# Electronic Supplementary Material (ESI) for Green Chemistry.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_mcm
_database_code_depnum_ccdc_archive 'CCDC 2023524'
loop_
_audit_author_name
_audit_author_address
'Haijun Haijun Pang'
;Harbin University of Science and Technology
China
;
_audit_update_record             
;
2020-08-16 deposited with the CCDC.	2021-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_mcm                 
;
PROBLEM: Short Inter D...A Contact O2   ..Ow4  .2.29 Ang.
x,y,z =   1_555 Check
RESPONSE: There are hydrogen bonds between atoms O2/Ow4,
Ow4/O15??Ow4/O24 and Ow2/O24.
;
_vrf_PLAT043_mcm                 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by..   92.78 Check
RESPONSE: Because individual oxygen atoms and water molecules are 
disordered, i did a half occupancy on these atoms. Meanwhile, there are 
also hydrogen atoms on the water molecules that are added directly. 
Therefore, the given formula is different from the calculated formula.
;
_vrf_PLAT306_mcm                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?).......   Ow1 Check
RESPONSE: H-atoms were not localized for Ow1/Ow2/Ow3 water molecules
because the H-atoms on water molecules cannot be found from the
residual peaks.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H46 Cu2 Ge N12 O48 W12'
_chemical_formula_weight         3772.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'Cm   '

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

_cell_length_a                   12.5419(5)
_cell_length_b                   22.4521(9)
_cell_length_c                   11.6246(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.9510(10)
_cell_angle_gamma                90.00
_cell_volume                     3076.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9902
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      28.34

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3256.3
_exptl_absorpt_coefficient_mu    23.593
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22556
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         28.38
_reflns_number_total             7802
_reflns_number_gt                6397
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0688P)²+182.8526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_number_reflns         7802
_refine_ls_number_parameters     441
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1487
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.8535(3) 0.67454(10) 1.0195(3) 0.0272(5) Uani 1 1 d . . .
Ge Ge 0.8552(3) 0.5000 0.5293(3) 0.0082(4) Uani 1 2 d S . .
W1 W 0.88118(9) 0.58015(5) 0.79254(9) 0.0314(3) Uani 1 1 d . . .
W2 W 0.81830(8) 0.57511(4) 0.25380(7) 0.0237(2) Uani 1 1 d . . .
W3 W 1.12241(12) 0.5000 0.76635(12) 0.0229(3) Uani 1 2 d S . .
W4 W 0.84976(10) 0.65794(3) 0.53686(10) 0.0240(2) Uani 1 1 d . . .
W5 W 1.09450(7) 0.57617(4) 0.50557(8) 0.0235(2) Uani 1 1 d . . .
W6 W 0.62488(8) 0.58211(4) 0.56064(8) 0.0240(2) Uani 1 1 d . . .
W7 W 0.59334(12) 0.5000 0.27896(12) 0.0226(3) Uani 1 2 d S . .
O1 O 1.1765(16) 0.5591(7) 0.6755(15) 0.032(4) Uani 1 1 d . . .
OW1 O 1.407(3) 0.5000 0.686(3) 0.048(7) Uani 1 2 d SU . .
O2 O 0.9768(12) 0.5709(6) 0.3538(13) 0.024(3) Uani 1 1 d DU . .
OW2 O 1.335(2) 0.5000 0.379(3) 0.063(10) Uani 1 2 d SD . .
OW3 O 0.643(2) 0.5000 0.913(2) 0.066(10) Uani 1 2 d S . .
O3 O 0.8018(13) 0.6258(6) 0.3742(13) 0.023(3) Uani 1 1 d . . .
O4 O 0.862(2) 0.7314(6) 0.5198(19) 0.035(4) Uani 1 1 d . . .
OW4 O 1.0285(17) 0.5000 0.2417(19) 0.039(11) Uani 0.50 2 d SPDU . .
O5 O 0.9978(14) 0.6270(7) 0.5545(15) 0.026(3) Uani 1 1 d . . .
O6 O 1.0030(17) 0.5000 0.5651(18) 0.021(4) Uani 1 2 d SU . .
O7 O 1.2361(17) 0.5000 0.911(2) 0.029(5) Uani 1 2 d SU . .
O8 O 1.0235(12) 0.5589(6) 0.7905(13) 0.020(3) Uani 1 1 d . . .
O9 O 0.845(2) 0.5000 0.812(2) 0.033(5) Uani 1 2 d S . .
O10 O 0.4593(19) 0.5000 0.184(2) 0.027(5) Uani 1 2 d SU . .
O11 O 0.7143(13) 0.5950(7) 0.7335(12) 0.025(3) Uani 1 1 d . . .
O12 O 0.9058(18) 0.6102(8) 0.9371(17) 0.039(4) Uani 1 1 d U . .
O13 O 0.8148(18) 0.6221(8) 0.1395(16) 0.037(4) Uani 1 1 d . . .
O14 O 0.5039(19) 0.6124(10) 0.5667(19) 0.047(5) Uani 1 1 d . . .
O15 O 0.8333(16) 0.5000 0.176(2) 0.034(6) Uani 1 2 d SD . .
O16 O 1.1931(19) 0.6203(10) 0.478(2) 0.050(6) Uani 1 1 d . . .
O17 O 0.8894(13) 0.6553(6) 0.7096(14) 0.027(3) Uani 1 1 d . . .
O18 O 0.6918(14) 0.6533(8) 0.5257(12) 0.031(4) Uani 1 1 d . . .
O19 O 0.5927(15) 0.5582(7) 0.4006(14) 0.029(4) Uani 1 1 d . . .
O20 O 0.611(2) 0.5000 0.597(2) 0.022(5) Uani 0.90 2 d SP . .
O21 O 0.6647(16) 0.5612(7) 0.2144(18) 0.039(5) Uani 1 1 d . . .
O22 O 0.7893(18) 0.5000 0.3744(17) 0.020(4) Uani 1 2 d S . .
O23 O 0.8158(12) 0.5618(5) 0.5905(12) 0.018(3) Uani 1 1 d U . .
O24 O 1.144(2) 0.5000 0.4648(19) 0.059(9) Uani 1 2 d SD . .
N1 N 0.7339(8) 0.7264(4) 0.9165(8) 0.018(4) Uani 1 1 d G . .
N2 N 0.992(2) 0.7208(9) 1.1274(17) 0.032(5) Uani 1 1 d . . .
N3 N 0.6962(10) 0.7149(5) 0.7934(10) 0.035(5) Uani 1 1 d GU . .
H3B H 0.7035 0.6818 0.7596 0.042 Uiso 1 1 calc R . .
N4 N 1.0289(16) 0.7081(7) 1.2432(16) 0.048(6) Uani 1 1 d . . .
