# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_compound_1
_database_code_depnum_ccdc_archive 'CCDC 1474350'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H108 Co5 N32 O100 P2 W24'
_chemical_formula_weight         8078.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   27.249(5)
_cell_length_b                   27.420(5)
_cell_length_c                   25.189(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     18820(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    535
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.48

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             14036
_exptl_absorpt_coefficient_mu    15.130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_T_max  0.004
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems. These atoms are as follows: P1 C5 O22 O24 C4 C6 O51 C23 O1 C1 C2 N13 C12 N5 C3 C8 C13 C28 O2 C37 N8 C7 C17 C31 C33 and C39. The command 'delu' was used to solve the non-H atoms with 'Large Hirshfeld Difference...' problems. These atoms are as follows: N1 C1. These restraint refinement leads to a relatively high restraint value 151. The coordination water molecule OW3 was refined isotropically to solve the ADP problem.
In the final refinement, the H atoms on coordination water molecules cannot be found from the residual peaks and directly included into the final molecular formula. Some free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. The SQUEEZE program indicates that there are at least fourteen solvent water molecules in the crystal structure. These water molecules were directly included in the final molecular formula based on the elemental analysis, and SQUEEZE analysis.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            114970
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.05
_diffrn_reflns_theta_max         28.22
_reflns_number_total             23245
_reflns_number_gt                17191
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0687P)²+1087.5214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         23082
_refine_ls_number_parameters     1099
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1211
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_restrained_S_all      0.808
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.124 0.250 18.0 0.0
2 0.000 0.500 0.197 2121.7 549.4
3 0.000 0.876 0.750 18.0 -0.2
4 0.500 0.000 0.146 2121.2 549.1
5 0.500 0.376 0.750 18.0 0.2
6 0.500 0.624 0.250 18.0 -0.3


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 0.191578(15) 0.819956(15) 0.623289(17) 0.01407(9) Uani 1 1 d . . .
W2 W 0.036846(15) 0.886586(16) 0.465668(18) 0.01607(9) Uani 1 1 d . . .
W3 W 0.207415(17) 0.762212(17) 0.391501(19) 0.01892(10) Uani 1 1 d . . .
W4 W 0.146024(18) 0.930207(17) 0.41937(2) 0.02127(10) Uani 1 1 d . . .
W5 W 0.256119(18) 0.755895(19) 0.51486(2) 0.02678(12) Uani 1 1 d . . .
W6 W 0.089188(19) 0.715183(19) 0.43969(2) 0.02522(11) Uani 1 1 d . . .
W7 W 0.137558(18) 0.709269(17) 0.56367(2) 0.02344(11) Uani 1 1 d . . .
W8 W 0.032336(17) 0.772421(18) 0.542647(19) 0.02031(10) Uani 1 1 d . . .
W9 W 0.260237(18) 0.863092(18) 0.44661(2) 0.02407(11) Uani 1 1 d . . .
W10 W 0.086138(18) 0.882818(18) 0.60168(2) 0.02263(11) Uani 1 1 d . . .
W11 W 0.196330(18) 0.926449(17) 0.55583(2) 0.02182(10) Uani 1 1 d . . .
W12 W 0.09440(2) 0.82986(2) 0.36378(2) 0.02982(12) Uani 1 1 d . . .
Co3 Co -0.09850(5) 0.91062(5) 0.47069(6) 0.0170(3) Uani 1 1 d . . .
Co2 Co 0.25113(5) 0.71621(5) 0.25760(5) 0.0093(3) Uani 1 1 d . . .
P1 P 0.14452(8) 0.82089(8) 0.49435(9) 0.0031(4) Uani 1 1 d U . .
O1 O 0.1527(2) 0.8485(2) 0.5465(3) 0.0088(13) Uani 1 1 d U . .
O2 O 0.1568(3) 0.9858(3) 0.3925(3) 0.0230(18) Uani 1 1 d U . .
O3 O -0.0196(3) 0.9139(3) 0.4640(3) 0.0223(18) Uani 1 1 d . . .
O4 O -0.0249(3) 0.7606(3) 0.5657(3) 0.0187(16) Uani 1 1 d . . .
O5 O 0.2259(3) 0.7326(3) 0.3353(3) 0.0235(18) Uani 1 1 d . . .
O6 O 0.2245(3) 0.9790(3) 0.5722(4) 0.0244(18) Uani 1 1 d . . .
O7 O 0.1946(2) 0.8065(2) 0.4709(3) 0.0086(13) Uani 1 1 d . . .
O8 O 0.1242(3) 0.8934(3) 0.3608(3) 0.0174(16) Uani 1 1 d . . .
O9 O 0.1561(3) 0.7226(2) 0.4154(3) 0.0156(15) Uani 1 1 d . . .
O10 O 0.2424(3) 0.8961(3) 0.5104(3) 0.0180(16) Uani 1 1 d . . .
O11 O 0.0758(3) 0.8222(4) 0.3011(3) 0.031(2) Uani 1 1 d . . .
O12 O 0.0478(3) 0.9092(3) 0.6450(3) 0.0246(18) Uani 1 1 d . . .
O13 O 0.0592(3) 0.9020(3) 0.5351(3) 0.0158(15) Uani 1 1 d . . .
O14 O 0.0677(3) 0.6686(3) 0.4015(4) 0.030(2) Uani 1 1 d . . .
O15 O 0.1354(3) 0.9324(3) 0.5939(3) 0.0146(15) Uani 1 1 d . . .
O16 O 0.1170(2) 0.8537(2) 0.4548(3) 0.0093(13) Uani 1 1 d . . .
O17 O 0.0558(3) 0.8215(3) 0.5892(3) 0.0156(15) Uani 1 1 d . . .
O18 O 0.0696(3) 0.7245(3) 0.5793(3) 0.0154(15) Uani 1 1 d . . .
O19 O 0.1151(3) 0.6801(3) 0.4997(3) 0.0166(16) Uani 1 1 d . . .
O20 O 0.2523(3) 0.8165(3) 0.3909(3) 0.0197(17) Uani 1 1 d . . .
O21 O 0.1617(3) 0.9434(3) 0.4929(3) 0.0164(16) Uani 1 1 d . . .
O22 O 0.1558(3) 0.7619(3) 0.6095(3) 0.0115(14) Uani 1 1 d U . .
O23 O 0.2388(3) 0.7951(3) 0.5748(3) 0.0168(16) Uani 1 1 d . . .
O24 O 0.2499(3) 0.7338(3) 0.4435(3) 0.0184(16) Uani 1 1 d U . .
O25 O 0.0219(3) 0.8244(3) 0.4928(3) 0.0144(15) Uani 1 1 d . . .
O26 O 0.2172(3) 0.8839(3) 0.6124(3) 0.0174(16) Uani 1 1 d . . .
O27 O 0.0387(3) 0.8596(3) 0.3958(3) 0.0185(16) Uani 1 1 d . . .
O28 O 0.1587(3) 0.8036(3) 0.3636(3) 0.0187(16) Uani 1 1 d . . .
O29 O 0.2895(3) 0.8124(3) 0.4870(3) 0.0154(15) Uani 1 1 d . . .
O30 O 0.2011(3) 0.7172(3) 0.5332(3) 0.0160(16) Uani 1 1 d . . .
O31 O 0.0327(3) 0.7291(3) 0.4815(3) 0.0140(15) Uani 1 1 d . . .
O32 O 0.0779(3) 0.9381(3) 0.4391(3) 0.0157(15) Uani 1 1 d . . .
O34 O 0.0764(3) 0.7701(3) 0.3969(3) 0.0155(15) Uani 1 1 d . . .
O35 O 0.1141(2) 0.7749(2) 0.5053(3) 0.0090(13) Uani 1 1 d . . .
O36 O 0.2189(3) 0.8061(3) 0.6823(3) 0.0160(15) Uani 1 1 d . . .
O37 O 0.1326(3) 0.8497(3) 0.6472(3) 0.0158(15) Uani 1 1 d . . .
O38 O 0.1455(3) 0.6590(3) 0.6025(4) 0.0261(19) Uani 1 1 d . . .
O39 O 0.3101(3) 0.8942(3) 0.4250(4) 0.028(2) Uani 1 1 d . . .
O40 O 0.3043(3) 0.7235(3) 0.5376(4) 0.029(2) Uani 1 1 d . . .
O33 O 0.2076(3) 0.8998(3) 0.4158(3) 0.0171(16) Uani 1 1 d . . .
OW2 O -0.0887(3) 0.9886(3) 0.4738(3) 0.0252(19) Uani 1 1 d . . .
OW1 O -0.1040(3) 0.8325(3) 0.4672(4) 0.032(2) Uani 1 1 d . . .
Co1 Co -0.5000 1.0472(3) 0.7500 0.126(2) Uani 1 2 d S . .
N1 N -0.4501(10) 0.9961(10) 0.7184(16) 0.170(16) Uani 1 1 d U . .
N2 N -0.2481(4) 0.9245(4) 0.5153(5) 0.032(3) Uani 1 1 d . . .
N3 N 0.3228(3) 0.7330(3) 0.2846(4) 0.019(2) Uani 1 1 d . . .
N4 N -0.3878(7) 0.9609(8) 0.6765(9) 0.087(6) Uani 1 1 d . . .
N5 N 0.4033(4) 0.7375(4) 0.2861(4) 0.028(2) Uani 1 1 d U . .
N6 N -0.0880(5) 0.9428(4) 0.3062(4) 0.033(3) Uani 1 1 d . . .
N7 N -0.1758(4) 0.9154(4) 0.4783(5) 0.028(2) Uani 1 1 d . . .
N8 N 0.2257(4) 1.0649(4) 0.2819(4) 0.027(2) Uani 1 1 d U . .
N9 N 0.2447(4) 0.7889(4) 0.2286(4) 0.024(2) Uani 1 1 d . . .
N10 N 0.2398(4) 0.8682(4) 0.2217(4) 0.029(2) Uani 1 1 d . . .
N11 N 0.1803(4) 0.7028(5) 0.2280(5) 0.034(3) Uani 1 1 d . . .
N12 N -0.0715(5) 0.9261(4) 0.6365(4) 0.031(3) Uani 1 1 d . . .
N13 N 0.0993(5) 0.6995(5) 0.2225(5) 0.042(3) Uani 1 1 d U . .
