# 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_k1
_database_code_depnum_ccdc_archive 'CCDC 967747'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H35 Cu3 N7 O46 Si W12'
_chemical_formula_weight         3726.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p2(1)/c

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

_cell_length_a                   23.4183(7)
_cell_length_b                   12.9661(3)
_cell_length_c                   22.7238(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.508(2)
_cell_angle_gamma                90.00
_cell_volume                     6503.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8735
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.25

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6625
_exptl_absorpt_coefficient_mu    22.209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0626
_exptl_absorpt_correction_T_max  0.1014
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1152 before and 0.0448 after correction. The Ratio 
of minimum to maximum transmission is 0.466454. The λ/2 
correction factor is 0.0015. 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47065
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         0.92
_diffrn_reflns_theta_max         28.35
_reflns_number_total             16161
_reflns_number_gt                10006
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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. 

restraints used:
ISOR 0.001 ow3 c7 c36 c21 c33
;

_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)+(0.0305P)²+30.0186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16161
_refine_ls_number_parameters     946
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.008
_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
W1 W -0.35447(3) 0.46549(4) -0.21419(3) 0.02149(14) Uani 1 1 d . . .
W2 W -0.17559(3) 0.70249(5) -0.16046(3) 0.02388(14) Uani 1 1 d . . .
W3 W -0.20584(3) 0.42787(5) -0.13670(3) 0.02374(14) Uani 1 1 d . . .
W4 W -0.32781(3) 0.38808(4) -0.41795(3) 0.02011(13) Uani 1 1 d . . .
W5 W -0.27852(3) 0.27710(4) -0.25822(3) 0.02438(15) Uani 1 1 d . . .
W6 W -0.40370(3) 0.57558(4) -0.37427(3) 0.02056(13) Uani 1 1 d . . .
W7 W -0.32353(3) 0.73842(4) -0.23860(3) 0.01975(13) Uani 1 1 d . . .
W8 W -0.16555(3) 0.34408(4) -0.33283(3) 0.01832(13) Uani 1 1 d . . .
W9 W -0.09247(3) 0.49551(4) -0.21045(3) 0.01817(13) Uani 1 1 d . . .
W10 W -0.29974(3) 0.63429(4) -0.44088(3) 0.01999(13) Uani 1 1 d . . .
W11 W -0.22107(3) 0.80084(4) -0.30557(3) 0.01966(13) Uani 1 1 d . . .
W12 W -0.13742(3) 0.59239(4) -0.35521(3) 0.01691(13) Uani 1 1 d . . .
Cu3 Cu -0.03892(8) -0.18324(14) -0.37489(9) 0.0249(4) Uani 1 1 d . . .
Cu1 Cu -0.42289(8) 0.00401(13) -0.57455(9) 0.0220(4) Uani 1 1 d . . .
Cu2 Cu -0.34877(8) 0.22103(13) -0.56986(9) 0.0213(4) Uani 1 1 d . . .
Si1 Si -0.24841(15) 0.5373(2) -0.28689(16) 0.0061(6) Uani 1 1 d . . .
O1 O -0.1402(5) 0.2394(8) -0.3605(5) 0.031(3) Uani 1 1 d . . .
O41 O -0.4159(4) 0.1469(7) -0.5607(5) 0.025(2) Uani 1 1 d . . .
O2 O -0.3710(4) 0.6866(7) -0.3171(5) 0.024(2) Uani 1 1 d . . .
OW1 O -0.0581(5) -0.1603(8) -0.2980(5) 0.028(2) Uani 1 1 d . . .
O3 O -0.1970(5) 0.5744(8) -0.1342(5) 0.028(3) Uani 1 1 d . . .
O4 O -0.3554(5) 0.2928(8) -0.4721(5) 0.030(3) Uani 1 1 d . . .
O5 O -0.1710(6) 0.3943(8) -0.0617(5) 0.037(3) Uani 1 1 d . . .
O6 O -0.2872(5) 0.4432(8) -0.1377(5) 0.025(2) Uani 1 1 d . . .
O7 O -0.2898(5) 0.1498(8) -0.2594(6) 0.040(3) Uani 1 1 d . . .
O8 O -0.1312(5) 0.7573(8) -0.0932(5) 0.036(3) Uani 1 1 d . . .
O9 O -0.1698(5) 0.8038(7) -0.2195(5) 0.024(2) Uani 1 1 d . . .
O10 O -0.3948(4) 0.4973(7) -0.3003(5) 0.023(2) Uani 1 1 d . . .
O11 O -0.3011(4) 0.5349(6) -0.3553(4) 0.015(2) Uani 1 1 d . . .
O12 O -0.3368(4) 0.6105(7) -0.2051(5) 0.025(2) Uani 1 1 d . . .
O14 O -0.4015(5) 0.4487(7) -0.4181(5) 0.026(2) Uani 1 1 d . . .
O15 O -0.3748(5) 0.8175(7) -0.2222(5) 0.030(3) Uani 1 1 d . . .
O16 O -0.4794(4) 0.6033(8) -0.3991(5) 0.030(3) Uani 1 1 d . . .
O17 O -0.1161(4) 0.6213(7) -0.1835(4) 0.022(2) Uani 1 1 d . . .
O18 O -0.3196(4) 0.4960(8) -0.4715(5) 0.024(2) Uani 1 1 d . . .
O19 O -0.1849(4) 0.5046(6) -0.2942(4) 0.016(2) Uani 1 1 d . . .
O20 O -0.0209(4) 0.4790(8) -0.1586(5) 0.028(3) Uani 1 1 d . . .
O21 O -0.3463(5) 0.3246(7) -0.2355(5) 0.027(2) Uani 1 1 d . . .
O22 O -0.2043(5) 0.9182(7) -0.3284(5) 0.029(3) Uani 1 1 d . . .
O23 O -0.3226(4) 0.3185(7) -0.3431(5) 0.022(2) Uani 1 1 d . . .
O24 O -0.1397(5) 0.4303(7) -0.1680(5) 0.023(2) Uani 1 1 d . . .
O25 O -0.2743(4) 0.7449(7) -0.3807(4) 0.019(2) Uani 1 1 d . . .
O26 O -0.2424(4) 0.3665(7) -0.3949(4) 0.020(2) Uani 1 1 d . . .
O27 O -0.4113(5) 0.4574(8) -0.1836(5) 0.029(3) Uani 1 1 d . . .
O28 O -0.2428(4) 0.6530(7) -0.2579(4) 0.0132(19) Uani 1 1 d . . .
O29 O -0.3060(5) 0.6943(8) -0.5095(5) 0.031(3) Uani 1 1 d . . .
O30 O -0.2155(4) 0.5977(7) -0.4142(4) 0.017(2) Uani 1 1 d . . .
O31 O -0.2528(4) 0.7569(7) -0.1651(5) 0.022(2) Uani 1 1 d . . .
O32 O -0.2877(5) 0.8364(7) -0.2805(5) 0.024(2) Uani 1 1 d . . .
O33 O -0.3807(5) 0.6480(7) -0.4373(5) 0.024(2) Uani 1 1 d . . .
O34 O -0.2278(5) 0.2934(7) -0.1721(5) 0.027(2) Uani 1 1 d . . .
O35 O -0.1589(4) 0.7144(7) -0.3193(5) 0.019(2) Uani 1 1 d . . .
O36 O -0.1322(4) 0.4512(7) -0.3734(5) 0.022(2) Uani 1 1 d . . .
O37 O -0.0935(4) 0.6444(8) -0.3954(5) 0.026(2) Uani 1 1 d . . .
O38 O -0.0760(4) 0.5692(7) -0.2761(4) 0.020(2) Uani 1 1 d . . .
O39 O -0.2657(4) 0.4570(6) -0.2407(4) 0.017(2) Uani 1 1 d . . .
O40 O -0.0981(4) 0.3734(7) -0.2600(5) 0.021(2) Uani 1 1 d . . .
O13 O -0.2087(4) 0.2891(7) -0.2837(4) 0.020(2) Uani 1 1 d . . .
O42 O -0.3354(4) -0.0255(8) -0.5405(5) 0.028(2) Uani 1 1 d . . .
O43 O -0.2890(4) 0.1274(7) -0.5150(4) 0.019(2) Uani 1 1 d . . .
N1 N -0.5119(6) 0.0100(9) -0.5868(7) 0.027(3) Uani 1 1 d . . .
C1 C -0.5444(7) 0.0927(11) -0.5827(9) 0.035(4) Uani 1 1 d . . .
H1A H -0.5248 0.1560 -0.5729 0.042 Uiso 1 1 calc R . .
C2 C -0.6055(7) 0.0881(12) -0.5922(8) 0.034(4) Uani 1 1 d . . .
H2A H -0.6267 0.1476 -0.5895 0.040 Uiso 1 1 calc R . .
C3 C -0.6349(8) -0.0043(12) -0.6057(9) 0.039(4) Uani 1 1 d . . .
H3A H -0.6763 -0.0092 -0.6126 0.046 Uiso 1 1 calc R . .
C4 C -0.6014(7) -0.0897(13) -0.6088(10) 0.044(5) Uani 1 1 d . . .
H4A H -0.6202 -0.1538 -0.6173 0.053 Uiso 1 1 calc R . .
C5 C -0.5418(7) -0.0819(11) -0.5998(9) 0.032(4) Uani 1 1 d . . .
C6 C -0.5029(7) -0.1674(11) -0.6061(8) 0.025(4) Uani 1 1 d . . .
C7 C -0.5217(8) -0.2675(13) -0.6200(8) 0.038(4) Uani 1 1 d U . .
H7A H -0.5620 -0.2848 -0.6272 0.046 Uiso 1 1 calc R . .
C8 C -0.4796(9) -0.3454(13) -0.6234(11) 0.058(6) Uani 1 1 d . . .
H8A H -0.4913 -0.4140 -0.6308 0.069 Uiso 1 1 calc R . .
C9 C -0.4215(7) -0.3152(12) -0.6154(8) 0.029(4) Uani 1 1 d . . .
H9A H -0.3931 -0.3630 -0.6187 0.035 Uiso 1 1 calc R . .
C10 C -0.4053(7) -0.2131(11) -0.6025(8) 0.030(4) Uani 1 1 d . . .
H10A H -0.3656 -0.1938 -0.5968 0.035 Uiso 1 1 calc R . .
N2 N -0.4440(6) -0.1412(9) -0.5979(6) 0.027(3) Uani 1 1 d . . .
N3 N -0.3995(5) 0.2983(9) -0.6431(6) 0.021(3) Uani 1 1 d . . .
C11 C -0.4558(8) 0.2782(13) -0.6780(8) 0.035(4) Uani 1 1 d . . .
H11A H -0.4742 0.2205 -0.6679 0.042 Uiso 1 1 calc R . .
C12 C -0.4897(7) 0.3369(14) -0.7289(8) 0.036(4) Uani 1 1 d . . .
H12A H -0.5298 0.3210 -0.7516 0.044 Uiso 1 1 calc R . .
C13 C -0.4599(9) 0.4218(14) -0.7439(8) 0.040(4) Uani 1 1 d . . .
H13A H -0.4809 0.4638 -0.7772 0.048 Uiso 1 1 calc R . .
C14 C -0.4021(8) 0.4437(13) -0.7115(8) 0.039(4) Uani 1 1 d . . .
H14A H -0.3821 0.4977 -0.7232 0.046 Uiso 1 1 calc R . .
C15 C -0.3726(7) 0.3822(12) -0.6588(8) 0.029(4) Uani 1 1 d . . .
C16 C -0.3093(6) 0.3985(11) -0.6137(7) 0.023(3) Uani 1 1 d . . .
C17 C -0.2759(10) 0.4869(13) -0.6175(9) 0.049(5) Uani 1 1 d . . .
H17A H -0.2908 0.5346 -0.6495 0.059 Uiso 1 1 calc R . .
C18 C -0.2198(8) 0.5005(13) -0.5717(10) 0.042(5) Uani 1 1 d . . .
H18A H -0.1968 0.5590 -0.5717 0.050 Uiso 1 1 calc R . .
C19 C -0.1986(7) 0.4260(12) -0.5261(8) 0.029(4) Uani 1 1 d . . .
H19A H -0.1618 0.4340 -0.4942 0.034 Uiso 1 1 calc R . .
C20 C -0.2337(7) 0.3398(11) -0.5295(7) 0.023(3) Uani 1 1 d . . .
H20A H -0.2187 0.2877 -0.5003 0.028 Uiso 1 1 calc R . .
C21 C -0.0275(8) -0.1343(13) -0.4970(8) 0.034(4) Uani 1 1 d U . .
H21A H -0.0608 -0.0915 -0.5029 0.041 Uiso 1 1 calc R . .
C22 C -0.0010(9) -0.1402(15) -0.5450(9) 0.049(5) Uani 1 1 d . . .
H22A H -0.0175 -0.1032 -0.5819 0.058 Uiso 1 1 calc R . .
C23 C 0.0482(9) -0.2003(16) -0.5362(11) 0.055(6) Uani 1 1 d . . .
H23A H 0.0672 -0.2048 -0.5661 0.066 Uiso 1 1 calc R . .
C24 C 0.0697(8) -0.2562(14) -0.4797(9) 0.041(5) Uani 1 1 d . . .
H24A H 0.1029 -0.2995 -0.4727 0.049 Uiso 1 1 calc R . .
C25 C 0.0429(7) -0.2482(12) -0.4350(8) 0.027(4) Uani 1 1 d . . .
C26 C 0.0620(7) -0.2997(11) -0.3748(8) 0.026(4) Uani 1 1 d . . .
C27 C 0.1109(9) -0.3678(14) -0.3581(10) 0.053(6) Uani 1 1 d . . .
H27A H 0.1334 -0.3784 -0.3844 0.063 Uiso 1 1 calc R . .
C28 C 0.1250(10) -0.4187(17) -0.3025(10) 0.067(7) Uani 1 1 d . . .
H28A H 0.1573 -0.4648 -0.2908 0.080 Uiso 1 1 calc R . .
C30 C 0.0428(7) -0.3297(12) -0.2846(7) 0.029(4) Uani 1 1 d . . .
H30A H 0.0190 -0.3160 -0.2600 0.035 Uiso 1 1 calc R . .
C31 C -0.1308(7) -0.0188(11) -0.4098(8) 0.027(4) Uani 1 1 d . . .
H31A H -0.1010 0.0167 -0.3789 0.033 Uiso 1 1 calc R . .
C32 C -0.1848(7) 0.0301(11) -0.4382(7) 0.027(4) Uani 1 1 d . . .
H32A H -0.1905 0.0979 -0.4280 0.032 Uiso 1 1 calc R . .
C33 C -0.2302(6) -0.0223(10) -0.4818(7) 0.018(3) Uani 1 1 d U . .
C34 C -0.2183(6) -0.1208(10) -0.4969(7) 0.021(3) Uani 1 1 d . . .
H34A H -0.2477 -0.1579 -0.5273 0.025 Uiso 1 1 calc R . .
C35 C -0.1618(7) -0.1644(12) -0.4665(8) 0.030(4) Uani 1 1 d . . .
H35A H -0.1545 -0.2315 -0.4765 0.036 Uiso 1 1 calc R . .
C36 C -0.2896(6) 0.0318(10) -0.5154(6) 0.014(3) Uani 1 1 d U . .
N4 N -0.2876(5) 0.3270(9) -0.5722(6) 0.021(3) Uani 1 1 d . . .
N5 N -0.0067(6) -0.1865(9) -0.4452(6) 0.026(3) Uani 1 1 d . . .
N6 N 0.0303(5) -0.2815(9) -0.3385(6) 0.022(3) Uani 1 1 d . . .
N7 N -0.1182(5) -0.1141(9) -0.4238(6) 0.022(3) Uani 1 1 d . . .
C29 C 0.0907(9) -0.4016(13) -0.2627(9) 0.046(5) Uani 1 1 d . . .
H29A H 0.0991 -0.4353 -0.2246 0.055 Uiso 1 1 calc R . .
OW2 O 0.0021(9) 0.360(2) -0.3243(8) 0.127(9) Uani 1 1 d . . .
OW3 O 0.0590(17) 1.068(3) 0.0122(18) 0.236(14) 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 O27 1.699(10) . ?
W1 O10 1.911(10) . ?
W1 O21 1.916(10) . ?
W1 O12 1.922(10) . ?
W1 O6 1.938(10) . ?
W1 O39 2.351(9) . ?
W2 O8 1.692(11) . ?
W2 O3 1.887(11) . ?
W2 O31 1.912(9) . ?
W2 O9 1.915(10) . ?
W2 O17 1.952(10) . ?
W2 O28 2.337(9) . ?
W3 O5 1.682(11) . ?
W3 O24 1.909(9) . ?
W3 O6 1.909(10) . ?
W3 O3 1.911(10) . ?
W3 O34 1.917(10) . ?
W3 O39 2.341(9) . ?
W4 O4 1.710(10) . ?
W4 O23 1.894(10) . ?
W4 O14 1.896(10) . ?
W4 O18 1.906(10) . ?
W4 O26 1.910(9) . ?
W4 O11 2.335(8) . ?
W5 O7 1.671(11) . ?
W5 O13 1.915(10) . ?
W5 O21 1.928(10) . ?
W5 O34 1.932(11) . ?
W5 O23 1.935(11) . ?
W5 O39 2.369(8) . ?
W6 O16 1.709(10) . ?
W6 O10 1.916(10) . ?
W6 O2 1.919(10) . ?
W6 O14 1.932(10) . ?
W6 O33 1.933(10) . ?
W6 O11 2.355(9) . ?
W7 O15 1.712(10) . ?
W7 O2 1.883(10) . ?
W7 O12 1.893(10) . ?
W7 O31 1.933(10) . ?
W7 O32 1.939(10) . ?
W7 O28 2.356(8) . ?
W8 O1 1.685(10) . ?
W8 O13 1.878(10) . ?
W8 O26 1.903(9) . ?
W8 O40 1.907(9) . ?
W8 O36 1.968(10) . ?
W8 O19 2.360(9) . ?
W9 O20 1.710(10) . ?
W9 O17 1.889(10) . ?
W9 O24 1.892(10) . ?
W9 O38 1.917(9) . ?
W9 O40 1.922(9) . ?
W9 O19 2.360(9) . ?
W10 O29 1.704(10) . ?
W10 O30 1.920(9) . ?
W10 O18 1.923(10) . ?
W10 O33 1.933(10) . ?
W10 O25 1.933(9) . ?
W10 O11 2.342(9) . ?
W11 O22 1.696(10) . ?
W11 O32 1.888(10) . ?
W11 O25 1.891(10) . ?
W11 O9 1.924(10) . ?
W11 O35 1.943(9) . ?
W11 O28 2.340(8) . ?
W12 O37 1.724(10) . ?
W12 O30 1.873(9) . ?
W12 O36 1.890(9) . ?
W12 O38 1.914(9) . ?
W12 O35 1.922(9) . ?
W12 O19 2.342(9) . ?
Cu3 OW1 1.967(10) . ?
Cu3 N5 1.983(13) . ?
Cu3 N6 2.010(12) . ?
Cu3 N7 2.027(12) . ?
Cu3 O20 2.502(11) 2_544 ?
Cu3 O37 2.539(10) 1_545 ?
Cu1 O41 1.877(10) . ?
Cu1 O42 1.971(10) . ?
Cu1 N2 1.974(12) . ?
Cu1 N1 2.009(12) . ?
Cu1 O27 2.629(11) 4_565 ?
Cu1 Cu2 3.289(2) . ?
Cu2 O41 1.913(10) . ?
Cu2 O43 1.955(9) . ?
Cu2 N3 1.966(12) . ?
Cu2 N4 1.997(11) . ?
Cu2 O4 2.461(10) . ?
Si1 O19 1.608(9) . ?
Si1 O39 1.623(10) . ?
Si1 O28 1.626(9) . ?
Si1 O11 1.630(10) . ?
O20 Cu3 2.502(11) 2_554 ?
O27 Cu1 2.629(11) 4_566 ?
O37 Cu3 2.539(10) 1_565 ?
O42 C36 1.273(16) . ?
O43 C36 1.240(15) . ?
N1 C1 1.335(18) . ?
N1 C5 1.365(17) . ?
C1 C2 1.38(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.36(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.37(2) . ?
C3 H3A 0.9300 . ?
C4 C5 1.34(2) . ?
C4 H4A 0.9300 . ?
C5 C6 1.47(2) . ?
C6 N2 1.370(18) . ?
C6 C7 1.37(2) . ?
C7 C8 1.43(2) . ?
C7 H7A 0.9300 . ?
C8 C9 1.37(2) . ?
C8 H8A 0.9300 . ?
C9 C10 1.38(2) . ?
C9 H9A 0.9300 . ?
C10 N2 1.329(19) . ?
C10 H10A 0.9300 . ?
N3 C11 1.32(2) . ?
N3 C15 1.36(2) . ?
C11 C12 1.39(2) . ?
C11 H11A 0.9300 . ?
C12 C13 1.40(2) . ?
C12 H12A 0.9300 . ?
C13 C14 1.34(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.41(2) . ?
C14 H14A 0.9300 . ?
C15 C16 1.51(2) . ?
C16 N4 1.299(18) . ?
C16 C17 1.41(2) . ?
C17 C18 1.39(3) . ?
C17 H17A 0.9300 . ?
C18 C19 1.38(2) . ?
C18 H18A 0.9300 . ?
C19 C20 1.37(2) . ?
C19 H19A 0.9300 . ?
C20 N4 1.321(18) . ?
C20 H20A 0.9300 . ?
C21 N5 1.30(2) . ?
C21 C22 1.42(2) . ?
C21 H21A 0.9300 . ?
C22 C23 1.35(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.41(3) . ?
C23 H23A 0.9300 . ?
C24 C25 1.36(2) . ?
C24 H24A 0.9300 . ?
C25 N5 1.365(18) . ?
C25 C26 1.45(2) . ?
C26 N6 1.302(19) . ?
C26 C27 1.39(2) . ?
C27 C28 1.36(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.41(3) . ?
C28 H28A 0.9300 . ?
C30 N6 1.318(18) . ?
C30 C29 1.42(2) . ?
C30 H30A 0.9300 . ?
C31 N7 1.333(17) . ?
C31 C32 1.37(2) . ?
C31 H31A 0.9300 . ?
C32 C33 1.37(2) . ?
C32 H32A 0.9300 . ?
C33 C34 1.375(19) . ?
C33 C36 1.517(18) . ?
C34 C35 1.39(2) . ?
C34 H34A 0.9300 . ?
C35 N7 1.322(18) . ?
C35 H35A 0.9300 . ?
C29 H29A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O27 W1 O10 104.2(5) . . ?
O27 W1 O21 101.7(5) . . ?
O10 W1 O21 90.2(4) . . ?
O27 W1 O12 100.8(5) . . ?
O10 W1 O12 85.1(4) . . ?
O21 W1 O12 157.6(4) . . ?
O27 W1 O6 97.8(5) . . ?
O10 W1 O6 157.8(4) . . ?
O21 W1 O6 88.0(4) . . ?
O12 W1 O6 88.2(4) . . ?
O27 W1 O39 169.2(4) . . ?
O10 W1 O39 85.7(4) . . ?
O21 W1 O39 73.7(4) . . ?
O12 W1 O39 84.0(4) . . ?
O6 W1 O39 72.5(4) . . ?
O8 W2 O3 103.4(5) . . ?
O8 W2 O31 100.3(5) . . ?
O3 W2 O31 89.8(4) . . ?
O8 W2 O9 100.3(5) . . ?
O3 W2 O9 156.0(4) . . ?
O31 W2 O9 89.7(4) . . ?
O8 W2 O17 101.1(5) . . ?
O3 W2 O17 84.2(4) . . ?
O31 W2 O17 158.6(4) . . ?
O9 W2 O17 87.6(4) . . ?
O8 W2 O28 170.9(4) . . ?
O3 W2 O28 83.8(4) . . ?
O31 W2 O28 73.9(4) . . ?
O9 W2 O28 73.0(4) . . ?
O17 W2 O28 85.0(4) . . ?
O5 W3 O24 101.7(5) . . ?
O5 W3 O6 100.6(5) . . ?
O24 W3 O6 157.7(4) . . ?
O5 W3 O3 102.5(5) . . ?
O24 W3 O3 84.3(4) . . ?
O6 W3 O3 89.7(4) . . ?
O5 W3 O34 99.3(5) . . ?
O24 W3 O34 89.7(4) . . ?
O6 W3 O34 87.9(4) . . ?
O3 W3 O34 158.2(4) . . ?
O5 W3 O39 171.4(5) . . ?
O24 W3 O39 84.7(4) . . ?
O6 W3 O39 73.2(4) . . ?
O3 W3 O39 83.8(4) . . ?
O34 W3 O39 74.8(4) . . ?
O4 W4 O23 101.4(5) . . ?
O4 W4 O14 100.0(5) . . ?
O23 W4 O14 89.1(4) . . ?
O4 W4 O18 99.5(5) . . ?
O23 W4 O18 159.0(4) . . ?
O14 W4 O18 88.9(4) . . ?
O4 W4 O26 101.6(4) . . ?
O23 W4 O26 86.4(4) . . ?
O14 W4 O26 158.4(4) . . ?
O18 W4 O26 87.9(4) . . ?
O4 W4 O11 171.0(4) . . ?
O23 W4 O11 85.2(4) . . ?
O14 W4 O11 73.8(4) . . ?
O18 W4 O11 74.1(4) . . ?
O26 W4 O11 84.8(4) . . ?
O7 W5 O13 102.8(5) . . ?
O7 W5 O21 100.4(5) . . ?
O13 W5 O21 156.7(4) . . ?
O7 W5 O34 99.4(5) . . ?
O13 W5 O34 89.9(4) . . ?
O21 W5 O34 88.7(4) . . ?
O7 W5 O23 103.3(5) . . ?
O13 W5 O23 84.4(4) . . ?
O21 W5 O23 88.0(4) . . ?
O34 W5 O23 157.2(4) . . ?
O7 W5 O39 170.5(5) . . ?
O13 W5 O39 84.1(4) . . ?
O21 W5 O39 73.1(4) . . ?
O34 W5 O39 73.8(4) . . ?
O23 W5 O39 83.7(3) . . ?
O16 W6 O10 101.4(5) . . ?
O16 W6 O2 101.6(5) . . ?
O10 W6 O2 84.4(4) . . ?
O16 W6 O14 102.2(5) . . ?
O10 W6 O14 89.3(4) . . ?
O2 W6 O14 156.1(4) . . ?
O16 W6 O33 99.7(5) . . ?
O10 W6 O33 158.8(4) . . ?
O2 W6 O33 89.4(4) . . ?
O14 W6 O33 88.3(4) . . ?
O16 W6 O11 171.8(4) . . ?
O10 W6 O11 85.2(4) . . ?
O2 W6 O11 83.8(4) . . ?
O14 W6 O11 72.7(4) . . ?
O33 W6 O11 74.0(4) . . ?
O15 W7 O2 100.6(5) . . ?
O15 W7 O12 102.5(5) . . ?
O2 W7 O12 86.8(4) . . ?
O15 W7 O31 101.5(5) . . ?
O2 W7 O31 157.9(4) . . ?
O12 W7 O31 88.2(4) . . ?
O15 W7 O32 99.5(5) . . ?
O2 W7 O32 89.1(4) . . ?
O12 W7 O32 158.0(4) . . ?
O31 W7 O32 87.5(4) . . ?
O15 W7 O28 170.8(4) . . ?
O2 W7 O28 85.0(4) . . ?
O12 W7 O28 85.0(4) . . ?
O31 W7 O28 73.1(4) . . ?
O32 W7 O28 73.2(4) . . ?
O1 W8 O13 104.1(5) . . ?
O1 W8 O26 102.2(5) . . ?
O13 W8 O26 86.3(4) . . ?
O1 W8 O40 101.0(5) . . ?
O13 W8 O40 90.7(4) . . ?
O26 W8 O40 156.6(4) . . ?
O1 W8 O36 98.5(5) . . ?
O13 W8 O36 157.4(4) . . ?
O26 W8 O36 88.3(4) . . ?
O40 W8 O36 85.6(4) . . ?
O1 W8 O19 169.7(4) . . ?
O13 W8 O19 84.6(4) . . ?
O26 W8 O19 83.7(4) . . ?
O40 W8 O19 73.0(3) . . ?
O36 W8 O19 73.0(3) . . ?
O20 W9 O17 102.1(4) . . ?
O20 W9 O24 101.4(5) . . ?
O17 W9 O24 86.3(4) . . ?
O20 W9 O38 101.2(5) . . ?
O17 W9 O38 88.8(4) . . ?
O24 W9 O38 157.4(4) . . ?
O20 W9 O40 99.2(4) . . ?
O17 W9 O40 158.6(4) . . ?
O24 W9 O40 89.6(4) . . ?
O38 W9 O40 87.0(4) . . ?
O20 W9 O19 170.4(4) . . ?
O17 W9 O19 85.9(4) . . ?
O24 W9 O19 84.2(4) . . ?
O38 W9 O19 73.5(4) . . ?
O40 W9 O19 72.8(4) . . ?
O29 W10 O30 99.7(5) . . ?
O29 W10 O18 99.1(5) . . ?
O30 W10 O18 89.0(4) . . ?
O29 W10 O33 102.2(5) . . ?
O30 W10 O33 158.1(4) . . ?
O18 W10 O33 88.8(4) . . ?
O29 W10 O25 102.7(5) . . ?
O30 W10 O25 85.3(4) . . ?
O18 W10 O25 158.1(4) . . ?
O33 W10 O25 88.7(4) . . ?
O29 W10 O11 171.8(4) . . ?
O30 W10 O11 84.2(4) . . ?
O18 W10 O11 73.7(4) . . ?
O33 W10 O11 74.3(4) . . ?
O25 W10 O11 84.7(3) . . ?
O22 W11 O32 99.9(4) . . ?
O22 W11 O25 102.6(5) . . ?
O32 W11 O25 90.3(4) . . ?
O22 W11 O9 99.4(5) . . ?
O32 W11 O9 89.2(4) . . ?
O25 W11 O9 157.7(4) . . ?
O22 W11 O35 101.8(4) . . ?
O32 W11 O35 158.2(4) . . ?
O25 W11 O35 86.4(4) . . ?
O9 W11 O35 85.9(4) . . ?
O22 W11 O28 170.2(4) . . ?
O32 W11 O28 74.4(3) . . ?
O25 W11 O28 85.7(4) . . ?
O9 W11 O28 72.8(4) . . ?
O35 W11 O28 83.8(3) . . ?
O37 W12 O30 102.7(4) . . ?
O37 W12 O36 99.7(4) . . ?
O30 W12 O36 89.9(4) . . ?
O37 W12 O38 99.5(4) . . ?
O30 W12 O38 157.8(4) . . ?
O36 W12 O38 88.3(4) . . ?
O37 W12 O35 100.9(4) . . ?
O30 W12 O35 86.7(4) . . ?
O36 W12 O35 159.3(4) . . ?
O38 W12 O35 87.3(4) . . ?
O37 W12 O19 171.4(4) . . ?
O30 W12 O19 84.2(4) . . ?
O36 W12 O19 74.8(4) . . ?
O38 W12 O19 74.0(4) . . ?
O35 W12 O19 84.6(3) . . ?
OW1 Cu3 N5 168.8(5) . . ?
OW1 Cu3 N6 97.1(5) . . ?
N5 Cu3 N6 81.1(5) . . ?
OW1 Cu3 N7 88.9(5) . . ?
N5 Cu3 N7 95.4(5) . . ?
N6 Cu3 N7 166.2(5) . . ?
OW1 Cu3 O20 82.8(4) . 2_544 ?
N5 Cu3 O20 86.4(4) . 2_544 ?
N6 Cu3 O20 96.6(4) . 2_544 ?
N7 Cu3 O20 96.4(4) . 2_544 ?
OW1 Cu3 O37 92.6(4) . 1_545 ?
N5 Cu3 O37 97.9(4) . 1_545 ?
N6 Cu3 O37 78.8(4) . 1_545 ?
N7 Cu3 O37 88.6(4) . 1_545 ?
O20 Cu3 O37 173.1(3) 2_544 1_545 ?
O41 Cu1 O42 96.0(4) . . ?
O41 Cu1 N2 170.6(5) . . ?
O42 Cu1 N2 93.1(5) . . ?
O41 Cu1 N1 90.8(5) . . ?
O42 Cu1 N1 162.9(5) . . ?
N2 Cu1 N1 81.0(5) . . ?
O41 Cu1 O27 86.5(4) . 4_565 ?
O42 Cu1 O27 89.2(4) . 4_565 ?
N2 Cu1 O27 91.4(5) . 4_565 ?
N1 Cu1 O27 106.9(5) . 4_565 ?
O41 Cu1 Cu2 30.1(3) . . ?
O42 Cu1 Cu2 71.7(3) . . ?
N2 Cu1 Cu2 155.1(4) . . ?
N1 Cu1 Cu2 118.9(3) . . ?
O27 Cu1 Cu2 69.4(2) 4_565 . ?
O41 Cu2 O43 93.3(4) . . ?
O41 Cu2 N3 93.6(5) . . ?
O43 Cu2 N3 163.3(5) . . ?
O41 Cu2 N4 166.2(5) . . ?
O43 Cu2 N4 94.4(5) . . ?
N3 Cu2 N4 82.1(5) . . ?
O41 Cu2 O4 77.9(4) . . ?
O43 Cu2 O4 84.7(4) . . ?
N3 Cu2 O4 111.7(4) . . ?
N4 Cu2 O4 91.5(4) . . ?
O41 Cu2 Cu1 29.5(3) . . ?
O43 Cu2 Cu1 75.4(3) . . ?
N3 Cu2 Cu1 104.2(4) . . ?
N4 Cu2 Cu1 164.3(3) . . ?
O4 Cu2 Cu1 99.3(2) . . ?
O19 Si1 O39 109.7(5) . . ?
O19 Si1 O28 109.4(5) . . ?
O39 Si1 O28 109.5(5) . . ?
O19 Si1 O11 109.2(5) . . ?
O39 Si1 O11 109.4(5) . . ?
O28 Si1 O11 109.7(5) . . ?
Cu1 O41 Cu2 120.4(5) . . ?
W7 O2 W6 152.2(6) . . ?
W2 O3 W3 154.6(6) . . ?
W4 O4 Cu2 143.1(6) . . ?
W3 O6 W1 122.4(5) . . ?
W2 O9 W11 122.2(5) . . ?
W1 O10 W6 152.1(6) . . ?
Si1 O11 W4 124.1(5) . . ?
Si1 O11 W10 124.4(5) . . ?
W4 O11 W10 91.0(3) . . ?
Si1 O11 W6 124.9(5) . . ?
W4 O11 W6 91.2(3) . . ?
W10 O11 W6 91.2(3) . . ?
W7 O12 W1 150.7(6) . . ?
W4 O14 W6 122.2(5) . . ?
W9 O17 W2 149.9(6) . . ?
W4 O18 W10 121.2(5) . . ?
Si1 O19 W12 124.8(5) . . ?
Si1 O19 W9 124.1(5) . . ?
W12 O19 W9 90.7(3) . . ?
Si1 O19 W8 124.7(5) . . ?
W12 O19 W8 91.2(3) . . ?
W9 O19 W8 91.0(3) . . ?
W9 O20 Cu3 129.4(5) . 2_554 ?
W1 O21 W5 122.2(5) . . ?
W4 O23 W5 151.7(5) . . ?
W9 O24 W3 152.0(5) . . ?
W11 O25 W10 151.4(5) . . ?
W8 O26 W4 150.5(6) . . ?
W1 O27 Cu1 135.7(6) . 4_566 ?
Si1 O28 W2 125.1(5) . . ?
Si1 O28 W11 124.7(5) . . ?
W2 O28 W11 91.8(3) . . ?
Si1 O28 W7 123.2(5) . . ?
W2 O28 W7 91.3(3) . . ?
W11 O28 W7 90.8(3) . . ?
W12 O30 W10 152.9(5) . . ?
W2 O31 W7 121.6(5) . . ?
W11 O32 W7 121.7(5) . . ?
W10 O33 W6 120.5(5) . . ?
W3 O34 W5 120.8(5) . . ?
W12 O35 W11 149.2(5) . . ?
W12 O36 W8 121.1(5) . . ?
W12 O37 Cu3 126.8(5) . 1_565 ?
W12 O38 W9 121.7(5) . . ?
Si1 O39 W3 124.1(5) . . ?
Si1 O39 W1 124.7(5) . . ?
W3 O39 W1 91.8(3) . . ?
Si1 O39 W5 124.6(5) . . ?
W3 O39 W5 90.6(3) . . ?
W1 O39 W5 90.9(3) . . ?
W8 O40 W9 123.2(5) . . ?
W8 O13 W5 153.3(5) . . ?
C36 O42 Cu1 132.3(9) . . ?
C36 O43 Cu2 127.7(9) . . ?
C1 N1 C5 116.9(14) . . ?
C1 N1 Cu1 127.6(10) . . ?
C5 N1 Cu1 115.5(10) . . ?
N1 C1 C2 122.8(14) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 118.6 . . ?
C3 C2 C1 119.5(15) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 117.8(16) . . ?
C2 C3 H3A 121.1 . . ?
C4 C3 H3A 121.1 . . ?
C5 C4 C3 120.9(16) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C4 C5 N1 122.1(14) . . ?
C4 C5 C6 125.0(13) . . ?
N1 C5 C6 112.8(13) . . ?
N2 C6 C7 119.8(15) . . ?
N2 C6 C5 115.3(12) . . ?
C7 C6 C5 124.9(14) . . ?
C6 C7 C8 120.4(17) . . ?
C6 C7 H7A 119.8 . . ?
C8 C7 H7A 119.8 . . ?
C9 C8 C7 117.6(15) . . ?
C9 C8 H8A 121.2 . . ?
C7 C8 H8A 121.2 . . ?
C8 C9 C10 119.4(15) . . ?
C8 C9 H9A 120.3 . . ?
C10 C9 H9A 120.3 . . ?
N2 C10 C9 122.9(15) . . ?
N2 C10 H10A 118.5 . . ?
C9 C10 H10A 118.5 . . ?
C10 N2 C6 119.8(13) . . ?
C10 N2 Cu1 125.0(11) . . ?
C6 N2 Cu1 115.1(10) . . ?
C11 N3 C15 117.2(13) . . ?
C11 N3 Cu2 127.5(11) . . ?
C15 N3 Cu2 115.3(10) . . ?
N3 C11 C12 124.8(16) . . ?
N3 C11 H11A 117.6 . . ?
C12 C11 H11A 117.6 . . ?
C11 C12 C13 116.0(15) . . ?
C11 C12 H12A 122.0 . . ?
C13 C12 H12A 122.0 . . ?
C14 C13 C12 121.8(17) . . ?
C14 C13 H13A 119.1 . . ?
C12 C13 H13A 119.1 . . ?
C13 C14 C15 117.8(17) . . ?
C13 C14 H14A 121.1 . . ?
C15 C14 H14A 121.1 . . ?
N3 C15 C14 122.3(16) . . ?
N3 C15 C16 111.6(13) . . ?
C14 C15 C16 126.1(16) . . ?
N4 C16 C17 122.3(16) . . ?
N4 C16 C15 116.8(13) . . ?
C17 C16 C15 120.9(15) . . ?
C18 C17 C16 117.7(16) . . ?
C18 C17 H17A 121.2 . . ?
C16 C17 H17A 121.2 . . ?
C19 C18 C17 119.1(16) . . ?
C19 C18 H18A 120.4 . . ?
C17 C18 H18A 120.4 . . ?
C20 C19 C18 117.9(15) . . ?
C20 C19 H19A 121.0 . . ?
C18 C19 H19A 121.0 . . ?
N4 C20 C19 123.4(14) . . ?
N4 C20 H20A 118.3 . . ?
C19 C20 H20A 118.3 . . ?
N5 C21 C22 122.5(17) . . ?
N5 C21 H21A 118.8 . . ?
C22 C21 H21A 118.8 . . ?
C23 C22 C21 119.1(19) . . ?
C23 C22 H22A 120.5 . . ?
C21 C22 H22A 120.5 . . ?
C22 C23 C24 117(2) . . ?
C22 C23 H23A 121.4 . . ?
C24 C23 H23A 121.4 . . ?
C25 C24 C23 121.7(17) . . ?
C25 C24 H24A 119.1 . . ?
C23 C24 H24A 119.1 . . ?
C24 C25 N5 119.6(15) . . ?
C24 C25 C26 126.3(15) . . ?
N5 C25 C26 114.1(14) . . ?
N6 C26 C27 122.1(16) . . ?
N6 C26 C25 116.8(14) . . ?
C27 C26 C25 121.1(15) . . ?
C28 C27 C26 118.9(18) . . ?
C28 C27 H27A 120.6 . . ?
C26 C27 H27A 120.6 . . ?
C27 C28 C29 120.2(18) . . ?
C27 C28 H28A 119.9 . . ?
C29 C28 H28A 119.9 . . ?
N6 C30 C29 122.9(17) . . ?
N6 C30 H30A 118.6 . . ?
C29 C30 H30A 118.6 . . ?
N7 C31 C32 124.1(14) . . ?
N7 C31 H31A 118.0 . . ?
C32 C31 H31A 118.0 . . ?
C31 C32 C33 118.9(14) . . ?
C31 C32 H32A 120.5 . . ?
C33 C32 H32A 120.5 . . ?
C32 C33 C34 117.9(13) . . ?
C32 C33 C36 119.7(13) . . ?
C34 C33 C36 122.2(12) . . ?
C33 C34 C35 119.5(13) . . ?
C33 C34 H34A 120.3 . . ?
C35 C34 H34A 120.3 . . ?
N7 C35 C34 122.5(14) . . ?
N7 C35 H35A 118.7 . . ?
C34 C35 H35A 118.7 . . ?
O43 C36 O42 126.4(13) . . ?
O43 C36 C33 116.9(11) . . ?
O42 C36 C33 116.7(12) . . ?
C16 N4 C20 119.3(13) . . ?
C16 N4 Cu2 113.6(10) . . ?
C20 N4 Cu2 125.8(10) . . ?
C21 N5 C25 119.9(14) . . ?
C21 N5 Cu3 126.1(11) . . ?
C25 N5 Cu3 113.9(10) . . ?
C26 N6 C30 120.4(14) . . ?
C26 N6 Cu3 114.0(11) . . ?
C30 N6 Cu3 125.5(11) . . ?
C35 N7 C31 117.0(13) . . ?
C35 N7 Cu3 121.7(10) . . ?
C31 N7 Cu3 121.0(10) . . ?
C28 C29 C30 115.5(17) . . ?
C28 C29 H29A 122.2 . . ?
C30 C29 H29A 122.2 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         3.209
_refine_diff_density_min         -2.631
_refine_diff_density_rms         0.426