H4B H 1.0239 0.6731 1.2713 0.057 Uiso 1 1 calc R . .
N5 N 0.7908(16) 0.8708(7) 1.2713(16) 0.079(10) Uani 1 1 d RU . .
N6 N 0.9316(16) 0.8688(7) 0.7804(16) 0.074(9) Uani 1 1 d RU . .
C1 C 0.6511(9) 0.8081(5) 0.8195(9) 0.027(5) Uani 1 1 d GU . .
H1A H 0.6229 0.8467 0.8039 0.032 Uiso 1 1 calc R . .
C2 C 0.7285(8) 0.8130(4) 1.0478(8) 0.031(6) Uani 1 1 d R . .
C3 C 0.7242(12) 0.8748(5) 1.0527(11) 0.070(11) Uani 1 1 d R . .
H3A H 0.7013 0.8969 0.9808 0.084 Uiso 1 1 d R . .
C4 C 0.7542(15) 0.9035(6) 1.1651(14) 0.067(10) Uani 1 1 d RU . .
H4A H 0.7501 0.9447 1.1684 0.081 Uiso 1 1 d R . .
C5 C 0.7927(13) 0.8087(7) 1.2677(12) 0.053(9) Uani 1 1 d R . .
H5A H 0.8143 0.7866 1.3397 0.064 Uiso 1 1 d R . .
C6 C 0.7627(10) 0.7800(5) 1.1553(9) 0.025(5) Uani 1 1 d RU . .
H6A H 0.7655 0.7387 1.1520 0.031 Uiso 1 1 d R . .
C7 C 1.0141(12) 0.7788(8) 1.1175(13) 0.028(5) Uani 1 1 d GU . .
C8 C 1.076(3) 0.7550(13) 1.316(3) 0.049(7) Uani 1 1 d U . .
H8A H 1.1116 0.7552 1.4001 0.058 Uiso 1 1 calc R . .
C9 C 1.0600(11) 0.8042(6) 1.2336(12) 0.060(10) Uani 1 1 d . . .
H9A H 1.0764 0.8441 1.2532 0.071 Uiso 1 1 calc R . .
C10 C 0.9822(11) 0.8086(6) 0.9989(12) 0.031(6) Uani 1 1 d R . .
C11 C 0.9605(11) 0.7777(6) 0.8896(12) 0.042(7) Uani 1 1 d R . .
H11A H 0.9637 0.7363 0.8900 0.050 Uiso 1 1 d R . .
C12 C 0.9341(11) 0.8086(6) 0.7799(12) 0.054(8) Uani 1 1 d R . .
H12A H 0.9190 0.7881 0.7065 0.065 Uiso 1 1 d R . .
C13 C 0.9509(11) 0.9014(6) 0.8886(12) 0.089(13) Uani 1 1 d RU . .
H13A H 0.9470 0.9428 0.8871 0.107 Uiso 1 1 d R . .
C14 C 0.9774(11) 0.8705(6) 0.9983(12) 0.064(10) Uani 1 1 d RU . .
H14A H 0.9918 0.8911 1.0714 0.076 Uiso 1 1 d R . .
C15 C 0.7060(7) 0.7841(3) 0.9327(7) 0.020(4) Uani 1 1 d G . .
C16 C 0.6451(10) 0.7654(6) 0.7334(11) 0.040(6) Uani 1 1 d GU . .
H16A H 0.6120 0.7698 0.6491 0.048 Uiso 0.47 1 calc PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.953(10) . ?
Cu1 O12 1.965(16) . ?
Cu1 O13 2.007(17) 1_556 ?
Cu1 N2 2.04(2) . ?
Ge O22 1.71(2) . ?
Ge O23 1.707(13) 2_565 ?
Ge O23 1.707(13) . ?
Ge O6 1.76(2) . ?
W1 O12 1.738(17) . ?
W1 O8 1.855(14) . ?
W1 O9 1.888(8) . ?
W1 O17 1.963(15) . ?
W1 O11 1.995(16) . ?
W1 O23 2.246(13) . ?
W2 O13 1.686(17) . ?
W2 O21 1.848(19) . ?
W2 O3 1.868(14) . ?
W2 O2 1.932(15) . ?
W2 O15 1.951(12) . ?
W2 O22 2.300(12) . ?
W3 O7 1.79(2) . ?
W3 O8 1.899(13) . ?
W3 O8 1.899(13) 2_565 ?
W3 O1 1.957(15) 2_565 ?
W3 O1 1.957(16) . ?
W3 O6 2.31(2) . ?
W4 O4 1.675(14) . ?
W4 O17 1.898(15) . ?
W4 O3 1.919(14) . ?
W4 O5 1.927(16) . ?
W4 O18 1.944(17) . ?
W4 O23 2.327(12) . ?
W5 O16 1.697(17) . ?
W5 O2 1.878(15) . ?
W5 O5 1.889(15) . ?
W5 O1 1.928(17) . ?
W5 O24 1.932(10) . ?
W5 O6 2.294(13) . ?
W6 O14 1.686(19) . ?
W6 O19 1.843(16) . ?
W6 O18 1.913(16) . ?
W6 O20 1.914(6) . ?
W6 O11 1.960(14) . ?
W6 O23 2.344(14) . ?
W7 O10 1.67(2) . ?
W7 O21 1.927(16) 2_565 ?
W7 O21 1.927(16) . ?
W7 O19 1.928(16) . ?
W7 O19 1.928(16) 2_565 ?
W7 O22 2.33(2) . ?
O6 W5 2.294(13) 2_565 ?
O9 W1 1.888(7) 2_565 ?
O13 Cu1 2.007(17) 1_554 ?
O15 W2 1.951(12) 2_565 ?
O20 W6 1.914(6) 2_565 ?
O22 W2 2.300(12) 2_565 ?
O24 W5 1.932(10) 2_565 ?
N1 N3 1.370(4) . ?
N1 C15 1.371(4) . ?
N2 N4 1.30(2) . ?
N2 C7 1.35(3) . ?
N3 C16 1.370(4) . ?
N4 C8 1.35(3) . ?
N5 C4 1.37(2) . ?
N5 C5 1.40(2) . ?
N6 C12 1.35(2) . ?
N6 C13 1.40(2) . ?
C1 C16 1.370(4) . ?
C1 C15 1.370(4) . ?
C2 C3 1.389(4) . ?
C2 C6 1.389(4) . ?
C2 C15 1.426(5) . ?
C3 C4 1.389(4) . ?
C5 C6 1.388(4) . ?
C7 C9 1.396(17) . ?
C7 C10 1.46(2) . ?
C8 C9 1.43(3) . ?
C10 C11 1.3901 . ?
C10 C14 1.3901 . ?
C11 C12 1.3899 . ?
C13 C14 1.3900 . ?

