4 C -0.0440(9) -0.1437(7) 0.5080(8) 0.094(5) Uani 1 1 d . . . . .
H4A H -0.0400 -0.1454 0.4660 0.113 Uiso 1 1 calc R U . . .
C3 C -0.0081(10) -0.1931(7) 0.5478(10) 0.108(7) Uani 1 1 d . . . . .
H3A H 0.0179 -0.2281 0.5317 0.130 Uiso 1 1 calc R U . . .
C9 C -0.1712(8) 0.0758(8) 0.4441(6) 0.084(5) Uani 1 1 d . . . . .
H9A H -0.1892 0.1148 0.4272 0.101 Uiso 1 1 calc R U . . .
C2 C -0.0106(10) -0.1906(6) 0.6082(9) 0.096(5) Uani 1 1 d . . . . .
H2A H 0.0182 -0.2220 0.6347 0.116 Uiso 1 1 calc R U . . .
C36 C -0.4206(5) 0.0881(3) 0.5879(3) 0.0269(15) Uani 1 1 d . . . . .
C35 C -0.3445(5) 0.0392(3) 0.5849(3) 0.0283(16) Uani 1 1 d . . . . .
C33 C -0.4065(7) 0.1386(4) 0.6270(4) 0.042(2) Uani 1 1 d . . . . .
H33A H -0.3475 0.1446 0.6541 0.051 Uiso 1 1 calc R U . . .
C31 C -0.4836(7) 0.1806(4) 0.6244(4) 0.046(2) Uani 1 1 d . . . . .
H31A H -0.4769 0.2151 0.6507 0.055 Uiso 1 1 calc R U . . .
C32 C -0.5683(6) 0.1715(4) 0.5839(4) 0.041(2) Uani 1 1 d . . . . .
H32A H -0.6199 0.1995 0.5821 0.049 Uiso 1 1 calc R U . . .
C34 C -0.5777(6) 0.1188(4) 0.5443(4) 0.0352(18) Uani 1 1 d . . . . .
H34A H -0.6360 0.1122 0.5165 0.042 Uiso 1 1 calc R U . . .
N7 N -0.5039(4) 0.0787(3) 0.5464(3) 0.0276(13) Uani 1 1 d . . . . .
OW2 O -0.1713(15) 0.5084(8) 0.7717(9) 0.118(8) Uani 0.5 1 d . . P . .
O41 O -0.3641(4) -0.0048(2) 0.5475(2) 0.0307(12) Uani 1 1 d . . . . .
O42 O -0.2629(4) 0.0451(3) 0.6214(3) 0.0445(15) Uani 1 1 d . . . . .
OW1 O -0.2053(5) -0.0612(3) 0.6874(3) 0.0595(19) Uani 1 1 d . . . . .
HW1A H -0.2088 -0.0454 0.7227 0.089 Uiso 1 1 d R U . . .
HW1B H -0.2137 -0.0999 0.6935 0.089 Uiso 1 1 d R U . . .
Cu3 Cu -0.5000 0.0000 0.5000 0.0263(3) Uani 1 2 d S . 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 O33 1.682(5) . ?
Mo1 O11 1.876(5) . ?
Mo1 O16 1.880(5) . ?
Mo1 O7 1.968(5) . ?
Mo1 O17 1.970(5) . ?
Mo1 O1 2.305(4) . ?
Mo2 O40 1.683(6) . ?
Mo2 O14 1.825(5) . ?
Mo2 O36 1.858(5) . ?
Mo2 O29 1.979(5) . ?
Mo2 O5 2.014(5) . ?
Mo2 O3 2.356(5) . ?
Mo3 O24 1.686(5) . ?
Mo3 O19 1.833(5) . ?
Mo3 O9 1.926(5) . ?
Mo3 O17 1.939(5) . ?
Mo3 O18 1.977(5) . ?
Mo3 O1 2.329(4) . ?
Mo4 O28 1.685(5) . ?
Mo4 O39 1.843(5) . ?
Mo4 O9 1.888(5) . ?
Mo4 O35 1.965(5) . ?
Mo4 O37 1.982(5) . ?
Mo4 O4 2.365(5) . ?
Mo5 O34 1.688(5) . ?
Mo5 O15 1.854(5) . ?
Mo5 O31 1.882(5) . ?
Mo5 O11 1.948(5) . ?
Mo5 O36 2.003(5) . ?
Mo5 O3 2.332(5) . ?
Mo6 O25 1.686(5) . ?
Mo6 O32 1.882(5) . ?
Mo6 O29 1.902(5) . ?
Mo6 O12 1.957(5) . ?
Mo6 O31 1.958(5) . ?
Mo6 O3 2.343(4) . ?
Mo7 O30 1.695(5) . ?
Mo7 O5 1.842(5) . ?
Mo7 O26 1.907(5) . ?
Mo7 O13 1.923(5) . ?
Mo7 O39 2.015(5) . ?
Mo7 O4 2.323(5) . ?
Mo8 O8 1.702(5) . ?
Mo8 O7 1.857(5) . ?
Mo8 O20 1.861(5) . ?
Mo8 O15 1.968(5) . ?
Mo8 O10 1.969(5) . ?
Mo8 O2 2.309(5) . ?
Mo9 O21 1.677(6) . ?
Mo9 O37 1.835(5) . ?
Mo9 O27 1.853(5) . ?
Mo9 O20 1.993(5) . ?
Mo9 O19 1.999(5) . ?
Mo9 O2 2.364(5) . ?
Mo10 O23 1.670(6) . ?
Mo10 O18 1.855(5) . ?
Mo10 O13 1.880(5) . ?
Mo10 O16 1.979(5) . ?
Mo10 O14 2.012(5) . ?
Mo10 O1 2.368(4) . ?
Mo11 O22 1.683(5) . ?
Mo11 O12 1.855(5) . ?
Mo11 O10 1.875(5) . ?
Mo11 O6 1.948(5) . ?
Mo11 O27 2.008(5) . ?
Mo11 O2 2.350(5) . ?
Mo12 O38 1.680(6) . ?
Mo12 O6 1.865(5) . ?
Mo12 O35 1.893(5) . ?
Mo12 O26 1.952(6) . ?
Mo12 O32 1.977(5) . ?
Mo12 O4 2.356(5) . ?
Cu1 O42 1.952(6) . ?
Cu1 OW1 1.957(6) . ?
Cu1 N1 1.973(7) . ?
Cu1 N2 1.987(8) . ?
Cu1 O8 2.278(5) . ?
Cu2 N4 1.950(6) . ?
Cu2 N6 1.957(7) . ?
Cu2 N5 2.020(7) . ?
Cu2 N3 2.029(6) . ?
Cu2 O17 2.410(5) . ?
Si1 O2 1.622(5) . ?
Si1 O3 1.625(5) . ?
Si1 O1 1.626(5) . ?
Si1 O4 1.628(5) . ?
O30 Cu3 2.380(5) 2_456 ?
N6 C30 1.345(10) . ?
N6 C26 1.354(10) . ?
N3 C14 1.323(10) . ?
N3 C15 1.353(9) . ?
N4 C20 1.341(10) . ?
N4 C16 1.354(10) . ?
N1 C1 1.344(14) . ?
N1 C5 1.374(13) . ?
N5 C21 1.325(11) . ?
N5 C25 1.334(10) . ?
N2 C10 1.333(13) . ?
N2 C6 1.333(12) . ?
C15 C11 1.395(11) . ?
C15 C16 1.478(11) . ?
C20 C19 1.359(11) . ?
C16 C17 1.378(11) . ?
C26 C27 1.355(11) . ?
C26 C25 1.487(11) . ?
C11 C12 1.357(13) . ?
C27 C28 1.376(13) . ?
C30 C29 1.385(12) . ?
C19 C18 1.398(13) . ?
C17 C18 1.373(13) . ?
C29 C28 1.386(14) . ?
C14 C13 1.370(12) . ?
C25 C24 1.387(12) . ?
C21 C22 1.395(13) . ?
C5 C4 1.369(14) . ?
C5 C6 1.457(16) . ?
C22 C23 1.387(15) . ?
C24 C23 1.383(14) . ?
C1 C2 1.402(16) . ?
C10 C9 1.374(14) . ?
C13 C12 1.398(13) . ?
C6 C7 1.399(16) . ?
C8 C7 1.34(2) . ?
C8 C9 1.35(2) . ?
C4 C3 1.41(2) . ?
C3 C2 1.33(2) . ?
C36 N7 1.350(9) . ?
C36 C33 1.373(10) . ?
C36 C35 1.497(10) . ?
C35 O41 1.246(8) . ?
C35 O42 1.269(8) . ?
C33 C31 1.391(12) . ?
C31 C32 1.353(12) . ?
C32 C34 1.417(11) . ?
C34 N7 1.332(9) . ?
N7 Cu3 1.975(6) . ?
O41 Cu3 1.984(5) . ?
Cu3 N7 1.975(6) 3_456 ?
Cu3 O41 1.984(5) 3_456 ?
Cu3 O30 2.380(5) 4_565 ?
Cu3 O30 2.380(5) 2_446 ?