# start Validation Reply Form

_vrf_PLAT306_k                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)..... Ow2
RESPONSE:  H-atoms of solvent water molecules and coordinated 
water were not located and included to refinement, however,
they were included to final formula to calculate actual 
cell metric values.
;
_vrf_PLAT342_k                   
;
PROBLEM: Low Bond Precision on  C-C Bonds .........0.0247 Ang
RESPONSE: The quality of this crystal was poor.
;
_vrf_PLAT430_k                   
;
PROBLEM: Short Inter D...A Contact  Ow1 ..  Ow2 .. 2.66 Ang
RESPONSE: there should be strong hydrogen bond between the two
water molecules.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_k2
_database_code_depnum_ccdc_archive 'CCDC 967748'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H68 Cl6 Cu6 N14 O50 Si W12'
_chemical_formula_weight         4901.69

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1

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

_cell_length_a                   11.702(2)
_cell_length_b                   14.419(3)
_cell_length_c                   18.071(4)
_cell_angle_alpha                71.19(3)
_cell_angle_beta                 88.84(3)
_cell_angle_gamma                80.19(3)
_cell_volume                     2842.1(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24255
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.53

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2247
_exptl_absorpt_coefficient_mu    13.425
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1032
_exptl_absorpt_correction_T_max  0.1961
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27840
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.49
_reflns_number_total             12791
_reflns_number_gt                10914
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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. 
restraints used:
ISOR 0.001 ow1 ow2 ow3 o5 o15 o20 o21 o22 o13 o17 o18
delu 0.02 c27 c28
;