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
N1 Cu1 O12 117.0(7) . . ?
N1 Cu1 O13 117.3(7) . 1_556 ?
O12 Cu1 O13 96.2(7) . 1_556 ?
N1 Cu1 N2 112.7(6) . . ?
O12 Cu1 N2 108.6(9) . . ?
O13 Cu1 N2 103.1(8) 1_556 . ?
O22 Ge O23 109.5(6) . 2_565 ?
O22 Ge O23 109.5(6) . . ?
O23 Ge O23 108.7(9) 2_565 . ?
O22 Ge O6 110.0(10) . . ?
O23 Ge O6 109.5(6) 2_565 . ?
O23 Ge O6 109.5(6) . . ?
O12 W1 O8 104.9(8) . . ?
O12 W1 O9 103.0(10) . . ?
O8 W1 O9 91.6(9) . . ?
O12 W1 O17 96.8(8) . . ?
O8 W1 O17 90.1(7) . . ?
O9 W1 O17 158.8(9) . . ?
O12 W1 O11 95.0(8) . . ?
O8 W1 O11 159.9(6) . . ?
O9 W1 O11 86.2(9) . . ?
O17 W1 O11 85.0(6) . . ?
O12 W1 O23 164.5(7) . . ?
O8 W1 O23 87.1(6) . . ?
O9 W1 O23 86.1(8) . . ?
O17 W1 O23 72.9(5) . . ?
O11 W1 O23 72.8(5) . . ?
O13 W2 O21 99.5(9) . . ?
O13 W2 O3 103.3(7) . . ?
O21 W2 O3 85.2(8) . . ?
O13 W2 O2 104.5(9) . . ?
O21 W2 O2 155.8(7) . . ?
O3 W2 O2 86.2(6) . . ?
O13 W2 O15 99.1(9) . . ?
O21 W2 O15 89.8(8) . . ?
O3 W2 O15 157.6(8) . . ?
O2 W2 O15 89.7(8) . . ?
O13 W2 O22 166.5(8) . . ?
O21 W2 O22 70.1(7) . . ?
O3 W2 O22 84.8(6) . . ?
O2 W2 O22 86.7(7) . . ?
O15 W2 O22 73.0(7) . . ?
O7 W3 O8 102.3(7) . . ?
O7 W3 O8 102.3(7) . 2_565 ?
O8 W3 O8 88.3(9) . 2_565 ?
O7 W3 O1 101.2(8) . 2_565 ?
O8 W3 O1 156.5(7) . 2_565 ?
O8 W3 O1 88.4(7) 2_565 2_565 ?
O7 W3 O1 101.2(8) . . ?
O8 W3 O1 88.4(7) . . ?
O8 W3 O1 156.5(7) 2_565 . ?
O1 W3 O1 85.4(9) 2_565 . ?
O7 W3 O6 169.3(9) . . ?
O8 W3 O6 85.3(6) . . ?
O8 W3 O6 85.3(6) 2_565 . ?
O1 W3 O6 71.2(6) 2_565 . ?
O1 W3 O6 71.2(6) . . ?
O4 W4 O17 98.9(9) . . ?
O4 W4 O3 105.3(8) . . ?
O17 W4 O3 155.7(7) . . ?
O4 W4 O5 104.0(9) . . ?
O17 W4 O5 88.9(7) . . ?
O3 W4 O5 86.3(6) . . ?
O4 W4 O18 100.3(10) . . ?
O17 W4 O18 87.8(6) . . ?
O3 W4 O18 86.8(6) . . ?
O5 W4 O18 155.7(7) . . ?
O4 W4 O23 168.1(9) . . ?
O17 W4 O23 72.1(5) . . ?
O3 W4 O23 83.7(5) . . ?
O5 W4 O23 84.0(6) . . ?
O18 W4 O23 72.1(6) . . ?
O16 W5 O2 104.5(9) . . ?
O16 W5 O5 106.7(9) . . ?
O2 W5 O5 86.6(6) . . ?
O16 W5 O1 98.0(10) . . ?
O2 W5 O1 157.4(7) . . ?
O5 W5 O1 89.1(7) . . ?
O16 W5 O24 99.0(9) . . ?
O2 W5 O24 85.9(9) . . ?
O5 W5 O24 154.3(8) . . ?
O1 W5 O24 88.4(8) . . ?
O16 W5 O6 164.4(10) . . ?
O2 W5 O6 85.6(7) . . ?
O5 W5 O6 85.5(6) . . ?
O1 W5 O6 71.9(7) . . ?
O24 W5 O6 69.5(7) . . ?
O14 W6 O19 105.6(9) . . ?
O14 W6 O18 97.9(10) . . ?
O19 W6 O18 89.4(6) . . ?
O14 W6 O20 103.0(11) . . ?
O19 W6 O20 86.5(8) . . ?
O18 W6 O20 159.0(9) . . ?
O14 W6 O11 96.1(9) . . ?
O19 W6 O11 158.3(7) . . ?
O18 W6 O11 87.4(6) . . ?
O20 W6 O11 88.8(9) . . ?
O14 W6 O23 163.9(9) . . ?
O19 W6 O23 87.3(6) . . ?
O18 W6 O23 72.2(6) . . ?
O20 W6 O23 87.0(8) . . ?
O11 W6 O23 71.3(6) . . ?
O10 W7 O21 103.8(8) . 2_565 ?
O10 W7 O21 103.8(8) . . ?
O21 W7 O21 91.1(10) 2_565 . ?
O10 W7 O19 103.3(7) . . ?
O21 W7 O19 152.7(8) 2_565 . ?
O21 W7 O19 85.4(7) . . ?
O10 W7 O19 103.3(8) . 2_565 ?
O21 W7 O19 85.4(7) 2_565 2_565 ?
O21 W7 O19 152.7(8) . 2_565 ?
O19 W7 O19 85.4(9) . 2_565 ?
O10 W7 O22 168.1(9) . . ?
O21 W7 O22 68.3(6) 2_565 . ?
O21 W7 O22 68.3(6) . . ?
O19 W7 O22 85.3(6) . . ?
O19 W7 O22 85.3(6) 2_565 . ?
W5 O1 W3 121.7(9) . . ?
W5 O2 W2 151.6(8) . . ?
W2 O3 W4 152.8(9) . . ?
W5 O5 W4 151.7(9) . . ?
Ge O6 W5 121.7(6) . 2_565 ?
Ge O6 W5 121.7(6) . . ?
W5 O6 W5 96.4(7) 2_565 . ?
Ge O6 W3 120.5(10) . . ?
W5 O6 W3 95.0(6) 2_565 . ?
W5 O6 W3 95.0(6) . . ?
W1 O8 W3 149.4(8) . . ?
W1 O9 W1 144.7(14) . 2_565 ?
W6 O11 W1 119.6(7) . . ?