N14 N -0.0985(4) 0.9142(4) 0.3869(4) 0.027(2) Uani 1 1 d . . .
N15 N 0.2371(4) 1.1443(4) 0.2828(4) 0.023(2) Uani 1 1 d . . .
N16 N -0.0836(4) 0.9053(4) 0.5522(4) 0.024(2) Uani 1 1 d . . .
C1 C -0.4195(10) 0.9963(11) 0.6809(11) 0.092(7) Uani 1 1 d U . .
H1A H -0.4195 1.0216 0.6564 0.111 Uiso 1 1 calc R . .
C2 C -0.394(2) 0.931(2) 0.716(2) 0.210(19) Uani 1 1 d U . .
H2A H -0.3794 0.9011 0.7241 0.252 Uiso 1 1 calc R . .
C3 C -0.4336(18) 0.9592(18) 0.747(2) 0.177(16) Uani 1 1 d U . .
H3A H -0.4445 0.9514 0.7805 0.213 Uiso 1 1 calc R . .
C4 C 0.1693(11) 0.7017(10) 0.1779(12) 0.095(8) Uani 1 1 d U . .
H4A H 0.1918 0.7023 0.1501 0.114 Uiso 1 1 calc R . .
C5 C 0.1174(12) 0.6992(12) 0.1719(13) 0.115(10) Uani 1 1 d U . .
H5A H 0.0996 0.6977 0.1404 0.138 Uiso 1 1 calc R . .
C6 C 0.0340(8) 0.7105(8) 0.2847(10) 0.073(6) Uani 1 1 d U . .
H6 H 0.0567 0.7226 0.3090 0.087 Uiso 1 1 calc R . .
C7 C 0.0149(7) 0.7032(9) 0.1996(9) 0.072(6) Uani 1 1 d U . .
H7 H 0.0232 0.7007 0.1639 0.086 Uiso 1 1 calc R . .
C8 C 0.2648(8) 0.8040(8) 0.1819(9) 0.064(5) Uani 1 1 d U . .
H8A H 0.2786 0.7831 0.1570 0.077 Uiso 1 1 calc R . .
C9 C -0.3529(6) 0.9515(8) 0.6319(9) 0.060(5) Uani 1 1 d . . .
C10 C -0.3430(7) 0.9056(8) 0.6175(9) 0.068(6) Uani 1 1 d . . .
H10A H -0.3597 0.8799 0.6335 0.081 Uiso 1 1 calc R . .
C11 C -0.3071(6) 0.8959(7) 0.5775(9) 0.058(5) Uani 1 1 d . . .
H11A H -0.2990 0.8642 0.5681 0.069 Uiso 1 1 calc R . .
C12 C 0.2623(6) 0.8532(7) 0.1760(7) 0.051(4) Uani 1 1 d U . .
H12A H 0.2732 0.8721 0.1477 0.061 Uiso 1 1 calc R . .
C13 C -0.2548(6) 0.8970(6) 0.4690(7) 0.045(4) Uani 1 1 d U . .
H13A H -0.2841 0.8853 0.4551 0.054 Uiso 1 1 calc R . .
C14 C 0.3876(5) 0.7597(8) 0.3303(7) 0.059(6) Uani 1 1 d . . .
H14A H 0.4068 0.7740 0.3566 0.071 Uiso 1 1 calc R . .
C15 C -0.1043(7) 0.8767(6) 0.3509(6) 0.053(5) Uani 1 1 d . . .
H15A H -0.1120 0.8446 0.3593 0.064 Uiso 1 1 calc R . .
C16 C -0.3286(8) 0.9910(7) 0.6088(9) 0.068(6) Uani 1 1 d . . .
H16A H -0.3346 1.0227 0.6202 0.081 Uiso 1 1 calc R . .
C17 C 0.4619(5) 0.7322(7) 0.2137(6) 0.044(4) Uani 1 1 d U . .
H17 H 0.4364 0.7318 0.1892 0.053 Uiso 1 1 calc R . .
C18 C 0.2261(6) 0.9540(5) 0.1977(6) 0.038(3) Uani 1 1 d . . .
H18A H 0.2231 0.9455 0.1621 0.045 Uiso 1 1 calc R . .
C19 C -0.2960(6) 0.9819(5) 0.5689(7) 0.045(4) Uani 1 1 d . . .
H19A H -0.2809 1.0078 0.5516 0.054 Uiso 1 1 calc R . .
C20 C -0.0754(7) 0.8766(5) 0.6344(6) 0.049(5) Uani 1 1 d . . .
H20A H -0.0734 0.8557 0.6634 0.059 Uiso 1 1 calc R . .
C21 C -0.0824(7) 0.8628(5) 0.5842(6) 0.043(4) Uani 1 1 d . . .
H21A H -0.0860 0.8309 0.5723 0.052 Uiso 1 1 calc R . .
C22 C 0.2330(7) 0.9799(5) 0.3032(6) 0.043(4) Uani 1 1 d . . .
H22A H 0.2338 0.9889 0.3388 0.051 Uiso 1 1 calc R . .
C23 C 0.3381(6) 0.7573(6) 0.3288(7) 0.049(4) Uani 1 1 d U . .
H23A H 0.3174 0.7703 0.3545 0.059 Uiso 1 1 calc R . .
C24 C -0.0566(6) 0.9626(6) 0.2185(5) 0.037(3) Uani 1 1 d . . .
H24 H -0.0433 0.9315 0.2156 0.044 Uiso 1 1 calc R . .
C25 C -0.2082(5) 0.8910(6) 0.4484(7) 0.043(4) Uani 1 1 d . . .
H25A H -0.2005 0.8728 0.4184 0.052 Uiso 1 1 calc R . .
C26 C 0.2064(6) 1.0816(5) 0.3286(5) 0.031(3) Uani 1 1 d . . .
H26A H 0.1914 1.0630 0.3549 0.038 Uiso 1 1 calc R . .
C27 C -0.0800(6) 0.9766(6) 0.2643(5) 0.039(4) Uani 1 1 d . . .
C28 C 0.4526(5) 0.7331(5) 0.2666(5) 0.026(3) Uani 1 1 d U . .
C29 C 0.1390(4) 0.7038(5) 0.2536(5) 0.028(3) Uani 1 1 d . . .
H29A H 0.1371 0.7072 0.2903 0.034 Uiso 1 1 calc R . .
C30 C -0.1999(4) 0.9351(5) 0.5177(5) 0.024(3) Uani 1 1 d . . .
H30A H -0.1855 0.9541 0.5440 0.029 Uiso 1 1 calc R . .
C31 C 0.4892(5) 0.7321(6) 0.3027(6) 0.041(3) Uani 1 1 d U . .
H31 H 0.4818 0.7312 0.3387 0.049 Uiso 1 1 calc R . .
C32 C 0.2431(6) 1.1040(4) 0.2561(5) 0.030(3) Uani 1 1 d . . .
H32A H 0.2578 1.1026 0.2228 0.036 Uiso 1 1 calc R . .
C33 C 0.2228(6) 1.0022(5) 0.2136(6) 0.038(3) Uani 1 1 d U . .
H33A H 0.2168 1.0264 0.1886 0.046 Uiso 1 1 calc R . .
C34 C -0.0979(6) 0.9752(5) 0.7699(5) 0.038(3) Uani 1 1 d . . .
H34 H -0.1124 0.9652 0.8014 0.045 Uiso 1 1 calc R . .
C35 C 0.2365(6) 0.9310(5) 0.2889(6) 0.041(4) Uani 1 1 d . . .
H35A H 0.2405 0.9072 0.3148 0.050 Uiso 1 1 calc R . .
C36 C -0.0715(5) 0.9583(5) 0.6808(5) 0.032(3) Uani 1 1 d . . .
C37 C -0.0766(4) 0.9410(4) 0.5845(5) 0.020(2) Uani 1 1 d U . .
H37A H -0.0751 0.9734 0.5738 0.024 Uiso 1 1 calc R . .
C38 C -0.0966(8) 0.8948(5) 0.3007(6) 0.053(5) Uani 1 1 d . . .
H38A H -0.0973 0.8772 0.2692 0.064 Uiso 1 1 calc R . .
C39 C 0.2313(5) 0.8293(4) 0.2515(5) 0.029(3) Uani 1 1 d U . .
H39A H 0.2173 0.8307 0.2852 0.035 Uiso 1 1 calc R . .
C40 C 0.2283(5) 1.0141(4) 0.2649(5) 0.029(3) Uani 1 1 d . . .
C41 C 0.3629(4) 0.7212(5) 0.2604(5) 0.024(3) Uani 1 1 d . . .
H41A H 0.3639 0.7036 0.2289 0.029 Uiso 1 1 calc R . .
C42 C 0.2341(5) 0.9181(4) 0.2367(5) 0.028(3) Uani 1 1 d . . .
C43 C 0.0480(4) 0.7002(6) 0.2357(5) 0.032(3) Uani 1 1 d . . .
C44 C 0.2135(6) 1.1305(4) 0.3290(5) 0.031(3) Uani 1 1 d . . .
H44A H 0.2040 1.1515 0.3561 0.037 Uiso 1 1 calc R . .
C45 C -0.0527(5) 1.0043(6) 0.6761(5) 0.033(3) Uani 1 1 d . . .
H45 H -0.0373 1.0137 0.6448 0.040 Uiso 1 1 calc R . .
C46 C -0.0901(6) 0.9531(5) 0.3589(5) 0.032(3) Uani 1 1 d . . .
H46A H -0.0860 0.9841 0.3732 0.038 Uiso 1 1 calc R . .
C47 C -0.2853(4) 0.9348(5) 0.5539(7) 0.034(3) Uani 1 1 d . . .
C48 C -0.0935(7) 0.9433(6) 0.7277(5) 0.044(4) Uani 1 1 d . . .
H48 H -0.1052 0.9116 0.7308 0.053 Uiso 1 1 calc R . .
OW3 O -0.4565(10) 1.0229(10) 0.8180(11) 0.155(9) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O36 1.705(8) . ?
W1 O23 1.901(8) . ?
W1 O22 1.899(7) . ?
W1 O37 1.900(7) . ?
W1 O26 1.908(8) . ?
W1 O1 2.339(7) . ?
W2 O3 1.711(7) . ?
W2 O25 1.882(7) . ?
W2 O13 1.900(8) . ?