_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)+(0.0284P)²+101.7622P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12791
_refine_ls_number_parameters     799
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1295
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.010
_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
O23 O 0.7154(10) 0.3359(7) 0.1553(6) 0.048(3) Uani 1 1 d . . .
O24 O 0.6626(9) 0.3031(6) 0.0481(6) 0.042(2) Uani 1 1 d . . .
N13 N 0.6640(11) 0.6667(8) -0.0450(7) 0.043(3) Uani 1 1 d . . .
W1 W 0.07448(4) 0.70996(4) 0.53503(3) 0.03017(12) Uani 1 1 d . . .
W2 W -0.01184(4) 0.72536(3) 0.34480(3) 0.03018(12) Uani 1 1 d . . .
W3 W 0.18864(5) 0.37087(4) 0.39635(3) 0.03376(13) Uani 1 1 d . . .
W4 W 0.25899(4) 0.58447(4) 0.42779(3) 0.03500(13) Uani 1 1 d . . .
W5 W 0.27050(4) 0.36286(4) 0.58505(3) 0.03472(13) Uani 1 1 d . . .
W6 W 0.08039(4) 0.48597(4) 0.69063(3) 0.02985(12) Uani 1 1 d . . .
Si1 Si 0.0000 0.5000 0.5000 0.0241(9) Uani 1 2 d S . .
O1 O 0.0008(12) 0.4414(11) 0.4377(8) 0.019(3) Uani 0.50 1 d P . .
O2 O 0.0650(13) 0.4320(11) 0.5826(9) 0.026(3) Uani 0.50 1 d P . .
O3 O 0.1394(12) 0.4609(11) 0.4831(8) 0.020(3) Uani 0.50 1 d P . .
O4 O 0.0550(12) 0.5994(10) 0.4647(8) 0.019(3) Uani 0.50 1 d P . .
O5 O 0.2124(12) 0.6622(10) 0.4938(8) 0.078(4) Uani 1 1 d U . .
O6 O 0.3795(8) 0.6245(8) 0.3933(6) 0.044(2) Uani 1 1 d . . .
O7 O 0.2783(9) 0.3113(8) 0.3469(6) 0.053(3) Uani 1 1 d . . .
O8 O 0.3969(8) 0.2941(7) 0.6280(6) 0.047(2) Uani 1 1 d . . .
O9 O -0.1704(9) 0.7287(9) 0.3684(8) 0.068(4) Uani 1 1 d . . .
O10 O -0.0830(8) 0.7158(8) 0.5665(7) 0.065(4) Uani 1 1 d . . .
O11 O 0.1187(10) 0.4793(10) 0.7820(6) 0.062(3) Uani 1 1 d . . .
O12 O 0.1092(9) 0.8109(8) 0.5511(8) 0.060(3) Uani 1 1 d . . .
O13 O 0.1502(12) 0.6767(10) 0.3504(8) 0.074(4) Uani 1 1 d U . .
O14 O -0.0197(11) 0.8332(7) 0.2719(6) 0.055(3) Uani 1 1 d . . .
O15 O 0.3177(13) 0.4791(11) 0.5210(8) 0.078(4) Uani 1 1 d U . .
O16 O -0.0287(10) 0.6357(9) 0.2893(9) 0.075(4) Uani 1 1 d . . .
O17 O 0.1169(12) 0.6099(10) 0.6322(8) 0.071(3) Uani 1 1 d U . .
O18 O 0.2223(11) 0.4299(10) 0.6573(8) 0.069(3) Uani 1 1 d U . .
O19 O 0.0752(9) 0.4529(8) 0.3151(7) 0.065(4) Uani 1 1 d . . .
O20 O 0.2553(13) 0.4867(11) 0.3789(9) 0.081(4) Uani 1 1 d U . .
O21 O 0.0119(12) 0.7689(10) 0.4305(8) 0.076(4) Uani 1 1 d U . .
O22 O 0.2632(13) 0.3206(11) 0.4956(9) 0.083(4) Uani 1 1 d U . .
N1 N 0.6549(10) 0.2856(7) 0.3109(7) 0.038(3) Uani 1 1 d . . .
N2 N 0.7418(10) 0.0961(7) 0.3403(6) 0.034(2) Uani 1 1 d . . .
N3 N 0.7024(10) 0.0087(7) 0.1189(6) 0.034(2) Uani 1 1 d . . .
N4 N 0.7648(10) 0.1424(8) -0.0043(6) 0.038(3) Uani 1 1 d . . .
N5 N 0.2284(11) 0.1993(10) 0.1731(8) 0.047(3) Uani 1 1 d . . .
N6 N 0.3515(10) 0.0386(8) 0.1509(7) 0.040(3) Uani 1 1 d . . .
C1 C 0.6202(14) 0.3836(11) 0.2960(10) 0.051(4) Uani 1 1 d . . .
H1A H 0.6341 0.4272 0.2474 0.062 Uiso 1 1 calc R . .
C2 C 0.5639(14) 0.4222(13) 0.3513(11) 0.056(4) Uani 1 1 d . . .
H2A H 0.5423 0.4906 0.3398 0.068 Uiso 1 1 calc R . .
C3 C 0.5403(13) 0.3590(12) 0.4227(11) 0.054(4) Uani 1 1 d . . .
H3A H 0.5014 0.3844 0.4593 0.064 Uiso 1 1 calc R . .
C4 C 0.5748(12) 0.2565(10) 0.4403(9) 0.042(3) Uani 1 1 d . . .
C5 C 0.5560(14) 0.1845(11) 0.5118(9) 0.049(4) Uani 1 1 d . . .
H5A H 0.5142 0.2048 0.5499 0.059 Uiso 1 1 calc R . .
C6 C 0.5972(15) 0.0875(13) 0.5260(9) 0.058(4) Uani 1 1 d . . .
H6A H 0.5839 0.0417 0.5737 0.070 Uiso 1 1 calc R . .
C7 C 0.6620(12) 0.0532(11) 0.4680(8) 0.041(3) Uani 1 1 d . . .
C8 C 0.7098(16) -0.0485(13) 0.4820(10) 0.059(4) Uani 1 1 d . . .
H8A H 0.6983 -0.0972 0.5285 0.071 Uiso 1 1 calc R . .
C9 C 0.7737(15) -0.0718(13) 0.4240(11) 0.059(4) Uani 1 1 d . . .
H9A H 0.8077 -0.1376 0.4317 0.071 Uiso 1 1 calc R . .
C10 C 0.7886(14) 0.0014(10) 0.3535(8) 0.046(4) Uani 1 1 d . . .
H10A H 0.8322 -0.0165 0.3151 0.056 Uiso 1 1 calc R . .
C11 C 0.6785(12) 0.1206(9) 0.3974(8) 0.036(3) Uani 1 1 d . . .
C12 C 0.6340(11) 0.2242(9) 0.3826(8) 0.034(3) Uani 1 1 d . . .
C13 C 0.6738(13) -0.0574(11) 0.1836(8) 0.042(3) Uani 1 1 d . . .
H13A H 0.6307 -0.0353 0.2204 0.051 Uiso 1 1 calc R . .
C14 C 0.7066(16) -0.1590(12) 0.1975(9) 0.059(5) Uani 1 1 d . . .
H14A H 0.6817 -0.2035 0.2420 0.071 Uiso 1 1 calc R . .
C15 C 0.7740(14) -0.1942(10) 0.1478(9) 0.047(4) Uani 1 1 d . . .
H15A H 0.7979 -0.2623 0.1584 0.056 Uiso 1 1 calc R . .
C16 C 0.8071(13) -0.1265(11) 0.0800(10) 0.046(3) Uani 1 1 d . . .
C17 C 0.8780(13) -0.1549(12) 0.0216(11) 0.054(4) Uani 1 1 d . . .
H17A H 0.9045 -0.2218 0.0285 0.065 Uiso 1 1 calc R . .
C18 C 0.9058(13) -0.0854(11) -0.0424(10) 0.049(4) Uani 1 1 d . . .
H18A H 0.9489 -0.1048 -0.0804 0.058 Uiso 1 1 calc R . .
C19 C 0.8702(11) 0.0173(10) -0.0530(8) 0.037(3) Uani 1 1 d . . .
C20 C 0.8989(15) 0.0935(14) -0.1188(9) 0.054(4) Uani 1 1 d . . .
H20A H 0.9435 0.0777 -0.1577 0.065 Uiso 1 1 calc R . .
C21 C 0.8605(16) 0.1897(17) -0.1245(9) 0.069(5) Uani 1 1 d . . .
H21A H 0.8780 0.2407 -0.1675 0.083 Uiso 1 1 calc R . .
C22 C 0.7945(15) 0.2118(12) -0.0652(9) 0.052(4) Uani 1 1 d . . .
H22A H 0.7707 0.2781 -0.0690 0.063 Uiso 1 1 calc R . .
C23 C 0.8026(11) 0.0457(10) 0.0022(8) 0.036(3) Uani 1 1 d . . .
C24 C 0.7683(12) -0.0254(10) 0.0682(8) 0.038(3) Uani 1 1 d . . .
C25 C 0.4099(14) -0.0389(10) 0.1341(11) 0.052(4) Uani 1 1 d . . .
H25A H 0.4523 -0.0274 0.0889 0.063 Uiso 1 1 calc R . .
C26 C 0.4103(17) -0.1359(11) 0.1808(12) 0.064(5) Uani 1 1 d . . .
H26A H 0.4500 -0.1891 0.1669 0.076 Uiso 1 1 calc R . .
C27 C 0.3524(17) -0.1507(14) 0.2458(13) 0.072(5) Uani 1 1 d U . .
H27A H 0.3572 -0.2154 0.2799 0.087 Uiso 1 1 calc R . .
C28 C 0.2827(17) -0.0718(15) 0.2661(10) 0.064(5) Uani 1 1 d U . .
C29 C 0.210(2) -0.084(2) 0.3317(11) 0.095(9) Uani 1 1 d . . .
H29A H 0.2084 -0.1470 0.3667 0.114 Uiso 1 1 calc R . .
C30 C 0.144(2) -0.003(2) 0.3430(12) 0.102(10) Uani 1 1 d . . .
H30A H 0.0983 -0.0116 0.3864 0.122 Uiso 1 1 calc R . .
C31 C 0.1441(15) 0.0944(18) 0.2886(10) 0.070(6) Uani 1 1 d . . .
C32 C 0.074(2) 0.178(3) 0.2966(18) 0.111(11) Uani 1 1 d . . .
H32A H 0.0242 0.1731 0.3381 0.134 Uiso 1 1 calc R . .
C33 C 0.079(2) 0.267(2) 0.2411(19) 0.105(10) Uani 1 1 d . . .
H33A H 0.0288 0.3234 0.2439 0.126 Uiso 1 1 calc R . .
C34 C 0.1584(17) 0.2789(16) 0.1789(14) 0.079(6) Uani 1 1 d . . .
H34A H 0.1608 0.3414 0.1430 0.095 Uiso 1 1 calc R . .
C35 C 0.2160(13) 0.1088(15) 0.2258(9) 0.056(5) Uani 1 1 d . . .
C36 C 0.2868(13) 0.0259(11) 0.2138(8) 0.045(3) Uani 1 1 d . . .
C37 C 0.7090(19) 0.6302(12) 0.0263(11) 0.070(6) Uani 1 1 d . . .
H37A H 0.7333 0.6727 0.0496 0.084 Uiso 1 1 calc R . .
C38 C 0.7216(17) 0.5276(10) 0.0685(9) 0.060(5) Uani 1 1 d . . .
H38A H 0.7572 0.5025 0.1182 0.073 Uiso 1 1 calc R . .
C39 C 0.6820(11) 0.4665(10) 0.0367(8) 0.037(3) Uani 1 1 d . . .
C40 C 0.6341(12) 0.5061(10) -0.0388(8) 0.037(3) Uani 1 1 d . . .
H40A H 0.6064 0.4657 -0.0628 0.044 Uiso 1 1 calc R . .
C41 C 0.6280(13) 0.6085(10) -0.0788(9) 0.044(3) Uani 1 1 d . . .
H41A H 0.5980 0.6351 -0.1300 0.052 Uiso 1 1 calc R . .
C42 C 0.6873(12) 0.3570(9) 0.0853(8) 0.036(3) Uani 1 1 d . . .
Cu1 Cu 0.73565(15) 0.21231(12) 0.24259(9) 0.0387(4) Uani 1 1 d . . .
Cu2 Cu 0.67191(15) 0.15697(12) 0.08847(9) 0.0374(4) Uani 1 1 d . . .
Cu3 Cu 0.35207(15) 0.18470(11) 0.09657(9) 0.0365(4) Uani 1 1 d . . .
Cl1 Cl 0.8676(3) 0.1354(3) 0.1791(2) 0.0488(8) Uani 1 1 d . . .
Cl2 Cl 0.5459(3) 0.1653(3) 0.18728(19) 0.0393(7) Uani 1 1 d . . .
Cl3 Cl 0.4637(3) 0.1602(3) -0.0011(2) 0.0499(9) Uani 1 1 d . . .
OW2 O 0.967(3) 0.347(2) 0.0392(18) 0.203(11) Uani 1 1 d U . .
OW1 O 1.105(4) 0.542(3) 0.125(3) 0.297(17) Uani 1 1 d U . .
OW3 O 1.299(3) 0.552(3) 0.205(2) 0.261(15) 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
O23 C42 1.238(16) . ?
O23 Cu1 1.944(9) . ?
O24 C42 1.251(16) . ?
O24 Cu2 1.979(9) . ?
N13 C37 1.307(19) . ?
N13 C41 1.311(17) . ?
N13 Cu3 2.019(10) 2_665 ?
W1 O12 1.688(10) . ?
W1 O5 1.881(14) . ?
W1 O17 1.889(13) . ?
W1 O21 1.907(14) . ?
W1 O10 1.913(10) . ?
W1 O4 2.377(14) . ?
W1 O1 2.393(14) 2_566 ?
W2 O14 1.672(9) . ?
W2 O21 1.890(14) . ?
W2 O9 1.892(10) . ?
W2 O13 1.900(14) . ?
W2 O16 1.909(11) . ?
W2 O4 2.377(13) . ?
W2 O2 2.405(15) 2_566 ?
W3 O7 1.670(9) . ?
W3 O10 1.869(10) 2_566 ?
W3 O22 1.875(15) . ?
W3 O20 1.894(15) . ?
W3 O19 1.935(11) . ?
W3 O3 2.344(14) . ?
W3 O1 2.468(14) . ?
W4 O6 1.649(9) . ?
W4 O20 1.897(14) . ?
W4 O5 1.899(14) . ?
W4 O13 1.907(14) . ?
W4 O15 1.912(14) . ?
W4 O3 2.403(14) . ?
W4 O4 2.458(14) . ?
W5 O8 1.680(9) . ?
W5 O15 1.869(14) . ?
W5 O18 1.886(13) . ?
W5 O9 1.896(10) 2_566 ?
W5 O22 1.910(14) . ?
W5 O3 2.333(14) . ?
W5 O2 2.437(16) . ?
W6 O11 1.688(10) . ?
W6 O19 1.872(10) 2_566 ?
W6 O17 1.875(13) . ?
W6 O16 1.876(11) 2_566 ?
W6 O18 1.895(13) . ?
W6 O2 2.343(15) . ?
W6 O1 2.358(14) 2_566 ?
Si1 O4 1.607(13) . ?
Si1 O4 1.607(13) 2_566 ?
Si1 O1 1.609(13) 2_566 ?
Si1 O1 1.609(13) . ?
Si1 O2 1.618(16) 2_566 ?
Si1 O2 1.618(16) . ?
Si1 O3 1.688(14) 2_566 ?
Si1 O3 1.688(14) . ?
O1 O2 1.78(2) 2_566 ?
O1 O4 1.815(19) 2_566 ?
O1 W6 2.358(14) 2_566 ?
O1 W1 2.393(14) 2_566 ?
O2 O1 1.78(2) 2_566 ?
O2 O4 1.85(2) 2_566 ?
O2 W2 2.405(15) 2_566 ?
O4 O1 1.815(19) 2_566 ?
O4 O2 1.85(2) 2_566 ?
O9 W5 1.896(10) 2_566 ?
O10 W3 1.869(10) 2_566 ?
O16 W6 1.876(11) 2_566 ?
O19 W6 1.872(10) 2_566 ?
N1 C1 1.342(17) . ?
N1 C12 1.357(17) . ?
N1 Cu1 1.997(11) . ?
N2 C10 1.326(17) . ?
N2 C11 1.363(16) . ?
N2 Cu1 1.997(10) . ?
N3 C13 1.327(16) . ?
N3 C24 1.347(17) . ?
N3 Cu2 1.997(10) . ?
N4 C22 1.314(17) . ?
N4 C23 1.357(17) . ?
N4 Cu2 2.027(11) . ?
N5 C34 1.32(2) . ?
N5 C35 1.37(2) . ?
N5 Cu3 2.013(12) . ?
N6 C25 1.326(19) . ?
N6 C36 1.332(18) . ?
N6 Cu3 2.019(11) . ?
C1 C2 1.40(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.37(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.40(2) . ?
C3 H3A 0.9300 . ?
C4 C12 1.400(18) . ?
C4 C5 1.41(2) . ?
C5 C6 1.34(2) . ?
C5 H5A 0.9300 . ?
C6 C7 1.45(2) . ?
C6 H6A 0.9300 . ?
C7 C11 1.365(19) . ?
C7 C8 1.42(2) . ?
C8 C9 1.37(2) . ?
C8 H8A 0.9300 . ?
C9 C10 1.40(2) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.434(17) . ?
C13 C14 1.39(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.35(2) . ?
C14 H14A 0.9300 . ?
C15 C16 1.39(2) . ?
C15 H15A 0.9300 . ?
C16 C24 1.398(19) . ?
C16 C17 1.45(2) . ?
C17 C18 1.34(2) . ?
C17 H17A 0.9300 . ?
C18 C19 1.419(19) . ?
C18 H18A 0.9300 . ?
C19 C23 1.381(18) . ?
C19 C20 1.41(2) . ?
C20 C21 1.35(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.39(2) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.402(19) . ?
C25 C26 1.38(2) . ?
C25 H25A 0.9300 . ?
C26 C27 1.32(3) . ?
C26 H26A 0.9300 . ?
C27 C28 1.43(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.43(3) . ?
C28 C36 1.43(2) . ?
C29 C30 1.35(4) . ?
C29 H29A 0.9300 . ?
C30 C31 1.44(3) . ?
C30 H30A 0.9300 . ?
C31 C35 1.38(2) . ?
C31 C32 1.38(3) . ?
C32 C33 1.37(4) . ?
C32 H32A 0.9300 . ?
C33 C34 1.43(3) . ?
C33 H33A 0.9300 . ?
C34 H34A 0.9300 . ?
C35 C36 1.41(2) . ?
C37 C38 1.413(19) . ?
C37 H37A 0.9300 . ?
C38 C39 1.342(19) . ?
C38 H38A 0.9300 . ?
C39 C40 1.386(18) . ?
C39 C42 1.530(17) . ?
C40 C41 1.408(18) . ?
C40 H40A 0.9300 . ?
C41 H41A 0.9300 . ?
Cu1 Cl1 2.258(4) . ?
Cu1 Cl2 2.726(4) . ?
Cu1 Cu2 3.266(2) . ?
Cu2 Cl2 2.313(4) . ?
Cu2 Cl1 2.757(4) . ?
Cu2 Cl3 2.938(5) . ?
Cu3 N13 2.019(10) 2_665 ?
Cu3 Cl3 2.257(4) . ?
Cu3 Cl2 2.748(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
C42 O23 Cu1 132.9(8) . . ?
C42 O24 Cu2 126.6(9) . . ?
C37 N13 C41 120.4(12) . . ?
C37 N13 Cu3 116.7(10) . 2_665 ?
C41 N13 Cu3 122.9(10) . 2_665 ?
O12 W1 O5 101.3(6) . . ?
O12 W1 O17 101.9(6) . . ?
O5 W1 O17 89.4(6) . . ?
O12 W1 O21 100.0(6) . . ?
O5 W1 O21 88.0(6) . . ?
O17 W1 O21 158.0(6) . . ?
O12 W1 O10 101.5(6) . . ?
O5 W1 O10 157.2(6) . . ?
O17 W1 O10 87.7(5) . . ?
O21 W1 O10 86.3(6) . . ?
O12 W1 O4 157.6(6) . . ?
O5 W1 O4 65.0(5) . . ?
O17 W1 O4 95.8(5) . . ?
O21 W1 O4 63.4(5) . . ?
O10 W1 O4 92.8(6) . . ?
O12 W1 O1 157.7(6) . 2_566 ?
O5 W1 O1 94.3(5) . 2_566 ?
O17 W1 O1 62.1(5) . 2_566 ?
O21 W1 O1 96.4(5) . 2_566 ?
O10 W1 O1 64.4(5) . 2_566 ?
O4 W1 O1 44.7(5) . 2_566 ?
O14 W2 O21 99.6(6) . . ?
O14 W2 O9 100.3(6) . . ?
O21 W2 O9 89.5(6) . . ?
O14 W2 O13 100.7(6) . . ?
O21 W2 O13 87.7(6) . . ?
O9 W2 O13 159.0(6) . . ?
O14 W2 O16 101.7(6) . . ?
O21 W2 O16 158.7(6) . . ?
O9 W2 O16 88.0(4) . . ?
O13 W2 O16 87.1(5) . . ?
O14 W2 O4 157.8(5) . . ?
O21 W2 O4 63.6(5) . . ?
O9 W2 O4 94.1(6) . . ?
O13 W2 O4 66.1(5) . . ?
O16 W2 O4 95.5(6) . . ?
O14 W2 O2 156.6(6) . 2_566 ?
O21 W2 O2 97.9(6) . 2_566 ?
O9 W2 O2 64.3(5) . 2_566 ?
O13 W2 O2 95.5(6) . 2_566 ?
O16 W2 O2 62.1(6) . 2_566 ?
O4 W2 O2 45.5(5) . 2_566 ?
O7 W3 O10 102.2(6) . 2_566 ?
O7 W3 O22 100.8(6) . . ?
O10 W3 O22 88.6(6) 2_566 . ?
O7 W3 O20 100.3(6) . . ?
O10 W3 O20 157.6(6) 2_566 . ?
O22 W3 O20 88.1(6) . . ?
O7 W3 O19 101.3(6) . . ?
O10 W3 O19 88.8(4) 2_566 . ?
O22 W3 O19 157.8(6) . . ?
O20 W3 O19 86.0(6) . . ?
O7 W3 O3 155.8(5) . . ?
O10 W3 O3 95.3(6) 2_566 . ?
O22 W3 O3 62.6(6) . . ?
O20 W3 O3 63.6(5) . . ?
O19 W3 O3 95.7(6) . . ?
O7 W3 O1 156.9(5) . . ?
O10 W3 O1 63.3(5) 2_566 . ?
O22 W3 O1 96.8(6) . . ?
O20 W3 O1 95.1(6) . . ?
O19 W3 O1 62.6(5) . . ?
O3 W3 O1 47.3(5) . . ?
O6 W4 O20 100.5(6) . . ?
O6 W4 O5 101.3(6) . . ?
O20 W4 O5 158.1(6) . . ?
O6 W4 O13 99.4(6) . . ?
O20 W4 O13 90.1(6) . . ?
O5 W4 O13 87.8(6) . . ?
O6 W4 O15 100.9(6) . . ?
O20 W4 O15 88.1(6) . . ?
O5 W4 O15 86.4(6) . . ?
O13 W4 O15 159.6(6) . . ?
O6 W4 O3 155.3(5) . . ?
O20 W4 O3 62.3(6) . . ?
O5 W4 O3 96.5(6) . . ?
O13 W4 O3 98.4(5) . . ?
O15 W4 O3 63.0(5) . . ?
O6 W4 O4 156.3(5) . . ?
O20 W4 O4 96.6(6) . . ?
O5 W4 O4 63.0(5) . . ?
O13 W4 O4 64.2(5) . . ?
O15 W4 O4 95.9(5) . . ?
O3 W4 O4 48.5(5) . . ?
O8 W5 O15 102.0(6) . . ?
O8 W5 O18 100.6(5) . . ?
O15 W5 O18 88.4(6) . . ?
O8 W5 O9 99.0(6) . 2_566 ?
O15 W5 O9 159.0(6) . 2_566 ?
O18 W5 O9 88.7(5) . 2_566 ?
O8 W5 O22 100.8(6) . . ?
O15 W5 O22 89.0(6) . . ?
O18 W5 O22 158.5(6) . . ?
O9 W5 O22 86.1(6) 2_566 . ?
O8 W5 O3 157.5(5) . . ?
O15 W5 O3 65.0(6) . . ?
O18 W5 O3 97.3(5) . . ?
O9 W5 O3 94.8(6) 2_566 . ?
O22 W5 O3 62.4(6) . . ?
O8 W5 O2 154.5(5) . . ?
O15 W5 O2 96.8(6) . . ?
O18 W5 O2 62.6(5) . . ?
O9 W5 O2 63.6(5) 2_566 . ?
O22 W5 O2 96.5(6) . . ?
O3 W5 O2 47.8(5) . . ?
O11 W6 O19 100.3(6) . 2_566 ?
O11 W6 O17 101.0(6) . . ?
O19 W6 O17 88.5(5) 2_566 . ?
O11 W6 O16 100.7(6) . 2_566 ?
O19 W6 O16 88.0(5) 2_566 2_566 ?
O17 W6 O16 158.2(6) . 2_566 ?
O11 W6 O18 101.2(6) . . ?
O19 W6 O18 158.5(6) 2_566 . ?
O17 W6 O18 86.2(6) . . ?
O16 W6 O18 89.2(5) 2_566 . ?
O11 W6 O2 157.8(6) . . ?
O19 W6 O2 95.2(6) 2_566 . ?
O17 W6 O2 95.1(6) . . ?
O16 W6 O2 63.9(6) 2_566 . ?
O18 W6 O2 64.6(5) . . ?
O11 W6 O1 157.7(6) . 2_566 ?
O19 W6 O1 65.7(5) 2_566 2_566 ?
O17 W6 O1 63.0(5) . 2_566 ?
O16 W6 O1 96.1(6) 2_566 2_566 ?
O18 W6 O1 93.4(5) . 2_566 ?
O2 W6 O1 44.4(5) . 2_566 ?
O4 Si1 O4 180.0(10) . 2_566 ?
O4 Si1 O1 68.7(7) . 2_566 ?
O4 Si1 O1 111.3(7) 2_566 2_566 ?
O4 Si1 O1 111.3(7) . . ?
O4 Si1 O1 68.7(7) 2_566 . ?
O1 Si1 O1 180.000(2) 2_566 . ?
O4 Si1 O2 70.0(7) . 2_566 ?
O4 Si1 O2 110.0(7) 2_566 2_566 ?
O1 Si1 O2 113.2(7) 2_566 2_566 ?
O1 Si1 O2 66.8(7) . 2_566 ?
O4 Si1 O2 110.0(7) . . ?
O4 Si1 O2 70.0(7) 2_566 . ?
O1 Si1 O2 66.8(7) 2_566 . ?
O1 Si1 O2 113.2(7) . . ?
O2 Si1 O2 180.0(8) 2_566 . ?
O4 Si1 O3 105.5(7) . 2_566 ?
O4 Si1 O3 74.5(7) 2_566 2_566 ?
O1 Si1 O3 71.8(7) 2_566 2_566 ?
O1 Si1 O3 108.2(7) . 2_566 ?
O2 Si1 O3 71.6(7) 2_566 2_566 ?
O2 Si1 O3 108.4(7) . 2_566 ?
O4 Si1 O3 74.5(7) . . ?
O4 Si1 O3 105.5(7) 2_566 . ?
O1 Si1 O3 108.2(7) 2_566 . ?
O1 Si1 O3 71.8(7) . . ?
O2 Si1 O3 108.4(7) 2_566 . ?
O2 Si1 O3 71.6(7) . . ?
O3 Si1 O3 180.0(9) 2_566 . ?
Si1 O1 O2 56.8(7) . 2_566 ?
Si1 O1 O4 55.6(6) . 2_566 ?
O2 O1 O4 94.6(9) 2_566 2_566 ?
Si1 O1 W6 124.1(8) . 2_566 ?
O2 O1 W6 67.3(7) 2_566 2_566 ?
O4 O1 W6 135.9(8) 2_566 2_566 ?
Si1 O1 W1 122.7(7) . 2_566 ?
O2 O1 W1 133.5(9) 2_566 2_566 ?
O4 O1 W1 67.2(6) 2_566 2_566 ?
W6 O1 W1 95.7(5) 2_566 2_566 ?
Si1 O1 W3 119.0(7) . . ?
O2 O1 W3 129.4(8) 2_566 . ?
O4 O1 W3 125.6(8) 2_566 . ?
W6 O1 W3 94.4(5) 2_566 . ?
W1 O1 W3 93.4(5) 2_566 . ?
Si1 O2 O1 56.4(7) . 2_566 ?
Si1 O2 O4 54.7(6) . 2_566 ?
O1 O2 O4 94.1(9) 2_566 2_566 ?
Si1 O2 W6 124.6(8) . . ?
O1 O2 W6 68.3(7) 2_566 . ?
O4 O2 W6 134.4(9) 2_566 . ?
Si1 O2 W2 121.2(8) . 2_566 ?
O1 O2 W2 134.9(9) 2_566 2_566 ?
O4 O2 W2 66.4(6) 2_566 2_566 ?
W6 O2 W2 96.0(6) . 2_566 ?
Si1 O2 W5 119.2(8) . . ?
O1 O2 W5 128.3(9) 2_566 . ?
O4 O2 W5 126.5(9) 2_566 . ?
W6 O2 W5 94.9(5) . . ?
W2 O2 W5 93.8(5) 2_566 . ?
Si1 O3 W5 121.4(7) . . ?
Si1 O3 W3 121.9(7) . . ?
W5 O3 W3 97.7(5) . . ?
Si1 O3 W4 118.1(7) . . ?
W5 O3 W4 95.6(5) . . ?
W3 O3 W4 96.3(5) . . ?
Si1 O4 O1 55.7(6) . 2_566 ?
Si1 O4 O2 55.3(6) . 2_566 ?
O1 O4 O2 94.6(9) 2_566 2_566 ?
Si1 O4 W1 123.8(7) . . ?
O1 O4 W1 68.1(6) 2_566 . ?
O2 O4 W1 136.6(9) 2_566 . ?
Si1 O4 W2 123.3(7) . . ?
O1 O4 W2 135.1(9) 2_566 . ?
O2 O4 W2 68.0(6) 2_566 . ?
W1 O4 W2 95.9(5) . . ?
Si1 O4 W4 118.9(7) . . ?
O1 O4 W4 127.6(8) 2_566 . ?
O2 O4 W4 126.1(8) 2_566 . ?
W1 O4 W4 93.7(5) . . ?
W2 O4 W4 93.7(5) . . ?
W1 O5 W4 138.0(8) . . ?
W2 O9 W5 138.0(7) . 2_566 ?
W3 O10 W1 138.5(7) 2_566 . ?
W2 O13 W4 135.9(8) . . ?
W5 O15 W4 136.3(8) . . ?
W6 O16 W2 137.5(8) 2_566 . ?
W6 O17 W1 138.9(8) . . ?
W5 O18 W6 137.4(7) . . ?
W6 O19 W3 136.9(7) 2_566 . ?
W3 O20 W4 137.6(8) . . ?
W2 O21 W1 136.7(8) . . ?
W3 O22 W5 137.0(8) . . ?
C1 N1 C12 117.5(13) . . ?
C1 N1 Cu1 129.6(11) . . ?
C12 N1 Cu1 112.8(8) . . ?
C10 N2 C11 118.3(11) . . ?
C10 N2 Cu1 129.6(9) . . ?
C11 N2 Cu1 111.8(8) . . ?
C13 N3 C24 117.9(12) . . ?
C13 N3 Cu2 128.7(10) . . ?
C24 N3 Cu2 113.2(8) . . ?
C22 N4 C23 118.6(12) . . ?
C22 N4 Cu2 129.2(10) . . ?
C23 N4 Cu2 112.2(8) . . ?
C34 N5 C35 117.2(15) . . ?
C34 N5 Cu3 131.1(14) . . ?
C35 N5 Cu3 111.6(10) . . ?
C25 N6 C36 120.9(13) . . ?
C25 N6 Cu3 128.7(10) . . ?
C36 N6 Cu3 110.3(10) . . ?
N1 C1 C2 121.9(16) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 119.9(15) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 119.8(14) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C3 C4 C12 116.7(14) . . ?
C3 C4 C5 124.8(14) . . ?
C12 C4 C5 118.5(12) . . ?
C6 C5 C4 121.4(13) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
C5 C6 C7 120.8(15) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C11 C7 C8 118.6(13) . . ?
C11 C7 C6 119.2(13) . . ?
C8 C7 C6 122.2(14) . . ?
C9 C8 C7 117.1(16) . . ?
C9 C8 H8A 121.4 . . ?
C7 C8 H8A 121.4 . . ?
C8 C9 C10 121.2(16) . . ?
C8 C9 H9A 119.4 . . ?
C10 C9 H9A 119.4 . . ?
N2 C10 C9 121.3(14) . . ?
N2 C10 H10A 119.4 . . ?
C9 C10 H10A 119.4 . . ?
N2 C11 C7 123.4(11) . . ?
N2 C11 C12 116.7(12) . . ?
C7 C11 C12 119.8(12) . . ?
N1 C12 C4 124.1(12) . . ?
N1 C12 C11 115.5(12) . . ?
C4 C12 C11 120.3(12) . . ?
N3 C13 C14 121.4(14) . . ?
N3 C13 H13A 119.3 . . ?
C14 C13 H13A 119.3 . . ?
C15 C14 C13 121.2(14) . . ?
C15 C14 H14A 119.4 . . ?
C13 C14 H14A 119.4 . . ?
C14 C15 C16 118.6(14) . . ?
C14 C15 H15A 120.7 . . ?
C16 C15 H15A 120.7 . . ?
C15 C16 C24 117.4(14) . . ?
C15 C16 C17 124.0(14) . . ?
C24 C16 C17 118.6(15) . . ?
C18 C17 C16 120.5(14) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C17 C18 C19 120.9(13) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C23 C19 C20 117.5(13) . . ?
C23 C19 C18 119.4(13) . . ?
C20 C19 C18 123.1(13) . . ?
C21 C20 C19 119.1(14) . . ?
C21 C20 H20A 120.4 . . ?
C19 C20 H20A 120.4 . . ?
C20 C21 C22 119.5(15) . . ?
C20 C21 H21A 120.2 . . ?
C22 C21 H21A 120.2 . . ?
N4 C22 C21 122.5(16) . . ?
N4 C22 H22A 118.7 . . ?
C21 C22 H22A 118.7 . . ?
N4 C23 C19 122.7(12) . . ?
N4 C23 C24 116.3(12) . . ?
C19 C23 C24 121.0(13) . . ?
N3 C24 C16 123.3(13) . . ?
N3 C24 C23 117.1(12) . . ?
C16 C24 C23 119.5(13) . . ?
N6 C25 C26 122.7(17) . . ?
N6 C25 H25A 118.6 . . ?
C26 C25 H25A 118.6 . . ?
C27 C26 C25 117.8(18) . . ?
C27 C26 H26A 121.1 . . ?
C25 C26 H26A 121.1 . . ?
C26 C27 C28 122.8(17) . . ?
C26 C27 H27A 118.6 . . ?
C28 C27 H27A 118.6 . . ?
C29 C28 C27 125(2) . . ?
C29 C28 C36 119(2) . . ?
C27 C28 C36 115.2(16) . . ?
C30 C29 C28 120(2) . . ?
C30 C29 H29A 120.0 . . ?
C28 C29 H29A 120.0 . . ?
C29 C30 C31 120.8(19) . . ?
C29 C30 H30A 119.6 . . ?
C31 C30 H30A 119.6 . . ?
C35 C31 C32 117(2) . . ?
C35 C31 C30 121(2) . . ?
C32 C31 C30 122(2) . . ?
C33 C32 C31 118(2) . . ?
C33 C32 H32A 121.2 . . ?
C31 C32 H32A 121.2 . . ?
C32 C33 C34 123(2) . . ?
C32 C33 H33A 118.5 . . ?
C34 C33 H33A 118.5 . . ?
N5 C34 C33 119(2) . . ?
N5 C34 H34A 120.5 . . ?
C33 C34 H34A 120.5 . . ?
N5 C35 C31 125.6(19) . . ?
N5 C35 C36 115.0(12) . . ?
C31 C35 C36 119.4(18) . . ?
N6 C36 C35 119.7(13) . . ?
N6 C36 C28 120.3(16) . . ?
C35 C36 C28 119.8(15) . . ?
N13 C37 C38 121.4(14) . . ?
N13 C37 H37A 119.3 . . ?
C38 C37 H37A 119.3 . . ?
C39 C38 C37 119.7(14) . . ?
C39 C38 H38A 120.2 . . ?
C37 C38 H38A 120.2 . . ?
C38 C39 C40 118.3(13) . . ?
C38 C39 C42 119.3(12) . . ?
C40 C39 C42 122.4(12) . . ?
C39 C40 C41 119.2(12) . . ?
C39 C40 H40A 120.4 . . ?
C41 C40 H40A 120.4 . . ?
N13 C41 C40 121.0(13) . . ?
N13 C41 H41A 119.5 . . ?
C40 C41 H41A 119.5 . . ?
O23 C42 O24 130.2(11) . . ?
O23 C42 C39 115.0(11) . . ?
O24 C42 C39 114.8(11) . . ?
O23 Cu1 N1 89.6(4) . . ?
O23 Cu1 N2 172.0(5) . . ?
N1 Cu1 N2 82.4(4) . . ?
O23 Cu1 Cl1 92.0(4) . . ?
N1 Cu1 Cl1 165.5(4) . . ?
N2 Cu1 Cl1 96.0(3) . . ?
O23 Cu1 Cl2 89.0(3) . . ?
N1 Cu1 Cl2 98.3(3) . . ?
N2 Cu1 Cl2 90.9(3) . . ?
Cl1 Cu1 Cl2 96.13(13) . . ?
O23 Cu1 Cu2 73.5(3) . . ?
N1 Cu1 Cu2 137.6(3) . . ?
N2 Cu1 Cu2 111.7(3) . . ?
Cl1 Cu1 Cu2 56.37(11) . . ?
Cl2 Cu1 Cu2 44.27(8) . . ?
O24 Cu2 N3 171.2(4) . . ?
O24 Cu2 N4 90.6(4) . . ?
N3 Cu2 N4 81.2(4) . . ?
O24 Cu2 Cl2 92.7(3) . . ?
N3 Cu2 Cl2 95.8(3) . . ?
N4 Cu2 Cl2 171.9(3) . . ?
O24 Cu2 Cl1 91.3(3) . . ?
N3 Cu2 Cl1 86.0(3) . . ?
N4 Cu2 Cl1 93.2(3) . . ?
Cl2 Cu2 Cl1 94.02(12) . . ?
O24 Cu2 Cl3 94.0(3) . . ?
N3 Cu2 Cl3 88.9(3) . . ?
N4 Cu2 Cl3 87.3(3) . . ?
Cl2 Cu2 Cl3 85.17(12) . . ?
Cl1 Cu2 Cl3 174.70(13) . . ?
O24 Cu2 Cu1 76.5(3) . . ?
N3 Cu2 Cu1 106.7(3) . . ?
N4 Cu2 Cu1 132.6(3) . . ?
Cl2 Cu2 Cu1 55.35(9) . . ?
Cl1 Cu2 Cu1 43.00(8) . . ?
Cl3 Cu2 Cu1 138.15(10) . . ?
N5 Cu3 N6 82.3(5) . . ?
N5 Cu3 N13 92.6(5) . 2_665 ?
N6 Cu3 N13 174.3(5) . 2_665 ?
N5 Cu3 Cl3 168.9(4) . . ?
N6 Cu3 Cl3 94.5(4) . . ?
N13 Cu3 Cl3 90.0(4) 2_665 . ?
N5 Cu3 Cl2 99.6(4) . . ?
N6 Cu3 Cl2 87.8(3) . . ?
N13 Cu3 Cl2 95.7(4) 2_665 . ?
Cl3 Cu3 Cl2 90.87(14) . . ?
Cu1 Cl1 Cu2 80.63(12) . . ?
Cu2 Cl2 Cu1 80.38(11) . . ?
Cu2 Cl2 Cu3 93.60(12) . . ?
Cu1 Cl2 Cu3 159.82(15) . . ?
Cu3 Cl3 Cu2 89.87(13) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         3.261
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.279