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
O33 Mo1 O11 100.1(2) . . ?
O33 Mo1 O16 101.6(3) . . ?
O11 Mo1 O16 92.0(2) . . ?
O33 Mo1 O7 99.2(3) . . ?
O11 Mo1 O7 85.5(2) . . ?
O16 Mo1 O7 159.2(2) . . ?
O33 Mo1 O17 98.6(2) . . ?
O11 Mo1 O17 160.7(2) . . ?
O16 Mo1 O17 88.8(2) . . ?
O7 Mo1 O17 87.0(2) . . ?
O33 Mo1 O1 173.1(2) . . ?
O11 Mo1 O1 86.52(19) . . ?
O16 Mo1 O1 75.86(19) . . ?
O7 Mo1 O1 83.37(19) . . ?
O17 Mo1 O1 75.00(18) . . ?
O40 Mo2 O14 103.2(3) . . ?
O40 Mo2 O36 100.8(3) . . ?
O14 Mo2 O36 96.0(2) . . ?
O40 Mo2 O29 97.1(3) . . ?
O14 Mo2 O29 157.8(2) . . ?
O36 Mo2 O29 88.7(2) . . ?
O40 Mo2 O5 99.9(3) . . ?
O14 Mo2 O5 84.9(2) . . ?
O36 Mo2 O5 158.6(2) . . ?
O29 Mo2 O5 83.0(2) . . ?
O40 Mo2 O3 169.5(2) . . ?
O14 Mo2 O3 87.00(19) . . ?
O36 Mo2 O3 75.58(19) . . ?
O29 Mo2 O3 73.15(18) . . ?
O5 Mo2 O3 83.10(19) . . ?
O24 Mo3 O19 102.9(3) . . ?
O24 Mo3 O9 99.7(2) . . ?
O19 Mo3 O9 88.1(2) . . ?
O24 Mo3 O17 99.8(2) . . ?
O19 Mo3 O17 94.1(2) . . ?
O9 Mo3 O17 159.4(2) . . ?
O24 Mo3 O18 97.5(3) . . ?
O19 Mo3 O18 159.4(2) . . ?
O9 Mo3 O18 85.7(2) . . ?
O17 Mo3 O18 85.2(2) . . ?
O24 Mo3 O1 169.6(2) . . ?
O19 Mo3 O1 86.57(19) . . ?
O9 Mo3 O1 84.71(18) . . ?
O17 Mo3 O1 75.00(18) . . ?
O18 Mo3 O1 73.32(18) . . ?
O28 Mo4 O39 101.0(3) . . ?
O28 Mo4 O9 102.6(3) . . ?
O39 Mo4 O9 93.3(2) . . ?
O28 Mo4 O35 98.9(3) . . ?
O39 Mo4 O35 89.6(2) . . ?
O9 Mo4 O35 157.3(2) . . ?
O28 Mo4 O37 100.3(2) . . ?
O39 Mo4 O37 158.5(2) . . ?
O9 Mo4 O37 84.4(2) . . ?
O35 Mo4 O37 84.8(2) . . ?
O28 Mo4 O4 171.9(2) . . ?
O39 Mo4 O4 75.15(19) . . ?
O9 Mo4 O4 84.84(19) . . ?
O35 Mo4 O4 74.13(19) . . ?
O37 Mo4 O4 83.38(19) . . ?
O34 Mo5 O15 103.7(3) . . ?
O34 Mo5 O31 101.0(2) . . ?
O15 Mo5 O31 94.8(2) . . ?
O34 Mo5 O11 99.8(2) . . ?
O15 Mo5 O11 86.1(2) . . ?
O31 Mo5 O11 158.4(2) . . ?
O34 Mo5 O36 96.8(3) . . ?
O15 Mo5 O36 158.9(2) . . ?
O31 Mo5 O36 86.6(2) . . ?
O11 Mo5 O36 85.1(2) . . ?
O34 Mo5 O3 169.8(2) . . ?
O15 Mo5 O3 86.22(19) . . ?
O31 Mo5 O3 75.35(19) . . ?
O11 Mo5 O3 83.18(18) . . ?
O36 Mo5 O3 73.68(18) . . ?
O25 Mo6 O32 101.9(3) . . ?
O25 Mo6 O29 99.9(3) . . ?
O32 Mo6 O29 93.0(2) . . ?
O25 Mo6 O12 101.3(3) . . ?
O32 Mo6 O12 85.3(2) . . ?
O29 Mo6 O12 158.6(2) . . ?
O25 Mo6 O31 98.1(3) . . ?
O32 Mo6 O31 159.3(2) . . ?
O29 Mo6 O31 88.6(2) . . ?
O12 Mo6 O31 85.8(2) . . ?
O25 Mo6 O3 170.2(2) . . ?
O32 Mo6 O3 86.76(19) . . ?
O29 Mo6 O3 74.78(18) . . ?
O12 Mo6 O3 83.78(19) . . ?
O31 Mo6 O3 73.78(18) . . ?
O30 Mo7 O5 103.5(3) . . ?
O30 Mo7 O26 100.5(3) . . ?
O5 Mo7 O26 94.4(2) . . ?
O30 Mo7 O13 100.3(3) . . ?
O5 Mo7 O13 87.3(2) . . ?
O26 Mo7 O13 158.2(2) . . ?
O30 Mo7 O39 95.2(3) . . ?
O5 Mo7 O39 160.9(2) . . ?
O26 Mo7 O39 85.7(2) . . ?
O13 Mo7 O39 85.8(2) . . ?
O30 Mo7 O4 167.4(2) . . ?
O5 Mo7 O4 88.4(2) . . ?
O26 Mo7 O4 74.2(2) . . ?
O13 Mo7 O4 84.12(19) . . ?
O39 Mo7 O4 73.25(18) . . ?
O8 Mo8 O7 103.0(2) . . ?
O8 Mo8 O20 100.7(2) . . ?
O7 Mo8 O20 94.0(2) . . ?
O8 Mo8 O15 100.4(2) . . ?
O7 Mo8 O15 84.8(2) . . ?
O20 Mo8 O15 158.6(2) . . ?
O8 Mo8 O10 97.2(2) . . ?
O7 Mo8 O10 158.9(2) . . ?
O20 Mo8 O10 88.1(2) . . ?
O15 Mo8 O10 85.6(2) . . ?
O8 Mo8 O2 170.4(2) . . ?
O7 Mo8 O2 86.29(19) . . ?
O20 Mo8 O2 75.92(19) . . ?
O15 Mo8 O2 82.68(18) . . ?
O10 Mo8 O2 73.87(19) . . ?
O21 Mo9 O37 102.8(3) . . ?
O21 Mo9 O27 101.7(3) . . ?
O37 Mo9 O27 95.6(2) . . ?
O21 Mo9 O20 97.6(3) . . ?
O37 Mo9 O20 158.1(2) . . ?
O27 Mo9 O20 88.0(2) . . ?
O21 Mo9 O19 100.4(3) . . ?
O37 Mo9 O19 84.9(2) . . ?
O27 Mo9 O19 157.2(2) . . ?
O20 Mo9 O19 83.6(2) . . ?
O21 Mo9 O2 169.3(2) . . ?
O37 Mo9 O2 87.6(2) . . ?
O27 Mo9 O2 74.96(19) . . ?
O20 Mo9 O2 72.35(18) . . ?
O19 Mo9 O2 82.25(19) . . ?
O23 Mo10 O18 102.0(3) . . ?
O23 Mo10 O13 103.3(3) . . ?
O18 Mo10 O13 94.1(2) . . ?
O23 Mo10 O16 98.7(3) . . ?
O18 Mo10 O16 89.1(2) . . ?
O13 Mo10 O16 156.6(2) . . ?
O23 Mo10 O14 99.7(3) . . ?
O18 Mo10 O14 157.9(2) . . ?
O13 Mo10 O14 84.7(2) . . ?
O16 Mo10 O14 83.6(2) . . ?
O23 Mo10 O1 170.5(2) . . ?
O18 Mo10 O1 74.41(19) . . ?
O13 Mo10 O1 85.84(19) . . ?
O16 Mo10 O1 72.66(18) . . ?
O14 Mo10 O1 83.50(18) . . ?
O22 Mo11 O12 103.9(3) . . ?
O22 Mo11 O10 101.2(3) . . ?
O12 Mo11 O10 94.8(2) . . ?
O22 Mo11 O6 99.8(3) . . ?
O12 Mo11 O6 86.6(2) . . ?
O10 Mo11 O6 158.0(2) . . ?
O22 Mo11 O27 97.4(3) . . ?
O12 Mo11 O27 158.0(2) . . ?
O10 Mo11 O27 86.6(2) . . ?
O6 Mo11 O27 84.2(2) . . ?
O22 Mo11 O2 169.2(3) . . ?
O12 Mo11 O2 86.44(19) . . ?
O10 Mo11 O2 74.50(19) . . ?
O6 Mo11 O2 83.69(19) . . ?
O27 Mo11 O2 72.71(18) . . ?
O38 Mo12 O6 101.8(3) . . ?
O38 Mo12 O35 100.2(3) . . ?
O6 Mo12 O35 93.4(2) . . ?
O38 Mo12 O26 99.6(3) . . ?
O6 Mo12 O26 157.7(2) . . ?
O35 Mo12 O26 88.8(2) . . ?
O38 Mo12 O32 100.6(3) . . ?
O6 Mo12 O32 84.8(2) . . ?
O35 Mo12 O32 159.0(2) . . ?
O26 Mo12 O32 85.2(2) . . ?
O38 Mo12 O4 171.1(2) . . ?
O6 Mo12 O4 86.4(2) . . ?
O35 Mo12 O4 75.60(19) . . ?
O26 Mo12 O4 72.66(19) . . ?
O32 Mo12 O4 83.36(18) . . ?
O42 Cu1 OW1 89.0(3) . . ?
O42 Cu1 N1 168.8(3) . . ?
OW1 Cu1 N1 94.2(3) . . ?
O42 Cu1 N2 92.9(3) . . ?
OW1 Cu1 N2 169.2(3) . . ?
N1 Cu1 N2 82.0(4) . . ?
O42 Cu1 O8 91.9(2) . . ?
OW1 Cu1 O8 88.9(2) . . ?
N1 Cu1 O8 98.8(2) . . ?
N2 Cu1 O8 101.6(2) . . ?
N4 Cu2 N6 168.5(3) . . ?
N4 Cu2 N5 99.2(3) . . ?
N6 Cu2 N5 81.8(3) . . ?
N4 Cu2 N3 81.8(3) . . ?
N6 Cu2 N3 104.8(3) . . ?
N5 Cu2 N3 140.4(3) . . ?
N4 Cu2 O17 87.4(2) . . ?
N6 Cu2 O17 81.5(2) . . ?
N5 Cu2 O17 108.4(2) . . ?
N3 Cu2 O17 111.2(2) . . ?
O2 Si1 O3 109.7(2) . . ?
O2 Si1 O1 109.2(3) . . ?
O3 Si1 O1 109.2(2) . . ?
O2 Si1 O4 109.9(3) . . ?
O3 Si1 O4 109.3(3) . . ?
O1 Si1 O4 109.5(2) . . ?
Si1 O1 Mo1 124.9(2) . . ?
Si1 O1 Mo3 123.6(2) . . ?
Mo1 O1 Mo3 92.38(16) . . ?
Si1 O1 Mo10 124.2(2) . . ?
Mo1 O1 Mo10 91.31(16) . . ?
Mo3 O1 Mo10 90.78(15) . . ?
Si1 O2 Mo8 125.3(3) . . ?
Si1 O2 Mo11 123.9(3) . . ?
Mo8 O2 Mo11 91.37(16) . . ?
Si1 O2 Mo9 123.8(2) . . ?
Mo8 O2 Mo9 91.35(17) . . ?
Mo11 O2 Mo9 91.09(16) . . ?
Si1 O3 Mo5 123.9(2) . . ?
Si1 O3 Mo6 124.3(2) . . ?
Mo5 O3 Mo6 90.76(16) . . ?
Si1 O3 Mo2 125.2(2) . . ?
Mo5 O3 Mo2 90.93(16) . . ?
Mo6 O3 Mo2 91.55(16) . . ?
Si1 O4 Mo7 124.1(3) . . ?
Si1 O4 Mo12 124.3(2) . . ?
Mo7 O4 Mo12 91.90(17) . . ?
Si1 O4 Mo4 125.1(3) . . ?
Mo7 O4 Mo4 91.19(16) . . ?
Mo12 O4 Mo4 90.14(16) . . ?
Mo7 O5 Mo2 149.1(3) . . ?
Mo12 O6 Mo11 151.6(3) . . ?
Mo8 O7 Mo1 151.7(3) . . ?
Mo8 O8 Cu1 138.2(3) . . ?
Mo4 O9 Mo3 150.8(3) . . ?
Mo11 O10 Mo8 120.3(2) . . ?
Mo1 O11 Mo5 150.6(3) . . ?
Mo11 O12 Mo6 151.0(3) . . ?
Mo10 O13 Mo7 151.3(3) . . ?
Mo2 O14 Mo10 152.1(3) . . ?
Mo5 O15 Mo8 151.9(3) . . ?
Mo1 O16 Mo10 120.0(2) . . ?
Mo3 O17 Mo1 117.6(2) . . ?
Mo3 O17 Cu2 123.5(2) . . ?
Mo1 O17 Cu2 117.8(2) . . ?
Mo10 O18 Mo3 121.5(2) . . ?
Mo3 O19 Mo9 149.6(3) . . ?
Mo8 O20 Mo9 120.3(3) . . ?
Mo7 O26 Mo12 121.2(3) . . ?
Mo9 O27 Mo11 121.2(3) . . ?
Mo6 O29 Mo2 120.4(2) . . ?
Mo7 O30 Cu3 146.7(3) . 2_456 ?
Mo5 O31 Mo6 120.1(2) . . ?
Mo6 O32 Mo12 151.0(3) . . ?
Mo12 O35 Mo4 120.0(3) . . ?
Mo2 O36 Mo5 119.8(3) . . ?
Mo9 O37 Mo4 153.2(3) . . ?
Mo4 O39 Mo7 120.4(2) . . ?
C30 N6 C26 118.6(7) . . ?
C30 N6 Cu2 124.9(6) . . ?
C26 N6 Cu2 115.6(5) . . ?
C14 N3 C15 118.8(7) . . ?
C14 N3 Cu2 128.3(6) . . ?
C15 N3 Cu2 112.8(5) . . ?
C20 N4 C16 119.0(7) . . ?
C20 N4 Cu2 124.8(5) . . ?
C16 N4 Cu2 116.1(5) . . ?
C1 N1 C5 121.8(9) . . ?
C1 N1 Cu1 126.5(8) . . ?
C5 N1 Cu1 111.5(7) . . ?
C21 N5 C25 118.8(8) . . ?
C21 N5 Cu2 127.3(6) . . ?
C25 N5 Cu2 113.5(6) . . ?
C10 N2 C6 118.5(9) . . ?
C10 N2 Cu1 126.8(7) . . ?
C6 N2 Cu1 113.9(8) . . ?
N3 C15 C11 121.2(8) . . ?
N3 C15 C16 115.2(7) . . ?
C11 C15 C16 123.6(7) . . ?
N4 C20 C19 122.3(8) . . ?
N4 C16 C17 121.4(8) . . ?
N4 C16 C15 113.9(7) . . ?
C17 C16 C15 124.4(8) . . ?
N6 C26 C27 121.3(8) . . ?
N6 C26 C25 113.8(7) . . ?
C27 C26 C25 124.7(8) . . ?
C12 C11 C15 119.2(9) . . ?
C26 C27 C28 120.2(9) . . ?
N6 C30 C29 122.8(9) . . ?
C20 C19 C18 118.9(9) . . ?
C18 C17 C16 119.2(9) . . ?
C30 C29 C28 117.2(9) . . ?
C27 C28 C29 119.7(9) . . ?
N3 C14 C13 123.1(8) . . ?
N5 C25 C24 121.4(8) . . ?
N5 C25 C26 115.3(7) . . ?
C24 C25 C26 123.0(8) . . ?
N5 C21 C22 122.8(9) . . ?
C4 C5 N1 118.9(13) . . ?
C4 C5 C6 124.9(12) . . ?
N1 C5 C6 116.2(8) . . ?
C23 C22 C21 119.1(10) . . ?
C23 C24 C25 120.6(9) . . ?
N1 C1 C2 119.6(13) . . ?
N2 C10 C9 123.2(12) . . ?
C17 C18 C19 119.1(9) . . ?
C14 C13 C12 118.3(9) . . ?
N2 C6 C7 120.1(12) . . ?
N2 C6 C5 113.7(9) . . ?
C7 C6 C5 126.1(11) . . ?
C24 C23 C22 117.1(10) . . ?
C7 C8 C9 120.4(13) . . ?
C11 C12 C13 119.4(9) . . ?
C8 C7 C6 119.9(13) . . ?
C5 C4 C3 119.1(14) . . ?
C2 C3 C4 121.2(13) . . ?
C8 C9 C10 117.9(15) . . ?
C3 C2 C1 119.3(15) . . ?
N7 C36 C33 123.1(7) . . ?
N7 C36 C35 112.9(6) . . ?
C33 C36 C35 123.9(7) . . ?
O41 C35 O42 123.6(7) . . ?
O41 C35 C36 119.1(6) . . ?
O42 C35 C36 117.3(6) . . ?
C36 C33 C31 117.6(8) . . ?
C32 C31 C33 120.2(8) . . ?
C31 C32 C34 119.4(8) . . ?
N7 C34 C32 120.6(7) . . ?
C34 N7 C36 119.1(7) . . ?
C34 N7 Cu3 128.7(5) . . ?
C36 N7 Cu3 112.0(5) . . ?
C35 O41 Cu3 112.4(5) . . ?
C35 O42 Cu1 114.4(5) . . ?
N7 Cu3 N7 180.0 . 3_456 ?
N7 Cu3 O41 83.4(2) . . ?
N7 Cu3 O41 96.6(2) 3_456 . ?
N7 Cu3 O41 96.6(2) . 3_456 ?
N7 Cu3 O41 83.4(2) 3_456 3_456 ?
O41 Cu3 O41 180.0 . 3_456 ?
N7 Cu3 O30 95.2(2) . 4_565 ?
N7 Cu3 O30 84.8(2) 3_456 4_565 ?
O41 Cu3 O30 95.6(2) . 4_565 ?
O41 Cu3 O30 84.4(2) 3_456 4_565 ?
N7 Cu3 O30 84.8(2) . 2_446 ?
N7 Cu3 O30 95.2(2) 3_456 2_446 ?
O41 Cu3 O30 84.4(2) . 2_446 ?
O41 Cu3 O30 95.6(2) 3_456 2_446 ?
O30 Cu3 O30 180.0 4_565 2_446 ?