W2 O27 1.909(8) . ?
W2 O32 1.923(8) . ?
W2 O16 2.378(6) . ?
W3 O5 1.707(8) . ?
W3 O9 1.871(8) . ?
W3 O28 1.883(8) . ?
W3 O24 1.914(8) . ?
W3 O20 1.927(8) . ?
W3 O7 2.367(7) . ?
W4 O2 1.692(8) . ?
W4 O33 1.875(7) . ?
W4 O8 1.883(8) . ?
W4 O21 1.934(8) . ?
W4 O32 1.934(7) . ?
W4 O16 2.412(7) . ?
W5 O40 1.685(8) . ?
W5 O30 1.894(7) . ?
W5 O24 1.905(8) . ?
W5 O23 1.913(8) . ?
W5 O29 1.929(7) . ?
W5 O7 2.442(7) . ?
W6 O14 1.702(8) . ?
W6 O34 1.884(7) . ?
W6 O31 1.903(7) . ?
W6 O9 1.934(7) . ?
W6 O19 1.926(8) . ?
W6 O35 2.422(7) . ?
W7 O38 1.705(8) . ?
W7 O19 1.901(8) . ?
W7 O30 1.906(7) . ?
W7 O22 1.914(7) . ?
W7 O18 1.938(7) . ?
W7 O35 2.410(7) . ?
W8 O4 1.696(7) . ?
W8 O17 1.897(7) . ?
W8 O18 1.900(7) . ?
W8 O25 1.920(7) . ?
W8 O31 1.946(7) . ?
W8 O35 2.419(6) . ?
W9 O39 1.693(8) . ?
W9 O29 1.898(7) . ?
W9 O10 1.907(8) . ?
W9 O20 1.910(8) . ?
W9 O33 1.917(7) . ?
W9 O7 2.445(7) . ?
W10 O12 1.674(8) . ?
W10 O17 1.899(7) . ?
W10 O13 1.905(8) . ?
W10 O15 1.921(8) . ?
W10 O37 1.935(7) . ?
W10 O1 2.471(7) . ?
W11 O6 1.683(8) . ?
W11 O10 1.892(8) . ?
W11 O21 1.904(8) . ?
W11 O15 1.924(8) . ?
W11 O26 1.927(7) . ?
W11 O1 2.456(7) . ?
W12 O11 1.673(9) . ?
W12 O28 1.894(7) . ?
W12 O27 1.904(7) . ?
W12 O34 1.902(8) . ?
W12 O8 1.925(8) . ?
W12 O16 2.464(7) . ?
Co3 N16 2.099(10) . ?
Co3 N7 2.118(11) . ?
Co3 N14 2.114(10) . ?
Co3 OW1 2.150(9) . ?
Co3 O3 2.159(8) . ?
Co3 OW2 2.156(9) . ?
Co2 N15 2.096(10) 7_655 ?
Co2 N11 2.102(10) . ?
Co2 N3 2.118(9) . ?
Co2 O5 2.123(8) . ?
Co2 N9 2.130(10) . ?
Co2 O36 2.154(8) 2_564 ?
P1 O1 1.534(7) . ?
P1 O7 1.538(7) . ?
P1 O16 1.538(7) . ?
P1 O35 1.536(7) . ?
O36 Co2 2.154(8) 2_565 ?
Co1 N1 2.11(3) . ?
Co1 N1 2.11(3) 4_456 ?
Co1 OW3 2.19(3) 4_456 ?
Co1 OW3 2.19(3) . ?
N1 C1 1.26(3) . ?
N1 C3 1.32(5) . ?
N2 C30 1.348(15) . ?
N2 C13 1.40(2) . ?
N2 C47 1.430(18) . ?
N3 C41 1.294(14) . ?
N3 C23 1.36(2) . ?
N4 C2 1.31(6) . ?
N4 C1 1.30(3) . ?
N4 C9 1.49(2) . ?
N5 C14 1.339(18) . ?
N5 C41 1.353(15) . ?
N5 C28 1.437(16) . ?
N6 C38 1.343(18) . ?
N6 C46 1.358(16) . ?
N6 C27 1.422(18) . ?
N7 C30 1.307(17) . ?
N7 C25 1.340(18) . ?
N8 C32 1.340(15) . ?
N8 C26 1.367(16) . ?
N8 C40 1.459(14) . ?
N9 C39 1.303(15) . ?
N9 C8 1.36(2) . ?
N10 C39 1.326(16) . ?
N10 C12 1.37(2) . ?
N10 C42 1.428(15) . ?
N11 C4 1.30(3) . ?
N11 C29 1.297(16) . ?
N12 C20 1.362(19) . ?
N12 C37 1.381(15) . ?
N12 C36 1.422(17) . ?
N13 C29 1.342(17) . ?
N13 C5 1.37(3) . ?
N13 C43 1.436(17) . ?
N14 C46 1.296(16) . ?
N14 C15 1.379(19) . ?
N15 C32 1.303(15) . ?
N15 C44 1.382(15) . ?
N15 Co2 2.096(10) 7_665 ?
N16 C37 1.286(15) . ?
N16 C21 1.416(17) . ?
C1 C3 1.98(6) . ?
C2 C3 1.53(6) . ?
C4 C5 1.43(4) . ?
C6 C43 1.32(3) . ?
C6 C7 1.40(3) 4 ?
C7 C43 1.28(2) . ?
C7 C6 1.40(3) 4 ?
C8 C12 1.36(3) . ?
C9 C10 1.34(3) . ?
C9 C16 1.39(3) . ?
C10 C11 1.43(3) . ?
C11 C47 1.36(2) . ?
C13 C25 1.38(2) . ?
C14 C23 1.35(2) . ?
C15 C38 1.37(2) . ?
C16 C19 1.36(2) . ?
C17 C28 1.35(2) . ?
C17 C31 1.395(19) 4_655 ?
C18 C33 1.384(19) . ?
C18 C42 1.405(18) . ?
C19 C47 1.376(19) . ?
C20 C21 1.33(2) . ?
C22 C40 1.352(19) . ?
C22 C35 1.391(18) . ?
C24 C27 1.37(2) . ?
C24 C45 1.406(19) 8_575 ?
C26 C44 1.356(17) . ?
C27 C34 1.42(2) 8_575 ?
C28 C31 1.349(19) . ?
C31 C17 1.395(19) 4_655 ?
C33 C40 1.34(2) . ?
C34 C48 1.381(19) . ?
C34 C27 1.42(2) 8_576 ?
C35 C42 1.36(2) . ?
C36 C45 1.37(2) . ?
C36 C48 1.387(19) . ?
C45 C24 1.406(19) 8_576 ?

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
O36 W1 O23 100.7(3) . . ?
O36 W1 O22 101.3(3) . . ?
O23 W1 O22 86.0(3) . . ?
O36 W1 O37 100.9(3) . . ?
O23 W1 O37 158.5(3) . . ?
O22 W1 O37 89.0(3) . . ?
O36 W1 O26 99.8(3) . . ?
O23 W1 O26 89.4(3) . . ?
O22 W1 O26 158.9(3) . . ?
O37 W1 O26 87.7(3) . . ?
O36 W1 O1 173.0(3) . . ?
O23 W1 O1 84.0(3) . . ?
O22 W1 O1 84.1(3) . . ?
O37 W1 O1 74.7(3) . . ?
O26 W1 O1 74.9(3) . . ?
O3 W2 O25 102.1(4) . . ?
O3 W2 O13 102.3(4) . . ?
O25 W2 O13 86.4(3) . . ?
O3 W2 O27 99.8(4) . . ?
O25 W2 O27 89.4(3) . . ?
O13 W2 O27 157.9(3) . . ?
O3 W2 O32 101.2(4) . . ?
O25 W2 O32 156.7(3) . . ?
O13 W2 O32 88.2(3) . . ?
O27 W2 O32 87.1(3) . . ?
O3 W2 O16 171.3(3) . . ?
O25 W2 O16 84.1(3) . . ?
O13 W2 O16 84.0(3) . . ?
O27 W2 O16 74.0(3) . . ?
O32 W2 O16 72.8(3) . . ?
O5 W3 O9 102.2(4) . . ?
O5 W3 O28 100.6(4) . . ?
O9 W3 O28 86.7(3) . . ?
O5 W3 O24 101.3(4) . . ?
O9 W3 O24 89.7(3) . . ?
O28 W3 O24 158.0(3) . . ?
O5 W3 O20 100.0(4) . . ?
O9 W3 O20 157.8(3) . . ?
O28 W3 O20 88.8(3) . . ?
O24 W3 O20 86.4(3) . . ?
O5 W3 O7 171.2(3) . . ?
O9 W3 O7 85.2(3) . . ?
O28 W3 O7 84.4(3) . . ?
O24 W3 O7 73.7(3) . . ?
O20 W3 O7 72.7(3) . . ?
O2 W4 O33 103.0(4) . . ?
O2 W4 O8 102.9(4) . . ?
O33 W4 O8 90.4(3) . . ?
O2 W4 O21 100.2(4) . . ?
O33 W4 O21 86.1(3) . . ?
O8 W4 O21 156.9(3) . . ?
O2 W4 O32 99.7(4) . . ?
O33 W4 O32 157.1(3) . . ?
O8 W4 O32 87.7(3) . . ?
O21 W4 O32 86.8(3) . . ?
O2 W4 O16 170.8(3) . . ?
O33 W4 O16 85.7(3) . . ?
O8 W4 O16 73.8(3) . . ?
O21 W4 O16 83.1(3) . . ?
O32 W4 O16 71.8(3) . . ?
O40 W5 O30 103.8(4) . . ?
O40 W5 O24 102.8(4) . . ?
O30 W5 O24 88.9(3) . . ?
O40 W5 O23 102.7(4) . . ?
O30 W5 O23 85.8(3) . . ?
O24 W5 O23 154.4(3) . . ?
O40 W5 O29 100.4(4) . . ?
O30 W5 O29 155.8(3) . . ?
O24 W5 O29 87.4(3) . . ?
O23 W5 O29 87.2(3) . . ?
O40 W5 O7 171.3(4) . . ?
O30 W5 O7 83.4(3) . . ?
O24 W5 O7 72.1(3) . . ?
O23 W5 O7 82.5(3) . . ?
O29 W5 O7 72.7(3) . . ?