# start Validation Reply Form

_vrf_PLAT306_k                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)..... Ow2
RESPONSE:  H-atoms of solvent water molecules and coordinated 
water were not located and included to refinement, however,
they were included to final formula to calculate actual 
cell metric values.
;
_vrf_PLAT342_k                   
;
PROBLEM: Low Bond Precision on  C-C Bonds .........0.0256 Ang
RESPONSE: The quality of this crystal was poor.
;
_vrf_PLAT430_k                   
;
PROBLEM: Short Inter D...A Contact  Ow1 ..  Ow3 ..  2.77Ang
RESPONSE: there should be strong hydrogen bond between the two
water molecules.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_k3
_database_code_depnum_ccdc_archive 'CCDC 967749'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl2 Cu4 N10 O46 Si W12'
_chemical_formula_weight         4100.29

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p2(1)/n

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

_cell_length_a                   15.070(4)
_cell_length_b                   13.496(3)
_cell_length_c                   18.814(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.953(4)
_cell_angle_gamma                90.00
_cell_volume                     3825.9(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    10087
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      35.28

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3684
_exptl_absorpt_coefficient_mu    19.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0687
_exptl_absorpt_correction_T_max  0.1071
_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  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15229
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.84
_reflns_number_total             7252
_reflns_number_gt                7110
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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. 

restraints used:
ISOR 0.001 c15 c5 c6 c7 c10 c12 c16 c19
ISOR 0.001 c3 c25 n4 c18 c24 c8 c23 o18
 
simu 0.02 0.04 3.8 $O
delu 0.02 w4 o2
delu 0.01 w3 o9
delu 0.01 w1 o8
;