W1 O12 Cu1 141.0(12) . . ?
W2 O13 Cu1 165.4(13) . 1_554 ?
W2 O15 W2 119.6(12) . 2_565 ?
W4 O17 W1 120.5(7) . . ?
W6 O18 W4 122.8(9) . . ?
W6 O19 W7 152.0(9) . . ?
W6 O20 W6 148.8(12) 2_565 . ?
W2 O21 W7 127.4(9) . . ?
Ge O22 W2 121.5(7) . 2_565 ?
Ge O22 W2 121.5(7) . . ?
W2 O22 W2 94.3(6) 2_565 . ?
Ge O22 W7 123.8(10) . . ?
W2 O22 W7 94.0(6) 2_565 . ?
W2 O22 W7 94.0(6) . . ?
Ge O23 W1 122.0(7) . . ?
Ge O23 W4 122.5(7) . . ?
W1 O23 W4 94.3(5) . . ?
Ge O23 W6 121.5(7) . . ?
W1 O23 W6 96.3(5) . . ?
W4 O23 W6 92.9(5) . . ?
W5 O24 W5 124.6(11) 2_565 . ?
N3 N1 C15 108.0 . . ?
N3 N1 Cu1 116.5(4) . . ?
C15 N1 Cu1 131.1(4) . . ?
N4 N2 C7 107.0(16) . . ?
N4 N2 Cu1 117.0(15) . . ?
C7 N2 Cu1 126.7(14) . . ?
C16 N3 N1 108.1 . . ?
N2 N4 C8 113.5(19) . . ?
C4 N5 C5 120.7(16) . . ?
C12 N6 C13 122.0(16) . . ?
C16 C1 C15 108.0 . . ?
C3 C2 C6 120.0 . . ?
C3 C2 C15 119.7 . . ?
C6 C2 C15 120.2 . . ?
C2 C3 C4 120.0 . . ?
N5 C4 C3 119.9(9) . . ?
C6 C5 N5 119.3(10) . . ?
C5 C6 C2 120.0 . . ?
N2 C7 C9 109.9(15) . . ?
N2 C7 C10 121.7(13) . . ?
C9 C7 C10 128.1(16) . . ?
N4 C8 C9 105(2) . . ?
C7 C9 C8 104.4(17) . . ?
C11 C10 C14 120.0 . . ?
C11 C10 C7 122.7(8) . . ?
C14 C10 C7 117.3(8) . . ?
C12 C11 C10 120.0 . . ?
N6 C12 C11 119.6(9) . . ?
C14 C13 N6 118.4(8) . . ?
C13 C14 C10 120.0 . . ?
C1 C15 N1 108.0 . . ?
C1 C15 C2 126.5 . . ?
N1 C15 C2 125.5 . . ?
N3 C16 C1 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.38
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         6.782
_refine_diff_density_min         -2.548
_refine_diff_density_rms         0.438
####################################################################### 
# 
# 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_sqb1
_database_code_depnum_ccdc_archive 'CCDC 2023544'
loop_
_audit_author_name
_audit_author_address
'Haijun Haijun Pang'
;Harbin University of Science and Technology
China
;
_audit_update_record             
;
2020-08-16 deposited with the CCDC.	2021-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_sqb1                
;
PROBLEM: Calculated and Reported Mol. Weight Differ by..   88.03 Check
RESPONSE: Because individual oxygen atoms and water molecules are disordered, 
i did a half occupancy on these atoms. Meanwhile, there are also hydrogen atoms
on the water molecules that are added directly. Therefore, the given formula 
is different from the calculated formula.
;
_vrf_PLAT342_sqb1                
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.058 Ang
RESPONSE: The ligand of 2-ptza is a flexible molecule collected at room 
temperature, it is unsurprising that low bond precision on C-C is present 
due to thermal motion.
;
_vrf_PLAT780_sqb1                
;
PROBLEM: Coordinates do not Form a Properly Connected Set  Please Do !
RESPONSE: The error represents some segments are out the cell,
however, if we move the segments would make the refinement difficult
because of the unit cell volumes is a little large. But it does not affect the
crystal structure analysis.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H32 Cu5 W12 N30 O44 Ge'
_chemical_formula_sum            'C36 H32 Cu5 W12 N30 O44 Ge'
_chemical_formula_weight         4121.2675

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.203(5)
_cell_length_b                   13.495(5)
_cell_length_c                   14.262(5)
_cell_angle_alpha                104.873(5)
_cell_angle_beta                 111.480(5)
_cell_angle_gamma                105.681(5)
_cell_volume                     1931.3(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2906
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      26.58

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1883
_exptl_absorpt_coefficient_mu    19.624
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11292
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.25
_reflns_number_total             6968
_reflns_number_gt                5720
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+400.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6968
_refine_ls_number_parameters     616
_refine_ls_number_restraints     918
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0934
_refine_ls_wR_factor_ref         0.2006
_refine_ls_wR_factor_gt          0.1908
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge 1.0000 -1.5000 -2.0000 0.0202(8) Uani 1 2 d S . .
W1 W 0.69784(11) -1.69745(9) -2.22296(10) 0.0277(3) Uani 1 1 d . . .
W2 W 0.84427(11) -1.75769(9) -1.99112(9) 0.0255(3) Uani 1 1 d . . .
W3 W 1.14740(14) -1.56214(12) -1.77010(10) 0.0344(3) Uani 1 1 d U . .
W4 W 0.71759(12) -1.55042(12) -1.96755(11) 0.0367(3) Uani 1 1 d . . .
W5 W 0.97910(17) -1.64570(10) -2.25510(11) 0.0454(4) Uani 1 1 d . . .
W6 W 1.12440(15) -1.70742(11) -2.02692(11) 0.0444(4) Uani 1 1 d U . .
Cu1 Cu 0.4670(3) -1.9517(3) -1.6269(3) 0.0255(7) Uani 1 1 d . . .
Cu2 Cu 0.6501(3) -1.4437(3) -1.5311(3) 0.0233(7) Uani 1 1 d . . .
Cu3 Cu 1.0000 -1.0000 -1.5000 0.0369(13) Uani 1 2 d S . .
N1 N 0.864(3) -1.226(2) -1.477(2) 0.036(6) Uani 1 1 d . . .
N2 N 0.758(3) -1.309(2) -1.541(2) 0.032(6) Uani 1 1 d . . .
N3 N 0.703(3) -1.299(2) -1.642(2) 0.040(7) Uani 1 1 d . . .
N4 N 0.862(2) -1.0403(19) -1.6523(19) 0.027(5) Uani 1 1 d . . .
N5 N 0.736(2) -1.540(2) -1.579(2) 0.029(5) Uani 1 1 d U . .