_refine_diff_density_max         2.673
_refine_diff_density_min         -2.832
_refine_diff_density_rms         0.190

####################################################################### 
# 
# 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_shelx_5
_database_code_depnum_ccdc_archive 'CCDC 1403342'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT342_shelx_5             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0243 Ang

RESPONSE: The quality of this crystal was poor.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 Cu2.50 Ge N7 O44 W12'
_chemical_formula_weight         3704.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'
O O 0.0106 0.0060 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.880(2)
_cell_length_b                   21.660(3)
_cell_length_c                   21.898(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.354(2)
_cell_angle_gamma                90
_cell_volume                     6476.6(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    12039
_cell_measurement_theta_min      3.1820
_cell_measurement_theta_max      28.6390

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.799
_exptl_crystal_F_000             6566
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    22.576
_shelx_estimated_absorpt_T_min   0.047
_shelx_estimated_absorpt_T_max   0.123
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_T_max  0.107
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
R(int) was 0.0734 before and 0.0602 after correction. The Ratio of minimum to 
maximum transmission is 0.1869.
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 15.9737
_diffrn_reflns_number            40698
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         29.145
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14978
_reflns_number_gt                10739
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0325P)²+74.6856P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14978
_refine_ls_number_parameters     922
_refine_ls_number_restraints     1668
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1211
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      0.991
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.24359(4) 0.70094(3) -0.14513(2) 0.02407(13) Uani 1 1 d . . . . .
W2 W 1.15645(4) 0.69968(3) -0.31523(3) 0.02823(14) Uani 1 1 d . . . . .
W3 W 0.80157(4) 0.65323(3) -0.19115(3) 0.02554(13) Uani 1 1 d . . . . .
W4 W 1.19477(4) 0.84842(3) -0.23010(3) 0.02752(14) Uani 1 1 d . . . . .
W5 W 0.92344(4) 0.73934(3) -0.37405(2) 0.02845(14) Uani 1 1 d . . . . .
W6 W 1.09340(4) 0.74229(3) -0.04853(2) 0.02672(14) Uani 1 1 d . . . . .
W7 W 0.75655(4) 0.78626(3) -0.26795(3) 0.02721(14) Uani 1 1 d . . . . .
W8 W 0.83619(4) 0.78631(3) -0.11278(3) 0.02760(14) Uani 1 1 d . . . . .
W9 W 1.05715(4) 0.60842(3) -0.12590(2) 0.02454(13) Uani 1 1 d . . . . .
W10 W 0.97070(4) 0.60690(3) -0.29633(2) 0.02541(13) Uani 1 1 d . . . . .
Ge1 Ge 1.00329(9) 0.74530(6) -0.21113(5) 0.0140(3) Uani 1 1 d . . . . .
W12 W 1.04085(4) 0.88909(3) -0.13543(3) 0.02818(14) Uani 1 1 d . . . . .
W11 W 0.96359(5) 0.88823(3) -0.29046(3) 0.03182(15) Uani 1 1 d . . . . .
Cu3 Cu 0.83228(13) 0.47770(9) -0.38565(8) 0.0319(4) Uani 1 1 d . . . . .
Cu2 Cu 1.30644(15) 0.53577(10) -0.07335(8) 0.0414(5) Uani 1 1 d . . . . .
Cu1 Cu 1.0000 1.0000 0.0000 0.0263(5) Uani 1 2 d S . P . .
O4 O 0.8832(6) 0.7434(4) -0.1996(4) 0.0216(17) Uani 1 1 d . U . . .
O40 O 0.8608(6) 0.6255(4) -0.2590(4) 0.0272(18) Uani 1 1 d . U . . .
O3 O 1.0405(6) 0.8209(4) -0.2156(4) 0.0240(17) Uani 1 1 d . U . . .
O39 O 1.1957(6) 0.6195(4) -0.1236(4) 0.0265(19) Uani 1 1 d . U . . .
O38 O 1.2387(6) 0.7847(4) -0.1714(4) 0.0268(19) Uani 1 1 d . U . . .
O37 O 1.0585(7) 0.7254(5) -0.3835(4) 0.032(2) Uani 1 1 d . U . . .
O36 O 0.7239(7) 0.5941(5) -0.1823(5) 0.038(2) Uani 1 1 d . U . . .
O35 O 0.9200(6) 0.6265(4) -0.1395(4) 0.0266(18) Uani 1 1 d . U . . .
O34 O 1.1798(7) 0.7833(4) -0.2909(4) 0.0297(19) Uani 1 1 d . U . . .
O33 O 1.0570(7) 0.5357(5) -0.0977(5) 0.039(3) Uani 1 1 d . U . . .
O32 O 0.8169(7) 0.7495(4) -0.3312(4) 0.0273(19) Uani 1 1 d . U . . .
O31 O 0.9607(7) 0.8207(4) -0.3458(4) 0.0287(19) Uani 1 1 d . U . . .
O30 O 0.7773(7) 0.7068(5) -0.1243(4) 0.033(2) Uani 1 1 d . U . . .
O29 O 0.7188(7) 0.7065(4) -0.2469(4) 0.031(2) Uani 1 1 d . U . . .
O2 O 1.0780(6) 0.7091(4) -0.1505(4) 0.0214(17) Uani 1 1 d . U . . .
O28 O 0.9157(7) 0.8544(4) -0.1279(4) 0.0300(19) Uani 1 1 d . U . . .
O27 O 1.0944(7) 0.6197(4) -0.3211(4) 0.0295(19) Uani 1 1 d . U . . .
O26 O 1.2222(7) 0.7278(5) -0.0650(4) 0.030(2) Uani 1 1 d . U . . .
O25 O 1.0396(7) 0.5939(4) -0.2132(4) 0.0269(18) Uani 1 1 d . U . . .
O24 O 1.0712(7) 0.6546(4) -0.0500(4) 0.0282(19) Uani 1 1 d . U . . .
O23 O 0.9487(7) 0.5326(5) -0.3228(4) 0.033(2) Uani 1 1 d . U . . .
O22 O 1.3028(7) 0.8820(5) -0.2393(5) 0.038(2) Uani 1 1 d . U . . .
O21 O 1.3660(7) 0.6891(4) -0.1278(4) 0.029(2) Uani 1 1 d . U . . .
O20 O 1.2123(7) 0.6803(4) -0.2300(4) 0.0287(19) Uani 1 1 d . U . . .
O19 O 1.0960(7) 0.8235(5) -0.0838(4) 0.0314(19) Uani 1 1 d . U . . .
O18 O 0.7779(8) 0.8148(5) -0.0571(5) 0.048(3) Uani 1 1 d . U . . .
O17 O 0.9526(7) 0.7518(4) -0.0679(4) 0.0294(19) Uani 1 1 d . U . . .
O16 O 0.6485(7) 0.8136(5) -0.3082(5) 0.041(3) Uani 1 1 d . U . . .
O15 O 1.2506(7) 0.6858(5) -0.3525(4) 0.043(3) Uani 1 1 d . U . . .
O1 O 1.0100(6) 0.7078(4) -0.2796(4) 0.0226(17) Uani 1 1 d . U . . .
O14 O 0.7440(7) 0.8122(5) -0.1854(4) 0.033(2) Uani 1 1 d . U . . .
O13 O 0.8436(7) 0.8532(5) -0.2731(4) 0.036(2) Uani 1 1 d . U . . .
O12 O 1.0516(7) 0.9498(5) -0.0858(5) 0.039(2) Uani 1 1 d . U . . .
O11 O 0.9108(7) 0.6511(5) -0.3690(4) 0.031(2) Uani 1 1 d . U . . .
O10 O 1.1031(7) 0.8960(4) -0.2872(4) 0.032(2) Uani 1 1 d . U . . .
O9 O 1.1183(8) 0.7550(5) 0.0287(4) 0.041(3) Uani 1 1 d . U . . .
O8 O 0.8712(8) 0.7525(5) -0.4494(4) 0.045(3) Uani 1 1 d . U . . .
O7 O 1.1627(7) 0.8980(4) -0.1645(4) 0.033(2) Uani 1 1 d . U . . .
O6 O 0.9811(8) 0.9291(5) -0.2111(5) 0.041(2) Uani 1 1 d . U . . .
O5 O 0.9215(8) 0.9464(5) -0.3396(5) 0.048(3) Uani 1 1 d . U . . .
O42 O 0.8651(7) 0.9933(5) -0.0489(4) 0.032(2) Uani 1 1 d . U . . .
N2 N 1.0011(8) 1.0773(5) -0.0481(5) 0.025(2) Uani 1 1 d . . . . .
OW1 O 0.782(2) 0.4419(16) -0.3167(16) 0.041(7) Uani 0.5 1 d . U P . .
OW3 O 0.809(2) 0.4344(19) -0.3086(18) 0.043(9) Uani 0.5 1 d . U P . .
N1 N 0.8522(8) 0.5054(6) -0.4674(4) 0.047(4) Uani 1 1 d G . . . .
C1 C 0.8842(8) 0.4590(5) -0.5029(5) 0.064(4) Uani 1 1 d G U . . .
C2 C 0.8901(9) 0.4700(6) -0.5646(5) 0.071(4) Uani 1 1 d G U . . .
H2A H 0.9115 0.4390 -0.5883 0.085 Uiso 1 1 calc R U . . .
C3 C 0.8641(10) 0.5274(7) -0.5909(4) 0.073(4) Uani 1 1 d G U . . .
H3A H 0.8680 0.5347 -0.6322 0.088 Uiso 1 1 calc R U . . .
C4 C 0.8321(9) 0.5737(5) -0.5555(6) 0.072(4) Uani 1 1 d G U . . .
H4A H 0.8147 0.6121 -0.5731 0.086 Uiso 1 1 calc R U . . .
C5 C 0.8261(8) 0.5627(5) -0.4937(5) 0.067(4) Uani 1 1 d G U . . .
H5A H 0.8048 0.5938 -0.4700 0.080 Uiso 1 1 calc R U . . .