_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)+(0.0001P)²+1223.2614P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7252
_refine_ls_number_parameters     593
_refine_ls_number_restraints     542
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.1076
_refine_ls_wR_factor_ref         0.2304
_refine_ls_wR_factor_gt          0.2300
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.58053(9) 1.48224(10) -0.67511(7) 0.0319(3) Uani 1 1 d . . .
W2 W 0.67646(9) 1.33973(10) -0.53742(7) 0.0311(3) Uani 1 1 d . . .
W3 W 0.59907(10) 1.36080(10) -0.36248(8) 0.0363(4) Uani 1 1 d U . .
W4 W 0.70832(9) 1.59958(11) -0.54081(8) 0.0335(3) Uani 1 1 d U . .
W5 W 0.46911(11) 1.23939(10) -0.49352(8) 0.0374(4) Uani 1 1 d . . .
W6 W 0.62784(10) 1.62053(11) -0.36707(8) 0.0392(4) Uani 1 1 d . . .
Si1 Si 0.5000 1.5000 -0.5000 0.030(3) Uani 1 2 d S . .
O1 O 0.454(3) 1.606(3) -0.520(3) 0.038(6) Uani 0.50 1 d PU . .
O2 O 0.585(4) 1.482(4) -0.544(3) 0.046(4) Uani 0.50 1 d PU . .
O3 O 0.475(4) 1.499(4) -0.586(3) 0.042(5) Uani 0.50 1 d PU . .
O4 O 0.431(3) 1.411(4) -0.515(3) 0.042(5) Uani 0.50 1 d PU . .
Cu2 Cu 0.8078(3) 1.1129(3) -0.6233(3) 0.0427(11) Uani 1 1 d . . .
Cu1 Cu 0.8942(3) 0.7977(4) -0.4774(3) 0.0475(12) Uani 1 1 d . . .
O22 O 0.4510(16) 1.1197(15) -0.4910(11) 0.030(5) Uani 1 1 d U . .
O21 O 0.7619(17) 1.2679(18) -0.5552(13) 0.042(5) Uani 1 1 d U . .
O20 O 0.6898(14) 1.6764(19) -0.3040(12) 0.038(5) Uani 1 1 d U . .
O18 O 0.6200(19) 1.475(2) -0.7555(15) 0.053(6) Uani 1 1 d U . .
O19 O 0.8054(18) 1.6509(18) -0.5592(13) 0.044(6) Uani 1 1 d U . .
O17 O 0.6481(16) 1.2950(19) -0.2950(13) 0.040(5) Uani 1 1 d U . .
O16 O 0.7345(19) 1.467(2) -0.5305(14) 0.048(4) Uani 1 1 d U . .
O15 O 0.6618(18) 1.5708(18) -0.6326(14) 0.046(4) Uani 1 1 d U . .
O14 O 0.683(2) 1.327(2) -0.4332(15) 0.055(4) Uani 1 1 d U . .
O13 O 0.522(2) 1.603(2) -0.3137(18) 0.058(5) Uani 1 1 d U . .
O12 O 0.713(2) 1.612(2) -0.4413(16) 0.057(4) Uani 1 1 d U . .
O11 O 0.6397(19) 1.3716(19) -0.6287(14) 0.047(4) Uani 1 1 d U . .
O10 O 0.5834(19) 1.246(2) -0.5360(14) 0.051(4) Uani 1 1 d U . .
O9 O 0.6489(19) 1.488(2) -0.3525(16) 0.054(4) Uani 1 1 d U . .
O8 O 0.4963(19) 1.411(2) -0.3202(17) 0.055(4) Uani 1 1 d U . .
O7 O 0.6346(19) 1.709(2) -0.5465(14) 0.049(4) Uani 1 1 d U . .
O6 O 0.5281(18) 1.257(2) -0.4042(14) 0.051(4) Uani 1 1 d U . .
O5 O 0.4222(19) 1.269(2) -0.5845(14) 0.048(4) Uani 1 1 d U . .
Cl1 Cl 0.9526(6) 1.1016(6) -0.5955(5) 0.045(2) Uani 1 1 d . . .
N4 N 0.8202(18) 1.202(2) -0.7080(14) 0.029(6) Uani 1 1 d U . .
O41 O 0.8382(18) 0.9038(18) -0.5275(12) 0.041(5) Uani 1 1 d U . .
N5 N 0.7584(19) 0.901(2) -0.3129(14) 0.038(7) Uani 1 1 d . . .
O43 O 0.8195(18) 0.8183(17) -0.3960(12) 0.041(6) Uani 1 1 d U . .
N2 N 0.9480(16) 0.6769(19) -0.4354(13) 0.026(6) Uani 1 1 d . . .
N1 N 0.9877(16) 0.7792(19) -0.5498(14) 0.025(5) Uani 1 1 d . . .
C1 C 1.006(2) 0.837(3) -0.6026(17) 0.042(10) Uani 1 1 d . . .
H1A H 0.9688 0.8908 -0.6117 0.051 Uiso 1 1 calc R . .
C16 C 0.738(2) 1.220(3) -0.7424(19) 0.037(8) Uani 1 1 d U . .
N3 N 0.6824(18) 1.1110(19) -0.6581(14) 0.029(6) Uani 1 1 d . . .
C23 C 0.714(3) 0.985(3) -0.288(2) 0.046(9) Uani 1 1 d U . .
H23A H 0.6987 0.9888 -0.2406 0.055 Uiso 1 1 calc R . .
C25 C 0.7650(19) 0.974(2) -0.4271(15) 0.021(6) Uani 1 1 d U . .
C6 C 1.0164(19) 0.648(2) -0.4712(15) 0.024(6) Uani 1 1 d U . .
C10 C 0.926(2) 0.636(3) -0.3764(18) 0.034(7) Uani 1 1 d U . .
H10A H 0.8785 0.6624 -0.3515 0.041 Uiso 1 1 calc R . .
O40 O 0.768(2) 1.046(2) -0.5383(13) 0.050(6) Uani 1 1 d U . .
C15 C 0.665(2) 1.168(2) -0.7170(17) 0.030(7) Uani 1 1 d U . .
C24 C 0.783(2) 0.893(2) -0.3821(17) 0.031(7) Uani 1 1 d U . .
C20 C 0.892(3) 1.245(3) -0.730(2) 0.054(11) Uani 1 1 d . . .
H20A H 0.9455 1.2330 -0.7066 0.065 Uiso 1 1 calc R . .
C5 C 1.042(2) 0.696(3) -0.5323(19) 0.037(8) Uani 1 1 d U . .
C22 C 0.693(2) 1.058(3) -0.332(2) 0.049(11) Uani 1 1 d . . .
H22A H 0.6609 1.1124 -0.3158 0.059 Uiso 1 1 calc R . .
C9 C 0.970(2) 0.555(2) -0.349(2) 0.041(9) Uani 1 1 d . . .
H9A H 0.9515 0.5252 -0.3072 0.049 Uiso 1 1 calc R . .
C17 C 0.744(3) 1.287(3) -0.8028(17) 0.050(11) Uani 1 1 d . . .
H17A H 0.6929 1.3037 -0.8286 0.060 Uiso 1 1 calc R . .
C18 C 0.822(3) 1.326(3) -0.822(2) 0.046(9) Uani 1 1 d U . .
H18A H 0.8245 1.3666 -0.8612 0.055 Uiso 1 1 calc R . .
C11 C 0.614(2) 1.065(2) -0.6271(18) 0.029(7) Uani 1 1 d . . .
H11A H 0.6233 1.0239 -0.5877 0.034 Uiso 1 1 calc R . .
C26 C 0.7916(19) 0.977(2) -0.5006(19) 0.031(7) Uani 1 1 d . . .
C21 C 0.720(2) 1.051(3) -0.402(2) 0.042(9) Uani 1 1 d . . .
H21A H 0.7053 1.1023 -0.4328 0.051 Uiso 1 1 calc R . .
C2 C 1.073(3) 0.824(3) -0.643(2) 0.048(10) Uani 1 1 d . . .
H2A H 1.0845 0.8698 -0.6780 0.058 Uiso 1 1 calc R . .
C12 C 0.527(2) 1.080(3) -0.6566(19) 0.038(8) Uani 1 1 d U . .
H12A H 0.4793 1.0464 -0.6369 0.045 Uiso 1 1 calc R . .
C8 C 1.042(3) 0.519(3) -0.386(2) 0.044(9) Uani 1 1 d U . .
H8A H 1.0764 0.4675 -0.3682 0.053 Uiso 1 1 calc R . .
C14 C 0.577(3) 1.182(4) -0.739(2) 0.058(12) Uani 1 1 d . . .
H14A H 0.5640 1.2243 -0.7771 0.069 Uiso 1 1 calc R . .
C19 C 0.892(3) 1.306(3) -0.786(2) 0.043(8) Uani 1 1 d U . .
H19A H 0.9448 1.3357 -0.7989 0.052 Uiso 1 1 calc R . .
C3 C 1.126(3) 0.745(3) -0.635(2) 0.042(8) Uani 1 1 d U . .
H3A H 1.1714 0.7333 -0.6665 0.051 Uiso 1 1 calc R . .
C13 C 0.514(3) 1.135(3) -0.706(2) 0.045(9) Uani 1 1 d . . .
H13A H 0.4556 1.1440 -0.7216 0.054 Uiso 1 1 calc R . .
C7 C 1.060(3) 0.558(3) -0.443(2) 0.043(8) Uani 1 1 d U . .
H7A H 1.1038 0.5287 -0.4703 0.052 Uiso 1 1 calc R . .
C4 C 1.111(2) 0.680(3) -0.5796(19) 0.038(8) Uani 1 1 d . . .
H4A H 1.1479 0.6252 -0.5735 0.046 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O18 1.64(3) . ?
W1 O8 1.85(3) 3_684 ?
W1 O15 1.88(3) . ?
W1 O13 1.93(3) 3_684 ?
W1 O11 1.94(3) . ?
W1 O3 2.35(5) . ?
W1 O2 2.46(5) . ?
W2 O21 1.65(3) . ?
W2 O11 1.85(3) . ?
W2 O10 1.89(3) . ?
W2 O16 1.93(3) . ?
W2 O14 1.97(3) . ?
W2 O2 2.37(5) . ?
W2 O1 2.37(5) 3_684 ?
W3 O17 1.71(2) . ?
W3 O8 1.88(3) . ?
W3 O9 1.88(3) . ?
W3 O14 1.91(3) . ?
W3 O6 1.93(3) . ?
W3 O1 2.39(5) 3_684 ?
W3 O3 2.39(5) 3_684 ?
W4 O19 1.66(3) . ?
W4 O16 1.84(3) . ?
W4 O7 1.85(3) . ?
W4 O12 1.88(3) . ?
W4 O15 1.89(3) . ?
W4 O4 2.37(5) 3_684 ?
W4 O2 2.45(5) . ?
W5 O22 1.64(2) . ?
W5 O7 1.88(3) 3_684 ?
W5 O5 1.88(3) . ?
W5 O6 1.90(3) . ?
W5 O10 1.91(3) . ?
W5 O1 2.39(5) 3_684 ?
W5 O4 2.43(5) . ?
W6 O20 1.68(2) . ?
W6 O9 1.84(3) . ?
W6 O5 1.89(3) 3_684 ?
W6 O12 1.92(3) . ?
W6 O13 1.92(3) . ?
W6 O3 2.39(5) 3_684 ?
W6 O4 2.41(5) 3_684 ?
Si1 O2 1.56(6) 3_684 ?
Si1 O2 1.56(6) . ?
Si1 O4 1.61(5) 3_684 ?
Si1 O4 1.61(5) . ?
Si1 O1 1.63(5) . ?
Si1 O1 1.63(5) 3_684 ?
Si1 O3 1.65(5) 3_684 ?
Si1 O3 1.65(5) . ?
O1 O2 1.80(7) 3_684 ?
O1 W2 2.37(5) 3_684 ?
O1 W3 2.39(5) 3_684 ?
O1 W5 2.39(5) 3_684 ?
O2 O1 1.80(7) 3_684 ?
O3 W3 2.39(5) 3_684 ?
O3 W6 2.39(5) 3_684 ?
O4 W4 2.37(5) 3_684 ?
O4 W6 2.41(5) 3_684 ?
Cu2 O40 1.94(2) . ?
Cu2 N3 1.99(3) . ?
Cu2 N4 2.00(3) . ?
Cu2 Cl1 2.240(11) . ?
Cu1 O41 1.90(2) . ?
Cu1 O43 1.94(2) . ?
Cu1 N2 1.98(3) . ?
Cu1 N1 1.99(3) . ?
O13 W1 1.93(3) 3_684 ?
O8 W1 1.85(3) 3_684 ?
O7 W5 1.88(3) 3_684 ?
O5 W6 1.89(3) 3_684 ?
N4 C20 1.31(5) . ?
N4 C16 1.41(4) . ?
O41 C26 1.32(4) . ?
N5 C24 1.36(4) . ?
N5 C23 1.40(5) . ?
O43 C24 1.18(4) . ?
N2 C10 1.29(4) . ?
N2 C6 1.30(4) . ?
N1 C1 1.30(5) . ?
N1 C5 1.43(4) . ?
C1 C2 1.28(5) . ?
C16 C15 1.39(5) . ?
C16 C17 1.46(5) . ?
N3 C11 1.35(4) . ?
N3 C15 1.38(4) . ?
C23 C22 1.31(6) . ?
C25 C21 1.33(5) . ?
C25 C24 1.41(4) . ?
C25 C26 1.45(4) . ?
C6 C5 1.38(5) . ?
C6 C7 1.47(5) . ?
C10 C9 1.37(5) . ?
O40 C26 1.22(4) . ?
C15 C14 1.39(5) . ?
C20 C19 1.33(6) . ?
C5 C4 1.40(5) . ?
C22 C21 1.40(5) . ?
C9 C8 1.39(5) . ?
C17 C18 1.33(6) . ?
C18 C19 1.27(5) . ?
C11 C12 1.43(5) . ?
C2 C3 1.34(6) . ?
C12 C13 1.20(5) . ?
C8 C7 1.22(5) . ?
C14 C13 1.32(6) . ?
C3 C4 1.38(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 W1 O8 103.8(14) . 3_684 ?
O18 W1 O15 100.7(14) . . ?
O8 W1 O15 85.9(12) 3_684 . ?
O18 W1 O13 99.5(14) . 3_684 ?
O8 W1 O13 87.9(12) 3_684 3_684 ?
O15 W1 O13 159.7(13) . 3_684 ?
O18 W1 O11 101.5(13) . . ?
O8 W1 O11 154.7(13) 3_684 . ?
O15 W1 O11 90.4(11) . . ?
O13 W1 O11 87.0(12) 3_684 . ?
O18 W1 O3 158.3(16) . . ?
O8 W1 O3 61.8(15) 3_684 . ?
O15 W1 O3 94.5(15) . . ?
O13 W1 O3 65.6(16) 3_684 . ?
O11 W1 O3 93.7(15) . . ?
O18 W1 O2 156.9(16) . . ?
O8 W1 O2 93.2(16) 3_684 . ?
O15 W1 O2 64.5(15) . . ?
O13 W1 O2 96.6(16) 3_684 . ?
O11 W1 O2 62.9(15) . . ?
O3 W1 O2 44.8(18) . . ?
O21 W2 O11 99.9(12) . . ?
O21 W2 O10 101.1(13) . . ?
O11 W2 O10 87.6(12) . . ?
O21 W2 O16 100.4(12) . . ?
O11 W2 O16 89.1(11) . . ?
O10 W2 O16 158.5(13) . . ?
O21 W2 O14 97.0(12) . . ?
O11 W2 O14 163.0(13) . . ?
O10 W2 O14 87.4(11) . . ?
O16 W2 O14 89.7(11) . . ?
O21 W2 O2 157.2(16) . . ?
O11 W2 O2 66.1(15) . . ?
O10 W2 O2 96.3(16) . . ?
O16 W2 O2 63.0(16) . . ?
O14 W2 O2 98.4(16) . . ?
O21 W2 O1 158.1(15) . 3_684 ?
O11 W2 O1 96.4(15) . 3_684 ?
O10 W2 O1 64.9(15) . 3_684 ?
O16 W2 O1 94.4(15) . 3_684 ?
O14 W2 O1 66.8(15) . 3_684 ?
O2 W2 O1 44.6(17) . 3_684 ?
O17 W3 O8 102.9(13) . . ?
O17 W3 O9 103.5(13) . . ?
O8 W3 O9 87.6(12) . . ?
O17 W3 O14 96.2(13) . . ?
O8 W3 O14 160.6(13) . . ?
O9 W3 O14 91.1(12) . . ?
O17 W3 O6 98.8(12) . . ?
O8 W3 O6 88.9(12) . . ?
O9 W3 O6 157.6(13) . . ?
O14 W3 O6 85.0(12) . . ?
O17 W3 O1 157.2(14) . 3_684 ?
O8 W3 O1 93.3(15) . 3_684 ?
O9 W3 O1 92.9(15) . 3_684 ?
O14 W3 O1 67.4(14) . 3_684 ?
O6 W3 O1 65.2(14) . 3_684 ?
O17 W3 O3 155.0(15) . 3_684 ?
O8 W3 O3 60.4(15) . 3_684 ?
O9 W3 O3 60.1(16) . 3_684 ?
O14 W3 O3 102.4(15) . 3_684 ?
O6 W3 O3 99.2(15) . 3_684 ?
O1 W3 O3 47.8(16) 3_684 3_684 ?
O19 W4 O16 103.8(13) . . ?
O19 W4 O7 100.7(13) . . ?
O16 W4 O7 155.3(13) . . ?
O19 W4 O12 98.7(13) . . ?
O16 W4 O12 88.7(12) . . ?
O7 W4 O12 90.1(12) . . ?
O19 W4 O15 102.1(12) . . ?
O16 W4 O15 88.4(11) . . ?
O7 W4 O15 84.1(11) . . ?
O12 W4 O15 159.1(13) . . ?
O19 W4 O4 155.4(16) . 3_684 ?
O16 W4 O4 94.7(15) . 3_684 ?
O7 W4 O4 62.6(15) . 3_684 ?
O12 W4 O4 65.3(16) . 3_684 ?
O15 W4 O4 94.4(15) . 3_684 ?
O19 W4 O2 159.7(16) . . ?
O16 W4 O2 62.2(15) . . ?
O7 W4 O2 93.4(16) . . ?
O12 W4 O2 95.8(16) . . ?
O15 W4 O2 64.7(15) . . ?
O4 W4 O2 44.9(18) 3_684 . ?
O22 W5 O7 102.4(12) . 3_684 ?
O22 W5 O5 100.2(12) . . ?
O7 W5 O5 89.0(11) 3_684 . ?
O22 W5 O6 99.8(12) . . ?
O7 W5 O6 88.9(12) 3_684 . ?
O5 W5 O6 159.9(12) . . ?
O22 W5 O10 102.2(12) . . ?
O7 W5 O10 155.4(12) 3_684 . ?
O5 W5 O10 86.4(12) . . ?
O6 W5 O10 87.2(11) . . ?
O22 W5 O1 159.3(14) . 3_684 ?
O7 W5 O1 92.1(14) 3_684 3_684 ?
O5 W5 O1 94.7(14) . 3_684 ?
O6 W5 O1 65.4(14) . 3_684 ?
O10 W5 O1 64.3(14) . 3_684 ?
O22 W5 O4 155.3(15) . . ?
O7 W5 O4 61.0(15) 3_684 . ?
O5 W5 O4 63.7(15) . . ?
O6 W5 O4 98.0(15) . . ?
O10 W5 O4 95.6(15) . . ?
O1 W5 O4 45.4(16) 3_684 . ?
O20 W6 O9 103.9(13) . . ?
O20 W6 O5 101.5(13) . 3_684 ?
O9 W6 O5 154.5(13) . 3_684 ?
O20 W6 O12 99.8(12) . . ?
O9 W6 O12 86.1(13) . . ?
O5 W6 O12 87.9(12) 3_684 . ?
O20 W6 O13 98.3(13) . . ?
O9 W6 O13 87.1(12) . . ?
O5 W6 O13 91.0(12) 3_684 . ?
O12 W6 O13 161.8(13) . . ?
O20 W6 O3 156.1(15) . 3_684 ?
O9 W6 O3 60.5(15) . 3_684 ?
O5 W6 O3 95.8(15) 3_684 3_684 ?
O12 W6 O3 97.2(15) . 3_684 ?
O13 W6 O3 64.8(15) . 3_684 ?
O20 W6 O4 157.3(15) . 3_684 ?
O9 W6 O4 91.3(15) . 3_684 ?
O5 W6 O4 64.0(15) 3_684 3_684 ?
O12 W6 O4 63.9(15) . 3_684 ?
O13 W6 O4 99.4(16) . 3_684 ?
O3 W6 O4 46.6(17) 3_684 3_684 ?
O2 Si1 O2 180(3) 3_684 . ?
O2 Si1 O4 109(3) 3_684 3_684 ?
O2 Si1 O4 71(3) . 3_684 ?
O2 Si1 O4 71(3) 3_684 . ?
O2 Si1 O4 109(3) . . ?
O4 Si1 O4 180(4) 3_684 . ?
O2 Si1 O1 69(3) 3_684 . ?
O2 Si1 O1 111(3) . . ?
O4 Si1 O1 70(2) 3_684 . ?
O4 Si1 O1 110(2) . . ?
O2 Si1 O1 111(3) 3_684 3_684 ?
O2 Si1 O1 69(3) . 3_684 ?
O4 Si1 O1 110(2) 3_684 3_684 ?
O4 Si1 O1 70(2) . 3_684 ?
O1 Si1 O1 180(3) . 3_684 ?
O2 Si1 O3 70(3) 3_684 3_684 ?
O2 Si1 O3 110(3) . 3_684 ?
O4 Si1 O3 71(3) 3_684 3_684 ?
O4 Si1 O3 109(3) . 3_684 ?
O1 Si1 O3 108(2) . 3_684 ?
O1 Si1 O3 72(2) 3_684 3_684 ?
O2 Si1 O3 110(3) 3_684 . ?
O2 Si1 O3 70(3) . . ?
O4 Si1 O3 109(3) 3_684 . ?
O4 Si1 O3 71(3) . . ?
O1 Si1 O3 72(2) . . ?
O1 Si1 O3 108(2) 3_684 . ?
O3 Si1 O3 180.000(7) 3_684 . ?
Si1 O1 O2 54(2) . 3_684 ?
Si1 O1 W2 121(3) . 3_684 ?
O2 O1 W2 67(2) 3_684 3_684 ?
Si1 O1 W3 121(2) . 3_684 ?
O2 O1 W3 129(3) 3_684 3_684 ?
W2 O1 W3 95.4(17) 3_684 3_684 ?
Si1 O1 W5 123(3) . 3_684 ?
O2 O1 W5 132(3) 3_684 3_684 ?
W2 O1 W5 95.1(16) 3_684 3_684 ?
W3 O1 W5 95.2(17) 3_684 3_684 ?
Si1 O2 O1 58(2) . 3_684 ?
Si1 O2 W2 126(3) . . ?
O1 O2 W2 68(2) 3_684 . ?
Si1 O2 W4 121(3) . . ?
O1 O2 W4 132(3) 3_684 . ?
W2 O2 W4 94.7(19) . . ?
Si1 O2 W1 122(3) . . ?
O1 O2 W1 132(3) 3_684 . ?
W2 O2 W1 93.5(18) . . ?
W4 O2 W1 91.8(19) . . ?
Si1 O3 W1 123(3) . . ?
Si1 O3 W3 119(3) . 3_684 ?
W1 O3 W3 95.8(17) . 3_684 ?
Si1 O3 W6 120(3) . 3_684 ?
W1 O3 W6 96.4(18) . 3_684 ?
W3 O3 W6 95.1(18) 3_684 3_684 ?
Si1 O4 W4 123(3) . 3_684 ?
Si1 O4 W6 122(3) . 3_684 ?
W4 O4 W6 94.9(18) 3_684 3_684 ?
Si1 O4 W5 122(3) . . ?
W4 O4 W5 94.3(18) 3_684 . ?
W6 O4 W5 93.8(18) 3_684 . ?
O40 Cu2 N3 87.5(12) . . ?
O40 Cu2 N4 165.0(11) . . ?
N3 Cu2 N4 81.2(11) . . ?
O40 Cu2 Cl1 95.4(9) . . ?
N3 Cu2 Cl1 172.7(8) . . ?
N4 Cu2 Cl1 97.1(8) . . ?
O41 Cu1 O43 91.4(10) . . ?
O41 Cu1 N2 172.9(11) . . ?
O43 Cu1 N2 92.4(10) . . ?
O41 Cu1 N1 93.9(11) . . ?
O43 Cu1 N1 170.6(11) . . ?
N2 Cu1 N1 83.1(11) . . ?
W4 O16 W2 139.5(16) . . ?
W1 O15 W4 138.3(15) . . ?
W3 O14 W2 130.4(16) . . ?
W6 O13 W1 133.2(17) . 3_684 ?
W4 O12 W6 135.6(17) . . ?
W2 O11 W1 136.6(15) . . ?
W2 O10 W5 135.4(16) . . ?
W6 O9 W3 143.7(17) . . ?
W1 O8 W3 141.4(18) 3_684 . ?
W4 O7 W5 140.9(16) . 3_684 ?
W5 O6 W3 134.2(16) . . ?
W5 O5 W6 138.2(16) . 3_684 ?
C20 N4 C16 120(3) . . ?
C20 N4 Cu2 128(3) . . ?
C16 N4 Cu2 112(2) . . ?
C26 O41 Cu1 128(2) . . ?
C24 N5 C23 122(3) . . ?
C24 O43 Cu1 125(2) . . ?
C10 N2 C6 122(3) . . ?
C10 N2 Cu1 126(2) . . ?
C6 N2 Cu1 111(2) . . ?
C1 N1 C5 122(3) . . ?
C1 N1 Cu1 128(2) . . ?
C5 N1 Cu1 110(2) . . ?
C2 C1 N1 123(4) . . ?
C15 C16 N4 116(3) . . ?
C15 C16 C17 130(3) . . ?
N4 C16 C17 114(3) . . ?
C11 N3 C15 118(3) . . ?
C11 N3 Cu2 126(2) . . ?
C15 N3 Cu2 115(2) . . ?
C22 C23 N5 121(4) . . ?
C21 C25 C24 119(3) . . ?
C21 C25 C26 118(3) . . ?
C24 C25 C26 123(3) . . ?
N2 C6 C5 121(3) . . ?
N2 C6 C7 115(3) . . ?
C5 C6 C7 124(3) . . ?
N2 C10 C9 122(3) . . ?
C26 O40 Cu2 137(3) . . ?
N3 C15 C14 119(3) . . ?
N3 C15 C16 115(3) . . ?
C14 C15 C16 125(4) . . ?
O43 C24 N5 115(3) . . ?
O43 C24 C25 128(3) . . ?
N5 C24 C25 117(3) . . ?
N4 C20 C19 123(4) . . ?
C6 C5 C4 133(3) . . ?
C6 C5 N1 113(3) . . ?
C4 C5 N1 114(3) . . ?
C23 C22 C21 118(4) . . ?
C10 C9 C8 118(4) . . ?
C18 C17 C16 121(4) . . ?
C19 C18 C17 120(4) . . ?
N3 C11 C12 118(3) . . ?
O40 C26 O41 120(3) . . ?
O40 C26 C25 119(3) . . ?
O41 C26 C25 120(3) . . ?
C25 C21 C22 123(3) . . ?
C1 C2 C3 121(4) . . ?
C13 C12 C11 122(4) . . ?
C7 C8 C9 118(4) . . ?
C13 C14 C15 119(4) . . ?
C18 C19 C20 122(4) . . ?
C2 C3 C4 119(4) . . ?
C12 C13 C14 124(4) . . ?
C8 C7 C6 124(4) . . ?
C3 C4 C5 121(3) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.84
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         3.604
_refine_diff_density_min         -2.689
_refine_diff_density_rms         0.493