N6 N 0.5530(17) -1.5875(15) -1.5289(14) 0.007(4) Uani 1 1 d U . .
N7 N 0.450(2) -1.6356(18) -1.5140(17) 0.020(5) Uani 1 1 d . . .
N8 N 0.520(2) -1.7627(18) -1.5552(19) 0.022(5) Uani 1 1 d . . .
N9 N 0.297(2) -1.9549(19) -1.7240(18) 0.026(5) Uani 1 1 d . . .
N10 N 0.634(2) -1.9898(18) -1.4424(18) 0.020(5) Uani 1 1 d . . .
N11 N 0.623(2) -1.9593(17) -1.5266(18) 0.022(5) Uani 1 1 d . . .
N12 N 0.735(3) -1.938(2) -1.532(2) 0.037(6) Uani 1 1 d U . .
N13 N 0.817(2) -1.9542(19) -1.455(2) 0.026(5) Uani 1 1 d . . .
N14 N 0.433(2) -1.7398(17) -1.5274(16) 0.015(4) Uani 1 1 d U . .
N15 N 0.884(2) -1.1536(19) -1.526(2) 0.029(5) Uani 1 1 d U . .
C1 C 0.854(3) -0.970(3) -1.706(3) 0.039(4) Uani 1 1 d U . .
H1A H 0.9171 -0.8974 -1.6732 0.047 Uiso 1 1 calc R . .
C2 C 0.753(3) -1.008(3) -1.811(3) 0.042(5) Uani 1 1 d U . .
H2A H 0.7496 -0.9624 -1.8496 0.050 Uiso 1 1 calc R . .
C3 C 0.658(3) -1.112(3) -1.855(3) 0.043(4) Uani 1 1 d U . .
H3A H 0.5883 -1.1346 -1.9231 0.052 Uiso 1 1 calc R . .
C4 C 0.661(3) -1.188(3) -1.803(3) 0.043(4) Uani 1 1 d U . .
H4A H 0.5993 -1.2614 -1.8347 0.051 Uiso 1 1 calc R . .
C5 C 0.828(3) -1.511(3) -1.609(3) 0.037(4) Uani 1 1 d U . .
H5A H 0.8531 -1.4409 -1.6127 0.044 Uiso 1 1 calc R . .
C6 C 0.888(3) -1.580(3) -1.636(3) 0.040(4) Uani 1 1 d U . .
H6A H 0.9531 -1.5565 -1.6548 0.048 Uiso 1 1 calc R . .
C7 C 0.847(3) -1.684(3) -1.634(3) 0.037(4) Uani 1 1 d U . .
H7A H 0.8812 -1.7336 -1.6562 0.045 Uiso 1 1 calc R . .
C8 C 0.756(3) -1.717(3) -1.600(3) 0.036(4) Uani 1 1 d U . .
H8A H 0.7322 -1.7848 -1.5928 0.044 Uiso 1 1 calc R . .
C9 C 0.701(3) -1.641(3) -1.577(3) 0.036(3) Uani 1 1 d U . .
C10 C 0.085(3) -1.997(3) -1.754(3) 0.036(4) Uani 1 1 d U . .
H10A H 0.0186 -2.0290 -1.7389 0.044 Uiso 1 1 calc R . .
C11 C 0.064(3) -1.952(3) -1.836(3) 0.038(5) Uani 1 1 d U . .
H11A H -0.0149 -1.9502 -1.8736 0.046 Uiso 1 1 calc R . .
C12 C 0.159(3) -1.914(3) -1.861(3) 0.036(4) Uani 1 1 d U . .
H12A H 0.1454 -1.8842 -1.9135 0.043 Uiso 1 1 calc R . .
C13 C 0.274(3) -1.919(3) -1.810(3) 0.037(4) Uani 1 1 d U . .
H13A H 0.3369 -1.8980 -1.8315 0.044 Uiso 1 1 calc R . .
C14 C 0.758(3) -1.979(2) -1.397(2) 0.025(6) Uani 1 1 d U . .
C15 C 0.596(3) -1.666(2) -1.555(2) 0.030(4) Uani 1 1 d U . .
C16 C 0.205(3) -1.988(3) -1.698(3) 0.033(4) Uani 1 1 d U . .
C17 C 0.767(3) -1.143(3) -1.700(3) 0.040(4) Uani 1 1 d U . .
C18 C 0.779(3) -1.205(3) -1.630(3) 0.039(4) Uani 1 1 d U . .
O1 O 0.743(3) -1.784(2) -2.140(2) 0.062(3) Uani 1 1 d U . .
OW1 O 0.5133(18) -1.9878(19) -1.7508(18) 0.040(6) Uani 1 1 d . . .
O2 O 0.651(3) -1.624(2) -2.119(2) 0.062(3) Uani 1 1 d U . .
OW2 O 0.499(2) -1.514(2) -1.730(2) 0.058(6) Uani 1 1 d U . .
O3 O 0.809(3) -1.725(2) -2.279(2) 0.062(3) Uani 1 1 d U . .
OW3 O 0.463(4) -1.102(4) -2.111(3) 0.041(12) Uani 0.50 1 d P . .
O4 O 0.581(3) -1.581(2) -1.956(2) 0.059(5) Uani 1 1 d U . .
OW4 O 0.464(5) -1.725(5) -1.863(4) 0.054(7) Uani 0.50 1 d PU . .
O5 O 1.029(3) -1.732(2) -2.173(2) 0.066(3) Uani 1 1 d U . .
O6 O 1.086(5) -1.559(5) -2.057(4) 0.058(3) Uani 0.50 1 d PU . .
O7 O 1.184(2) -1.806(2) -2.036(2) 0.049(5) Uani 1 1 d U . .
O8 O 1.191(3) -1.640(2) -1.871(2) 0.060(3) Uani 1 1 d U . .
O9 O 0.772(3) -1.877(2) -1.984(2) 0.067(6) Uani 1 1 d U . .
O10 O 0.861(5) -1.598(5) -2.035(5) 0.061(3) Uani 0.50 1 d PU . .
O11 O 0.976(2) -1.7092(19) -2.375(2) 0.045(5) Uani 1 1 d U . .
O12 O 0.554(3) -1.792(2) -2.324(2) 0.065(6) Uani 1 1 d U . .
O13 O 1.217(2) -1.592(2) -1.661(2) 0.049(5) Uani 1 1 d U . .
O14 O 1.083(3) -1.466(2) -1.710(2) 0.062(3) Uani 1 1 d U . .
O15 O 0.758(3) -1.675(2) -1.948(2) 0.062(3) Uani 1 1 d U . .
O16 O 0.846(3) -1.465(2) -1.822(2) 0.064(3) Uani 1 1 d U . .
O17 O 0.751(3) -1.419(2) -1.994(2) 0.069(4) Uani 1 1 d U . .