C8 C 1.0730(11) 1.1178(7) -0.0461(6) 0.032(3) Uani 1 1 d . U . . .
H8A H 1.1308 1.1117 -0.0179 0.039 Uiso 1 1 calc R U . . .
C12 C 0.8428(10) 1.0387(6) -0.0859(6) 0.022(3) Uani 1 1 d . U . . .
N7 N 0.9096(9) 0.4049(6) -0.4057(7) 0.046(4) Uani 1 1 d . . . . .
C10 C 0.9792(12) 1.1779(8) -0.1248(7) 0.041(3) Uani 1 1 d . U . . .
H10A H 0.9721 1.2117 -0.1514 0.049 Uiso 1 1 calc R U . . .
C9 C 1.0651(11) 1.1686(7) -0.0843(7) 0.034(3) Uani 1 1 d . U . . .
H9A H 1.1171 1.1960 -0.0827 0.041 Uiso 1 1 calc R U . . .
C6 C 0.9160(14) 0.4043(10) -0.4665(9) 0.062(4) Uani 1 1 d . U . . .
C7 C 0.9180(10) 1.0868(6) -0.0883(6) 0.026(3) Uani 1 1 d . U . . .
C11 C 0.9033(12) 1.1369(7) -0.1258(7) 0.039(3) Uani 1 1 d . U . . .
H11A H 0.8433 1.1434 -0.1516 0.047 Uiso 1 1 calc R U . . .
N6 N 1.3454(10) 0.5376(6) -0.1551(6) 0.039(3) Uani 1 1 d . . . . .
N4 N 1.2517(9) 0.5514(6) 0.0007(5) 0.030(3) Uani 1 1 d . . . . .
C36 C 1.4339(12) 0.5635(8) -0.1559(7) 0.044(3) Uani 1 1 d . U . . .
N3 N 1.2328(9) 0.4570(6) -0.0719(6) 0.035(3) Uani 1 1 d . . . . .
N5 N 1.4396(9) 0.5739(6) -0.0475(6) 0.043(3) Uani 1 1 d . . . . .
C29 C 1.2109(13) 0.6169(9) 0.0803(7) 0.049(4) Uani 1 1 d . U . . .
H29A H 1.2157 0.6550 0.1002 0.059 Uiso 1 1 calc R U . . .
C40 C 1.2883(13) 0.5246(8) -0.2090(7) 0.045(3) Uani 1 1 d . U . . .
H40A H 1.2270 0.5073 -0.2091 0.054 Uiso 1 1 calc R U . . .
C34 C 1.5738(14) 0.6176(9) -0.0849(9) 0.056(4) Uani 1 1 d . U . . .
H34A H 1.6075 0.6228 -0.1176 0.067 Uiso 1 1 calc R U . . .
C35 C 1.4867(12) 0.5857(8) -0.0940(8) 0.045(3) Uani 1 1 d . U . . .
C30 C 1.2554(12) 0.6060(8) 0.0290(7) 0.045(3) Uani 1 1 d . U . . .
H30A H 1.2891 0.6381 0.0141 0.054 Uiso 1 1 calc R U . . .
C26 C 1.1981(13) 0.5056(8) 0.0189(7) 0.044(3) Uani 1 1 d . U . . .
C24 C 1.1355(13) 0.3979(8) -0.0133(8) 0.051(3) Uani 1 1 d . U . . .
H24A H 1.1058 0.3937 0.0212 0.062 Uiso 1 1 calc R U . . .
C31 C 1.4790(13) 0.5961(9) 0.0102(9) 0.055(4) Uani 1 1 d . U . . .
H31A H 1.4479 0.5867 0.0434 0.066 Uiso 1 1 calc R U . . .
C37 C 1.4652(14) 0.5745(9) -0.2117(8) 0.052(3) Uani 1 1 d . U . . .
H37A H 1.5263 0.5920 -0.2119 0.062 Uiso 1 1 calc R U . . .
C21 C 1.2267(13) 0.4095(8) -0.1109(8) 0.050(3) Uani 1 1 d . U . . .
H21A H 1.2600 0.4120 -0.1441 0.060 Uiso 1 1 calc R U . . .
C38 C 1.4070(13) 0.5596(8) -0.2649(7) 0.047(3) Uani 1 1 d . U . . .
H38A H 1.4281 0.5655 -0.3024 0.056 Uiso 1 1 calc R U . . .
C39 C 1.3173(14) 0.5359(8) -0.2641(8) 0.049(4) Uani 1 1 d . U . . .
H39A H 1.2752 0.5273 -0.3012 0.058 Uiso 1 1 calc R U . . .
C25 C 1.1880(12) 0.4511(8) -0.0209(7) 0.043(3) Uani 1 1 d . U . . .
C27 C 1.1540(13) 0.5121(9) 0.0701(7) 0.051(3) Uani 1 1 d . U . . .
H27A H 1.1211 0.4793 0.0844 0.061 Uiso 1 1 calc R U . . .
C32 C 1.5602(13) 0.6305(10) 0.0210(9) 0.058(4) Uani 1 1 d . U . . .
H32A H 1.5822 0.6466 0.0604 0.070 Uiso 1 1 calc R U . . .
C28 C 1.1601(14) 0.5693(9) 0.0999(8) 0.054(4) Uani 1 1 d . U . . .
H28A H 1.1289 0.5750 0.1336 0.065 Uiso 1 1 calc R U . . .
C22 C 1.1738(15) 0.3571(9) -0.1047(8) 0.057(4) Uani 1 1 d . U . . .
H22A H 1.1700 0.3256 -0.1339 0.068 Uiso 1 1 calc R U . . .
C33 C 1.6116(14) 0.6423(10) -0.0265(9) 0.063(4) Uani 1 1 d . U . . .
H33A H 1.6688 0.6656 -0.0198 0.075 Uiso 1 1 calc R U . . .
C23 C 1.1275(15) 0.3519(9) -0.0561(9) 0.061(4) Uani 1 1 d . U . . .
H23A H 1.0903 0.3170 -0.0518 0.073 Uiso 1 1 calc R U . . .
C16 C 0.9413(15) 0.3597(10) -0.3668(11) 0.069(4) Uani 1 1 d . U . . .
H16A H 0.9354 0.3614 -0.3252 0.082 Uiso 1 1 calc R U . . .
C14 C 0.9870(16) 0.3077(11) -0.4511(12) 0.080(4) Uani 1 1 d . U . . .
H14A H 1.0124 0.2725 -0.4667 0.096 Uiso 1 1 calc R U . . .
C15 C 0.9851(16) 0.3084(11) -0.3916(12) 0.078(5) Uani 1 1 d . U . . .
H15A H 1.0118 0.2760 -0.3661 0.094 Uiso 1 1 calc R U . . .
C13 C 0.9553(16) 0.3537(11) -0.4928(11) 0.078(4) Uani 1 1 d . U . . .
H13A H 0.9596 0.3515 -0.5346 0.093 Uiso 1 1 calc R U . . .
OW5 O 0.8333(12) 1.0103(7) -0.2294(7) 0.098(4) Uani 1 1 d . U . . .
HW5A H 0.8937 1.0010 -0.2211 0.147 Uiso 1 1 d R U . . .
HW5B H 0.8155 1.0203 -0.1956 0.147 Uiso 1 1 d R U . . .
O43 O 0.7603(8) 1.0442(5) -0.1200(5) 0.044(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O21 1.693(9) . ?
W1 O20 1.884(9) . ?
W1 O38 1.901(9) . ?
W1 O26 1.923(9) . ?
W1 O39 1.972(9) . ?
W1 O2 2.288(8) . ?
W2 O15 1.688(9) . ?
W2 O34 1.901(10) . ?
W2 O37 1.914(10) . ?
W2 O27 1.929(9) . ?
W2 O20 1.934(9) . ?
W2 O1 2.312(8) . ?
W3 O36 1.708(10) . ?
W3 O29 1.907(10) . ?
W3 O35 1.910(9) . ?
W3 O40 1.919(8) . ?
W3 O30 1.945(9) . ?
W3 O4 2.283(9) . ?
W4 O22 1.710(10) . ?
W4 O7 1.909(9) . ?
W4 O38 1.909(9) . ?
W4 O10 1.916(10) . ?
W4 O34 1.924(9) . ?
W4 O3 2.299(9) . ?
W5 O8 1.703(10) . ?
W5 O32 1.901(9) . ?
W5 O31 1.909(9) . ?
W5 O11 1.923(10) . ?
W5 O37 1.947(9) . ?
W5 O1 2.301(9) . ?
W6 O9 1.686(9) . ?
W6 O26 1.912(9) . ?
W6 O19 1.923(10) . ?
W6 O24 1.923(10) . ?
W6 O17 1.935(9) . ?
W6 O2 2.318(8) . ?
W7 O16 1.704(10) . ?
W7 O29 1.887(10) . ?
W7 O13 1.904(10) . ?
W7 O32 1.916(9) . ?
W7 O14 1.931(9) . ?
W7 O4 2.291(9) . ?
W8 O18 1.696(10) . ?
W8 O17 1.888(9) . ?
W8 O30 1.903(10) . ?
W8 O28 1.907(10) . ?
W8 O14 1.935(10) . ?
W8 O4 2.312(8) . ?
W9 O33 1.692(10) . ?
W9 O25 1.909(9) . ?
W9 O35 1.914(9) . ?
W9 O24 1.919(9) . ?
W9 O39 1.930(9) . ?
W9 O2 2.277(9) . ?
W10 O23 1.720(10) . ?
W10 O40 1.899(8) . ?
W10 O27 1.911(9) . ?
W10 O11 1.915(9) . ?
W10 O25 1.919(9) . ?
W10 O1 2.267(9) . ?
Ge1 O2 1.720(8) . ?
Ge1 O1 1.722(8) . ?
Ge1 O3 1.726(9) . ?
Ge1 O4 1.730(8) . ?
W12 O12 1.695(10) . ?
W12 O19 1.891(10) . ?
W12 O7 1.921(9) . ?
W12 O6 1.922(10) . ?
W12 O28 1.926(9) . ?
W12 O3 2.293(9) . ?
W11 O5 1.690(11) . ?
W11 O31 1.895(9) . ?
W11 O6 1.926(10) . ?
W11 O13 1.929(10) . ?
W11 O10 1.932(10) . ?
W11 O3 2.307(9) . ?
Cu3 OW1 1.93(3) . ?
Cu3 O43 1.949(11) 2_644 ?
Cu3 N1 1.955(8) . ?
Cu3 N7 2.000(13) . ?
Cu3 OW3 2.01(4) . ?
Cu3 O23 2.263(9) . ?
Cu2 N4 1.939(11) . ?
Cu2 N6 1.961(11) . ?
Cu2 N3 1.993(13) . ?
Cu2 N5 2.011(13) . ?
Cu1 N2 1.980(11) . ?
Cu1 N2 1.980(11) 3_775 ?
Cu1 O42 1.988(9) 3_775 ?
Cu1 O42 1.988(9) . ?
Cu1 O12 2.390(10) 3_775 ?
Cu1 O12 2.390(10) . ?
O42 C12 1.277(15) . ?
N2 C8 1.323(17) . ?
N2 C7 1.335(17) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C1 C6 1.45(2) . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C8 C9 1.374(19) . ?
C12 O43 1.255(16) . ?
C12 C7 1.483(18) . ?
N7 C16 1.32(2) . ?
N7 C6 1.35(2) . ?
C10 C9 1.37(2) . ?
C10 C11 1.38(2) . ?
C6 C13 1.39(3) . ?
C7 C11 1.353(19) . ?
N6 C40 1.33(2) . ?
N6 C36 1.35(2) . ?
N4 C30 1.33(2) . ?
N4 C26 1.342(19) . ?
C36 C37 1.39(2) . ?
C36 C35 1.50(2) . ?
N3 C21 1.329(19) . ?
N3 C25 1.377(17) . ?
N5 C35 1.330(18) . ?
N5 C31 1.37(2) . ?
C29 C28 1.36(2) . ?
C29 C30 1.40(2) . ?
C40 C39 1.36(2) . ?
C34 C35 1.38(2) . ?
C34 C33 1.40(2) . ?
C26 C27 1.377(19) . ?
C26 C25 1.46(2) . ?
C24 C23 1.36(2) . ?
C24 C25 1.39(2) . ?
C31 C32 1.34(2) . ?
C37 C38 1.33(2) . ?
C21 C22 1.37(2) . ?
C38 C39 1.35(2) . ?
C27 C28 1.40(2) . ?
C32 C33 1.39(2) . ?
C22 C23 1.34(2) . ?
C16 C15 1.42(3) . ?
C14 C15 1.31(3) . ?
C14 C13 1.37(3) . ?
O43 Cu3 1.949(11) 2_654 ?