# start Validation Reply Form

_vrf_PLAT342_k                   
;
PROBLEM: Low Bond Precision on  C-C Bonds .........0.0509 Ang
RESPONSE: The quality of this crystal was poor.
;
_vrf_PLAT430_k                   
;
PROBLEM: Short Inter D...A Contact  O17 ..  N5 .. 2.84 Ang
RESPONSE: there should be strong hydrogen bond between the two
water molecules.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_k4
_database_code_depnum_ccdc_archive 'CCDC 967750'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H40 Cl4 Cu4 N10 O44 Si W12'
_chemical_formula_weight         4235.19

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1

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

_cell_length_a                   12.186(2)
_cell_length_b                   12.977(3)
_cell_length_c                   14.887(3)
_cell_angle_alpha                102.93(3)
_cell_angle_beta                 91.43(3)
_cell_angle_gamma                102.46(3)
_cell_volume                     2233.8(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13048
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      35.33

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1907
_exptl_absorpt_coefficient_mu    16.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1548
_exptl_absorpt_correction_T_max  0.1906
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16247
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.94
_reflns_number_total             8463
_reflns_number_gt                8332
_reflns_threshold_expression     >2sigma(I)

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

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

restraints used:
ISOR 0.001 o4 o2 c18 c7 o7 o11 o14 o17 o18 c17 c23 c28 o1 o3 o8 o9 c30
ISOR 0.001 c13 o5 o6 o10 o15
SIMU 0.02 2.0 si1 o1 o2 o3 o4
delu 0.02 c14 c15
;

_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+525.6360P] 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     SHELXL
_refine_ls_extinction_coef       0.00112(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8463
_refine_ls_number_parameters     629
_refine_ls_number_restraints     157
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.1001
_refine_ls_wR_factor_ref         0.2181
_refine_ls_wR_factor_gt          0.2179
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      0.998
_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 1.2674(3) 0.2468(3) 0.5826(3) 0.0409(9) Uani 1 1 d . . .
Cu2 Cu 1.3156(4) 0.0099(3) 0.5320(3) 0.0466(10) Uani 1 1 d . . .
Cl1 Cl 1.4438(7) 0.1536(6) 0.5102(6) 0.0447(18) Uani 1 1 d . . .
Cl2 Cl 1.1904(6) 0.1072(6) 0.6454(5) 0.0375(15) Uani 1 1 d . . .
Si1 Si 1.0000 0.5000 0.0000 0.033(2) Uani 1 2 d SU . .
O1 O 0.973(3) 0.597(3) -0.041(3) 0.036(7) Uani 0.50 1 d PU . .
O2 O 0.892(3) 0.395(3) -0.024(2) 0.025(6) Uani 0.50 1 d PU . .
O3 O 1.106(3) 0.466(3) -0.051(3) 0.031(7) Uani 0.50 1 d PU . .
O4 O 0.960(3) 0.464(3) -0.112(2) 0.021(6) Uani 0.50 1 d PU . .
W6 W 0.71704(10) 0.41117(13) 0.04292(10) 0.0481(4) Uani 1 1 d . . .
W5 W 0.89561(10) 0.23081(10) 0.01695(9) 0.0358(3) Uani 1 1 d . . .
W4 W 0.91660(10) 0.58569(9) -0.19543(8) 0.0322(3) Uani 1 1 d . . .
W3 W 0.81746(11) 0.67828(10) 0.02091(9) 0.0406(3) Uani 1 1 d . . .
W2 W 0.80962(10) 0.31855(10) -0.17684(8) 0.0374(3) Uani 1 1 d . . .
W1 W 0.90605(12) 0.59734(11) 0.21740(8) 0.0436(4) Uani 1 1 d . . .
O21 O 0.5849(19) 0.3685(17) 0.0654(14) 0.041(5) Uani 1 1 d . . .
O20 O 0.8626(18) 0.6424(17) 0.3244(14) 0.037(5) Uani 1 1 d . . .
O119 O 0.7210(18) 0.2285(16) -0.2610(14) 0.041(5) Uani 1 1 d . . .
O18 O 0.7324(19) 0.7653(19) 0.0320(16) 0.047(5) Uani 1 1 d U . .
O17 O 0.850(2) 0.106(2) 0.0275(17) 0.054(6) Uani 1 1 d U . .
O16 O 0.8188(17) 0.638(2) -0.1089(16) 0.058(8) Uani 1 1 d . . .
O14 O 1.038(2) 0.2200(19) -0.0236(16) 0.048(5) Uani 1 1 d U . .
O15 O 0.967(2) 0.294(2) 0.1350(17) 0.054(6) Uani 1 1 d U . .
O22 O 0.8165(19) 0.4476(18) -0.211(3) 0.075(10) Uani 1 1 d . . .
O12 O 0.8765(19) 0.628(2) -0.2898(16) 0.055(7) Uani 1 1 d . . .
O11 O 0.712(2) 0.354(2) -0.0898(19) 0.064(7) Uani 1 1 d U . .
O10 O 0.774(3) 0.289(3) 0.057(2) 0.075(8) Uani 1 1 d U . .
O9 O 0.863(3) 0.685(3) 0.146(2) 0.082(9) Uani 1 1 d U . .
O8 O 0.781(2) 0.482(2) 0.161(2) 0.066(7) Uani 1 1 d U . .
O7 O 0.714(3) 0.547(3) 0.018(2) 0.082(9) Uani 1 1 d U . .
O6 O 0.849(3) 0.223(2) -0.105(2) 0.073(8) Uani 1 1 d U . .
O5 O 0.949(2) 0.310(2) -0.226(2) 0.067(7) Uani 1 1 d U . .
O24 O 1.1816(19) 0.1778(15) 0.4632(14) 0.038(5) Uani 1 1 d . . .
O23 O 1.2160(17) 0.0116(15) 0.4283(13) 0.036(5) Uani 1 1 d . . .
N4 N 1.3131(17) 0.3876(17) 0.5411(14) 0.024(4) Uani 1 1 d . . .
N3 N 1.3763(17) 0.3285(17) 0.6917(15) 0.027(5) Uani 1 1 d . . .
C24 C 1.425(2) 0.431(2) 0.686(2) 0.032(6) Uani 1 1 d . . .
N5 N 1.0021(19) -0.077(2) 0.1991(15) 0.034(5) Uani 1 1 d . . .
N2 N 1.225(2) -0.140(2) 0.5357(19) 0.040(6) Uani 1 1 d . . .
N1 N 1.4034(19) -0.014(2) 0.6371(18) 0.038(6) Uani 1 1 d . . .
C22 C 1.277(2) 0.418(2) 0.471(2) 0.031(6) Uani 1 1 d . . .
H22A H 1.2237 0.3662 0.4287 0.037 Uiso 1 1 calc R . .
C30 C 1.168(2) 0.082(2) 0.4144(19) 0.031(6) Uani 1 1 d U . .
C12 C 1.356(2) -0.101(2) 0.6653(19) 0.030(6) Uani 1 1 d . . .
C23 C 1.389(2) 0.464(2) 0.6040(17) 0.024(5) Uani 1 1 d U . .
C13 C 1.399(2) 0.298(2) 0.7675(19) 0.032(6) Uani 1 1 d U . .
H13A H 1.3618 0.2300 0.7753 0.038 Uiso 1 1 calc R . .
C18 C 1.517(2) 0.640(2) 0.6606(19) 0.033(6) Uani 1 1 d U . .
H18A H 1.5481 0.7095 0.6536 0.039 Uiso 1 1 calc R . .
C21 C 1.310(2) 0.515(3) 0.453(2) 0.039(7) Uani 1 1 d . . .
H21A H 1.2794 0.5320 0.4016 0.046 Uiso 1 1 calc R . .
C16 C 1.506(2) 0.502(3) 0.7536(19) 0.044(8) Uani 1 1 d . . .
C11 C 1.256(2) -0.1767(19) 0.6078(18) 0.027(5) Uani 1 1 d . . .
C25 C 1.088(3) 0.054(2) 0.3298(19) 0.032(6) Uani 1 1 d . . .
C4 C 1.394(2) -0.132(3) 0.744(2) 0.045(8) Uani 1 1 d . . .
C19 C 1.433(2) 0.564(2) 0.592(2) 0.039(7) Uani 1 1 d . . .
C8 C 1.109(3) -0.334(3) 0.573(3) 0.048(8) Uani 1 1 d . . .
H8A H 1.0667 -0.3964 0.5866 0.057 Uiso 1 1 calc R . .
C28 C 0.955(3) 0.090(2) 0.228(2) 0.038(7) Uani 1 1 d U . .
H28A H 0.9153 0.1369 0.2103 0.046 Uiso 1 1 calc R . .
C29 C 1.027(3) 0.123(2) 0.3089(19) 0.034(6) Uani 1 1 d . . .
H29A H 1.0326 0.1914 0.3478 0.040 Uiso 1 1 calc R . .
C9 C 1.081(3) -0.300(3) 0.494(3) 0.060(10) Uani 1 1 d . . .
H9A H 1.0218 -0.3434 0.4531 0.072 Uiso 1 1 calc R . .
C6 C 1.246(3) -0.294(3) 0.712(2) 0.052(9) Uani 1 1 d . . .
H6A H 1.2100 -0.3593 0.7253 0.063 Uiso 1 1 calc R . .
C20 C 1.393(3) 0.594(3) 0.517(2) 0.044(8) Uani 1 1 d . . .
H20A H 1.4198 0.6633 0.5074 0.053 Uiso 1 1 calc R . .
C17 C 1.550(3) 0.606(3) 0.734(3) 0.053(8) Uani 1 1 d U . .
H17A H 1.6058 0.6546 0.7755 0.063 Uiso 1 1 calc R . .
C14 C 1.478(2) 0.367(3) 0.836(2) 0.042(7) Uani 1 1 d U . .
H14A H 1.4931 0.3444 0.8889 0.050 Uiso 1 1 calc R . .
C26 C 1.078(3) -0.047(3) 0.270(2) 0.048(8) Uani 1 1 d . . .
H26A H 1.1238 -0.0923 0.2801 0.057 Uiso 1 1 calc R . .
C1 C 1.491(3) 0.048(3) 0.687(3) 0.049(8) Uani 1 1 d . . .
H1A H 1.5269 0.1097 0.6679 0.059 Uiso 1 1 calc R . .
C15 C 1.531(3) 0.462(3) 0.827(2) 0.048(8) Uani 1 1 d U . .
H15A H 1.5874 0.5038 0.8722 0.057 Uiso 1 1 calc R . .
C7 C 1.206(3) -0.266(3) 0.633(2) 0.039(7) Uani 1 1 d U . .
C10 C 1.140(3) -0.204(2) 0.476(3) 0.050(8) Uani 1 1 d . . .
H10A H 1.1210 -0.1841 0.4224 0.059 Uiso 1 1 calc R . .
C27 C 0.943(3) -0.011(2) 0.1750(19) 0.037(7) Uani 1 1 d . . .
H27A H 0.8937 -0.0341 0.1220 0.045 Uiso 1 1 calc R . .
C5 C 1.332(3) -0.231(3) 0.767(2) 0.053(9) Uani 1 1 d . . .
H5A H 1.3533 -0.2494 0.8212 0.064 Uiso 1 1 calc R . .
C2 C 1.534(3) 0.028(4) 0.768(3) 0.079(15) Uani 1 1 d . . .
H2A H 1.5941 0.0794 0.8030 0.094 Uiso 1 1 calc R . .
C3 C 1.491(3) -0.062(4) 0.795(3) 0.068(12) Uani 1 1 d . . .
H3A H 1.5239 -0.0785 0.8462 0.082 Uiso 1 1 calc R . .
O25 O 0.973(2) 0.486(2) 0.242(3) 0.081(10) 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
Cu1 O24 1.96(2) . ?
Cu1 N3 2.01(2) . ?
Cu1 N4 2.03(2) . ?
Cu1 Cl2 2.260(8) . ?
Cu1 O20 2.59(2) 2_766 ?
Cu1 Cl1 2.812(9) . ?
Cu1 Cu2 3.183(6) . ?
Cu2 O23 1.946(19) . ?
Cu2 N1 1.99(2) . ?
Cu2 N2 2.03(2) . ?
Cu2 Cl1 2.250(8) . ?
Cu2 Cl2 2.602(9) . ?
Si1 O1 1.61(4) 2_765 ?
Si1 O1 1.61(4) . ?
Si1 O3 1.61(4) . ?
Si1 O3 1.61(4) 2_765 ?
Si1 O2 1.65(3) 2_765 ?
Si1 O2 1.65(3) . ?
Si1 O4 1.66(3) . ?
Si1 O4 1.66(3) 2_765 ?
O1 O4 1.79(5) . ?
O1 W4 2.35(4) . ?
O1 W5 2.40(4) 2_765 ?
O1 W3 2.46(4) . ?
O2 W5 2.35(3) . ?
O2 W2 2.37(3) . ?
O2 W6 2.40(3) . ?
O3 W6 2.37(4) 2_765 ?
O3 W3 2.38(4) 2_765 ?
O3 W1 2.42(4) 2_765 ?
O4 W2 2.33(3) . ?
O4 W4 2.35(3) . ?
O4 W1 2.42(3) 2_765 ?
W6 O21 1.65(2) . ?
W6 O8 1.86(3) . ?
W6 O7 1.88(3) . ?
W6 O10 1.91(3) . ?
W6 O11 1.94(3) . ?
W6 O3 2.37(4) 2_765 ?
W5 O17 1.63(2) . ?
W5 O10 1.86(3) . ?
W5 O15 1.87(2) . ?
W5 O6 1.87(3) . ?
W5 O14 1.87(2) . ?
W5 O1 2.40(4) 2_765 ?
W4 O12 1.71(2) . ?
W4 O25 1.86(3) 2_765 ?
W4 O16 1.891(19) . ?
W4 O15 1.90(3) 2_765 ?
W4 O22 1.90(2) . ?
W3 O18 1.68(2) . ?
W3 O7 1.88(3) . ?
W3 O16 1.89(2) . ?
W3 O9 1.91(3) . ?
W3 O14 1.96(2) 2_765 ?
W3 O3 2.38(4) 2_765 ?
W2 O119 1.684(17) . ?
W2 O11 1.83(3) . ?
W2 O22 1.84(2) . ?
W2 O5 1.89(3) . ?
W2 O6 1.92(3) . ?
W1 O20 1.708(19) . ?
W1 O9 1.86(3) . ?
W1 O5 1.89(3) 2_765 ?
W1 O25 1.91(3) . ?
W1 O8 1.91(3) . ?
W1 O3 2.42(4) 2_765 ?
W1 O4 2.42(3) 2_765 ?
O20 Cu1 2.59(2) 2_766 ?
O14 W3 1.96(2) 2_765 ?
O15 W4 1.90(2) 2_765 ?
O5 W1 1.89(3) 2_765 ?
O24 C30 1.27(3) . ?
O23 C30 1.23(3) . ?
N4 C22 1.29(4) . ?
N4 C23 1.36(3) . ?
N3 C13 1.32(4) . ?
N3 C24 1.36(3) . ?
C24 C16 1.41(4) . ?
C24 C23 1.46(4) . ?
N5 C26 1.32(4) . ?
N5 C27 1.34(4) . ?
N2 C10 1.34(4) . ?
N2 C11 1.35(4) . ?
N1 C1 1.28(4) . ?
N1 C12 1.32(4) . ?
C22 C21 1.33(4) . ?
C22 H22A 0.9300 . ?
C30 C25 1.50(4) . ?
C12 C4 1.41(4) . ?
C12 C11 1.49(4) . ?
C23 C19 1.35(4) . ?
C13 C14 1.39(4) . ?
C13 H13A 0.9300 . ?
C18 C17 1.34(5) . ?
C18 C19 1.46(4) . ?
C18 H18A 0.9300 . ?
C21 C20 1.43(4) . ?
C21 H21A 0.9300 . ?
C16 C15 1.37(5) . ?
C16 C17 1.44(5) . ?
C11 C7 1.33(4) . ?
C25 C29 1.37(4) . ?
C25 C26 1.38(4) . ?
C4 C3 1.41(5) . ?
C4 C5 1.47(4) . ?
C19 C20 1.38(4) . ?
C8 C9 1.39(5) . ?
C8 C7 1.45(5) . ?
C8 H8A 0.9300 . ?
C28 C27 1.33(4) . ?
C28 C29 1.41(4) . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9300 . ?
C9 C10 1.39(5) . ?
C9 H9A 0.9300 . ?
C6 C5 1.32(5) . ?
C6 C7 1.41(5) . ?
C6 H6A 0.9300 . ?
C20 H20A 0.9300 . ?
C17 H17A 0.9300 . ?
C14 C15 1.30(5) . ?
C14 H14A 0.9300 . ?
C26 H26A 0.9300 . ?
C1 C2 1.40(5) . ?
C1 H1A 0.9300 . ?
C15 H15A 0.9300 . ?
C10 H10A 0.9300 . ?
C27 H27A 0.9300 . ?
C5 H5A 0.9300 . ?
C2 C3 1.34(5) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
O25 W4 1.86(2) 2_765 ?