O18 O 0.712(3) -1.573(2) -2.266(2) 0.062(3) Uani 1 1 d U . .
O19 O 0.981(3) -1.675(2) -1.846(2) 0.064(3) Uani 1 1 d U . .
O20 O 0.963(3) -1.787(2) -2.035(2) 0.063(3) Uani 1 1 d U . .
O21 O 1.104(5) -1.439(5) -1.854(4) 0.059(3) Uani 0.50 1 d PU . .
O22 O 1.010(5) -1.610(5) -1.960(4) 0.060(3) Uani 0.50 1 d PU . .


_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
Ge O10 1.65(6) . ?
Ge O10 1.65(6) 2_721 ?
Ge O22 1.74(6) . ?
Ge O22 1.74(6) 2_721 ?
Ge O6 1.77(5) 2_721 ?
Ge O6 1.77(5) . ?
Ge O21 1.81(6) . ?
Ge O21 1.81(6) 2_721 ?
W1 O12 1.66(3) . ?
W1 O3 1.88(3) . ?
W1 O18 1.91(3) . ?
W1 O1 1.92(3) . ?
W1 O2 1.92(3) . ?
W1 O21 2.25(6) 2_721 ?
W1 O10 2.40(6) . ?
W2 O9 1.66(3) . ?
W2 O15 1.87(3) . ?
W2 O20 1.88(3) . ?
W2 O1 1.90(3) . ?
W2 O19 1.90(3) . ?
W2 O22 2.23(6) . ?
W2 O10 2.37(6) . ?
W3 O13 1.68(2) . ?
W3 O19 1.87(3) . ?
W3 O14 1.87(3) . ?
W3 O8 1.89(3) . ?
W3 O18 1.93(3) 2_721 ?
W3 O21 2.34(5) . ?
W3 O22 2.40(6) . ?
W4 O4 1.68(3) . ?
W4 O16 1.87(3) . ?
W4 O2 1.87(3) . ?
W4 O17 1.87(3) . ?
W4 O15 1.93(3) . ?
W4 O6 2.30(6) 2_721 ?
W4 O10 2.43(6) . ?
W5 O11 1.68(2) . ?
W5 O5 1.91(3) . ?
W5 O3 1.92(3) . ?
W5 O16 1.93(3) 2_721 ?
W5 O14 1.96(3) 2_721 ?
W5 O21 2.38(5) 2_721 ?
W5 O6 2.42(5) . ?
W6 O7 1.68(2) . ?
W6 O17 1.83(3) 2_721 ?
W6 O5 1.87(3) . ?
W6 O20 1.91(3) . ?
W6 O8 1.92(3) . ?
W6 O6 2.28(5) . ?
W6 O22 2.43(6) . ?
Cu1 N11 1.97(2) . ?
Cu1 N10 1.97(2) 2_612 ?
Cu1 N9 2.01(2) . ?
Cu1 OW1 2.03(2) . ?
Cu1 N8 2.29(2) . ?
Cu2 N7 1.99(2) 2_622 ?
Cu2 N6 1.997(19) . ?
Cu2 N2 2.00(2) . ?
Cu2 N5 2.02(2) . ?
Cu3 N15 2.02(2) . ?
Cu3 N15 2.02(2) 2_732 ?
Cu3 N4 2.02(2) 2_732 ?
Cu3 N4 2.02(2) . ?
N1 N2 1.26(4) . ?
N1 N15 1.36(3) . ?
N2 N3 1.41(3) . ?
N3 C18 1.28(4) . ?
N4 C17 1.34(4) . ?
N4 C1 1.36(4) . ?
N5 C9 1.32(4) . ?
N5 C5 1.34(4) . ?
N6 C15 1.33(3) . ?
N6 N7 1.37(3) . ?
N7 N14 1.32(3) . ?
N7 Cu2 1.99(2) 2_622 ?
N8 N14 1.35(3) . ?
N8 C15 1.37(4) . ?
N9 C16 1.31(4) . ?
N9 C13 1.39(4) . ?
N10 N11 1.34(3) . ?
N10 C14 1.36(3) . ?
N10 Cu1 1.97(2) 2_612 ?
N11 N12 1.35(3) . ?
N12 N13 1.30(3) . ?
N13 C14 1.33(4) . ?
N15 C18 1.38(4) . ?
C1 C2 1.39(5) . ?
C2 C3 1.35(5) . ?
C3 C4 1.42(5) . ?
C4 C17 1.39(5) . ?
C5 C6 1.39(4) . ?
C6 C7 1.37(5) . ?
C7 C8 1.38(5) . ?
C8 C9 1.39(4) . ?
C9 C15 1.42(4) . ?
C10 C16 1.35(4) . ?
C10 C11 1.43(4) . ?
C11 C12 1.33(5) . ?
C12 C13 1.35(4) . ?
C14 C16 1.49(4) 2_612 ?
C16 C14 1.49(4) 2_612 ?
C17 C18 1.46(5) . ?
O6 W4 2.30(6) 2_721 ?
O10 O22 1.82(8) . ?
O14 W5 1.96(3) 2_721 ?
O16 W5 1.93(3) 2_721 ?
O17 W6 1.83(3) 2_721 ?
O18 W3 1.93(3) 2_721 ?
O21 W1 2.25(6) 2_721 ?
O21 W5 2.38(5) 2_721 ?

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
O10 Ge O10 180.000(10) . 2_721 ?
O10 Ge O22 65(3) . . ?
O10 Ge O22 115(3) 2_721 . ?
O10 Ge O22 115(3) . 2_721 ?
O10 Ge O22 65(3) 2_721 2_721 ?
O22 Ge O22 180.00(5) . 2_721 ?
O10 Ge O6 70(3) . 2_721 ?
O10 Ge O6 110(3) 2_721 2_721 ?
O22 Ge O6 107(3) . 2_721 ?
O22 Ge O6 73(3) 2_721 2_721 ?
O10 Ge O6 110(3) . . ?
O10 Ge O6 70(3) 2_721 . ?
O22 Ge O6 73(3) . . ?
O22 Ge O6 107(3) 2_721 . ?
O6 Ge O6 180(3) 2_721 . ?
O10 Ge O21 112(3) . . ?
O10 Ge O21 68(3) 2_721 . ?
O22 Ge O21 73(3) . . ?
O22 Ge O21 107(3) 2_721 . ?
O6 Ge O21 76(2) 2_721 . ?
O6 Ge O21 104(3) . . ?
O10 Ge O21 68(3) . 2_721 ?
O10 Ge O21 112(3) 2_721 2_721 ?
O22 Ge O21 107(3) . 2_721 ?
O22 Ge O21 73(3) 2_721 2_721 ?
O6 Ge O21 104(3) 2_721 2_721 ?