O14 W6 O34 102.3(4) . . ?
O14 W6 O31 100.6(4) . . ?
O34 W6 O31 90.4(3) . . ?
O14 W6 O9 103.0(4) . . ?
O34 W6 O9 84.8(3) . . ?
O31 W6 O9 156.4(3) . . ?
O14 W6 O19 101.2(4) . . ?
O34 W6 O19 156.3(3) . . ?
O31 W6 O19 87.9(3) . . ?
O9 W6 O19 87.4(3) . . ?
O14 W6 O35 171.2(4) . . ?
O34 W6 O35 84.3(3) . . ?
O31 W6 O35 73.3(3) . . ?
O9 W6 O35 83.1(3) . . ?
O19 W6 O35 72.5(3) . . ?
O38 W7 O19 100.7(4) . . ?
O38 W7 O30 102.0(4) . . ?
O19 W7 O30 89.9(3) . . ?
O38 W7 O22 103.4(4) . . ?
O19 W7 O22 155.9(3) . . ?
O30 W7 O22 85.5(3) . . ?
O38 W7 O18 100.3(4) . . ?
O19 W7 O18 87.5(3) . . ?
O30 W7 O18 157.6(3) . . ?
O22 W7 O18 87.9(3) . . ?
O38 W7 O35 171.0(3) . . ?
O19 W7 O35 73.2(3) . . ?
O30 W7 O35 84.8(3) . . ?
O22 W7 O35 82.8(3) . . ?
O18 W7 O35 73.1(3) . . ?
O4 W8 O17 103.5(4) . . ?
O4 W8 O18 101.2(4) . . ?
O17 W8 O18 90.6(3) . . ?
O4 W8 O25 103.2(3) . . ?
O17 W8 O25 85.8(3) . . ?
O18 W8 O25 155.5(3) . . ?
O4 W8 O31 99.2(3) . . ?
O17 W8 O31 157.1(3) . . ?
O18 W8 O31 87.7(3) . . ?
O25 W8 O31 86.3(3) . . ?
O4 W8 O35 170.3(3) . . ?
O17 W8 O35 84.9(3) . . ?
O18 W8 O35 73.5(3) . . ?
O25 W8 O35 82.0(3) . . ?
O31 W8 O35 72.8(3) . . ?
O39 W9 O29 101.8(4) . . ?
O39 W9 O10 103.6(4) . . ?
O29 W9 O10 90.2(3) . . ?
O39 W9 O20 101.0(4) . . ?
O29 W9 O20 87.2(3) . . ?
O10 W9 O20 155.2(3) . . ?
O39 W9 O33 101.8(4) . . ?
O29 W9 O33 156.4(3) . . ?
O10 W9 O33 84.3(3) . . ?
O20 W9 O33 88.2(3) . . ?
O39 W9 O7 170.6(3) . . ?
O29 W9 O7 73.1(3) . . ?
O10 W9 O7 84.5(3) . . ?
O20 W9 O7 71.2(3) . . ?
O33 W9 O7 83.6(3) . . ?
O12 W10 O17 102.6(4) . . ?
O12 W10 O13 102.4(4) . . ?
O17 W10 O13 86.1(3) . . ?
O12 W10 O15 101.3(4) . . ?
O17 W10 O15 156.1(3) . . ?
O13 W10 O15 89.1(3) . . ?
O12 W10 O37 103.0(4) . . ?
O17 W10 O37 88.1(3) . . ?
O13 W10 O37 154.6(3) . . ?
O15 W10 O37 86.3(3) . . ?
O12 W10 O1 171.3(3) . . ?
O17 W10 O1 83.7(3) . . ?
O13 W10 O1 83.9(3) . . ?
O15 W10 O1 72.5(3) . . ?
O37 W10 O1 71.0(3) . . ?
O6 W11 O10 102.8(4) . . ?
O6 W11 O21 102.8(4) . . ?
O10 W11 O21 86.1(3) . . ?
O6 W11 O15 101.5(4) . . ?
O10 W11 O15 155.8(3) . . ?
O21 W11 O15 88.1(3) . . ?
O6 W11 O26 101.7(4) . . ?
O10 W11 O26 89.2(3) . . ?
O21 W11 O26 155.5(3) . . ?
O15 W11 O26 86.4(3) . . ?
O6 W11 O1 171.2(3) . . ?
O10 W11 O1 83.2(3) . . ?
O21 W11 O1 83.9(3) . . ?
O15 W11 O1 72.8(3) . . ?
O26 W11 O1 71.8(3) . . ?
O11 W12 O28 103.3(4) . . ?
O11 W12 O27 102.3(4) . . ?
O28 W12 O27 154.4(3) . . ?
O11 W12 O34 103.2(4) . . ?
O28 W12 O34 84.9(3) . . ?
O27 W12 O34 88.7(3) . . ?
O11 W12 O8 101.9(4) . . ?
O28 W12 O8 87.4(3) . . ?
O27 W12 O8 88.0(3) . . ?
O34 W12 O8 154.9(3) . . ?
O11 W12 O16 171.4(4) . . ?
O28 W12 O16 82.6(3) . . ?
O27 W12 O16 72.0(3) . . ?
O34 W12 O16 83.4(3) . . ?
O8 W12 O16 71.9(3) . . ?
N16 Co3 N7 96.2(4) . . ?
N16 Co3 N14 168.8(4) . . ?
N7 Co3 N14 95.0(5) . . ?
N16 Co3 OW1 89.1(4) . . ?
N7 Co3 OW1 89.7(4) . . ?
N14 Co3 OW1 90.3(4) . . ?
N16 Co3 O3 83.5(4) . . ?
N7 Co3 O3 174.1(4) . . ?
N14 Co3 O3 85.5(4) . . ?
OW1 Co3 O3 96.2(3) . . ?
N16 Co3 OW2 90.6(4) . . ?
N7 Co3 OW2 93.4(4) . . ?
N14 Co3 OW2 89.4(4) . . ?
OW1 Co3 OW2 176.9(4) . . ?
O3 Co3 OW2 80.7(3) . . ?
N15 Co2 N11 94.8(5) 7_655 . ?
N15 Co2 N3 88.1(4) 7_655 . ?
N11 Co2 N3 176.9(5) . . ?
N15 Co2 O5 88.3(4) 7_655 . ?
N11 Co2 O5 93.8(4) . . ?
N3 Co2 O5 87.5(4) . . ?
N15 Co2 N9 175.3(4) 7_655 . ?
N11 Co2 N9 88.1(5) . . ?
N3 Co2 N9 89.0(4) . . ?
O5 Co2 N9 95.2(4) . . ?
N15 Co2 O36 86.6(3) 7_655 2_564 ?
N11 Co2 O36 89.2(4) . 2_564 ?
N3 Co2 O36 89.7(3) . 2_564 ?
O5 Co2 O36 174.3(3) . 2_564 ?
N9 Co2 O36 89.7(3) . 2_564 ?
O1 P1 O7 109.0(4) . . ?
O1 P1 O16 109.6(4) . . ?
O7 P1 O16 109.6(4) . . ?
O1 P1 O35 109.3(4) . . ?
O7 P1 O35 109.8(4) . . ?
O16 P1 O35 109.5(4) . . ?
P1 O1 W1 127.5(4) . . ?
P1 O1 W11 125.6(4) . . ?
W1 O1 W11 89.6(2) . . ?
P1 O1 W10 124.2(4) . . ?
W1 O1 W10 89.7(2) . . ?
W11 O1 W10 88.3(2) . . ?
W2 O3 Co3 151.1(5) . . ?
W3 O5 Co2 163.9(5) . . ?
P1 O7 W3 125.9(4) . . ?
P1 O7 W5 125.5(4) . . ?
W3 O7 W5 89.4(2) . . ?
P1 O7 W9 125.6(4) . . ?
W3 O7 W9 90.3(2) . . ?
W5 O7 W9 88.4(2) . . ?
W4 O8 W12 126.0(4) . . ?
W3 O9 W6 150.2(4) . . ?
W11 O10 W9 152.5(4) . . ?
W2 O13 W10 150.7(4) . . ?
W10 O15 W11 126.4(4) . . ?
P1 O16 W2 126.6(4) . . ?
P1 O16 W4 126.1(4) . . ?
W2 O16 W4 90.8(2) . . ?
P1 O16 W12 124.7(4) . . ?
W2 O16 W12 88.7(2) . . ?
W4 O16 W12 88.2(2) . . ?
W8 O17 W10 151.3(4) . . ?
W8 O18 W7 124.1(4) . . ?
W7 O19 W6 124.9(4) . . ?
W9 O20 W3 125.7(4) . . ?
W11 O21 W4 149.5(4) . . ?
W1 O22 W7 151.1(4) . . ?
W1 O23 W5 151.1(4) . . ?
W5 O24 W3 124.7(4) . . ?
W2 O25 W8 151.4(4) . . ?
W1 O26 W11 123.7(4) . . ?
W12 O27 W2 125.3(4) . . ?
W3 O28 W12 151.8(5) . . ?
W9 O29 W5 125.8(4) . . ?
W5 O30 W7 151.8(4) . . ?
W6 O31 W8 124.4(4) . . ?
W2 O32 W4 124.4(4) . . ?
W6 O34 W12 153.1(4) . . ?
P1 O35 W7 125.4(4) . . ?
P1 O35 W8 126.2(4) . . ?
W7 O35 W8 89.2(2) . . ?
P1 O35 W6 125.7(4) . . ?
W7 O35 W6 89.2(2) . . ?
W8 O35 W6 89.4(2) . . ?
W1 O36 Co2 175.2(4) . 2_565 ?
W1 O37 W10 124.6(4) . . ?
W4 O33 W9 152.0(4) . . ?
N1 Co1 N1 96.7(13) . 4_456 ?
N1 Co1 OW3 81.4(14) . 4_456 ?
N1 Co1 OW3 75.1(14) 4_456 4_456 ?
N1 Co1 OW3 75.1(14) . . ?
N1 Co1 OW3 81.4(14) 4_456 . ?
OW3 Co1 OW3 144.4(15) 4_456 . ?
C1 N1 C3 100(3) . . ?
C1 N1 Co1 135(3) . . ?
C3 N1 Co1 122(3) . . ?
C30 N2 C13 106.2(12) . . ?
C30 N2 C47 128.1(12) . . ?