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
O24 Cu1 N3 169.9(9) . . ?
O24 Cu1 N4 89.8(8) . . ?
N3 Cu1 N4 82.9(9) . . ?
O24 Cu1 Cl2 92.6(6) . . ?
N3 Cu1 Cl2 95.9(6) . . ?
N4 Cu1 Cl2 168.1(7) . . ?
O24 Cu1 O20 104.4(8) . 2_766 ?
N3 Cu1 O20 81.3(8) . 2_766 ?
N4 Cu1 O20 79.8(7) . 2_766 ?
Cl2 Cu1 O20 88.3(5) . 2_766 ?
O24 Cu1 Cl1 87.2(7) . . ?
N3 Cu1 Cl1 86.7(7) . . ?
N4 Cu1 Cl1 97.3(6) . . ?
Cl2 Cu1 Cl1 94.5(3) . . ?
O20 Cu1 Cl1 167.9(5) 2_766 . ?
O24 Cu1 Cu2 75.8(6) . . ?
N3 Cu1 Cu2 105.0(7) . . ?
N4 Cu1 Cu2 137.8(6) . . ?
Cl2 Cu1 Cu2 54.0(2) . . ?
O20 Cu1 Cu2 141.9(5) 2_766 . ?
Cl1 Cu1 Cu2 43.55(17) . . ?
O23 Cu2 N1 171.5(10) . . ?
O23 Cu2 N2 90.1(10) . . ?
N1 Cu2 N2 81.4(11) . . ?
O23 Cu2 Cl1 92.3(7) . . ?
N1 Cu2 Cl1 95.9(7) . . ?
N2 Cu2 Cl1 166.4(8) . . ?
O23 Cu2 Cl2 89.7(7) . . ?
N1 Cu2 Cl2 90.9(8) . . ?
N2 Cu2 Cl2 92.7(8) . . ?
Cl1 Cu2 Cl2 100.7(3) . . ?
O23 Cu2 Cu1 76.2(6) . . ?
N1 Cu2 Cu1 110.0(8) . . ?
N2 Cu2 Cu1 134.0(8) . . ?
Cl1 Cu2 Cu1 59.4(2) . . ?
Cl2 Cu2 Cu1 44.61(18) . . ?
Cu2 Cl1 Cu1 77.0(3) . . ?
Cu1 Cl2 Cu2 81.4(3) . . ?
O1 Si1 O1 180(2) 2_765 . ?
O1 Si1 O3 73.2(19) 2_765 . ?
O1 Si1 O3 107(2) . . ?
O1 Si1 O3 106.8(19) 2_765 2_765 ?
O1 Si1 O3 73.2(19) . 2_765 ?
O3 Si1 O3 180(3) . 2_765 ?
O1 Si1 O2 110.3(19) 2_765 2_765 ?
O1 Si1 O2 69.7(19) . 2_765 ?
O3 Si1 O2 71.2(18) . 2_765 ?
O3 Si1 O2 108.8(18) 2_765 2_765 ?
O1 Si1 O2 69.7(19) 2_765 . ?
O1 Si1 O2 110.3(19) . . ?
O3 Si1 O2 108.8(18) . . ?
O3 Si1 O2 71.2(18) 2_765 . ?
O2 Si1 O2 180.0(19) 2_765 . ?
O1 Si1 O4 113.5(18) 2_765 . ?
O1 Si1 O4 66.5(18) . . ?
O3 Si1 O4 74.0(17) . . ?
O3 Si1 O4 106.0(17) 2_765 . ?
O2 Si1 O4 111.3(16) 2_765 . ?
O2 Si1 O4 68.7(16) . . ?
O1 Si1 O4 66.5(18) 2_765 2_765 ?
O1 Si1 O4 113.5(18) . 2_765 ?
O3 Si1 O4 106.0(17) . 2_765 ?
O3 Si1 O4 74.0(17) 2_765 2_765 ?
O2 Si1 O4 68.7(16) 2_765 2_765 ?
O2 Si1 O4 111.3(16) . 2_765 ?
O4 Si1 O4 180.0(8) . 2_765 ?
Si1 O1 O4 58.2(17) . . ?
Si1 O1 W4 126(2) . . ?
O4 O1 W4 67.7(16) . . ?
Si1 O1 W5 122(2) . 2_765 ?
O4 O1 W5 136(2) . 2_765 ?
W4 O1 W5 96.2(14) . 2_765 ?
Si1 O1 W3 118(2) . . ?
O4 O1 W3 127(2) . . ?
W4 O1 W3 94.0(14) . . ?
W5 O1 W3 93.7(14) 2_765 . ?
Si1 O2 W5 122.4(18) . . ?
Si1 O2 W2 121.5(18) . . ?
W5 O2 W2 97.4(13) . . ?
Si1 O2 W6 119.1(17) . . ?
W5 O2 W6 94.7(12) . . ?
W2 O2 W6 95.3(12) . . ?
Si1 O3 W6 123(2) . 2_765 ?
Si1 O3 W3 122.0(19) . 2_765 ?
W6 O3 W3 95.3(13) 2_765 2_765 ?
Si1 O3 W1 120.1(19) . 2_765 ?
W6 O3 W1 94.6(13) 2_765 2_765 ?
W3 O3 W1 95.2(13) 2_765 2_765 ?
Si1 O4 O1 55.3(16) . . ?
Si1 O4 W2 122.9(17) . . ?
O1 O4 W2 135(2) . . ?
Si1 O4 W4 122.7(17) . . ?
O1 O4 W4 67.4(16) . . ?
W2 O4 W4 96.9(12) . . ?
Si1 O4 W1 117.7(16) . 2_765 ?
O1 O4 W1 127(2) . 2_765 ?
W2 O4 W1 95.2(12) . 2_765 ?
W4 O4 W1 94.7(11) . 2_765 ?
O21 W6 O8 100.2(11) . . ?
O21 W6 O7 101.7(13) . . ?
O8 W6 O7 89.1(13) . . ?
O21 W6 O10 99.0(12) . . ?
O8 W6 O10 88.0(13) . . ?
O7 W6 O10 159.3(14) . . ?
O21 W6 O11 102.3(11) . . ?
O8 W6 O11 157.5(12) . . ?
O7 W6 O11 87.4(13) . . ?
O10 W6 O11 87.5(12) . . ?
O21 W6 O3 157.2(12) . 2_765 ?
O8 W6 O3 64.2(13) . 2_765 ?
O7 W6 O3 63.4(14) . 2_765 ?
O10 W6 O3 97.0(13) . 2_765 ?
O11 W6 O3 94.5(12) . 2_765 ?
O21 W6 O2 155.8(11) . . ?
O8 W6 O2 96.1(12) . . ?
O7 W6 O2 96.3(13) . . ?
O10 W6 O2 63.7(12) . . ?
O11 W6 O2 62.3(12) . . ?
O3 W6 O2 47.0(12) 2_765 . ?
O17 W5 O10 100.2(13) . . ?
O17 W5 O15 99.5(12) . . ?
O10 W5 O15 87.5(12) . . ?
O17 W5 O6 103.2(13) . . ?
O10 W5 O6 89.9(13) . . ?
O15 W5 O6 157.2(12) . . ?
O17 W5 O14 98.8(11) . . ?
O10 W5 O14 160.9(12) . . ?
O15 W5 O14 87.3(10) . . ?
O6 W5 O14 87.7(12) . . ?
O17 W5 O2 158.4(12) . . ?
O10 W5 O2 65.6(13) . . ?
O15 W5 O2 96.1(11) . . ?
O6 W5 O2 62.4(13) . . ?
O14 W5 O2 96.8(11) . . ?
O17 W5 O1 155.3(13) . 2_765 ?
O10 W5 O1 94.9(14) . 2_765 ?
O15 W5 O1 61.5(12) . 2_765 ?
O6 W5 O1 96.1(13) . 2_765 ?
O14 W5 O1 66.5(12) . 2_765 ?
O2 W5 O1 46.2(13) . 2_765 ?
O12 W4 O25 100.9(15) . 2_765 ?
O12 W4 O16 100.9(13) . . ?
O25 W4 O16 158.2(15) 2_765 . ?
O12 W4 O15 101.9(11) . 2_765 ?
O25 W4 O15 88.7(11) 2_765 2_765 ?
O16 W4 O15 88.0(10) . 2_765 ?
O12 W4 O22 102.0(13) . . ?
O25 W4 O22 88.1(10) 2_765 . ?
O16 W4 O22 86.2(10) . . ?
O15 W4 O22 156.1(13) 2_765 . ?
O12 W4 O1 158.2(14) . . ?
O25 W4 O1 94.0(16) 2_765 . ?
O16 W4 O1 65.5(13) . . ?
O15 W4 O1 62.4(12) 2_765 . ?
O22 W4 O1 94.3(15) . . ?
O12 W4 O4 156.9(12) . . ?
O25 W4 O4 64.8(13) 2_765 . ?
O16 W4 O4 94.1(12) . . ?
O15 W4 O4 96.1(11) 2_765 . ?
O22 W4 O4 61.3(13) . . ?
O1 W4 O4 44.9(12) . . ?
O18 W3 O7 101.6(13) . . ?
O18 W3 O16 100.7(12) . . ?
O7 W3 O16 89.8(12) . . ?
O18 W3 O9 102.9(13) . . ?
O7 W3 O9 88.7(14) . . ?
O16 W3 O9 156.2(13) . . ?
O18 W3 O14 99.4(10) . 2_765 ?
O7 W3 O14 158.9(12) . 2_765 ?
O16 W3 O14 88.1(9) . 2_765 ?
O9 W3 O14 84.9(12) . 2_765 ?
O18 W3 O3 157.3(12) . 2_765 ?
O7 W3 O3 63.2(14) . 2_765 ?
O16 W3 O3 96.2(13) . 2_765 ?
O9 W3 O3 62.2(13) . 2_765 ?
O14 W3 O3 96.2(11) 2_765 2_765 ?
O18 W3 O1 155.8(12) . . ?
O7 W3 O1 96.4(14) . . ?
O16 W3 O1 63.1(12) . . ?
O9 W3 O1 93.5(14) . . ?
O14 W3 O1 64.2(12) 2_765 . ?
O3 W3 O1 46.8(13) 2_765 . ?
O119 W2 O11 101.3(12) . . ?
O119 W2 O22 102.5(13) . . ?
O11 W2 O22 90.2(12) . . ?
O119 W2 O5 100.4(12) . . ?
O11 W2 O5 157.7(12) . . ?
O22 W2 O5 89.9(11) . . ?
O119 W2 O6 100.6(12) . . ?
O11 W2 O6 87.7(13) . . ?
O22 W2 O6 156.8(14) . . ?
O5 W2 O6 83.5(13) . . ?
O119 W2 O4 157.2(11) . . ?
O11 W2 O4 96.0(12) . . ?
O22 W2 O4 62.4(12) . . ?
O5 W2 O4 64.6(12) . . ?
O6 W2 O4 94.9(12) . . ?
O119 W2 O2 155.8(11) . . ?
O11 W2 O2 64.3(12) . . ?
O22 W2 O2 97.1(14) . . ?
O5 W2 O2 93.6(12) . . ?
O6 W2 O2 61.3(12) . . ?
O4 W2 O2 46.9(11) . . ?
O20 W1 O9 104.8(12) . . ?
O20 W1 O5 101.0(11) . 2_765 ?
O9 W1 O5 85.2(13) . 2_765 ?
O20 W1 O25 99.1(12) . . ?
O9 W1 O25 156.1(15) . . ?
O5 W1 O25 89.8(11) 2_765 . ?
O20 W1 O8 102.0(11) . . ?
O9 W1 O8 89.7(13) . . ?
O5 W1 O8 156.9(12) 2_765 . ?
O25 W1 O8 85.8(12) . . ?
O20 W1 O3 157.9(11) . 2_765 ?
O9 W1 O3 61.8(13) . 2_765 ?
O5 W1 O3 95.4(12) 2_765 2_765 ?
O25 W1 O3 95.6(14) . 2_765 ?
O8 W1 O3 62.6(12) . 2_765 ?
O20 W1 O4 153.9(10) . 2_765 ?
O9 W1 O4 94.5(13) . 2_765 ?
O5 W1 O4 62.7(12) 2_765 2_765 ?
O25 W1 O4 62.7(12) . 2_765 ?
O8 W1 O4 95.4(12) . 2_765 ?
O3 W1 O4 48.2(12) 2_765 2_765 ?
W1 O20 Cu1 145.4(11) . 2_766 ?
W3 O16 W4 137.0(15) . . ?
W5 O14 W3 135.5(13) . 2_765 ?
W5 O15 W4 139.4(14) . 2_765 ?
W2 O22 W4 139.0(18) . . ?
W2 O11 W6 138.1(16) . . ?
W5 O10 W6 135.9(17) . . ?
W1 O9 W3 139.9(19) . . ?
W6 O8 W1 138.0(16) . . ?
W6 O7 W3 137.8(19) . . ?
W5 O6 W2 138.1(17) . . ?
W2 O5 W1 136.8(16) . 2_765 ?
C30 O24 Cu1 130.1(18) . . ?
C30 O23 Cu2 131.1(18) . . ?
C22 N4 C23 117(2) . . ?
C22 N4 Cu1 131.2(18) . . ?
C23 N4 Cu1 111.5(16) . . ?
C13 N3 C24 119(2) . . ?
C13 N3 Cu1 128.6(18) . . ?
C24 N3 Cu1 112.7(19) . . ?
N3 C24 C16 122(3) . . ?
N3 C24 C23 116(3) . . ?
C16 C24 C23 122(3) . . ?
C26 N5 C27 123(3) . . ?
C10 N2 C11 118(3) . . ?
C10 N2 Cu2 128(2) . . ?
C11 N2 Cu2 114(2) . . ?
C1 N1 C12 116(3) . . ?
C1 N1 Cu2 130(2) . . ?
C12 N1 Cu2 113.4(19) . . ?
N4 C22 C21 126(3) . . ?
N4 C22 H22A 117.1 . . ?
C21 C22 H22A 117.1 . . ?
O23 C30 O24 126(3) . . ?
O23 C30 C25 118(2) . . ?
O24 C30 C25 116(2) . . ?
N1 C12 C4 125(3) . . ?
N1 C12 C11 118(2) . . ?
C4 C12 C11 117(2) . . ?
C19 C23 N4 123(2) . . ?
C19 C23 C24 120(3) . . ?
N4 C23 C24 117(2) . . ?
N3 C13 C14 120(3) . . ?
N3 C13 H13A 120.1 . . ?
C14 C13 H13A 120.1 . . ?
C17 C18 C19 118(3) . . ?
C17 C18 H18A 120.9 . . ?
C19 C18 H18A 120.9 . . ?
C22 C21 C20 117(3) . . ?
C22 C21 H21A 121.4 . . ?
C20 C21 H21A 121.4 . . ?
C15 C16 C24 116(3) . . ?
C15 C16 C17 130(3) . . ?
C24 C16 C17 114(3) . . ?
C7 C11 N2 128(3) . . ?
C7 C11 C12 120(3) . . ?
N2 C11 C12 112(2) . . ?
C29 C25 C26 119(3) . . ?
C29 C25 C30 123(2) . . ?
C26 C25 C30 118(3) . . ?
C12 C4 C3 117(3) . . ?
C12 C4 C5 120(3) . . ?
C3 C4 C5 124(3) . . ?
C23 C19 C20 118(3) . . ?
C23 C19 C18 120(3) . . ?
C20 C19 C18 122(3) . . ?
C9 C8 C7 117(3) . . ?
C9 C8 H8A 121.4 . . ?
C7 C8 H8A 121.4 . . ?
C27 C28 C29 120(3) . . ?
C27 C28 H28A 120.1 . . ?
C29 C28 H28A 120.1 . . ?
C25 C29 C28 119(3) . . ?
C25 C29 H29A 120.6 . . ?
C28 C29 H29A 120.6 . . ?
C10 C9 C8 122(4) . . ?
C10 C9 H9A 119.1 . . ?
C8 C9 H9A 119.1 . . ?
C5 C6 C7 122(3) . . ?
C5 C6 H6A 118.8 . . ?
C7 C6 H6A 118.8 . . ?
C19 C20 C21 118(3) . . ?
C19 C20 H20A 120.9 . . ?
C21 C20 H20A 120.9 . . ?
C18 C17 C16 126(3) . . ?
C18 C17 H17A 117.0 . . ?
C16 C17 H17A 117.0 . . ?
C15 C14 C13 122(3) . . ?
C15 C14 H14A 119.0 . . ?
C13 C14 H14A 119.0 . . ?
N5 C26 C25 119(3) . . ?
N5 C26 H26A 120.4 . . ?
C25 C26 H26A 120.4 . . ?
N1 C1 C2 124(3) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
C14 C15 C16 121(3) . . ?
C14 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C11 C7 C6 122(3) . . ?
C11 C7 C8 116(3) . . ?
C6 C7 C8 123(3) . . ?
N2 C10 C9 120(3) . . ?
N2 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C28 C27 N5 120(3) . . ?
C28 C27 H27A 120.2 . . ?
N5 C27 H27A 120.2 . . ?
C6 C5 C4 119(3) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C3 C2 C1 122(4) . . ?
C3 C2 H2A 119.2 . . ?
C1 C2 H2A 119.2 . . ?
C2 C3 C4 116(3) . . ?
C2 C3 H3A 121.8 . . ?
C4 C3 H3A 121.8 . . ?
W4 O25 W1 137.6(18) 2_765 . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.94
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         3.067
_refine_diff_density_min         -4.933
_refine_diff_density_rms         0.445

# start Validation Reply Form

_vrf_PLAT342_k                   
;
PROBLEM: Low Bond Precision on  C-C Bonds .........0.0469 Ang
RESPONSE: The quality of this crystal was poor.
;
_vrf_PLAT430_k                   
;
PROBLEM: Short Inter D...A Contact  O14 ..  N5 .. 2.81 Ang
RESPONSE: there should be strong hydrogen bond between the two
atoms.
;
_vrf_PLAT601_k                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 190.00 A**3
RESPONSE: The existance of large voids containing loosely bound water
solvent is typical for POM structures
;
_vrf_PLAT780_k                   
;
PROBLEM: Coordinates do not Form a Properly Connected Set ?
RESPONSE: the POM anion forms a complicated network which can not 
fit to asymmetric to make traditional connected set.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_k5
_database_code_depnum_ccdc_archive 'CCDC 967751'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl2 Cu4 N10 O44 Si W12'
_chemical_formula_weight         4068.29

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   14.797(3)
_cell_length_b                   13.334(3)
_cell_length_c                   23.821(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.20(2)
_cell_angle_gamma                90.00
_cell_volume                     3792.7(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    32706
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3652
_exptl_absorpt_coefficient_mu    19.397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0679
_exptl_absorpt_correction_T_max  0.1060
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34560
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8628
_reflns_number_gt                8096
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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. 

restraints used:
simu 0.02 0.04 3.8 $O
 
ISOR 0.001 c6 c21 c5 n5 c12
;

_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+999.4719P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8628
_refine_ls_number_parameters     584
_refine_ls_number_restraints     492
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.2051
_refine_ls_wR_factor_gt          0.2027
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.27887(8) -0.34982(8) 0.36837(5) 0.0220(2) Uani 1 1 d . . .
W2 W 1.24236(8) -0.61188(8) 0.36943(5) 0.0260(3) Uani 1 1 d . . .
W3 W 1.58258(8) -0.48467(7) 0.67332(5) 0.0159(2) Uani 1 1 d . . .
W4 W 1.36235(8) -0.33456(7) 0.54092(5) 0.0174(2) Uani 1 1 d . . .
W8 W 1.32454(8) -0.59666(8) 0.54179(5) 0.0206(2) Uani 1 1 d . . .
W11 W 1.46288(11) -0.76271(8) 0.50111(5) 0.0274(3) Uani 1 1 d . . .
Cu1 Cu 1.0834(3) 0.1853(3) 0.47713(18) 0.0347(9) Uani 1 1 d . . .
Cu2 Cu 1.3323(2) -0.1127(2) 0.63225(15) 0.0200(6) Uani 1 1 d . . .
Si1 Si 1.5000 -0.5000 0.5000 0.024(2) Uani 1 2 d S . .
O1 O 1.540(3) -0.517(3) 0.452(2) 0.025(5) Uani 0.50 1 d PU . .
O2 O 1.602(3) -0.503(3) 0.5823(19) 0.026(5) Uani 0.50 1 d PU . .
O3 O 1.407(3) -0.586(3) 0.484(2) 0.036(5) Uani 0.50 1 d PU . .
O4 O 1.435(3) -0.391(3) 0.482(2) 0.032(5) Uani 0.50 1 d PU . .
O21 O 1.1724(17) -0.2791(17) 0.3057(11) 0.035(4) Uani 1 1 d U . .
O20 O 1.445(2) -0.8854(17) 0.5021(11) 0.041(5) Uani 1 1 d U . .
O19 O 1.1205(16) -0.6644(17) 0.3081(11) 0.035(4) Uani 1 1 d U . .
O18 O 1.2900(19) -0.4563(18) 0.5329(12) 0.048(4) Uani 1 1 d U . .
O17 O 1.2927(15) -0.2576(17) 0.5597(11) 0.035(4) Uani 1 1 d U . .
O16 O 1.2397(16) -0.6395(18) 0.5605(12) 0.041(5) Uani 1 1 d U . .
O15 O 1.6200(19) -0.4770(14) 0.7538(10) 0.034(5) Uani 1 1 d U . .
O14 O 1.4806(18) -0.3744(18) 0.6297(13) 0.049(5) Uani 1 1 d U . .
N5 N 1.0932(17) 0.1092(16) 0.4084(11) 0.021(4) Uani 1 1 d U . .
O12 O 1.4549(19) -0.5694(19) 0.6292(13) 0.052(5) Uani 1 1 d U . .
O11 O 1.3069(18) -0.5973(17) 0.3221(13) 0.043(4) Uani 1 1 d U . .
O10 O 1.2033(19) -0.4718(18) 0.3532(13) 0.045(4) Uani 1 1 d U . .
O9 O 1.3325(18) -0.4030(18) 0.3194(14) 0.045(4) Uani 1 1 d U . .
O8 O 1.4611(19) -0.244(2) 0.5400(12) 0.049(5) Uani 1 1 d U . .
O7 O 1.335(2) -0.727(2) 0.4130(12) 0.049(4) Uani 1 1 d U . .
O6 O 1.268(2) -0.328(2) 0.4427(12) 0.050(4) Uani 1 1 d U . .
O5 O 1.390(2) -0.718(2) 0.5419(12) 0.054(5) Uani 1 1 d U . .
Cl1 Cl 1.1576(5) -0.0999(5) 0.6035(4) 0.0322(15) Uani 1 1 d . . .
N4 N 1.3971(15) -0.2049(13) 0.7127(10) 0.016(4) Uani 1 1 d . . .
N3 N 1.4911(18) -0.1143(16) 0.6662(10) 0.022(5) Uani 1 1 d . . .
O30 O 1.2985(18) -0.0375(17) 0.5518(11) 0.038(4) Uani 1 1 d U . .
O29 O 1.205(2) 0.0998(17) 0.5434(10) 0.041(5) Uani 1 1 d U . .
N1 N 0.9913(16) 0.3052(18) 0.4289(10) 0.023(5) Uani 1 1 d . . .
N2 N 1.0530(19) 0.2176(17) 0.5446(13) 0.028(5) Uani 1 1 d . . .
C15 C 1.560(2) -0.1728(19) 0.7215(13) 0.023(5) Uani 1 1 d . . .
C16 C 1.508(2) -0.2236(19) 0.7488(13) 0.024(5) Uani 1 1 d . . .
C21 C 1.030(2) 0.108(2) 0.3385(15) 0.029(6) Uani 1 1 d U . .
H21A H 0.9760 0.1581 0.3147 0.035 Uiso 1 1 calc R . .
C22 C 1.039(2) 0.036(2) 0.2993(13) 0.028(6) Uani 1 1 d . . .
H22A H 0.9924 0.0380 0.2509 0.034 Uiso 1 1 calc R . .
C7 C 0.956(2) 0.331(2) 0.5681(13) 0.026(6) Uani 1 1 d . . .
H7A H 0.9098 0.3859 0.5556 0.032 Uiso 1 1 calc R . .
C9 C 1.061(3) 0.193(3) 0.6450(16) 0.040(8) Uani 1 1 d . . .
H9A H 1.0845 0.1551 0.6842 0.047 Uiso 1 1 calc R . .
C26 C 1.232(2) 0.034(2) 0.5194(15) 0.027(6) Uani 1 1 d . . .
C11 C 1.536(2) -0.068(2) 0.6349(15) 0.028(6) Uani 1 1 d . . .
H11A H 1.4895 -0.0267 0.5969 0.034 Uiso 1 1 calc R . .
C6 C 0.9865(18) 0.3013(17) 0.5267(12) 0.014(4) Uani 1 1 d U . .
C24 C 1.182(2) -0.041(2) 0.4057(16) 0.030(6) Uani 1 1 d . . .
H24A H 1.2328 -0.0925 0.4305 0.036 Uiso 1 1 calc R . .
C20 C 1.338(3) -0.257(2) 0.7302(16) 0.034(7) Uani 1 1 d . . .
H20A H 1.2606 -0.2476 0.7039 0.041 Uiso 1 1 calc R . .
O22 O 1.230(2) -0.601(2) 0.4417(13) 0.055(5) Uani 1 1 d U . .
C25 C 1.1669(19) 0.034(2) 0.4390(13) 0.022(5) Uani 1 1 d . . .
C19 C 1.388(3) -0.323(2) 0.7857(15) 0.037(7) Uani 1 1 d . . .
H19A H 1.3461 -0.3576 0.7965 0.044 Uiso 1 1 calc R . .
C14 C 1.671(2) -0.185(2) 0.7475(16) 0.036(7) Uani 1 1 d . . .
H14A H 1.7176 -0.2268 0.7856 0.043 Uiso 1 1 calc R . .
C23 C 1.118(2) -0.037(2) 0.3343(15) 0.032(6) Uani 1 1 d . . .
H23A H 1.1288 -0.0846 0.3100 0.038 Uiso 1 1 calc R . .
C1 C 0.969(3) 0.349(2) 0.3719(15) 0.035(7) Uani 1 1 d . . .
H1A H 1.0012 0.3224 0.3518 0.042 Uiso 1 1 calc R . .
C12 C 1.645(3) -0.082(2) 0.6576(17) 0.037(7) Uani 1 1 d U . .
H12A H 1.6698 -0.0557 0.6330 0.045 Uiso 1 1 calc R . .
C8 C 0.994(2) 0.279(3) 0.6281(13) 0.031(6) Uani 1 1 d . . .
H8A H 0.9755 0.3007 0.6573 0.037 Uiso 1 1 calc R . .
C18 C 1.501(3) -0.335(2) 0.8241(15) 0.043(9) Uani 1 1 d . . .
H18A H 1.5370 -0.3769 0.8627 0.052 Uiso 1 1 calc R . .
C4 C 0.884(3) 0.435(3) 0.4338(18) 0.041(8) Uani 1 1 d . . .
H4A H 0.8531 0.4625 0.4547 0.050 Uiso 1 1 calc R . .
C17 C 1.561(3) -0.287(2) 0.8066(13) 0.035(7) Uani 1 1 d . . .
H17A H 1.6377 -0.2954 0.8333 0.042 Uiso 1 1 calc R . .
C13 C 1.714(2) -0.135(3) 0.7159(19) 0.045(9) Uani 1 1 d . . .
H13A H 1.7896 -0.1378 0.7356 0.054 Uiso 1 1 calc R . .
C10 C 1.091(3) 0.166(2) 0.6016(15) 0.034(6) Uani 1 1 d . . .
H10A H 1.1377 0.1111 0.6129 0.041 Uiso 1 1 calc R . .
C5 C 0.961(2) 0.350(2) 0.4652(16) 0.033(6) Uani 1 1 d U . .
C2 C 0.899(2) 0.435(2) 0.3390(15) 0.032(6) Uani 1 1 d . . .
H2A H 0.8802 0.4618 0.2974 0.039 Uiso 1 1 calc R . .
C3 C 0.861(3) 0.474(3) 0.376(2) 0.049(9) Uani 1 1 d . . .
H3A H 0.8153 0.5304 0.3580 0.059 Uiso 1 1 calc R . .
O23 O 1.601(2) -0.742(2) 0.5879(11) 0.046(4) 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 1.68(2) . ?
W1 O10 1.88(2) . ?
W1 O6 1.89(3) . ?
W1 O23 1.89(2) 3_846 ?
W1 O9 1.89(2) . ?
W1 O4 2.37(4) . ?
W1 O2 2.43(4) 3_846 ?
W2 O19 1.66(2) . ?
W2 O22 1.84(3) . ?
W2 O11 1.87(2) . ?
W2 O7 1.90(2) . ?
W2 O10 1.93(2) . ?
W2 O3 2.37(4) . ?
W2 O2 2.43(4) 3_846 ?
W3 O15 1.656(19) . ?
W3 O9 1.90(2) 3_846 ?
W3 O12 1.90(2) . ?
W3 O14 1.91(2) . ?
W3 O11 1.92(2) 3_846 ?
W3 O2 2.36(3) . ?
W3 O1 2.41(4) 3_846 ?
W4 O17 1.69(2) . ?
W4 O14 1.86(2) . ?
W4 O6 1.89(2) . ?
W4 O18 1.89(2) . ?
W4 O8 1.91(2) . ?
W4 O4 2.33(4) . ?
W4 O1 2.39(3) 3_846 ?
W8 O16 1.66(2) . ?
W8 O12 1.86(2) . ?
W8 O5 1.89(2) . ?
W8 O18 1.92(2) . ?
W8 O22 1.92(2) . ?
W8 O3 2.32(4) . ?
W8 O1 2.45(4) 3_846 ?
W11 O20 1.66(2) . ?
W11 O23 1.88(2) . ?
W11 O7 1.88(2) . ?
W11 O8 1.88(3) 3_846 ?
W11 O5 1.93(3) . ?
W11 O4 2.44(4) 3_846 ?
W11 O3 2.45(4) . ?
Cu1 O29 1.92(2) . ?
Cu1 N2 1.96(2) . ?
Cu1 N1 1.97(2) . ?
Cu1 N5 2.00(2) . ?
Cu2 O30 1.95(2) . ?
Cu2 N3 1.98(2) . ?
Cu2 N4 1.98(2) . ?
Cu2 Cl1 2.254(7) . ?
Cu2 O17 2.42(2) . ?
Si1 O1 1.59(3) 3_846 ?
Si1 O1 1.59(3) . ?
Si1 O2 1.62(4) . ?
Si1 O2 1.62(4) 3_846 ?
Si1 O4 1.65(4) . ?
Si1 O4 1.65(4) 3_846 ?
Si1 O3 1.65(5) . ?
Si1 O3 1.65(5) 3_846 ?
O1 O2 1.77(5) 3_846 ?
O1 W4 2.39(3) 3_846 ?
O1 W3 2.41(4) 3_846 ?
O1 W8 2.45(4) 3_846 ?
O2 O1 1.77(5) 3_846 ?
O2 W2 2.43(4) 3_846 ?
O2 W1 2.43(4) 3_846 ?
O4 W11 2.44(4) 3_846 ?
N5 C25 1.34(3) . ?
N5 C21 1.34(3) . ?
O11 W3 1.92(2) 3_846 ?
O9 W3 1.90(2) 3_846 ?
O8 W11 1.88(3) 3_846 ?
N4 C16 1.35(3) . ?
N4 C20 1.36(4) . ?
N3 C15 1.34(3) . ?
N3 C11 1.39(3) . ?
O30 C26 1.25(3) . ?
O29 C26 1.24(3) . ?
N1 C1 1.33(3) . ?
N1 C5 1.34(4) . ?
N2 C10 1.32(4) . ?
N2 C6 1.38(3) . ?
C15 C14 1.39(4) . ?
C15 C16 1.44(4) . ?
C16 C17 1.39(4) . ?
C21 C22 1.40(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.37(4) . ?
C22 H22A 0.9300 . ?
C7 C6 1.36(3) . ?
C7 C8 1.37(4) . ?
C7 H7A 0.9300 . ?
C9 C10 1.39(4) . ?
C9 C8 1.41(5) . ?
C9 H9A 0.9300 . ?
C26 C25 1.55(4) . ?
C11 C12 1.38(4) . ?
C11 H11A 0.9300 . ?
C6 C5 1.43(4) . ?
C24 C25 1.37(4) . ?
C24 C23 1.37(4) . ?
C24 H24A 0.9300 . ?
C20 C19 1.38(4) . ?
C20 H20A 0.9300 . ?
C19 C18 1.36(5) . ?
C19 H19A 0.9300 . ?
C14 C13 1.40(5) . ?
C14 H14A 0.9300 . ?
C23 H23A 0.9300 . ?
C1 C2 1.42(4) . ?
C1 H1A 0.9300 . ?
C12 C13 1.34(5) . ?
C12 H12A 0.9300 . ?
C8 H8A 0.9300 . ?
C18 C17 1.34(5) . ?
C18 H18A 0.9300 . ?
C4 C3 1.31(5) . ?
C4 C5 1.46(4) . ?
C4 H4A 0.9300 . ?
C17 H17A 0.9300 . ?
C13 H13A 0.9300 . ?
C10 H10A 0.9300 . ?
C2 C3 1.39(4) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
O23 W1 1.89(2) 3_846 ?