O6 Ge O21 76(2) . 2_721 ?
O21 Ge O21 180.00(5) . 2_721 ?
O12 W1 O3 101.9(14) . . ?
O12 W1 O18 100.5(13) . . ?
O3 W1 O18 87.5(12) . . ?
O12 W1 O1 99.8(13) . . ?
O3 W1 O1 87.6(12) . . ?
O18 W1 O1 159.7(13) . . ?
O12 W1 O2 101.5(14) . . ?
O3 W1 O2 156.6(13) . . ?
O18 W1 O2 87.4(12) . . ?
O1 W1 O2 89.3(12) . . ?
O12 W1 O21 156.4(17) . 2_721 ?
O3 W1 O21 63.0(17) . 2_721 ?
O18 W1 O21 62.8(17) . 2_721 ?
O1 W1 O21 97.5(17) . 2_721 ?
O2 W1 O21 94.5(17) . 2_721 ?
O12 W1 O10 154.4(18) . . ?
O3 W1 O10 96.0(17) . . ?
O18 W1 O10 98.5(17) . . ?
O1 W1 O10 62.4(16) . . ?
O2 W1 O10 62.3(16) . . ?
O21 W1 O10 49.2(19) 2_721 . ?
O9 W2 O15 99.9(14) . . ?
O9 W2 O20 102.7(14) . . ?
O15 W2 O20 157.4(13) . . ?
O9 W2 O1 102.3(14) . . ?
O15 W2 O1 90.1(12) . . ?
O20 W2 O1 85.9(12) . . ?
O9 W2 O19 101.6(13) . . ?
O15 W2 O19 86.0(13) . . ?
O20 W2 O19 88.7(13) . . ?
O1 W2 O19 156.1(13) . . ?
O9 W2 O22 156.4(18) . . ?
O15 W2 O22 95.4(17) . . ?
O20 W2 O22 63.0(17) . . ?
O1 W2 O22 95.5(17) . . ?
O19 W2 O22 61.5(17) . . ?
O9 W2 O10 157.1(18) . . ?
O15 W2 O10 64.3(16) . . ?
O20 W2 O10 94.3(17) . . ?
O1 W2 O10 63.3(16) . . ?
O19 W2 O10 93.9(17) . . ?
O22 W2 O10 46(2) . . ?
O13 W3 O19 102.5(13) . . ?
O13 W3 O14 98.8(12) . . ?
O19 W3 O14 88.1(12) . . ?
O13 W3 O8 101.7(12) . . ?
O19 W3 O8 90.1(12) . . ?
O14 W3 O8 159.3(12) . . ?
O13 W3 O18 99.3(12) . 2_721 ?
O19 W3 O18 158.0(13) . 2_721 ?
O14 W3 O18 85.4(12) . 2_721 ?
O8 W3 O18 88.7(12) . 2_721 ?
O13 W3 O21 153.1(17) . . ?
O19 W3 O21 97.5(17) . . ?
O14 W3 O21 63.9(16) . . ?
O8 W3 O21 96.0(16) . . ?
O18 W3 O21 60.8(16) 2_721 . ?
O13 W3 O22 154.2(16) . . ?
O19 W3 O22 58.3(16) . . ?
O14 W3 O22 97.6(16) . . ?
O8 W3 O22 64.3(16) . . ?
O18 W3 O22 101.8(16) 2_721 . ?
O21 W3 O22 52.6(19) . . ?
O4 W4 O16 102.9(13) . . ?
O4 W4 O2 100.8(13) . . ?
O16 W4 O2 156.3(13) . . ?
O4 W4 O17 108.4(13) . . ?
O16 W4 O17 88.2(13) . . ?
O2 W4 O17 84.7(13) . . ?
O4 W4 O15 99.6(13) . . ?
O16 W4 O15 86.2(12) . . ?
O2 W4 O15 89.5(12) . . ?
O17 W4 O15 152.0(13) . . ?
O4 W4 O6 157.7(17) . 2_721 ?
O16 W4 O6 63.7(16) . 2_721 ?
O2 W4 O6 93.8(16) . 2_721 ?
O17 W4 O6 56.0(17) . 2_721 ?
O15 W4 O6 97.3(16) . 2_721 ?
O4 W4 O10 153.4(18) . . ?
O16 W4 O10 95.4(17) . . ?
O2 W4 O10 62.2(16) . . ?
O17 W4 O10 91.1(17) . . ?
O15 W4 O10 62.2(16) . . ?
O6 W4 O10 48.9(19) 2_721 . ?
O11 W5 O5 103.6(12) . . ?
O11 W5 O3 103.5(12) . . ?
O5 W5 O3 85.5(13) . . ?
O11 W5 O16 98.7(12) . 2_721 ?
O5 W5 O16 89.8(13) . 2_721 ?
O3 W5 O16 157.8(12) . 2_721 ?
O11 W5 O14 98.8(12) . 2_721 ?
O5 W5 O14 157.3(12) . 2_721 ?
O3 W5 O14 85.6(12) . 2_721 ?
O16 W5 O14 90.6(12) 2_721 2_721 ?
O11 W5 O21 153.7(17) . 2_721 ?
O5 W5 O21 95.6(16) . 2_721 ?
O3 W5 O21 59.8(16) . 2_721 ?
O16 W5 O21 99.2(17) 2_721 2_721 ?
O14 W5 O21 62.0(15) 2_721 2_721 ?
O11 W5 O6 151.7(16) . . ?
O5 W5 O6 60.7(16) . . ?
O3 W5 O6 98.7(16) . . ?
O16 W5 O6 60.5(16) 2_721 . ?
O14 W5 O6 100.2(15) 2_721 . ?
O21 W5 O6 54.4(19) 2_721 . ?
O7 W6 O17 105.8(14) . 2_721 ?
O7 W6 O5 103.2(13) . . ?
O17 W6 O5 90.8(13) 2_721 . ?
O7 W6 O20 101.3(13) . . ?
O17 W6 O20 152.8(13) 2_721 . ?
O5 W6 O20 86.1(13) . . ?
O7 W6 O8 99.8(12) . . ?
O17 W6 O8 84.7(13) 2_721 . ?
O5 W6 O8 156.9(12) . . ?
O20 W6 O8 87.7(12) . . ?
O7 W6 O6 155.8(17) . . ?
O17 W6 O6 56.6(17) 2_721 . ?
O5 W6 O6 64.0(16) . . ?
O20 W6 O6 98.3(17) . . ?
O8 W6 O6 95.1(16) . . ?
O7 W6 O22 152.1(16) . . ?
O17 W6 O22 95.0(17) 2_721 . ?
O5 W6 O22 94.8(16) . . ?
O20 W6 O22 58.4(16) . . ?
O8 W6 O22 63.2(15) . . ?
O6 W6 O22 52.1(19) . . ?