C13 N2 C47 125.5(12) . . ?
C41 N3 C23 104.4(11) . . ?
C41 N3 Co2 124.9(8) . . ?
C23 N3 Co2 130.7(10) . . ?
C2 N4 C1 108(3) . . ?
C2 N4 C9 124(3) . . ?
C1 N4 C9 128(2) . . ?
C14 N5 C41 106.7(11) . . ?
C14 N5 C28 128.5(12) . . ?
C41 N5 C28 124.7(11) . . ?
C38 N6 C46 107.3(12) . . ?
C38 N6 C27 126.1(12) . . ?
C46 N6 C27 126.6(12) . . ?
C30 N7 C25 107.6(12) . . ?
C30 N7 Co3 126.4(9) . . ?
C25 N7 Co3 125.0(10) . . ?
C32 N8 C26 106.6(10) . . ?
C32 N8 C40 127.2(11) . . ?
C26 N8 C40 126.2(11) . . ?
C39 N9 C8 103.7(13) . . ?
C39 N9 Co2 131.9(9) . . ?
C8 N9 Co2 123.3(11) . . ?
C39 N10 C12 108.3(12) . . ?
C39 N10 C42 127.1(11) . . ?
C12 N10 C42 124.1(12) . . ?
C4 N11 C29 106.5(16) . . ?
C4 N11 Co2 124.1(15) . . ?
C29 N11 Co2 128.0(9) . . ?
C20 N12 C37 104.5(11) . . ?
C20 N12 C36 130.6(12) . . ?
C37 N12 C36 124.1(11) . . ?
C29 N13 C5 104.7(18) . . ?
C29 N13 C43 130.4(13) . . ?
C5 N13 C43 124.6(19) . . ?
C46 N14 C15 106.0(11) . . ?
C46 N14 Co3 125.5(9) . . ?
C15 N14 Co3 128.4(9) . . ?
C32 N15 C44 105.2(10) . . ?
C32 N15 Co2 128.4(9) . 7_665 ?
C44 N15 Co2 125.7(8) . 7_665 ?
C37 N16 C21 105.3(11) . . ?
C37 N16 Co3 126.4(8) . . ?
C21 N16 Co3 128.2(9) . . ?
N1 C1 N4 120(3) . . ?
N1 C1 C3 41(2) . . ?
N4 C1 C3 80(2) . . ?
N4 C2 C3 99(4) . . ?
N1 C3 C2 111(5) . . ?
N1 C3 C1 39(2) . . ?
C2 C3 C1 73(3) . . ?
N11 C4 C5 109(3) . . ?
N13 C5 C4 105(3) . . ?
C43 C6 C7 120(2) . 4 ?
C43 C7 C6 119(2) . 4 ?
C12 C8 N9 112.2(18) . . ?
C10 C9 C16 121.4(17) . . ?
C10 C9 N4 119.5(18) . . ?
C16 C9 N4 118.9(18) . . ?
C9 C10 C11 120.3(17) . . ?
C47 C11 C10 117.6(17) . . ?
C8 C12 N10 103.2(17) . . ?
C25 C13 N2 105.0(14) . . ?
N5 C14 C23 105.9(14) . . ?
C38 C15 N14 108.6(13) . . ?
C19 C16 C9 118.4(17) . . ?
C28 C17 C31 117.9(14) . 4_655 ?
C33 C18 C42 118.4(13) . . ?
C16 C19 C47 120.8(16) . . ?
C21 C20 N12 109.3(13) . . ?
C20 C21 N16 108.0(13) . . ?
C40 C22 C35 119.3(13) . . ?
C14 C23 N3 110.7(15) . . ?
C27 C24 C45 119.5(15) . 8_575 ?
N7 C25 C13 109.6(15) . . ?
C44 C26 N8 106.4(11) . . ?
C24 C27 C34 120.3(14) . 8_575 ?
C24 C27 N6 120.8(15) . . ?
C34 C27 N6 118.9(13) 8_575 . ?
C31 C28 C17 121.6(13) . . ?
C31 C28 N5 117.6(12) . . ?
C17 C28 N5 120.8(12) . . ?
N11 C29 N13 114.0(12) . . ?
N7 C30 N2 111.5(12) . . ?
C28 C31 C17 120.4(14) . 4_655 ?
N15 C32 N8 112.6(11) . . ?
C40 C33 C18 120.3(13) . . ?
C48 C34 C27 119.0(14) . 8_576 ?
C42 C35 C22 119.8(13) . . ?
C45 C36 C48 120.6(13) . . ?
C45 C36 N12 120.5(12) . . ?
C48 C36 N12 118.9(13) . . ?
N16 C37 N12 112.9(11) . . ?
N6 C38 C15 106.5(13) . . ?
N9 C39 N10 112.6(11) . . ?
C33 C40 C22 121.9(12) . . ?
C33 C40 N8 120.7(12) . . ?
C22 C40 N8 117.2(12) . . ?
N3 C41 N5 112.3(11) . . ?
C35 C42 C18 119.9(12) . . ?
C35 C42 N10 119.9(12) . . ?
C18 C42 N10 120.2(12) . . ?
C7 C43 C6 116.3(16) . . ?
C7 C43 N13 121.3(15) . . ?
C6 C43 N13 120.0(15) . . ?
C26 C44 N15 109.3(11) . . ?
C36 C45 C24 120.2(13) . 8_576 ?
N14 C46 N6 111.6(12) . . ?
C11 C47 C19 121.4(15) . . ?
C11 C47 N2 116.8(14) . . ?
C19 C47 N2 121.6(13) . . ?
C34 C48 C36 120.3(15) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.22
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         3.366
_refine_diff_density_min         -3.547
_refine_diff_density_rms         0.336
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound_2
_database_code_depnum_ccdc_archive 'CCDC 1474351'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-06-28 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 H34 Co2 Ge N12 O42 W12'
_chemical_formula_weight         3703.29

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   26.8635(13)
_cell_length_b                   20.0627(10)
_cell_length_c                   13.1107(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7066.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8611
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.48

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6496
_exptl_absorpt_coefficient_mu    20.411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems. These atoms are as follows: Ge1 O7 O23 O25 O22 C17 C3 C16 O9 and O13. These restraint refinement leads to a relatively high restraint value 54. In the final refinement, the H atoms on coordination water molecules cannot be found from the residual peaks and directly included into the final molecular formula. Some free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. The SQUEEZE program indicates that there are at least fourteen solvent water molecules in the crystal structure. These water molecules were directly included in the final molecular formula based on the elemental analysis, and SQUEEZE analysis. The highest residual peak 6.08 eA-3 should be assigned to free water molecule.
;

_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  'phi and omega scans'
_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            46878
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         27.31
_reflns_number_total             8191
_reflns_number_gt                6348
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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. 
The reported refinements are of the guest-free structures using the *.hkp files produced by using the SQUEEZE routine. The SQUEEZE programe indicats that there is two solvent water molecules in the crystal structure. 
;

_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)+(0.0587P)²+784.9310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8191
_refine_ls_number_parameters     481
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1834
_refine_ls_wR_factor_gt          0.1701
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.017 0.250 0.052 263.8 1050.4
2 0.017 0.750 -0.053 263.8 977.4
3 0.483 0.250 0.447 263.9 997.7
4 0.517 0.750 0.552 263.9 993.2
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 0.26675(3) 0.16699(4) 0.87631(6) 0.0234(2) Uani 1 1 d . . .
W2 W 0.26703(3) 0.07466(4) 1.12006(6) 0.02052(19) Uani 1 1 d . . .
W3 W 0.26819(3) 0.15799(4) 1.33997(6) 0.0222(2) Uani 1 1 d . . .
W4 W 0.36929(3) 0.15759(4) 1.19155(6) 0.01984(19) Uani 1 1 d . . .
W6 W 0.15442(3) 0.16649(4) 1.03839(6) 0.02002(19) Uani 1 1 d . . .
W7 W 0.15514(4) 0.2500 1.25969(9) 0.0207(2) Uani 1 2 d S . .
W5 W 0.36851(4) 0.2500 0.94782(9) 0.0230(3) Uani 1 2 d S . .
Ge1 Ge 0.26413(8) 0.2500 1.11195(17) 0.0044(4) Uani 1 2 d SU . .
Co1 Co 0.25868(14) 0.10972(19) 0.6135(3) 0.0421(8) Uani 1 1 d . . .
O1 O 0.3753(5) 0.1845(7) 1.0536(10) 0.020(3) Uani 1 1 d . . .
O2 O 0.2012(4) 0.1074(6) 1.1031(9) 0.015(2) Uani 1 1 d . . .
O3 O 0.2791(4) 0.1083(6) 0.9863(9) 0.015(3) Uani 1 1 d . . .
O4 O 0.3369(5) 0.0759(6) 1.1457(10) 0.018(3) Uani 1 1 d . . .
O6 O 0.2592(5) -0.0081(7) 1.1025(12) 0.026(3) Uani 1 1 d . . .
O7 O 0.2601(5) 0.1272(7) 1.4601(11) 0.027(3) Uani 1 1 d U . .
O8 O 0.3386(4) 0.1442(6) 1.3243(10) 0.017(3) Uani 1 1 d . . .
O10 O 0.2597(5) 0.1139(7) 0.7743(11) 0.026(3) Uani 1 1 d . . .
O11 O 0.4275(5) 0.1285(7) 1.2184(11) 0.023(3) Uani 1 1 d . . .
O12 O 0.3376(5) 0.1829(7) 0.8645(10) 0.022(3) Uani 1 1 d . . .
O14 O 0.2575(5) 0.0762(6) 1.2642(9) 0.016(3) Uani 1 1 d . . .
O15 O 0.2031(5) 0.1857(7) 1.3066(9) 0.017(3) Uani 1 1 d . . .
O16 O 0.2860(4) 0.1801(6) 1.1741(9) 0.013(2) Uani 1 1 d . . .
O17 O 0.2013(5) 0.1716(6) 0.9317(9) 0.016(3) Uani 1 1 d . . .
O18 O 0.4272(8) 0.2500 0.8962(15) 0.030(5) Uani 1 2 d S . .
O19 O 0.1249(6) 0.2500 0.9965(14) 0.015(4) Uani 1 2 d S . .
O20 O 0.1139(7) 0.2500 1.3584(15) 0.025(4) Uani 1 2 d S . .