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 O10 100.1(10) . . ?
O21 W1 O6 101.2(11) . . ?
O10 W1 O6 86.8(11) . . ?
O21 W1 O23 102.0(11) . 3_846 ?
O10 W1 O23 157.8(11) . 3_846 ?
O6 W1 O23 87.5(10) . 3_846 ?
O21 W1 O9 100.2(10) . . ?
O10 W1 O9 88.6(10) . . ?
O6 W1 O9 158.6(11) . . ?
O23 W1 O9 88.9(10) 3_846 . ?
O21 W1 O4 156.6(13) . . ?
O10 W1 O4 95.0(13) . . ?
O6 W1 O4 61.7(12) . . ?
O23 W1 O4 63.6(12) 3_846 . ?
O9 W1 O4 98.0(12) . . ?
O21 W1 O2 156.4(12) . 3_846 ?
O10 W1 O2 65.0(11) . 3_846 ?
O6 W1 O2 96.3(11) . 3_846 ?
O23 W1 O2 94.4(12) 3_846 3_846 ?
O9 W1 O2 63.0(11) . 3_846 ?
O4 W1 O2 47.0(13) . 3_846 ?
O19 W2 O22 101.3(11) . . ?
O19 W2 O11 100.9(10) . . ?
O22 W2 O11 157.7(11) . . ?
O19 W2 O7 101.3(11) . . ?
O22 W2 O7 89.3(10) . . ?
O11 W2 O7 87.5(10) . . ?
O19 W2 O10 101.0(11) . . ?
O22 W2 O10 86.0(11) . . ?
O11 W2 O10 88.7(10) . . ?
O7 W2 O10 157.7(11) . . ?
O19 W2 O3 156.1(14) . . ?
O22 W2 O3 61.2(13) . . ?
O11 W2 O3 97.7(13) . . ?
O7 W2 O3 64.7(13) . . ?
O10 W2 O3 94.2(13) . . ?
O19 W2 O2 156.7(12) . 3_846 ?
O22 W2 O2 95.9(12) . 3_846 ?
O11 W2 O2 62.4(11) . 3_846 ?
O7 W2 O2 94.5(12) . 3_846 ?
O10 W2 O2 64.5(11) . 3_846 ?
O3 W2 O2 47.1(14) . 3_846 ?
O15 W3 O9 101.1(10) . 3_846 ?
O15 W3 O12 102.7(12) . . ?
O9 W3 O12 88.2(10) 3_846 . ?
O15 W3 O14 101.4(11) . . ?
O9 W3 O14 157.5(12) 3_846 . ?
O12 W3 O14 87.1(10) . . ?
O15 W3 O11 102.0(11) . 3_846 ?
O9 W3 O11 87.1(9) 3_846 3_846 ?
O12 W3 O11 155.3(11) . 3_846 ?
O14 W3 O11 88.0(10) . 3_846 ?
O15 W3 O2 158.7(12) . . ?
O9 W3 O2 64.5(12) 3_846 . ?
O12 W3 O2 92.8(13) . . ?
O14 W3 O2 93.8(13) . . ?
O11 W3 O2 63.4(12) 3_846 . ?
O15 W3 O1 157.8(11) . 3_846 ?
O9 W3 O1 95.5(11) 3_846 3_846 ?
O12 W3 O1 62.9(12) . 3_846 ?
O14 W3 O1 62.9(11) . 3_846 ?
O11 W3 O1 93.4(11) 3_846 3_846 ?
O2 W3 O1 43.5(12) . 3_846 ?
O17 W4 O14 100.6(11) . . ?
O17 W4 O6 100.5(11) . . ?
O14 W4 O6 158.9(12) . . ?
O17 W4 O18 98.7(11) . . ?
O14 W4 O18 88.0(10) . . ?
O6 W4 O18 87.5(10) . . ?
O17 W4 O8 102.0(11) . . ?
O14 W4 O8 89.0(10) . . ?
O6 W4 O8 88.0(10) . . ?
O18 W4 O8 159.3(12) . . ?
O17 W4 O4 157.2(13) . . ?
O14 W4 O4 97.6(13) . . ?
O6 W4 O4 62.4(13) . . ?
O18 W4 O4 95.5(13) . . ?
O8 W4 O4 64.6(13) . . ?
O17 W4 O1 156.7(12) . 3_846 ?
O14 W4 O1 63.9(12) . 3_846 ?
O6 W4 O1 95.6(13) . 3_846 ?
O18 W4 O1 65.2(12) . 3_846 ?
O8 W4 O1 95.2(12) . 3_846 ?
O4 W4 O1 45.9(14) . 3_846 ?
O16 W8 O12 102.4(12) . . ?
O16 W8 O5 99.8(13) . . ?
O12 W8 O5 88.6(11) . . ?
O16 W8 O18 99.8(12) . . ?
O12 W8 O18 88.0(10) . . ?
O5 W8 O18 160.4(12) . . ?
O16 W8 O22 102.0(12) . . ?
O12 W8 O22 155.5(13) . . ?
O5 W8 O22 88.4(10) . . ?
O18 W8 O22 86.8(10) . . ?
O16 W8 O3 157.6(14) . . ?
O12 W8 O3 95.4(14) . . ?
O5 W8 O3 66.8(14) . . ?
O18 W8 O3 94.3(14) . . ?
O22 W8 O3 61.3(14) . . ?
O16 W8 O1 156.6(12) . 3_846 ?
O12 W8 O1 62.6(13) . 3_846 ?
O5 W8 O1 97.8(12) . 3_846 ?
O18 W8 O1 63.7(11) . 3_846 ?
O22 W8 O1 93.8(13) . 3_846 ?
O3 W8 O1 45.7(14) . 3_846 ?
O20 W11 O23 101.7(11) . . ?
O20 W11 O7 101.6(12) . . ?
O23 W11 O7 156.6(12) . . ?
O20 W11 O8 101.5(12) . 3_846 ?
O23 W11 O8 88.4(9) . 3_846 ?
O7 W11 O8 85.9(10) . 3_846 ?
O20 W11 O5 99.0(12) . . ?
O23 W11 O5 88.2(10) . . ?
O7 W11 O5 89.3(10) . . ?
O8 W11 O5 159.5(12) 3_846 . ?
O20 W11 O4 156.2(12) . 3_846 ?
O23 W11 O4 62.3(12) . 3_846 ?
O7 W11 O4 95.1(13) . 3_846 ?
O8 W11 O4 62.7(12) 3_846 3_846 ?
O5 W11 O4 98.0(13) . 3_846 ?
O20 W11 O3 155.6(13) . . ?
O23 W11 O3 95.0(13) . . ?
O7 W11 O3 63.2(13) . . ?
O8 W11 O3 96.6(13) 3_846 . ?
O5 W11 O3 63.6(13) . . ?
O4 W11 O3 48.2(14) 3_846 . ?
O29 Cu1 N2 90.9(9) . . ?
O29 Cu1 N1 162.2(10) . . ?
N2 Cu1 N1 83.4(9) . . ?
O29 Cu1 N5 83.4(9) . . ?
N2 Cu1 N5 161.1(9) . . ?
N1 Cu1 N5 107.1(9) . . ?
O30 Cu2 N3 87.7(9) . . ?
O30 Cu2 N4 165.0(9) . . ?
N3 Cu2 N4 79.6(8) . . ?
O30 Cu2 Cl1 94.6(7) . . ?
N3 Cu2 Cl1 173.8(6) . . ?
N4 Cu2 Cl1 98.9(6) . . ?
O30 Cu2 O17 84.0(9) . . ?
N3 Cu2 O17 90.6(7) . . ?
N4 Cu2 O17 88.3(8) . . ?
Cl1 Cu2 O17 95.3(5) . . ?
O1 Si1 O1 180.0(11) 3_846 . ?
O1 Si1 O2 66.8(18) 3_846 . ?
O1 Si1 O2 113.2(18) . . ?
O1 Si1 O2 113.2(18) 3_846 3_846 ?
O1 Si1 O2 66.8(18) . 3_846 ?
O2 Si1 O2 180(2) . 3_846 ?
O1 Si1 O4 69(2) 3_846 . ?
O1 Si1 O4 111(2) . . ?
O2 Si1 O4 108(2) . . ?
O2 Si1 O4 72(2) 3_846 . ?
O1 Si1 O4 111(2) 3_846 3_846 ?
O1 Si1 O4 69(2) . 3_846 ?
O2 Si1 O4 72(2) . 3_846 ?
O2 Si1 O4 108(2) 3_846 3_846 ?
O4 Si1 O4 180(4) . 3_846 ?
O1 Si1 O3 70(2) 3_846 . ?
O1 Si1 O3 110(2) . . ?
O2 Si1 O3 108(2) . . ?
O2 Si1 O3 72(2) 3_846 . ?
O4 Si1 O3 106(2) . . ?
O4 Si1 O3 74(2) 3_846 . ?
O1 Si1 O3 110(2) 3_846 3_846 ?
O1 Si1 O3 70(2) . 3_846 ?
O2 Si1 O3 72(2) . 3_846 ?
O2 Si1 O3 108(2) 3_846 3_846 ?
O4 Si1 O3 74(2) . 3_846 ?
O4 Si1 O3 106(2) 3_846 3_846 ?
O3 Si1 O3 180.000(6) . 3_846 ?
Si1 O1 O2 57.5(16) . 3_846 ?
Si1 O1 W4 122(2) . 3_846 ?
O2 O1 W4 132(2) 3_846 3_846 ?
Si1 O1 W3 124.2(18) . 3_846 ?
O2 O1 W3 66.7(17) 3_846 3_846 ?
W4 O1 W3 94.5(12) 3_846 3_846 ?
Si1 O1 W8 120(2) . 3_846 ?
O2 O1 W8 130(2) 3_846 3_846 ?
W4 O1 W8 94.1(11) 3_846 3_846 ?
W3 O1 W8 93.5(13) 3_846 3_846 ?
Si1 O2 O1 55.8(17) . 3_846 ?
Si1 O2 W3 125.5(18) . . ?
O1 O2 W3 69.8(16) 3_846 . ?
Si1 O2 W2 120(2) . 3_846 ?
O1 O2 W2 131(2) 3_846 3_846 ?
W3 O2 W2 95.4(13) . 3_846 ?
Si1 O2 W1 119.9(19) . 3_846 ?
O1 O2 W1 133(2) 3_846 3_846 ?
W3 O2 W1 95.1(14) . 3_846 ?
W2 O2 W1 93.6(12) 3_846 3_846 ?
Si1 O3 W8 124(2) . . ?
Si1 O3 W2 121(2) . . ?
W8 O3 W2 97.6(16) . . ?
Si1 O3 W11 118(2) . . ?
W8 O3 W11 94.9(16) . . ?
W2 O3 W11 94.0(16) . . ?
Si1 O4 W4 122(2) . . ?
Si1 O4 W1 122(2) . . ?
W4 O4 W1 97.4(14) . . ?
Si1 O4 W11 119.1(19) . 3_846 ?
W4 O4 W11 95.3(15) . 3_846 ?
W1 O4 W11 94.7(15) . 3_846 ?
W4 O18 W8 136.7(14) . . ?
W4 O17 Cu2 138.2(10) . . ?
W4 O14 W3 138.4(15) . . ?
C25 N5 C21 115(2) . . ?
C25 N5 Cu1 111.4(17) . . ?
C21 N5 Cu1 133.0(19) . . ?
W8 O12 W3 140.5(16) . . ?
W2 O11 W3 138.4(14) . 3_846 ?
W1 O10 W2 136.5(13) . . ?
W1 O9 W3 137.3(15) . 3_846 ?
W11 O8 W4 137.2(15) 3_846 . ?
W11 O7 W2 137.7(14) . . ?
W1 O6 W4 138.2(15) . . ?
W8 O5 W11 134.6(16) . . ?
C16 N4 C20 118(2) . . ?
C16 N4 Cu2 116.2(17) . . ?
C20 N4 Cu2 125.4(18) . . ?
C15 N3 C11 117(2) . . ?
C15 N3 Cu2 115.8(19) . . ?
C11 N3 Cu2 126.7(17) . . ?
C26 O30 Cu2 130(2) . . ?
C26 O29 Cu1 116.5(19) . . ?
C1 N1 C5 119(3) . . ?
C1 N1 Cu1 128.8(19) . . ?
C5 N1 Cu1 111.7(19) . . ?
C10 N2 C6 122(2) . . ?
C10 N2 Cu1 125(2) . . ?
C6 N2 Cu1 113.0(17) . . ?
N3 C15 C14 121(3) . . ?
N3 C15 C16 115(2) . . ?
C14 C15 C16 124(3) . . ?
N4 C16 C17 120(3) . . ?
N4 C16 C15 113(2) . . ?
C17 C16 C15 127(3) . . ?
N5 C21 C22 124(3) . . ?
N5 C21 H21A 117.9 . . ?
C22 C21 H21A 117.9 . . ?
C23 C22 C21 118(2) . . ?
C23 C22 H22A 121.0 . . ?
C21 C22 H22A 121.0 . . ?
C6 C7 C8 121(3) . . ?
C6 C7 H7A 119.7 . . ?
C8 C7 H7A 119.7 . . ?
C10 C9 C8 119(3) . . ?
C10 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
O29 C26 O30 127(3) . . ?
O29 C26 C25 116(2) . . ?
O30 C26 C25 117(2) . . ?
C12 C11 N3 123(3) . . ?
C12 C11 H11A 118.5 . . ?
N3 C11 H11A 118.5 . . ?
C7 C6 N2 119(2) . . ?
C7 C6 C5 127(2) . . ?
N2 C6 C5 113(2) . . ?
C25 C24 C23 118(2) . . ?
C25 C24 H24A 121.1 . . ?
C23 C24 H24A 121.1 . . ?
N4 C20 C19 122(3) . . ?
N4 C20 H20A 118.9 . . ?
C19 C20 H20A 118.9 . . ?
W2 O22 W8 139.3(15) . . ?
N5 C25 C24 126(2) . . ?
N5 C25 C26 113(2) . . ?
C24 C25 C26 121(2) . . ?
C18 C19 C20 118(3) . . ?
C18 C19 H19A 120.8 . . ?
C20 C19 H19A 120.8 . . ?
C15 C14 C13 120(3) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C22 C23 C24 120(3) . . ?
C22 C23 H23A 120.2 . . ?
C24 C23 H23A 120.2 . . ?
N1 C1 C2 126(3) . . ?
N1 C1 H1A 117.2 . . ?
C2 C1 H1A 117.2 . . ?
C13 C12 C11 118(3) . . ?
C13 C12 H12A 120.8 . . ?
C11 C12 H12A 120.8 . . ?
C7 C8 C9 119(3) . . ?
C7 C8 H8A 120.5 . . ?
C9 C8 H8A 120.5 . . ?
C17 C18 C19 120(3) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C3 C4 C5 119(3) . . ?
C3 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
C18 C17 C16 121(3) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C12 C13 C14 120(3) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
N2 C10 C9 120(3) . . ?
N2 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
N1 C5 C6 118(3) . . ?
N1 C5 C4 118(3) . . ?
C6 C5 C4 123(3) . . ?
C3 C2 C1 113(3) . . ?
C3 C2 H2A 123.7 . . ?
C1 C2 H2A 123.7 . . ?
C4 C3 C2 124(3) . . ?
C4 C3 H3A 117.9 . . ?
C2 C3 H3A 117.9 . . ?
W11 O23 W1 139.1(13) . 3_846 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         3.785
_refine_diff_density_min         -3.041
_refine_diff_density_rms         0.500

# start Validation Reply Form

_vrf_PLAT342_k                   
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PROBLEM: Low Bond Precision on  C-C Bonds .........0.0478 Ang
RESPONSE: The quality of this crystal was poor.
;

# end Validation Reply Form