N11 Cu1 N10 93.2(9) . 2_612 ?
N11 Cu1 N9 173.9(10) . . ?
N10 Cu1 N9 81.0(9) 2_612 . ?
N11 Cu1 OW1 90.9(8) . . ?
N10 Cu1 OW1 146.5(10) 2_612 . ?
N9 Cu1 OW1 93.1(9) . . ?
N11 Cu1 N8 100.5(8) . . ?
N10 Cu1 N8 103.2(8) 2_612 . ?
N9 Cu1 N8 82.6(9) . . ?
OW1 Cu1 N8 108.7(9) . . ?
N7 Cu2 N6 94.4(8) 2_622 . ?
N7 Cu2 N2 92.3(10) 2_622 . ?
N6 Cu2 N2 173.2(9) . . ?
N7 Cu2 N5 173.4(10) 2_622 . ?
N6 Cu2 N5 79.1(9) . . ?
N2 Cu2 N5 94.2(10) . . ?
N15 Cu3 N15 180.000(6) . 2_732 ?
N15 Cu3 N4 98.6(10) . 2_732 ?
N15 Cu3 N4 81.4(10) 2_732 2_732 ?
N15 Cu3 N4 81.4(10) . . ?
N15 Cu3 N4 98.6(10) 2_732 . ?
N4 Cu3 N4 180.000(12) 2_732 . ?
N2 N1 N15 110(2) . . ?
N1 N2 N3 109(2) . . ?
N1 N2 Cu2 136(2) . . ?
N3 N2 Cu2 114(2) . . ?
C18 N3 N2 106(3) . . ?
C17 N4 C1 119(3) . . ?
C17 N4 Cu3 116(2) . . ?
C1 N4 Cu3 125(2) . . ?
C9 N5 C5 117(3) . . ?
C9 N5 Cu2 117(2) . . ?
C5 N5 Cu2 126(2) . . ?
C15 N6 N7 107(2) . . ?
C15 N6 Cu2 112.8(17) . . ?
N7 N6 Cu2 140.3(14) . . ?
N14 N7 N6 109(2) . . ?
N14 N7 Cu2 125.9(17) . 2_622 ?
N6 N7 Cu2 125.0(15) . 2_622 ?
N14 N8 C15 107(2) . . ?
N14 N8 Cu1 111.8(15) . . ?
C15 N8 Cu1 139.0(19) . . ?
C16 N9 C13 119(3) . . ?
C16 N9 Cu1 115.3(19) . . ?
C13 N9 Cu1 125(2) . . ?
N11 N10 C14 103(2) . . ?
N11 N10 Cu1 142.1(17) . 2_612 ?
C14 N10 Cu1 114.9(18) . 2_612 ?
N10 N11 N12 109(2) . . ?
N10 N11 Cu1 124.5(17) . . ?
N12 N11 Cu1 126.4(18) . . ?
N13 N12 N11 110(2) . . ?
N12 N13 C14 104(2) . . ?
N7 N14 N8 109(2) . . ?
N1 N15 C18 105(2) . . ?
N1 N15 Cu3 143(2) . . ?
C18 N15 Cu3 111.8(19) . . ?
N4 C1 C2 120(3) . . ?
C3 C2 C1 120(3) . . ?
C2 C3 C4 123(3) . . ?
C17 C4 C3 113(3) . . ?
N5 C5 C6 123(3) . . ?
C7 C6 C5 117(3) . . ?
C6 C7 C8 122(3) . . ?
C7 C8 C9 116(3) . . ?
N5 C9 C8 125(3) . . ?
N5 C9 C15 111(3) . . ?
C8 C9 C15 124(3) . . ?
C16 C10 C11 116(3) . . ?
C12 C11 C10 120(3) . . ?
C11 C12 C13 121(3) . . ?
C12 C13 N9 119(3) . . ?
N13 C14 N10 113(2) . . ?
N13 C14 C16 132(3) . 2_612 ?
N10 C14 C16 114(3) . 2_612 ?
N6 C15 N8 109(2) . . ?
N6 C15 C9 120(3) . . ?
N8 C15 C9 132(3) . . ?
N9 C16 C10 124(3) . . ?
N9 C16 C14 115(3) . 2_612 ?
C10 C16 C14 121(3) . 2_612 ?
N4 C17 C4 126(3) . . ?
N4 C17 C18 114(3) . . ?
C4 C17 C18 120(3) . . ?
N3 C18 N15 110(3) . . ?
N3 C18 C17 132(3) . . ?
N15 C18 C17 117(3) . . ?
W2 O1 W1 137.3(16) . . ?
W4 O2 W1 140.0(16) . . ?
W1 O3 W5 137.5(16) . . ?
W6 O5 W5 137.9(16) . . ?
Ge O6 W6 121(3) . . ?
Ge O6 W4 121(3) . 2_721 ?
W6 O6 W4 101(2) . 2_721 ?
Ge O6 W5 115(3) . . ?
W6 O6 W5 97(2) . . ?
W4 O6 W5 98(2) 2_721 . ?
W3 O8 W6 137.8(15) . . ?
Ge O10 O22 60(3) . . ?
Ge O10 W2 123(3) . . ?
O22 O10 W2 63(2) . . ?
Ge O10 W1 121(3) . . ?
O22 O10 W1 131(3) . . ?
W2 O10 W1 96(2) . . ?
Ge O10 W4 120(3) . . ?
O22 O10 W4 129(3) . . ?
W2 O10 W4 95(2) . . ?
W1 O10 W4 95(2) . . ?
W3 O14 W5 136.3(16) . 2_721 ?
W2 O15 W4 137.7(16) . . ?
W4 O16 W5 138.1(16) . 2_721 ?
W6 O17 W4 145.3(18) 2_721 . ?
W1 O18 W3 135.0(16) . 2_721 ?
W3 O19 W2 139.9(17) . . ?
W2 O20 W6 139.2(16) . . ?
Ge O21 W1 122(3) . 2_721 ?
Ge O21 W3 117(3) . . ?
W1 O21 W3 101(2) 2_721 . ?
Ge O21 W5 115(3) . 2_721 ?
W1 O21 W5 100(2) 2_721 2_721 ?
W3 O21 W5 98(2) . 2_721 ?
Ge O22 O10 55(2) . . ?
Ge O22 W2 126(3) . . ?
O10 O22 W2 71(3) . . ?
Ge O22 W3 117(3) . . ?
O10 O22 W3 135(3) . . ?
W2 O22 W3 99(2) . . ?
Ge O22 W6 115(3) . . ?
O10 O22 W6 130(3) . . ?
W2 O22 W6 99(2) . . ?
W3 O22 W6 94.6(19) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.276
_refine_diff_density_min         -3.251
_refine_diff_density_rms         0.425