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
O21 W1 O20 103.3(4) . . ?
O21 W1 O38 101.1(4) . . ?
O20 W1 O38 86.5(4) . . ?
O21 W1 O26 98.9(4) . . ?
O20 W1 O26 157.8(4) . . ?
O38 W1 O26 89.1(4) . . ?
O21 W1 O39 100.3(4) . . ?
O20 W1 O39 89.7(4) . . ?
O38 W1 O39 158.6(4) . . ?
O26 W1 O39 86.5(4) . . ?
O21 W1 O2 169.2(4) . . ?
O20 W1 O2 85.2(4) . . ?
O38 W1 O2 86.0(3) . . ?
O26 W1 O2 72.8(3) . . ?
O39 W1 O2 72.7(3) . . ?
O15 W2 O34 101.4(5) . . ?
O15 W2 O37 100.2(4) . . ?
O34 W2 O37 90.2(4) . . ?
O15 W2 O27 100.6(5) . . ?
O34 W2 O27 157.9(4) . . ?
O37 W2 O27 87.9(4) . . ?
O15 W2 O20 102.5(5) . . ?
O34 W2 O20 85.3(4) . . ?
O37 W2 O20 157.3(4) . . ?
O27 W2 O20 88.0(4) . . ?
O15 W2 O1 168.9(4) . . ?
O34 W2 O1 87.1(3) . . ?
O37 W2 O1 72.4(3) . . ?
O27 W2 O1 71.4(3) . . ?
O20 W2 O1 85.1(3) . . ?
O36 W3 O29 101.9(5) . . ?
O36 W3 O35 101.5(4) . . ?
O29 W3 O35 156.6(4) . . ?
O36 W3 O40 102.7(4) . . ?
O29 W3 O40 89.2(4) . . ?
O35 W3 O40 85.5(4) . . ?
O36 W3 O30 99.5(4) . . ?
O29 W3 O30 87.4(4) . . ?
O35 W3 O30 88.9(4) . . ?
O40 W3 O30 157.8(4) . . ?
O36 W3 O4 169.7(4) . . ?
O29 W3 O4 71.4(4) . . ?
O35 W3 O4 85.4(4) . . ?
O40 W3 O4 85.3(3) . . ?
O30 W3 O4 72.9(3) . . ?
O22 W4 O7 100.2(4) . . ?
O22 W4 O38 101.9(4) . . ?
O7 W4 O38 89.4(4) . . ?
O22 W4 O10 100.9(4) . . ?
O7 W4 O10 88.3(4) . . ?
O38 W4 O10 157.2(4) . . ?
O22 W4 O34 102.5(4) . . ?
O7 W4 O34 157.2(4) . . ?
O38 W4 O34 85.3(4) . . ?
O10 W4 O34 88.1(4) . . ?
O22 W4 O3 169.8(4) . . ?
O7 W4 O3 72.1(4) . . ?
O38 W4 O3 85.0(3) . . ?
O10 W4 O3 72.8(3) . . ?
O34 W4 O3 85.3(3) . . ?
O8 W5 O32 103.0(5) . . ?
O8 W5 O31 101.7(5) . . ?
O32 W5 O31 85.5(4) . . ?
O8 W5 O11 101.2(5) . . ?
O32 W5 O11 90.0(4) . . ?
O31 W5 O11 157.1(4) . . ?
O8 W5 O37 100.0(4) . . ?
O32 W5 O37 157.0(4) . . ?
O31 W5 O37 88.2(4) . . ?
O11 W5 O37 87.2(4) . . ?
O8 W5 O1 169.6(4) . . ?
O32 W5 O1 85.3(3) . . ?
O31 W5 O1 85.1(4) . . ?
O11 W5 O1 72.1(4) . . ?
O37 W5 O1 72.1(3) . . ?
O9 W6 O26 100.7(5) . . ?
O9 W6 O19 103.7(5) . . ?
O26 W6 O19 89.4(4) . . ?
O9 W6 O24 100.5(5) . . ?
O26 W6 O24 89.2(4) . . ?
O19 W6 O24 155.6(4) . . ?
O9 W6 O17 102.6(4) . . ?
O26 W6 O17 156.7(4) . . ?
O19 W6 O17 84.6(4) . . ?
O24 W6 O17 87.1(4) . . ?
O9 W6 O2 169.4(4) . . ?
O26 W6 O2 72.3(3) . . ?
O19 W6 O2 84.4(3) . . ?
O24 W6 O2 72.0(3) . . ?
O17 W6 O2 84.7(3) . . ?
O16 W7 O29 100.8(5) . . ?
O16 W7 O13 102.3(5) . . ?
O29 W7 O13 156.8(4) . . ?
O16 W7 O32 103.2(4) . . ?
O29 W7 O32 88.5(4) . . ?
O13 W7 O32 84.8(4) . . ?
O16 W7 O14 99.5(4) . . ?
O29 W7 O14 87.8(4) . . ?
O13 W7 O14 89.9(4) . . ?
O32 W7 O14 157.3(4) . . ?
O16 W7 O4 168.5(4) . . ?
O29 W7 O4 71.6(4) . . ?
O13 W7 O4 85.8(4) . . ?
O32 W7 O4 85.4(3) . . ?
O14 W7 O4 72.1(3) . . ?
O18 W8 O17 104.1(5) . . ?
O18 W8 O30 100.1(5) . . ?
O17 W8 O30 91.0(4) . . ?
O18 W8 O28 102.1(5) . . ?
O17 W8 O28 85.9(4) . . ?
O30 W8 O28 157.7(4) . . ?
O18 W8 O14 98.9(5) . . ?
O17 W8 O14 156.9(4) . . ?
O30 W8 O14 87.1(4) . . ?
O28 W8 O14 87.2(4) . . ?
O18 W8 O4 168.1(4) . . ?
O17 W8 O4 85.9(3) . . ?
O30 W8 O4 72.9(3) . . ?
O28 W8 O4 84.8(3) . . ?
O14 W8 O4 71.6(3) . . ?
O33 W9 O25 101.7(4) . . ?
O33 W9 O35 100.4(4) . . ?
O25 W9 O35 86.2(4) . . ?
O33 W9 O24 100.2(4) . . ?
O25 W9 O24 158.1(4) . . ?
O35 W9 O24 88.3(4) . . ?
O33 W9 O39 100.0(4) . . ?
O25 W9 O39 89.6(4) . . ?
O35 W9 O39 159.6(4) . . ?
O24 W9 O39 88.1(4) . . ?
O33 W9 O2 170.5(4) . . ?
O25 W9 O2 85.4(3) . . ?
O35 W9 O2 86.1(4) . . ?
O24 W9 O2 73.0(3) . . ?
O39 W9 O2 73.7(3) . . ?
O23 W10 O40 103.6(4) . . ?
O23 W10 O27 98.9(4) . . ?
O40 W10 O27 157.4(4) . . ?
O23 W10 O11 99.4(4) . . ?
O40 W10 O11 89.4(4) . . ?
O27 W10 O11 88.2(4) . . ?
O23 W10 O25 102.1(4) . . ?
O40 W10 O25 85.7(4) . . ?
O27 W10 O25 88.3(4) . . ?
O11 W10 O25 158.4(4) . . ?
O23 W10 O1 168.6(4) . . ?
O40 W10 O1 85.1(4) . . ?
O27 W10 O1 72.8(3) . . ?
O11 W10 O1 73.0(4) . . ?
O25 W10 O1 85.6(4) . . ?
O2 Ge1 O1 109.8(4) . . ?
O2 Ge1 O3 109.4(4) . . ?
O1 Ge1 O3 109.6(4) . . ?
O2 Ge1 O4 109.8(4) . . ?
O1 Ge1 O4 108.7(4) . . ?
O3 Ge1 O4 109.6(4) . . ?
O12 W12 O19 102.8(4) . . ?
O12 W12 O7 98.8(4) . . ?
O19 W12 O7 89.3(4) . . ?
O12 W12 O6 100.2(5) . . ?
O19 W12 O6 157.0(4) . . ?
O7 W12 O6 86.5(4) . . ?
O12 W12 O28 103.0(4) . . ?
O19 W12 O28 86.0(4) . . ?
O7 W12 O28 158.2(4) . . ?
O6 W12 O28 89.6(4) . . ?
O12 W12 O3 167.9(4) . . ?
O19 W12 O3 85.3(3) . . ?
O7 W12 O3 72.0(3) . . ?
O6 W12 O3 71.9(4) . . ?
O28 W12 O3 86.4(3) . . ?
O5 W11 O31 101.7(5) . . ?
O5 W11 O6 101.8(5) . . ?
O31 W11 O6 156.4(4) . . ?
O5 W11 O13 101.9(5) . . ?
O31 W11 O13 84.4(4) . . ?
O6 W11 O13 88.6(4) . . ?
O5 W11 O10 100.8(5) . . ?
O31 W11 O10 89.8(4) . . ?
O6 W11 O10 87.9(4) . . ?
O13 W11 O10 157.2(4) . . ?
O5 W11 O3 170.2(4) . . ?
O31 W11 O3 85.5(4) . . ?
O6 W11 O3 71.5(4) . . ?
O13 W11 O3 85.3(4) . . ?
O10 W11 O3 72.3(3) . . ?
OW1 Cu3 O43 85.1(10) . 2_644 ?
OW1 Cu3 N1 165.5(11) . . ?
O43 Cu3 N1 92.0(5) 2_644 . ?
OW1 Cu3 N7 97.8(10) . . ?
O43 Cu3 N7 169.3(5) 2_644 . ?
N1 Cu3 N7 82.6(6) . . ?
OW1 Cu3 OW3 11.9(14) . . ?
O43 Cu3 OW3 94.9(11) 2_644 . ?
N1 Cu3 OW3 169.8(13) . . ?
N7 Cu3 OW3 89.3(12) . . ?
OW1 Cu3 O23 93.0(11) . . ?
O43 Cu3 O23 88.8(4) 2_644 . ?
N1 Cu3 O23 101.2(4) . . ?
N7 Cu3 O23 101.2(5) . . ?
OW3 Cu3 O23 86.5(11) . . ?
N4 Cu2 N6 166.6(5) . . ?
N4 Cu2 N3 81.7(5) . . ?
N6 Cu2 N3 105.0(5) . . ?
N4 Cu2 N5 99.9(5) . . ?
N6 Cu2 N5 81.9(6) . . ?
N3 Cu2 N5 142.7(5) . . ?
N2 Cu1 N2 180.0(6) . 3_775 ?
N2 Cu1 O42 97.4(4) . 3_775 ?
N2 Cu1 O42 82.6(4) 3_775 3_775 ?
N2 Cu1 O42 82.6(4) . . ?
N2 Cu1 O42 97.4(4) 3_775 . ?
O42 Cu1 O42 180.0 3_775 . ?
N2 Cu1 O12 93.8(4) . 3_775 ?
N2 Cu1 O12 86.2(4) 3_775 3_775 ?
O42 Cu1 O12 86.0(4) 3_775 3_775 ?
O42 Cu1 O12 94.0(4) . 3_775 ?
N2 Cu1 O12 86.2(4) . . ?
N2 Cu1 O12 93.8(4) 3_775 . ?
O42 Cu1 O12 94.0(4) 3_775 . ?
O42 Cu1 O12 86.0(4) . . ?
O12 Cu1 O12 180.0 3_775 . ?
Ge1 O4 W3 122.5(4) . . ?
Ge1 O4 W7 122.8(4) . . ?
W3 O4 W7 93.7(3) . . ?
Ge1 O4 W8 122.2(5) . . ?
W3 O4 W8 93.4(3) . . ?
W7 O4 W8 94.5(3) . . ?
W10 O40 W3 152.7(5) . . ?
Ge1 O3 W12 121.8(4) . . ?
Ge1 O3 W4 123.3(5) . . ?
W12 O3 W4 93.7(3) . . ?
Ge1 O3 W11 122.3(5) . . ?
W12 O3 W11 94.3(3) . . ?
W4 O3 W11 93.5(3) . . ?
W9 O39 W1 118.8(4) . . ?
W1 O38 W4 152.1(5) . . ?
W2 O37 W5 121.6(4) . . ?
W3 O35 W9 151.7(5) . . ?
W2 O34 W4 152.2(5) . . ?
W5 O32 W7 152.2(5) . . ?
W11 O31 W5 153.3(5) . . ?
W8 O30 W3 120.7(4) . . ?
W7 O29 W3 123.3(5) . . ?
Ge1 O2 W9 122.3(4) . . ?
Ge1 O2 W1 122.4(4) . . ?
W9 O2 W1 94.8(3) . . ?
Ge1 O2 W6 122.7(4) . . ?
W9 O2 W6 93.6(3) . . ?
W1 O2 W6 93.3(3) . . ?
W8 O28 W12 151.1(5) . . ?
W10 O27 W2 121.7(5) . . ?
W6 O26 W1 121.6(5) . . ?
W9 O25 W10 151.4(5) . . ?
W9 O24 W6 121.4(4) . . ?
W10 O23 Cu3 139.6(5) . . ?
W1 O20 W2 151.8(5) . . ?
W12 O19 W6 153.2(6) . . ?
W8 O17 W6 153.2(5) . . ?
Ge1 O1 W10 123.1(4) . . ?
Ge1 O1 W5 122.8(5) . . ?
W10 O1 W5 94.0(3) . . ?
Ge1 O1 W2 121.2(4) . . ?
W10 O1 W2 94.1(3) . . ?
W5 O1 W2 93.9(3) . . ?
W7 O14 W8 121.8(5) . . ?
W7 O13 W11 152.9(6) . . ?
W12 O12 Cu1 148.5(6) . . ?
W10 O11 W5 120.9(5) . . ?
W4 O10 W11 121.4(4) . . ?
W4 O7 W12 122.1(5) . . ?
W12 O6 W11 122.4(5) . . ?
C12 O42 Cu1 112.6(9) . . ?
C8 N2 C7 118.4(12) . . ?
C8 N2 Cu1 128.4(10) . . ?
C7 N2 Cu1 113.1(9) . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Cu3 113.7(7) . . ?
C5 N1 Cu3 125.8(7) . . ?
N1 C1 C2 120.0 . . ?
N1 C1 C6 112.3(11) . . ?
C2 C1 C6 127.5(11) . . ?
C3 C2 C1 120.0 . . ?
C2 C3 C4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 N1 120.0 . . ?
N2 C8 C9 122.2(14) . . ?
O43 C12 O42 122.8(12) . . ?
O43 C12 C7 119.1(12) . . ?
O42 C12 C7 118.1(12) . . ?
C16 N7 C6 123.7(16) . . ?
C16 N7 Cu3 125.0(13) . . ?
C6 N7 Cu3 110.9(13) . . ?
C9 C10 C11 119.4(15) . . ?
C10 C9 C8 118.5(15) . . ?
N7 C6 C13 121(2) . . ?
N7 C6 C1 117.8(16) . . ?
C13 C6 C1 121.1(19) . . ?
N2 C7 C11 122.8(13) . . ?
N2 C7 C12 113.6(12) . . ?
C11 C7 C12 123.6(13) . . ?
C7 C11 C10 118.5(15) . . ?
C40 N6 C36 118.3(13) . . ?
C40 N6 Cu2 126.1(11) . . ?
C36 N6 Cu2 114.9(11) . . ?
C30 N4 C26 119.6(13) . . ?
C30 N4 Cu2 123.8(10) . . ?
C26 N4 Cu2 116.2(10) . . ?
N6 C36 C37 120.7(16) . . ?
N6 C36 C35 114.8(13) . . ?
C37 C36 C35 124.1(16) . . ?
C21 N3 C25 117.6(14) . . ?
C21 N3 Cu2 128.7(11) . . ?
C25 N3 Cu2 113.6(10) . . ?
C35 N5 C31 118.0(15) . . ?
C35 N5 Cu2 114.6(11) . . ?
C31 N5 Cu2 126.7(11) . . ?
C28 C29 C30 117.1(17) . . ?
N6 C40 C39 121.7(17) . . ?
C35 C34 C33 120.0(17) . . ?
N5 C35 C34 121.7(17) . . ?
N5 C35 C36 113.7(14) . . ?
C34 C35 C36 124.5(15) . . ?
N4 C30 C29 122.6(15) . . ?
N4 C26 C27 121.2(16) . . ?
N4 C26 C25 114.7(13) . . ?
C27 C26 C25 124.0(16) . . ?
C23 C24 C25 120.4(16) . . ?
C32 C31 N5 122.8(17) . . ?
C38 C37 C36 119.4(17) . . ?
N3 C21 C22 123.3(16) . . ?
C37 C38 C39 119.8(15) . . ?
C38 C39 C40 120.0(17) . . ?
N3 C25 C24 119.8(14) . . ?
N3 C25 C26 113.6(14) . . ?
C24 C25 C26 126.6(14) . . ?
C26 C27 C28 118.2(16) . . ?
C31 C32 C33 120.1(19) . . ?
C29 C28 C27 121.0(16) . . ?
C23 C22 C21 119.3(17) . . ?
C32 C33 C34 117.2(18) . . ?
C22 C23 C24 119.5(19) . . ?
N7 C16 C15 117(2) . . ?
C15 C14 C13 126(2) . . ?
C14 C15 C16 118(2) . . ?
C14 C13 C6 114(2) . . ?
C12 O43 Cu3 115.7(9) . 2_654 ?