O21 O 0.1107(5) 0.1135(7) 0.9902(12) 0.027(3) Uani 1 1 d . . .
O22 O 0.2551(7) 0.2500 0.8032(15) 0.021(4) Uani 1 2 d SU . .
O23 O 0.2822(7) 0.2500 1.3621(14) 0.018(4) Uani 1 2 d SU . .
O24 O 0.3755(6) 0.2500 1.2241(15) 0.019(4) Uani 1 2 d S . .
O13 O 0.1271(4) 0.1820(6) 1.1731(9) 0.015(2) Uani 1 1 d U . .
N1 N 0.3363(8) 0.0820(12) 0.6106(16) 0.043(5) Uani 1 1 d . . .
N2 N 0.1804(7) 0.1240(12) 0.6155(15) 0.042(5) Uani 1 1 d . . .
N3 N 0.4182(8) 0.0709(11) 0.6484(15) 0.038(5) Uani 1 1 d . . .
N4 N 0.0996(8) 0.1188(11) 0.6547(18) 0.043(5) Uani 1 1 d . . .
C1 C 0.3727(11) 0.0984(13) 0.674(2) 0.047(7) Uani 1 1 d . . .
H1 H 0.3680 0.1256 0.7311 0.057 Uiso 1 1 calc R . .
C2 C 0.4657(10) 0.0825(15) 0.700(2) 0.047(7) Uani 1 1 d . . .
C3 C 0.4719(13) 0.1378(18) 0.749(3) 0.064(8) Uani 1 1 d U . .
H3 H 0.4467 0.1696 0.7507 0.076 Uiso 1 1 calc R . .
C4 C 0.4081(14) 0.0313(16) 0.564(2) 0.065(9) Uani 1 1 d . . .
H4 H 0.4312 0.0062 0.5280 0.078 Uiso 1 1 calc R . .
C5 C 0.3594(11) 0.0357(13) 0.544(2) 0.049(7) Uani 1 1 d . . .
H5 H 0.3430 0.0117 0.4938 0.059 Uiso 1 1 calc R . .
C6 C 0.5024(12) 0.0365(18) 0.694(3) 0.070(10) Uani 1 1 d . . .
H6 H 0.4970 -0.0036 0.6601 0.084 Uiso 1 1 calc R . .
C7 C 0.1453(12) 0.1016(18) 0.683(2) 0.064(9) Uani 1 1 d . . .
H7 H 0.1526 0.0775 0.7419 0.077 Uiso 1 1 calc R . .
C8 C 0.1535(11) 0.1562(15) 0.538(2) 0.049(7) Uani 1 1 d . . .
H8 H 0.1675 0.1751 0.4798 0.059 Uiso 1 1 calc R . .
C9 C 0.5479(11) 0.0493(16) 0.739(3) 0.065(10) Uani 1 1 d . . .
H9 H 0.5742 0.0197 0.7305 0.078 Uiso 1 1 calc R . .
C10 C 0.0540(10) 0.1054(14) 0.705(2) 0.045(6) Uani 1 1 d . . .
C11 C 0.5163(12) 0.1492(17) 0.799(3) 0.071(11) Uani 1 1 d . . .
H11 H 0.5203 0.1881 0.8364 0.085 Uiso 1 1 calc R . .
C12 C 0.1047(8) 0.1555(13) 0.5597(17) 0.034(5) Uani 1 1 d . . .
H12 H 0.0793 0.1747 0.5217 0.040 Uiso 1 1 calc R . .
N5 N 0.0902(5) 0.0183(8) 0.3964(12) 0.019(3) Uani 1 1 d . . .
N6 N 0.1467(6) 0.0557(10) 0.2938(15) 0.030(4) Uani 1 1 d . . .
C13 C 0.1697(9) 0.0079(11) 0.3564(18) 0.035(6) Uani 1 1 d . . .
H13 H 0.2029 -0.0052 0.3550 0.042 Uiso 1 1 calc R . .
C14 C 0.1334(8) -0.0154(13) 0.4193(17) 0.033(5) Uani 1 1 d . . .
H14 H 0.1371 -0.0482 0.4688 0.040 Uiso 1 1 calc R . .
C15 C 0.0441(7) 0.0085(10) 0.4481(15) 0.022(4) Uani 1 1 d . . .
C16 C 0.0070(11) 0.0549(17) 0.446(2) 0.056(7) Uani 1 1 d U . .
H16 H 0.0112 0.0932 0.4072 0.068 Uiso 1 1 calc R . .
C17 C 0.0352(11) -0.0470(15) 0.502(2) 0.052(7) Uani 1 1 d U . .
H17 H 0.0590 -0.0807 0.5025 0.062 Uiso 1 1 calc R . .
C18 C 0.0997(8) 0.0617(11) 0.3181(16) 0.027(5) Uani 1 1 d . . .
H18 H 0.0768 0.0902 0.2876 0.033 Uiso 1 1 calc R . .
O5 O 0.2003(6) 0.2500 1.1116(12) 0.009(3) Uani 1 2 d S . .
O9 O 0.2851(6) 0.2500 0.9883(12) 0.008(3) Uani 1 2 d SU . .


_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 O10 1.720(14) . ?
W1 O3 1.891(13) . ?
W1 O17 1.905(12) . ?
W1 O12 1.936(13) . ?
W1 O22 1.947(10) . ?
W1 O9 2.274(11) . ?
W2 O6 1.689(14) . ?
W2 O2 1.898(12) . ?
W2 O4 1.908(13) . ?
W2 O14 1.907(12) . ?
W2 O3 1.907(12) . ?
W2 O16 2.289(12) . ?
W3 O7 1.706(15) . ?
W3 O15 1.887(13) . ?
W3 O23 1.906(5) . ?
W3 O8 1.921(12) . ?
W3 O14 1.940(13) . ?
W3 O16 2.271(12) . ?
W4 O11 1.705(12) . ?
W4 O1 1.895(13) . ?
W4 O24 1.910(5) . ?
W4 O8 1.945(13) . ?
W4 O4 1.950(13) . ?
W4 O16 2.293(12) . ?
W6 O21 1.706(13) . ?
W6 O17 1.884(12) . ?
W6 O2 1.926(12) . ?
W6 O19 1.934(9) . ?
W6 O13 1.938(12) . ?
W6 O5 2.291(10) . ?
W7 O20 1.704(19) . ?
W7 O15 1.924(13) 8_565 ?
W7 O15 1.924(13) . ?
W7 O13 1.929(12) . ?
W7 O13 1.929(12) 8_565 ?
W7 O5 2.289(16) . ?
W5 O18 1.71(2) . ?
W5 O1 1.919(14) 8_565 ?
W5 O1 1.919(14) . ?
W5 O12 1.923(14) . ?
W5 O12 1.923(14) 8_565 ?
W5 O9 2.304(15) . ?
Ge1 O9 1.716(16) . ?
Ge1 O5 1.715(15) . ?
Ge1 O16 1.725(12) 8_565 ?
Ge1 O16 1.725(12) . ?
Co1 O7 2.042(15) 1_554 ?
Co1 O6 2.101(14) 2_554 ?
Co1 O10 2.109(14) . ?
Co1 N2 2.12(2) . ?
Co1 N1 2.16(2) . ?
O6 Co1 2.101(14) 2 ?
O7 Co1 2.042(15) 1_556 ?
O19 W6 1.934(9) 8_565 ?
O22 W1 1.947(10) 8_565 ?
O23 W3 1.906(5) 8_565 ?
O24 W4 1.910(5) 8_565 ?
N1 C1 1.33(3) . ?
N1 C5 1.41(4) . ?
N2 C7 1.37(4) . ?
N2 C8 1.41(3) . ?
N3 C1 1.38(3) . ?
N3 C4 1.39(3) . ?
N3 C2 1.46(3) . ?
N4 C7 1.33(3) . ?
N4 C10 1.42(3) . ?
N4 C12 1.45(3) . ?
C2 C3 1.29(4) . ?
C2 C6 1.35(4) . ?
C3 C11 1.38(4) . ?
C4 C5 1.34(4) . ?
C6 C9 1.38(4) . ?
C8 C12 1.34(3) . ?
C9 C10 1.35(4) 6_657 ?
C10 C9 1.35(4) 6_557 ?
C10 C11 1.34(4) 6_557 ?
C11 C10 1.34(4) 6_657 ?
N5 C18 1.37(3) . ?
N5 C14 1.38(3) . ?
N5 C15 1.43(2) . ?
N6 C18 1.31(3) . ?
N6 C13 1.41(3) . ?
C13 C14 1.36(3) . ?
C15 C17 1.34(3) . ?
C15 C16 1.36(4) . ?
C16 C17 1.33(4) 5_556 ?
C17 C16 1.33(4) 5_556 ?
O5 W6 2.291(10) 8_565 ?
O9 W1 2.274(11) 8_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 W1 O3 103.1(6) . . ?
O10 W1 O17 103.0(6) . . ?
O3 W1 O17 84.4(5) . . ?
O10 W1 O12 98.5(6) . . ?
O3 W1 O12 89.5(5) . . ?
O17 W1 O12 158.5(5) . . ?
O10 W1 O22 97.4(7) . . ?
O3 W1 O22 159.4(6) . . ?
O17 W1 O22 89.9(7) . . ?
O12 W1 O22 88.7(7) . . ?
O10 W1 O9 168.3(6) . . ?
O3 W1 O9 85.7(5) . . ?
O17 W1 O9 85.3(5) . . ?
O12 W1 O9 73.6(5) . . ?
O22 W1 O9 74.1(6) . . ?
O6 W2 O2 102.0(6) . . ?
O6 W2 O4 99.2(6) . . ?
O2 W2 O4 158.8(5) . . ?
O6 W2 O14 97.7(6) . . ?
O2 W2 O14 89.2(5) . . ?
O4 W2 O14 87.5(5) . . ?
O6 W2 O3 104.1(6) . . ?
O2 W2 O3 85.9(5) . . ?
O4 W2 O3 89.4(5) . . ?
O14 W2 O3 158.2(5) . . ?
O6 W2 O16 168.1(6) . . ?
O2 W2 O16 85.7(5) . . ?
O4 W2 O16 73.4(5) . . ?
O14 W2 O16 73.0(5) . . ?
O3 W2 O16 85.4(5) . . ?