_refine_diff_density_max         2.958
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.372

####################################################################### 
# 
# 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_shelx_6
_database_code_depnum_ccdc_archive 'CCDC 1403343'
_audit_update_record             
;
2015-07-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;

_vrf_PLAT306_shelx_6             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow5 Check

RESPONSE: The hydrogens of the water molecule were not added.
;

_vrf_PLAT342_shelx_6             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0297 Ang

RESPONSE: The quality of this crystal was poor.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H35 Cu3 Ge N6 O49.50 W12'
_chemical_formula_weight         3813.04

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'
Ge Ge 0.1547 1.8001 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.010(3)
_cell_length_b                   14.252(3)
_cell_length_c                   17.350(3)
_cell_angle_alpha                99.63(3)
_cell_angle_beta                 94.38(3)
_cell_angle_gamma                94.97(3)
_cell_volume                     3388.0(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13380
_cell_measurement_theta_min      3.3300
_cell_measurement_theta_max      28.7530

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.738
_exptl_crystal_F_000             3391
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    21.740
_shelx_estimated_absorpt_T_min   0.046
_shelx_estimated_absorpt_T_max   0.129
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_T_max  0.079
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;  
R(int) was 0.0460 before and 0.0421 after correction. The Ratio of minimum to 
maximum transmission is 0.2152.
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 15.9737
_diffrn_reflns_number            32952
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.914
_diffrn_reflns_theta_max         29.114
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15650
_reflns_number_gt                13059
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0508P)²+126.8366P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15650
_refine_ls_number_parameters     973
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.1522
_refine_ls_wR_factor_gt          0.1436
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.24495(9) 0.73485(10) -0.25160(7) 0.0142(3) Uani 1 1 d . . . . .
W12 W 0.05869(4) 0.88631(4) -0.23911(4) 0.02402(13) Uani 1 1 d . . . . .
W11 W -0.00218(4) 0.64854(4) -0.27956(4) 0.02474(14) Uani 1 1 d . . . . .
W10 W 0.42015(5) 0.57085(5) -0.26015(4) 0.02816(15) Uani 1 1 d . . . . .
W9 W 0.28173(4) 0.59083(5) -0.10682(4) 0.02500(14) Uani 1 1 d . . . . .
W8 W 0.34771(4) 0.85256(5) -0.06351(4) 0.02766(14) Uani 1 1 d . . . . .
W7 W 0.18609(5) 0.48348(4) -0.28897(4) 0.02744(14) Uani 1 1 d . . . . .
W6 W 0.09164(4) 0.75415(5) -0.09731(4) 0.02559(14) Uani 1 1 d . . . . .
W5 W 0.31501(4) 0.98352(4) -0.20614(4) 0.02548(14) Uani 1 1 d . . . . .
W4 W 0.21145(4) 0.86632(5) -0.40498(4) 0.02550(14) Uani 1 1 d . . . . .
W3 W 0.48759(4) 0.83300(5) -0.21606(4) 0.02770(14) Uani 1 1 d . . . . .
W2 W 0.38517(5) 0.71698(5) -0.41507(4) 0.02762(14) Uani 1 1 d . . . . .
W1 W 0.15108(5) 0.62762(5) -0.44497(3) 0.02643(14) Uani 1 1 d . . . . .
Cu3 Cu 0.30810(15) 0.47387(15) 0.09120(12) 0.0327(4) Uani 1 1 d . . . . .
Cu2 Cu 0.24684(14) 0.22148(14) 0.24668(11) 0.0304(4) Uani 1 1 d . . . . .
Cu1 Cu 0.20445(16) 0.97306(15) -0.59322(12) 0.0351(5) Uani 1 1 d . . . . .
O38 O 0.1846(8) 0.5352(8) -0.3827(7) 0.032(2) Uani 1 1 d . . . . .
O37 O 0.1646(8) 0.6478(8) -0.0969(7) 0.031(2) Uani 1 1 d . . . . .
O36 O 0.3281(8) 0.8254(8) -0.4472(7) 0.034(3) Uani 1 1 d . . . . .
O35 O 0.5189(9) 0.5112(9) -0.2688(8) 0.041(3) Uani 1 1 d . . . . .
O34 O 0.2931(9) 0.5352(9) -0.0272(7) 0.036(3) Uani 1 1 d . . . . .
O33 O 0.0749(9) 0.5478(8) -0.2673(7) 0.034(3) Uani 1 1 d . . . . .
O32 O 0.4044(9) 0.6171(9) -0.3568(7) 0.039(3) Uani 1 1 d . . . . .
O31 O -0.0129(8) 0.9779(8) -0.2424(7) 0.035(3) Uani 1 1 d . . . . .
O30 O 0.2855(8) 0.9403(9) -0.3176(6) 0.035(3) Uani 1 1 d . . . . .
O29 O 0.1930(9) 0.9504(8) -0.4637(6) 0.033(3) Uani 1 1 d . . . . .
O28 O 0.3825(10) 0.8925(10) 0.0321(7) 0.045(3) Uani 1 1 d . . . . .
O27 O 0.4458(8) 0.9567(9) -0.2175(7) 0.035(3) Uani 1 1 d . . . . .
O26 O 0.3450(8) 0.7151(8) -0.0725(7) 0.034(3) Uani 1 1 d . . . . .
O25 O 0.0407(9) 0.8623(8) -0.1344(6) 0.034(3) Uani 1 1 d . . . . .
O24 O 0.3345(9) 0.9713(10) -0.0967(6) 0.039(3) Uani 1 1 d . . . . .
O23 O 0.4727(7) 0.6972(9) -0.2172(7) 0.032(3) Uani 1 1 d . . . . .
O22 O 0.0402(8) 0.7619(9) -0.0115(7) 0.036(3) Uani 1 1 d . . . . .
O21 O 0.2747(7) 0.6274(8) -0.2308(6) 0.029(2) Uani 1 1 d . . . . .
O20 O 0.2800(9) 0.6361(9) -0.4770(7) 0.038(3) Uani 1 1 d . . . . .
O19 O 0.1300(7) 0.7509(7) -0.2249(6) 0.024(2) Uani 1 1 d . . . . .
O18 O 0.3247(9) 1.1034(9) -0.2000(8) 0.044(3) Uani 1 1 d . . . . .
O17 O 0.1072(8) 0.8735(8) -0.3399(6) 0.031(2) Uani 1 1 d . . . . .
O16 O -0.1129(8) 0.5896(10) -0.3055(8) 0.043(3) Uani 1 1 d . . . . .
O15 O 0.4717(9) 0.7075(10) -0.4782(7) 0.043(3) Uani 1 1 d . . . . .
O14 O 0.0508(8) 0.6499(8) -0.3767(6) 0.028(2) Uani 1 1 d . . . . .
O13 O 0.3247(7) 0.8238(8) -0.1996(6) 0.025(2) Uani 1 1 d . . . . .
O12 O 0.2471(7) 0.7354(7) -0.3509(6) 0.024(2) Uani 1 1 d . . . . .
O11 O 0.4702(9) 0.8537(9) -0.1048(7) 0.038(3) Uani 1 1 d . . . . .
O10 O 0.3218(9) 0.4668(9) -0.2985(7) 0.040(3) Uani 1 1 d . . . . .
O9 O 0.4477(8) 0.8002(8) -0.3264(7) 0.032(2) Uani 1 1 d . . . . .
O8 O 0.6081(8) 0.8559(9) -0.2149(8) 0.040(3) Uani 1 1 d . . . . .
O7 O 0.1406(10) 0.3664(9) -0.3190(8) 0.045(3) Uani 1 1 d . . . . .
O6 O 0.1805(8) 0.9537(8) -0.2018(6) 0.030(2) Uani 1 1 d . . . . .
O5 O 0.3964(8) 0.5536(10) -0.1532(7) 0.039(3) Uani 1 1 d . . . . .
O4 O -0.0355(9) 0.7782(8) -0.2787(6) 0.035(3) Uani 1 1 d . . . . .
O3 O -0.0078(9) 0.6733(8) -0.1655(7) 0.034(3) Uani 1 1 d . . . . .
O2 O 0.1418(9) 0.7541(9) -0.4705(7) 0.035(3) Uani 1 1 d . . . . .
O1 O 0.2119(8) 0.8301(8) -0.0683(7) 0.032(3) Uani 1 1 d . . . . .
N4 N 0.1925(11) 0.5409(11) 0.1143(8) 0.037(3) Uani 1 1 d . . . . .
O39 O 0.2117(8) 0.4823(9) -0.1785(7) 0.036(3) Uani 1 1 d . . . . .
N2 N 0.1805(10) 0.8328(10) -0.6306(8) 0.033(3) Uani 1 1 d . . . . .
O40 O 0.0920(10) 0.5612(10) -0.5269(7) 0.046(3) Uani 1 1 d . . . . .
C24 C 0.3120(12) 0.6729(11) 0.1433(9) 0.030(4) Uani 1 1 d . . . . .
N3 N 0.3759(10) 0.6031(10) 0.1289(8) 0.033(3) Uani 1 1 d . . . . .
N1 N 0.3408(12) 0.9495(10) -0.6041(9) 0.039(4) Uani 1 1 d . . . . .
C23 C 0.2147(14) 0.6369(14) 0.1340(10) 0.040(4) Uani 1 1 d . . . . .
C4 C 0.4401(14) 0.8169(13) -0.6330(10) 0.037(4) Uani 1 1 d . . . . .
C12 C 0.3525(12) 0.8533(12) -0.6245(8) 0.029(3) Uani 1 1 d . . . . .
C11 C 0.2633(11) 0.7915(11) -0.6387(9) 0.026(3) Uani 1 1 d . . . . .
C19 C 0.1432(14) 0.6988(15) 0.1436(10) 0.041(4) Uani 1 1 d . . . . .
C6 C 0.3599(17) 0.6595(13) -0.6671(11) 0.048(5) Uani 1 1 d . . . . .
H6A H 0.3623 0.5940 -0.6820 0.057 Uiso 1 1 calc R U . . .
C16 C 0.3413(14) 0.7700(14) 0.1626(10) 0.041(4) Uani 1 1 d . . . . .
C17 C 0.2692(18) 0.8349(14) 0.1735(12) 0.053(6) Uani 1 1 d . . . . .
H17A H 0.2876 0.9003 0.1865 0.063 Uiso 1 1 calc R U . . .
C18 C 0.1743(18) 0.8023(14) 0.1652(10) 0.051(6) Uani 1 1 d . . . . .
H18A H 0.1284 0.8455 0.1732 0.061 Uiso 1 1 calc R U . . .
C7 C 0.2675(14) 0.6942(14) -0.6586(9) 0.038(4) Uani 1 1 d . . . . .
C1 C 0.4209(16) 1.0092(14) -0.5939(13) 0.051(5) Uani 1 1 d . . . . .
H1A H 0.4159 1.0743 -0.5788 0.061 Uiso 1 1 calc R U . . .
C22 C 0.1008(15) 0.5037(16) 0.1066(13) 0.052(5) Uani 1 1 d . . . . .
H22A H 0.0865 0.4376 0.0956 0.063 Uiso 1 1 calc R U . . .
C5 C 0.4408(14) 0.7148(15) -0.6550(12) 0.045(5) Uani 1 1 d . . . . .
H5A H 0.4989 0.6884 -0.6606 0.054 Uiso 1 1 calc R U . . .
C15 C 0.4399(17) 0.7970(15) 0.1694(11) 0.051(6) Uani 1 1 d . . . . .
H15A H 0.4627 0.8615 0.1825 0.062 Uiso 1 1 calc R U . . .
C10 C 0.0994(16) 0.7774(18) -0.6439(11) 0.056(6) Uani 1 1 d . . . . .
H10A H 0.0414 0.8043 -0.6398 0.068 Uiso 1 1 calc R U . . .
C9 C 0.0988(17) 0.6763(18) -0.6647(13) 0.062(7) Uani 1 1 d . . . . .
H9A H 0.0404 0.6381 -0.6725 0.074 Uiso 1 1 calc R U . . .
C2 C 0.5087(16) 0.980(2) -0.6044(13) 0.062(7) Uani 1 1 d . . . . .
H2A H 0.5616 1.0255 -0.6012 0.074 Uiso 1 1 calc R U . . .
C8 C 0.1809(15) 0.6349(14) -0.6732(11) 0.044(5) Uani 1 1 d . . . . .
H8A H 0.1801 0.5691 -0.6884 0.053 Uiso 1 1 calc R U . . .
C21 C 0.0282(15) 0.5607(17) 0.1145(13) 0.053(5) Uani 1 1 d . . . . .
H21A H -0.0352 0.5332 0.1064 0.064 Uiso 1 1 calc R U . . .
C20 C 0.0472(16) 0.6604(17) 0.1348(12) 0.055(6) Uani 1 1 d . . . . .
H20A H -0.0024 0.6995 0.1421 0.066 Uiso 1 1 calc R U . . .
C13 C 0.4691(14) 0.6340(13) 0.1380(11) 0.041(4) Uani 1 1 d . . . . .
H13A H 0.5133 0.5889 0.1312 0.049 Uiso 1 1 calc R U . . .
C14 C 0.5035(13) 0.7297(14) 0.1570(12) 0.044(5) Uani 1 1 d . . . . .
H14A H 0.5693 0.7481 0.1613 0.053 Uiso 1 1 calc R U . . .
C3 C 0.5210(15) 0.8813(18) -0.6201(13) 0.055(6) Uani 1 1 d . . . . .
H3A H 0.5821 0.8606 -0.6217 0.066 Uiso 1 1 calc R U . . .
O42 O 0.2637(8) 0.3226(8) 0.1826(7) 0.032(3) Uani 1 1 d . . . . .
N6 N 0.1931(10) 0.1441(10) 0.1467(7) 0.029(3) Uani 1 1 d . . . . .
O41 O 0.2337(10) 0.3500(8) 0.0603(7) 0.040(3) Uani 1 1 d . . . . .
N5 N 0.2919(10) 0.3050(10) 0.3464(8) 0.031(3) Uani 1 1 d . . . . .
C34 C 0.1907(11) 0.1957(12) 0.0869(9) 0.027(3) Uani 1 1 d . . . . .
C33 C 0.1596(14) 0.1521(15) 0.0103(10) 0.043(4) Uani 1 1 d . . . . .
H33A H 0.1589 0.1872 -0.0303 0.052 Uiso 1 1 calc R U . . .
C35 C 0.2314(11) 0.2975(13) 0.1107(10) 0.031(4) Uani 1 1 d . . . . .
C30 C 0.1641(12) 0.0512(12) 0.1310(10) 0.034(4) Uani 1 1 d . . . . .
H30A H 0.1653 0.0167 0.1720 0.041 Uiso 1 1 calc R U . . .
C25 C 0.3257(12) 0.3969(13) 0.3586(10) 0.035(4) Uani 1 1 d . . . . .
H25A H 0.3323 0.4270 0.3155 0.042 Uiso 1 1 calc R U . . .
C29 C 0.2824(13) 0.2611(12) 0.4098(9) 0.032(4) Uani 1 1 d . . . . .
C31 C 0.1326(15) 0.0043(15) 0.0574(12) 0.049(5) Uani 1 1 d . . . . .
H31A H 0.1132 -0.0610 0.0478 0.059 Uiso 1 1 calc R U . . .
C27 C 0.3372(17) 0.4054(16) 0.4952(12) 0.053(5) Uani 1 1 d . . . . .
H27A H 0.3509 0.4407 0.5456 0.064 Uiso 1 1 calc R U . . .
C28 C 0.3033(18) 0.3100(15) 0.4861(11) 0.055(6) Uani 1 1 d . . . . .
H28A H 0.2948 0.2799 0.5290 0.066 Uiso 1 1 calc R U . . .
C32 C 0.1303(17) 0.0576(16) -0.0037(11) 0.053(5) Uani 1 1 d . . . . .
H32A H 0.1083 0.0274 -0.0545 0.064 Uiso 1 1 calc R U . . .
C26 C 0.3513(15) 0.4493(14) 0.4327(13) 0.049(5) Uani 1 1 d . . . . .
H26A H 0.3774 0.5127 0.4397 0.059 Uiso 1 1 calc R U . . .
O43 O 0.2256(9) 0.1245(8) 0.3142(6) 0.033(3) Uani 1 1 d . . . . .
OW3 O 0.4231(9) 0.4102(10) 0.0638(9) 0.049(3) Uani 1 1 d . . . . .
HW3A H 0.4246 0.3529 0.0404 0.073 Uiso 1 1 d R U . . .
HW3B H 0.4806 0.4260 0.0843 0.073 Uiso 1 1 d R U . . .
O44 O 0.2398(10) 1.1075(9) -0.5599(7) 0.043(3) Uani 1 1 d . . . . .
OW1 O 0.0671(10) 0.9941(12) -0.5977(9) 0.059(4) Uani 1 1 d . . . . .
C36 C 0.2468(13) 0.1601(12) 0.3865(9) 0.033(4) Uani 1 1 d . . . . .
OW5 O 0.3933(12) 0.2220(13) 0.0047(12) 0.078(6) Uani 1 1 d . . . . .
OW7 O 0.755(2) 0.6976(19) 0.1225(17) 0.157(13) Uani 1 1 d . . . . .
HW7A H 0.7568 0.6587 0.0803 0.236 Uiso 1 1 d R U . . .
HW7B H 0.7512 0.6657 0.1597 0.236 Uiso 1 1 d R U . . .
OW6 O 0.048(2) 0.158(3) 0.492(3) 0.12(2) Uani 0.5 1 d . . P . .
HW6A H -0.0007 0.1826 0.4766 0.181 Uiso 0.5 1 d R U P . .
HW6B H 0.0669 0.1221 0.4536 0.181 Uiso 0.5 1 d R U P . .
OW8 O -0.098(2) 0.829(2) 0.225(2) 0.168(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O13 1.700(10) . ?
Ge1 O21 1.709(11) . ?
Ge1 O12 1.727(10) . ?
Ge1 O19 1.732(10) . ?
W12 O31 1.720(12) . ?
W12 O6 1.896(11) . ?
W12 O17 1.910(10) . ?
W12 O25 1.934(11) . ?
W12 O4 1.935(12) . ?
W12 O19 2.289(10) . ?
W11 O16 1.690(12) . ?
W11 O14 1.896(10) . ?
W11 O33 1.900(13) . ?
W11 O4 1.943(12) . ?
W11 O3 1.959(11) . ?
W11 O19 2.293(10) . ?
W10 O35 1.689(11) . ?
W10 O23 1.892(13) . ?
W10 O32 1.906(11) . ?
W10 O10 1.927(13) . ?
W10 O5 1.961(12) . ?
W10 O21 2.317(10) . ?
W9 O34 1.708(11) . ?
W9 O26 1.890(12) . ?
W9 O37 1.900(11) . ?
W9 O5 1.927(12) . ?
W9 O39 1.951(12) . ?
W9 O21 2.294(11) . ?
W8 O28 1.681(11) . ?
W8 O1 1.895(11) . ?
W8 O24 1.896(14) . ?
W8 O11 1.910(12) . ?
W8 O26 1.936(12) . ?
W8 O13 2.320(10) . ?
W7 O7 1.713(12) . ?
W7 O38 1.894(11) . ?
W7 O33 1.905(12) . ?
W7 O39 1.926(11) . ?
W7 O10 1.953(12) . ?
W7 O21 2.333(11) . ?
W6 O22 1.695(11) . ?
W6 O37 1.901(12) . ?
W6 O1 1.907(11) . ?
W6 O3 1.920(12) . ?
W6 O25 1.937(12) . ?
W6 O19 2.312(10) . ?
W5 O18 1.687(13) . ?
W5 O6 1.906(11) . ?
W5 O27 1.922(11) . ?
W5 O30 1.929(11) . ?
W5 O24 1.936(11) . ?
W5 O13 2.313(11) . ?
W4 O29 1.721(11) . ?
W4 O30 1.877(11) . ?
W4 O17 1.913(11) . ?
W4 O36 1.937(12) . ?
W4 O2 1.937(11) . ?
W4 O12 2.299(10) . ?
W3 O8 1.690(12) . ?
W3 O27 1.908(12) . ?
W3 O9 1.921(11) . ?
W3 O23 1.924(12) . ?
W3 O11 1.940(12) . ?
W3 O13 2.317(10) . ?
W2 O15 1.694(12) . ?
W2 O9 1.882(12) . ?
W2 O32 1.904(11) . ?
W2 O20 1.925(12) . ?
W2 O36 1.942(12) . ?
W2 O12 2.317(10) . ?
W1 O40 1.685(13) . ?
W1 O38 1.905(11) . ?
W1 O14 1.919(10) . ?
W1 O20 1.929(12) . ?
W1 O2 1.939(12) . ?
W1 O12 2.302(10) . ?
Cu3 O41 1.941(12) . ?
Cu3 OW3 1.967(13) . ?
Cu3 N3 1.981(13) . ?
Cu3 N4 1.983(17) . ?
Cu3 O34 2.366(11) . ?
Cu2 N6 1.952(14) . ?
Cu2 N5 1.956(14) . ?
Cu2 O42 1.971(11) . ?
Cu2 O43 1.973(11) . ?
Cu2 O8 2.450(13) 2_665 ?
Cu1 O44 1.916(13) . ?
Cu1 OW1 1.971(15) . ?
Cu1 N2 1.986(14) . ?
Cu1 N1 1.986(16) . ?
Cu1 O29 2.338(10) . ?
O8 Cu2 2.450(13) 2_665 ?
N4 C22 1.33(2) . ?
N4 C23 1.36(2) . ?
N2 C10 1.31(2) . ?
N2 C11 1.35(2) . ?
C24 C16 1.39(2) . ?
C24 N3 1.40(2) . ?
C24 C23 1.40(2) . ?
N3 C13 1.33(2) . ?
N1 C1 1.33(2) . ?
N1 C12 1.38(2) . ?
C23 C19 1.39(3) . ?
C4 C3 1.37(3) . ?
C4 C12 1.38(2) . ?
C4 C5 1.44(3) . ?
C12 C11 1.44(2) . ?
C11 C7 1.38(2) . ?
C19 C20 1.39(3) . ?
C19 C18 1.48(3) . ?
C6 C5 1.31(3) . ?
C6 C7 1.43(3) . ?
C6 H6A 0.9300 . ?
C16 C15 1.39(3) . ?
C16 C17 1.43(3) . ?
C17 C18 1.36(3) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C7 C8 1.40(3) . ?
C1 C2 1.35(3) . ?
C1 H1A 0.9300 . ?
C22 C21 1.36(3) . ?
C22 H22A 0.9300 . ?
C5 H5A 0.9300 . ?
C15 C14 1.37(3) . ?
C15 H15A 0.9300 . ?
C10 C9 1.42(3) . ?
C10 H10A 0.9300 . ?
C9 C8 1.34(3) . ?
C9 H9A 0.9300 . ?
C2 C3 1.42(3) . ?
C2 H2A 0.9300 . ?
C8 H8A 0.9300 . ?
C21 C20 1.40(3) . ?
C21 H21A 0.9300 . ?
C20 H20A 0.9300 . ?
C13 C14 1.38(3) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C3 H3A 0.9300 . ?
O42 C35 1.27(2) . ?
N6 C30 1.33(2) . ?
N6 C34 1.37(2) . ?
O41 C35 1.24(2) . ?
N5 C25 1.33(2) . ?
N5 C29 1.36(2) . ?
C34 C33 1.39(2) . ?
C34 C35 1.49(2) . ?
C33 C32 1.35(3) . ?
C33 H33A 0.9300 . ?
C30 C31 1.36(3) . ?
C30 H30A 0.9300 . ?
C25 C26 1.38(3) . ?
C25 H25A 0.9300 . ?
C29 C28 1.39(2) . ?
C29 C36 1.46(2) . ?
C31 C32 1.40(3) . ?
C31 H31A 0.9300 . ?
C27 C26 1.36(3) . ?
C27 C28 1.38(3) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
C32 H32A 0.9300 . ?
C26 H26A 0.9300 . ?
O43 C36 1.274(19) . ?
OW3 HW3A 0.8518 . ?
OW3 HW3B 0.8514 . ?
O44 C36 1.292(19) 1_564 ?
C36 O44 1.292(19) 1_546 ?
OW7 HW7A 0.8445 . ?
OW7 HW7B 0.8520 . ?
OW6 HW6A 0.8423 . ?
OW6 HW6B 0.8399 . ?