O7 W3 O15 101.7(6) . . ?
O7 W3 O23 103.6(7) . . ?
O15 W3 O23 86.2(7) . . ?
O7 W3 O8 99.9(6) . . ?
O15 W3 O8 158.4(5) . . ?
O23 W3 O8 87.8(7) . . ?
O7 W3 O14 98.5(6) . . ?
O15 W3 O14 89.6(5) . . ?
O23 W3 O14 157.9(7) . . ?
O8 W3 O14 88.2(5) . . ?
O7 W3 O16 169.1(6) . . ?
O15 W3 O16 85.2(5) . . ?
O23 W3 O16 85.1(6) . . ?
O8 W3 O16 73.6(5) . . ?
O14 W3 O16 72.9(5) . . ?
O11 W4 O1 102.5(6) . . ?
O11 W4 O24 101.9(7) . . ?
O1 W4 O24 85.9(7) . . ?
O11 W4 O8 99.0(6) . . ?
O1 W4 O8 158.4(5) . . ?
O24 W4 O8 88.4(7) . . ?
O11 W4 O4 100.6(6) . . ?
O1 W4 O4 89.1(6) . . ?
O24 W4 O4 157.5(6) . . ?
O8 W4 O4 88.3(5) . . ?
O11 W4 O16 169.1(6) . . ?
O1 W4 O16 86.1(5) . . ?
O24 W4 O16 85.2(6) . . ?
O8 W4 O16 72.7(5) . . ?
O4 W4 O16 72.6(5) . . ?
O21 W6 O17 102.6(7) . . ?
O21 W6 O2 103.2(6) . . ?
O17 W6 O2 85.7(5) . . ?
O21 W6 O19 98.8(6) . . ?
O17 W6 O19 90.9(6) . . ?
O2 W6 O19 158.0(6) . . ?
O21 W6 O13 100.2(6) . . ?
O17 W6 O13 157.1(5) . . ?
O2 W6 O13 86.9(5) . . ?
O19 W6 O13 87.9(7) . . ?
O21 W6 O5 169.0(6) . . ?
O17 W6 O5 85.0(6) . . ?
O2 W6 O5 85.1(5) . . ?
O19 W6 O5 72.9(5) . . ?
O13 W6 O5 72.8(5) . . ?
O20 W7 O15 101.1(6) . 8_565 ?
O20 W7 O15 101.1(6) . . ?
O15 W7 O15 84.3(8) 8_565 . ?
O20 W7 O13 101.1(6) . . ?
O15 W7 O13 157.6(5) 8_565 . ?
O15 W7 O13 88.6(5) . . ?
O20 W7 O13 101.1(6) . 8_565 ?
O15 W7 O13 88.6(5) 8_565 8_565 ?
O15 W7 O13 157.6(5) . 8_565 ?
O13 W7 O13 90.0(7) . 8_565 ?
O20 W7 O5 171.4(8) . . ?
O15 W7 O5 85.2(5) 8_565 . ?
O15 W7 O5 85.2(5) . . ?
O13 W7 O5 73.0(4) . . ?
O13 W7 O5 73.0(4) 8_565 . ?
O18 W5 O1 101.4(6) . 8_565 ?
O18 W5 O1 101.4(6) . . ?
O1 W5 O1 86.4(8) 8_565 . ?
O18 W5 O12 99.9(6) . . ?
O1 W5 O12 158.6(5) 8_565 . ?
O1 W5 O12 88.4(6) . . ?
O18 W5 O12 99.9(6) . 8_565 ?
O1 W5 O12 88.4(6) 8_565 8_565 ?
O1 W5 O12 158.6(5) . 8_565 ?
O12 W5 O12 88.9(8) . 8_565 ?
O18 W5 O9 170.1(8) . . ?
O1 W5 O9 85.8(5) 8_565 . ?
O1 W5 O9 85.8(5) . . ?
O12 W5 O9 73.2(5) . . ?
O12 W5 O9 73.2(5) 8_565 . ?
O9 Ge1 O5 109.0(8) . . ?
O9 Ge1 O16 109.5(5) . 8_565 ?
O5 Ge1 O16 110.0(5) . 8_565 ?
O9 Ge1 O16 109.5(5) . . ?
O5 Ge1 O16 110.0(5) . . ?
O16 Ge1 O16 108.8(8) 8_565 . ?
O7 Co1 O6 95.9(6) 1_554 2_554 ?
O7 Co1 O10 167.7(6) 1_554 . ?
O6 Co1 O10 96.4(6) 2_554 . ?
O7 Co1 N2 90.4(7) 1_554 . ?
O6 Co1 N2 84.6(8) 2_554 . ?
O10 Co1 N2 89.7(7) . . ?
O7 Co1 N1 90.5(7) 1_554 . ?
O6 Co1 N1 88.2(7) 2_554 . ?
O10 Co1 N1 90.9(7) . . ?
N2 Co1 N1 172.8(9) . . ?
W4 O1 W5 151.3(8) . . ?
W2 O2 W6 150.8(7) . . ?
W1 O3 W2 153.0(7) . . ?
W2 O4 W4 120.2(7) . . ?
W2 O6 Co1 166.7(10) . 2 ?
W3 O7 Co1 167.0(9) . 1_556 ?
W3 O8 W4 119.6(6) . . ?
W1 O10 Co1 143.4(9) . . ?
W5 O12 W1 119.6(7) . . ?
W2 O14 W3 120.1(6) . . ?
W3 O15 W7 153.1(7) . . ?
Ge1 O16 W3 122.6(6) . . ?
Ge1 O16 W4 122.7(6) . . ?
W3 O16 W4 94.1(4) . . ?
Ge1 O16 W2 122.0(6) . . ?
W3 O16 W2 93.9(4) . . ?
W4 O16 W2 93.8(4) . . ?
W6 O17 W1 153.7(7) . . ?
W6 O19 W6 120.1(9) 8_565 . ?
W1 O22 W1 117.6(10) 8_565 . ?
W3 O23 W3 151.1(10) 8_565 . ?
W4 O24 W4 152.3(11) 8_565 . ?
W7 O13 W6 120.1(6) . . ?
C1 N1 C5 103(2) . . ?
C1 N1 Co1 129.4(19) . . ?
C5 N1 Co1 127.1(16) . . ?
C7 N2 C8 105(2) . . ?
C7 N2 Co1 130.2(17) . . ?
C8 N2 Co1 124.2(17) . . ?
C1 N3 C4 105(2) . . ?
C1 N3 C2 126(2) . . ?
C4 N3 C2 129(2) . . ?
C7 N4 C10 128(3) . . ?
C7 N4 C12 107(2) . . ?
C10 N4 C12 125(2) . . ?
N1 C1 N3 113(2) . . ?
C3 C2 C6 121(3) . . ?
C3 C2 N3 119(3) . . ?
C6 C2 N3 120(2) . . ?
C2 C3 C11 119(3) . . ?
C5 C4 N3 108(2) . . ?
C4 C5 N1 111(2) . . ?
C2 C6 C9 120(3) . . ?
N4 C7 N2 112(2) . . ?
C12 C8 N2 110(2) . . ?
C10 C9 C6 120(3) 6_657 . ?
C9 C10 C11 118(3) 6_557 6_557 ?
C9 C10 N4 121(2) 6_557 . ?
C11 C10 N4 121(3) 6_557 . ?
C10 C11 C3 122(3) 6_657 . ?
C8 C12 N4 106(2) . . ?
C18 N5 C14 108.6(16) . . ?
C18 N5 C15 127.3(16) . . ?
C14 N5 C15 124.1(16) . . ?
C18 N6 C13 110.1(19) . . ?
C14 C13 N6 105.9(19) . . ?
C13 C14 N5 107.6(19) . . ?
C17 C15 C16 117(2) . . ?
C17 C15 N5 121(2) . . ?
C16 C15 N5 122(2) . . ?
C17 C16 C15 122(3) 5_556 . ?
C16 C17 C15 121(3) 5_556 . ?
N6 C18 N5 107.7(18) . . ?
Ge1 O5 W7 121.8(8) . . ?
Ge1 O5 W6 122.6(5) . . ?
W7 O5 W6 94.0(5) . . ?
Ge1 O5 W6 122.6(5) . 8_565 ?
W7 O5 W6 94.0(5) . 8_565 ?
W6 O5 W6 94.0(6) . 8_565 ?
Ge1 O9 W1 122.6(5) . . ?
Ge1 O9 W1 122.6(5) . 8_565 ?
W1 O9 W1 94.2(6) . 8_565 ?
Ge1 O9 W5 122.4(8) . . ?
W1 O9 W5 93.5(5) . . ?
W1 O9 W5 93.5(5) 8_565 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.31
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         6.066
_refine_diff_density_min         -4.206
_refine_diff_density_rms         0.532
####################################################################### 
# 
# 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_compound_3
_database_code_depnum_ccdc_archive 'CCDC 1474352'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-06-28 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 H34 B Co2 N12 O42 W12'
_chemical_formula_weight         3641.47

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'
B B 0.0013 0.0007 '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'
Co Co 0.3494 0.9721 '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           Orthorhombic
_symmetry_space_group_name_H-M   'P n m a'

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

_cell_length_a                   26.780(5)
_cell_length_b                   19.963(5)
_cell_length_c                   12.980(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6939(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6692
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.70

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6420
_exptl_absorpt_coefficient_mu    20.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_T_max  0.001
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems. These atoms are as follows: O19 O18 C6 C16 C18 C3 C17 C8 and O17. These restraint refinement leads to a relatively high restraint value 54. In the previous version, even after a 60-cycle refinement run, the refinement had not fully converged. There is a major problem with the anisotropic vibration parameters for the B1 atom. The reason for the problem may be that the atomic mass of B atom is small, which may probably result in the B with an NDP problem. Therefore, in this version, the B atom in the refinement with unit-occupancy and a fixed (not refined) Uiso value of 0.02. Consequently, with this change a 60-cycle refinement run will give complete convergence. 