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
O13 Ge1 O21 109.2(5) . . ?
O13 Ge1 O12 110.1(5) . . ?
O21 Ge1 O12 109.9(5) . . ?
O13 Ge1 O19 109.8(5) . . ?
O21 Ge1 O19 108.5(5) . . ?
O12 Ge1 O19 109.4(5) . . ?
O31 W12 O6 102.0(5) . . ?
O31 W12 O17 101.7(5) . . ?
O6 W12 O17 85.0(5) . . ?
O31 W12 O25 99.7(6) . . ?
O6 W12 O25 89.8(5) . . ?
O17 W12 O25 158.6(5) . . ?
O31 W12 O4 99.6(5) . . ?
O6 W12 O4 158.3(5) . . ?
O17 W12 O4 89.3(5) . . ?
O25 W12 O4 87.9(5) . . ?
O31 W12 O19 169.2(5) . . ?
O6 W12 O19 86.0(4) . . ?
O17 W12 O19 86.1(4) . . ?
O25 W12 O19 72.8(5) . . ?
O4 W12 O19 72.7(4) . . ?
O16 W11 O14 103.7(6) . . ?
O16 W11 O33 102.6(6) . . ?
O14 W11 O33 86.4(5) . . ?
O16 W11 O4 98.6(6) . . ?
O14 W11 O4 89.9(5) . . ?
O33 W11 O4 158.8(5) . . ?
O16 W11 O3 98.5(6) . . ?
O14 W11 O3 157.8(5) . . ?
O33 W11 O3 88.7(5) . . ?
O4 W11 O3 86.9(5) . . ?
O16 W11 O19 167.0(5) . . ?
O14 W11 O19 86.0(4) . . ?
O33 W11 O19 86.4(4) . . ?
O4 W11 O19 72.5(4) . . ?
O3 W11 O19 72.1(4) . . ?
O35 W10 O23 102.8(6) . . ?
O35 W10 O32 103.6(6) . . ?
O23 W10 O32 85.3(5) . . ?
O35 W10 O10 99.6(6) . . ?
O23 W10 O10 157.6(5) . . ?
O32 W10 O10 90.6(5) . . ?
O35 W10 O5 98.1(6) . . ?
O23 W10 O5 87.7(5) . . ?
O32 W10 O5 158.2(6) . . ?
O10 W10 O5 88.1(5) . . ?
O35 W10 O21 167.0(5) . . ?
O23 W10 O21 84.4(4) . . ?
O32 W10 O21 87.7(5) . . ?
O10 W10 O21 73.4(5) . . ?
O5 W10 O21 71.0(5) . . ?
O34 W9 O26 105.0(5) . . ?
O34 W9 O37 104.0(5) . . ?
O26 W9 O37 86.7(5) . . ?
O34 W9 O5 98.1(6) . . ?
O26 W9 O5 88.9(5) . . ?
O37 W9 O5 157.9(5) . . ?
O34 W9 O39 96.6(5) . . ?
O26 W9 O39 158.4(5) . . ?
O37 W9 O39 89.1(5) . . ?
O5 W9 O39 87.1(5) . . ?
O34 W9 O21 165.0(5) . . ?
O26 W9 O21 86.5(5) . . ?
O37 W9 O21 86.0(4) . . ?
O5 W9 O21 72.1(4) . . ?
O39 W9 O21 72.1(4) . . ?
O28 W8 O1 104.5(6) . . ?
O28 W8 O24 99.3(6) . . ?
O1 W8 O24 89.3(5) . . ?
O28 W8 O11 100.0(6) . . ?
O1 W8 O11 155.5(5) . . ?
O24 W8 O11 87.8(5) . . ?
O28 W8 O26 103.1(6) . . ?
O1 W8 O26 84.8(5) . . ?
O24 W8 O26 157.6(5) . . ?
O11 W8 O26 88.6(5) . . ?
O28 W8 O13 167.4(5) . . ?
O1 W8 O13 84.9(4) . . ?
O24 W8 O13 72.1(4) . . ?
O11 W8 O13 71.0(4) . . ?
O26 W8 O13 85.8(4) . . ?
O7 W7 O38 104.3(6) . . ?
O7 W7 O33 103.6(6) . . ?
O38 W7 O33 86.7(5) . . ?
O7 W7 O39 98.8(6) . . ?
O38 W7 O39 156.8(5) . . ?
O33 W7 O39 89.4(5) . . ?
O7 W7 O10 98.0(6) . . ?
O38 W7 O10 88.1(5) . . ?
O33 W7 O10 158.4(5) . . ?
O39 W7 O10 87.2(5) . . ?
O7 W7 O21 166.6(5) . . ?
O38 W7 O21 85.3(4) . . ?
O33 W7 O21 86.0(4) . . ?
O39 W7 O21 71.6(4) . . ?
O10 W7 O21 72.6(5) . . ?
O22 W6 O37 103.2(6) . . ?
O22 W6 O1 103.2(5) . . ?
O37 W6 O1 85.3(5) . . ?
O22 W6 O3 99.6(5) . . ?
O37 W6 O3 89.6(5) . . ?
O1 W6 O3 157.2(5) . . ?
O22 W6 O25 98.7(6) . . ?
O37 W6 O25 158.0(5) . . ?
O1 W6 O25 88.7(5) . . ?
O3 W6 O25 87.8(5) . . ?
O22 W6 O19 167.7(5) . . ?
O37 W6 O19 86.2(4) . . ?
O1 W6 O19 85.2(4) . . ?
O3 W6 O19 72.3(4) . . ?
O25 W6 O19 72.2(4) . . ?
O18 W5 O6 102.4(6) . . ?
O18 W5 O27 101.4(6) . . ?
O6 W5 O27 156.1(5) . . ?
O18 W5 O30 101.7(6) . . ?
O6 W5 O30 84.2(5) . . ?
O27 W5 O30 89.0(5) . . ?
O18 W5 O24 101.6(6) . . ?
O6 W5 O24 88.5(5) . . ?
O27 W5 O24 88.7(5) . . ?
O30 W5 O24 156.6(5) . . ?
O18 W5 O13 170.3(5) . . ?
O6 W5 O13 84.7(4) . . ?
O27 W5 O13 71.9(4) . . ?
O30 W5 O13 85.5(5) . . ?
O24 W5 O13 71.7(5) . . ?
O29 W4 O30 101.6(5) . . ?
O29 W4 O17 104.0(5) . . ?
O30 W4 O17 85.5(5) . . ?
O29 W4 O36 96.9(5) . . ?
O30 W4 O36 89.7(5) . . ?
O17 W4 O36 159.1(5) . . ?
O29 W4 O2 100.1(5) . . ?
O30 W4 O2 158.4(5) . . ?
O17 W4 O2 89.0(5) . . ?
O36 W4 O2 88.0(5) . . ?
O29 W4 O12 167.4(5) . . ?
O30 W4 O12 86.4(5) . . ?
O17 W4 O12 86.1(4) . . ?
O36 W4 O12 73.3(4) . . ?
O2 W4 O12 72.3(4) . . ?
O8 W3 O27 101.7(6) . . ?
O8 W3 O9 102.4(6) . . ?
O27 W3 O9 88.6(5) . . ?
O8 W3 O23 102.2(5) . . ?
O27 W3 O23 156.1(5) . . ?
O9 W3 O23 85.3(5) . . ?
O8 W3 O11 101.8(6) . . ?
O27 W3 O11 87.1(5) . . ?
O9 W3 O11 155.8(5) . . ?
O23 W3 O11 89.1(5) . . ?
O8 W3 O13 170.0(5) . . ?
O27 W3 O13 72.0(4) . . ?
O9 W3 O13 85.5(4) . . ?
O23 W3 O13 84.4(4) . . ?
O11 W3 O13 70.6(4) . . ?
O15 W2 O9 103.0(6) . . ?
O15 W2 O32 103.4(6) . . ?
O9 W2 O32 86.0(5) . . ?
O15 W2 O20 100.8(6) . . ?
O9 W2 O20 156.3(5) . . ?
O32 W2 O20 88.7(5) . . ?
O15 W2 O36 98.5(6) . . ?
O9 W2 O36 88.7(5) . . ?
O32 W2 O36 158.2(5) . . ?
O20 W2 O36 87.6(5) . . ?
O15 W2 O12 168.1(5) . . ?
O9 W2 O12 85.1(4) . . ?
O32 W2 O12 85.7(5) . . ?
O20 W2 O12 71.4(4) . . ?
O36 W2 O12 72.8(4) . . ?
O40 W1 O38 103.7(6) . . ?
O40 W1 O14 103.0(6) . . ?
O38 W1 O14 85.2(5) . . ?
O40 W1 O20 99.9(6) . . ?
O38 W1 O20 89.7(5) . . ?
O14 W1 O20 157.0(5) . . ?
O40 W1 O2 99.4(6) . . ?
O38 W1 O2 156.9(5) . . ?
O14 W1 O2 88.7(5) . . ?
O20 W1 O2 87.3(5) . . ?
O40 W1 O12 168.1(5) . . ?
O38 W1 O12 85.1(4) . . ?
O14 W1 O12 85.5(4) . . ?
O20 W1 O12 71.7(4) . . ?
O2 W1 O12 72.2(4) . . ?
O41 Cu3 OW3 87.8(6) . . ?
O41 Cu3 N3 175.2(6) . . ?
OW3 Cu3 N3 96.4(6) . . ?
O41 Cu3 N4 93.0(6) . . ?
OW3 Cu3 N4 177.3(6) . . ?
N3 Cu3 N4 82.9(6) . . ?
O41 Cu3 O34 101.0(5) . . ?
OW3 Cu3 O34 93.6(5) . . ?
N3 Cu3 O34 81.1(5) . . ?
N4 Cu3 O34 83.7(5) . . ?
N6 Cu2 N5 175.4(6) . . ?
N6 Cu2 O42 83.2(5) . . ?
N5 Cu2 O42 95.0(5) . . ?
N6 Cu2 O43 98.3(5) . . ?
N5 Cu2 O43 83.3(5) . . ?
O42 Cu2 O43 177.0(5) . . ?
N6 Cu2 O8 83.0(5) . 2_665 ?
N5 Cu2 O8 101.4(5) . 2_665 ?
O42 Cu2 O8 97.4(5) . 2_665 ?
O43 Cu2 O8 85.4(5) . 2_665 ?
O44 Cu1 OW1 90.5(7) . . ?
O44 Cu1 N2 174.6(6) . . ?
OW1 Cu1 N2 94.6(7) . . ?
O44 Cu1 N1 91.4(6) . . ?
OW1 Cu1 N1 172.4(6) . . ?
N2 Cu1 N1 83.2(6) . . ?
O44 Cu1 O29 91.6(5) . . ?
OW1 Cu1 O29 87.5(5) . . ?
N2 Cu1 O29 90.3(5) . . ?
N1 Cu1 O29 99.8(5) . . ?
W7 O38 W1 152.5(6) . . ?
W9 O37 W6 151.2(6) . . ?
W4 O36 W2 120.4(6) . . ?
W9 O34 Cu3 174.1(7) . . ?
W11 O33 W7 150.4(6) . . ?
W2 O32 W10 151.6(7) . . ?
W4 O30 W5 152.7(6) . . ?
W4 O29 Cu1 140.4(7) . . ?
W3 O27 W5 122.9(6) . . ?
W9 O26 W8 150.6(7) . . ?
W12 O25 W6 120.9(6) . . ?
W8 O24 W5 123.0(6) . . ?
W10 O23 W3 152.8(6) . . ?
Ge1 O21 W9 123.4(6) . . ?
Ge1 O21 W10 121.7(6) . . ?
W9 O21 W10 94.9(4) . . ?
Ge1 O21 W7 121.8(5) . . ?
W9 O21 W7 94.3(4) . . ?
W10 O21 W7 93.1(4) . . ?
W2 O20 W1 122.7(6) . . ?
Ge1 O19 W12 121.8(5) . . ?
Ge1 O19 W11 122.6(5) . . ?
W12 O19 W11 94.5(4) . . ?
Ge1 O19 W6 122.0(5) . . ?
W12 O19 W6 94.1(4) . . ?
W11 O19 W6 94.4(4) . . ?
W12 O17 W4 151.3(6) . . ?
W11 O14 W1 152.1(6) . . ?
Ge1 O13 W5 122.7(5) . . ?
Ge1 O13 W3 122.3(6) . . ?
W5 O13 W3 93.2(4) . . ?
Ge1 O13 W8 123.0(5) . . ?
W5 O13 W8 93.2(4) . . ?
W3 O13 W8 94.4(4) . . ?
Ge1 O12 W4 121.7(5) . . ?
Ge1 O12 W1 122.7(5) . . ?
W4 O12 W1 94.4(4) . . ?
Ge1 O12 W2 122.6(5) . . ?
W4 O12 W2 93.6(4) . . ?
W1 O12 W2 94.1(4) . . ?
W8 O11 W3 124.1(6) . . ?
W10 O10 W7 120.8(7) . . ?
W2 O9 W3 152.3(6) . . ?
W3 O8 Cu2 142.0(7) . 2_665 ?
W12 O6 W5 153.7(7) . . ?
W9 O5 W10 121.9(7) . . ?
W12 O4 W11 120.3(6) . . ?
W6 O3 W11 121.2(6) . . ?
W4 O2 W1 121.1(6) . . ?
W8 O1 W6 153.8(7) . . ?
C22 N4 C23 120.0(18) . . ?
C22 N4 Cu3 128.1(14) . . ?
C23 N4 Cu3 111.7(12) . . ?
W7 O39 W9 122.0(6) . . ?
C10 N2 C11 118.0(18) . . ?
C10 N2 Cu1 129.9(16) . . ?
C11 N2 Cu1 112.0(11) . . ?
C16 C24 N3 123.3(16) . . ?
C16 C24 C23 122.2(18) . . ?
N3 C24 C23 114.5(15) . . ?
C13 N3 C24 116.5(14) . . ?
C13 N3 Cu3 131.2(13) . . ?
C24 N3 Cu3 112.2(10) . . ?
C1 N1 C12 116.0(17) . . ?
C1 N1 Cu1 131.2(14) . . ?
C12 N1 Cu1 112.8(11) . . ?
N4 C23 C19 121.3(18) . . ?
N4 C23 C24 118.2(18) . . ?
C19 C23 C24 120.5(18) . . ?
C3 C4 C12 117.2(18) . . ?
C3 C4 C5 124(2) . . ?
C12 C4 C5 118.3(17) . . ?
C4 C12 N1 124.7(16) . . ?
C4 C12 C11 121.3(15) . . ?
N1 C12 C11 114.0(15) . . ?
N2 C11 C7 123.9(15) . . ?
N2 C11 C12 117.7(14) . . ?
C7 C11 C12 118.4(15) . . ?
C23 C19 C20 119(2) . . ?
C23 C19 C18 117.5(18) . . ?
C20 C19 C18 124(2) . . ?
C5 C6 C7 123.6(18) . . ?
C5 C6 H6A 118.2 . . ?
C7 C6 H6A 118.2 . . ?
C24 C16 C15 117(2) . . ?
C24 C16 C17 118.4(18) . . ?
C15 C16 C17 124.7(19) . . ?
C18 C17 C16 120.9(18) . . ?
C18 C17 H17A 119.5 . . ?
C16 C17 H17A 119.5 . . ?
C17 C18 C19 120.6(19) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C11 C7 C8 118.1(18) . . ?
C11 C7 C6 118.4(16) . . ?
C8 C7 C6 123.4(19) . . ?
N1 C1 C2 123(2) . . ?
N1 C1 H1A 118.3 . . ?
C2 C1 H1A 118.3 . . ?
N4 C22 C21 121(2) . . ?
N4 C22 H22A 119.4 . . ?
C21 C22 H22A 119.4 . . ?
C6 C5 C4 119.9(18) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C14 C15 C16 120.6(18) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
N2 C10 C9 121(2) . . ?
N2 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C8 C9 C10 121.4(19) . . ?
C8 C9 H9A 119.3 . . ?
C10 C9 H9A 119.3 . . ?
C1 C2 C3 120(2) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
C9 C8 C7 117.8(19) . . ?
C9 C8 H8A 121.1 . . ?
C7 C8 H8A 121.1 . . ?
C22 C21 C20 121(2) . . ?
C22 C21 H21A 119.4 . . ?
C20 C21 H21A 119.4 . . ?
C19 C20 C21 117(2) . . ?
C19 C20 H20A 121.3 . . ?
C21 C20 H20A 121.3 . . ?
N3 C13 C14 123.3(19) . . ?
N3 C13 H13A 118.3 . . ?
C14 C13 H13A 118.3 . . ?
C15 C14 C13 119.3(18) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3A 120.9 . . ?
C2 C3 H3A 120.9 . . ?
C35 O42 Cu2 114.6(10) . . ?
C30 N6 C34 119.1(14) . . ?
C30 N6 Cu2 128.5(12) . . ?
C34 N6 Cu2 112.4(11) . . ?
C35 O41 Cu3 116.4(11) . . ?
C25 N5 C29 118.5(15) . . ?
C25 N5 Cu2 128.2(12) . . ?
C29 N5 Cu2 113.2(11) . . ?
N6 C34 C33 121.1(16) . . ?
N6 C34 C35 114.1(14) . . ?
C33 C34 C35 124.6(15) . . ?
C32 C33 C34 118.4(18) . . ?
C32 C33 H33A 120.8 . . ?
C34 C33 H33A 120.8 . . ?
O41 C35 O42 125.3(16) . . ?
O41 C35 C34 119.1(15) . . ?
O42 C35 C34 115.6(14) . . ?
N6 C30 C31 122.8(17) . . ?
N6 C30 H30A 118.6 . . ?
C31 C30 H30A 118.6 . . ?
N5 C25 C26 122.6(17) . . ?
N5 C25 H25A 118.7 . . ?
C26 C25 H25A 118.7 . . ?
N5 C29 C28 122.1(17) . . ?
N5 C29 C36 111.8(13) . . ?
C28 C29 C36 126.0(16) . . ?
C30 C31 C32 117.9(18) . . ?
C30 C31 H31A 121.1 . . ?
C32 C31 H31A 121.1 . . ?
C26 C27 C28 121.9(19) . . ?
C26 C27 H27A 119.1 . . ?
C28 C27 H27A 119.1 . . ?
C27 C28 C29 116.8(19) . . ?
C27 C28 H28A 121.6 . . ?
C29 C28 H28A 121.6 . . ?
C33 C32 C31 120.8(18) . . ?
C33 C32 H32A 119.6 . . ?
C31 C32 H32A 119.6 . . ?
C27 C26 C25 117.9(18) . . ?
C27 C26 H26A 121.0 . . ?
C25 C26 H26A 121.0 . . ?
C36 O43 Cu2 111.5(10) . . ?
Cu3 OW3 HW3A 127.0 . . ?
Cu3 OW3 HW3B 127.2 . . ?
HW3A OW3 HW3B 103.3 . . ?
C36 O44 Cu1 117.8(11) 1_564 . ?
O43 C36 O44 121.0(16) . 1_546 ?
O43 C36 C29 120.0(14) . . ?
O44 C36 C29 119.0(15) 1_546 . ?
HW7A OW7 HW7B 108.0 . . ?
HW6A OW6 HW6B 109.4 . . ?

_refine_diff_density_max         6.947
_refine_diff_density_min         -4.023
_refine_diff_density_rms         0.388