In the final refinement, the H atoms on coordination water molecules cannot be found from the residual peaks and directly included into the final molecular formula. Some free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. The SQUEEZE program indicates that there are at least two solvent water molecules in the crystal structure. These two molecules were directly included in the final molecular formula based on the elemental analysis, and SQUEEZE analysis. The highest residual peak 5.55 eA-3 is close to the Co1 positions, which is featureless, and should be due to the "series termination errors". 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'phi and omega scans'
_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            49640
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         28.30
_reflns_number_total             8880
_reflns_number_gt                6433
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8874
_refine_ls_number_parameters     483
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1780
_refine_ls_wR_factor_gt          0.1622
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.466 0.250 0.095 223.2 60.1
2 0.534 0.750 -0.095 223.4 59.3
3 -0.034 0.250 0.405 223.1 61.5
4 0.870 0.750 0.249 19.1 2.9
5 0.370 0.750 0.251 19.0 1.4
6 0.034 0.750 0.595 223.3 60.4
7 0.630 0.250 0.749 19.2 2.3
8 0.130 0.250 0.751 19.3 0.9

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 0.15367(3) 0.2500 -0.74349(7) 0.0204(2) Uani 1 2 d S . .
W2 W 0.15436(2) 0.16726(3) -0.52234(5) 0.02020(16) Uani 1 1 d . . .
W3 W 0.36756(3) 0.2500 -0.43986(7) 0.0198(2) Uani 1 2 d S . .
W4 W 0.26523(2) 0.07694(3) -0.60737(5) 0.02123(16) Uani 1 1 d . . .
W5 W 0.26661(2) 0.16761(3) -0.36542(5) 0.02216(16) Uani 1 1 d . . .
W6 W 0.26503(2) 0.15932(4) -0.82678(5) 0.02631(18) Uani 1 1 d . . .
W7 W 0.36667(2) 0.15871(3) -0.68231(5) 0.02073(16) Uani 1 1 d . . .
Co1 Co 0.24085(12) -0.10895(17) -0.6009(2) 0.0534(8) Uani 1 1 d . . .
B1 B 0.2628(8) 0.2500 -0.599(2) 0.020 Uiso 1 2 d S . .
O1 O 0.1258(5) 0.2500 -0.4794(11) 0.020(3) Uani 1 2 d S . .
OW1 O 0.5118(9) 0.2500 -0.536(2) 0.078(8) Uani 1 2 d S . .
O2 O 0.1988(3) 0.1062(5) -0.5885(8) 0.019(2) Uani 1 1 d . . .
O3 O 0.3759(4) 0.1824(5) -0.5441(7) 0.017(2) Uani 1 1 d . . .
O4 O 0.2552(5) 0.2500 -0.2929(11) 0.023(3) Uani 1 2 d S . .
O24 O 0.2389(4) -0.1159(6) -0.7626(8) 0.026(2) Uani 1 1 d . . .
O5 O 0.2425(4) -0.1281(7) -0.4470(9) 0.035(3) Uani 1 1 d . . .
O6 O 0.4255(5) 0.2500 -0.3838(13) 0.031(4) Uani 1 2 d S . .
O7 O 0.2006(4) 0.1695(5) -0.4117(7) 0.018(2) Uani 1 1 d . . .
O8 O 0.3365(4) 0.1843(5) -0.3557(8) 0.019(2) Uani 1 1 d . . .
O9 O 0.3363(4) 0.0779(5) -0.6350(9) 0.025(2) Uani 1 1 d . . .
O10 O 0.1992(3) 0.1848(5) -0.7970(8) 0.022(2) Uani 1 1 d . . .
O11 O 0.4242(4) 0.1274(6) -0.7110(9) 0.031(3) Uani 1 1 d . . .
O12 O 0.1262(4) 0.1823(5) -0.6562(8) 0.018(2) Uani 1 1 d . . .
O13 O 0.3355(3) 0.1452(5) -0.8120(8) 0.020(2) Uani 1 1 d . . .
O14 O 0.2782(4) 0.1057(5) -0.4703(8) 0.018(2) Uani 1 1 d . . .
O15 O 0.1105(4) 0.1144(5) -0.4761(9) 0.026(2) Uani 1 1 d . . .
O16 O 0.2543(4) 0.0780(6) -0.7520(8) 0.024(2) Uani 1 1 d . . .
O17 O 0.2825(5) 0.2500 -0.4867(11) 0.015(3) Uani 1 2 d SU . .
O18 O 0.2063(5) 0.2500 -0.5972(11) 0.016(3) Uani 1 2 d SU . .
O19 O 0.3758(5) 0.2500 -0.7180(12) 0.020(3) Uani 1 2 d SU . .
O20 O 0.2777(5) 0.2500 -0.8572(11) 0.025(4) Uani 1 2 d S . .
O21 O 0.2814(4) 0.1868(5) -0.6550(8) 0.017(2) Uani 1 1 d . . .
O22 O 0.2580(4) -0.0078(5) -0.5892(9) 0.026(2) Uani 1 1 d . . .
O23 O 0.1108(6) 0.2500 -0.8404(12) 0.027(4) Uani 1 2 d S . .
C1 C 0.4573(5) -0.0085(7) -0.4466(12) 0.021(3) Uani 1 1 d . . .
C2 C 0.0341(7) -0.0827(9) -0.6857(14) 0.035(4) Uani 1 1 d . . .
C3 C 0.0264(8) -0.1435(12) -0.7376(18) 0.053(5) Uani 1 1 d U . .
H3A H 0.0501 -0.1776 -0.7353 0.063 Uiso 1 1 calc R . .
C4 C -0.0017(8) -0.0329(9) -0.6853(16) 0.046(5) Uani 1 1 d . . .
H4A H 0.0035 0.0069 -0.6496 0.055 Uiso 1 1 calc R . .
C5 C 0.4654(5) 0.0504(8) -0.4945(15) 0.033(4) Uani 1 1 d . . .
H5 H 0.4426 0.0855 -0.4900 0.040 Uiso 1 1 calc R . .
C6 C 0.0873(10) -0.0341(13) -0.556(2) 0.064(6) Uani 1 1 d U . .
H6A H 0.0630 -0.0092 -0.5227 0.077 Uiso 1 1 calc R . .
C7 C 0.4032(5) -0.0610(9) -0.3162(14) 0.034(4) Uani 1 1 d . . .
H7A H 0.4268 -0.0905 -0.2898 0.041 Uiso 1 1 calc R . .
C8 C 0.3681(6) 0.0149(9) -0.4093(15) 0.034(4) Uani 1 1 d U . .
H8A H 0.3633 0.0469 -0.4603 0.041 Uiso 1 1 calc R . .
C9 C 0.3328(6) -0.0075(8) -0.3413(15) 0.032(4) Uani 1 1 d . . .
H9A H 0.3000 0.0075 -0.3345 0.039 Uiso 1 1 calc R . .
C10 C 0.5087(7) 0.0563(11) -0.5501(15) 0.044(5) Uani 1 1 d . . .
H10 H 0.5143 0.0955 -0.5870 0.052 Uiso 1 1 calc R . .
C11 C 0.1378(9) -0.0380(11) -0.5290(15) 0.051(6) Uani 1 1 d . . .
H11A H 0.1525 -0.0144 -0.4751 0.062 Uiso 1 1 calc R . .
C12 C 0.1247(7) -0.0989(10) -0.6666(14) 0.039(5) Uani 1 1 d . . .
H12A H 0.1292 -0.1248 -0.7254 0.046 Uiso 1 1 calc R . .
C13 C -0.0188(9) -0.1510(12) -0.794(2) 0.075(9) Uani 1 1 d . . .
H13A H -0.0237 -0.1893 -0.8333 0.090 Uiso 1 1 calc R . .
C14 C -0.0476(7) -0.0442(10) -0.7422(15) 0.042(5) Uani 1 1 d . . .
H14A H -0.0721 -0.0112 -0.7455 0.050 Uiso 1 1 calc R . .
C15 C -0.0542(7) -0.1046(10) -0.7909(14) 0.036(4) Uani 1 1 d . . .
C16 C -0.1467(8) -0.0985(11) -0.8200(17) 0.047(5) Uani 1 1 d U . .
H16A H -0.1553 -0.0742 -0.7615 0.056 Uiso 1 1 calc R . .
C17 C -0.1019(7) -0.1553(9) -0.9349(15) 0.034(4) Uani 1 1 d U . .
H17A H -0.0761 -0.1760 -0.9707 0.040 Uiso 1 1 calc R . .
N2 N -0.1810(7) -0.1219(9) -0.8921(13) 0.051(5) Uani 1 1 d . . .
N1 N -0.0991(6) -0.1156(8) -0.8455(12) 0.039(4) Uani 1 1 d . . .
C18 C -0.1528(7) -0.1561(10) -0.9565(17) 0.045(5) Uani 1 1 d U . .
H18A H -0.1660 -0.1791 -1.0126 0.054 Uiso 1 1 calc R . .
N3 N 0.4114(4) -0.0180(6) -0.3890(10) 0.021(3) Uani 1 1 d . . .
N4 N 0.1631(7) -0.0819(9) -0.5937(13) 0.049(5) Uani 1 1 d . . .
N5 N 0.0805(5) -0.0712(8) -0.6360(13) 0.040(4) Uani 1 1 d . . .
N6 N 0.3561(5) -0.0568(8) -0.2850(12) 0.034(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O23 1.703(15) . ?
W1 O12 1.911(10) . ?
W1 O12 1.911(10) 8_565 ?
W1 O10 1.914(10) 8_565 ?
W1 O10 1.914(10) . ?
W1 O18 2.364(14) . ?
W2 O15 1.689(10) . ?
W2 O7 1.897(10) . ?
W2 O1 1.904(7) . ?
W2 O2 1.909(10) . ?
W2 O12 1.917(10) . ?
W2 O18 2.367(10) . ?
W3 O6 1.714(15) . ?
W3 O8 1.898(10) . ?
W3 O8 1.898(10) 8_565 ?
W3 O3 1.924(10) . ?
W3 O3 1.924(10) 8_565 ?
W3 O17 2.358(13) . ?
W4 O22 1.718(11) . ?
W4 O14 1.902(10) . ?
W4 O2 1.887(9) . ?
W4 O16 1.901(11) . ?
W4 O9 1.936(10) . ?
W4 O21 2.320(10) . ?
W5 O24 1.693(11) 2 ?
W5 O7 1.868(10) . ?
W5 O14 1.865(10) . ?
W5 O8 1.906(10) . ?
W5 O4 1.919(7) . ?
W5 O17 2.316(10) . ?
W6 O5 1.693(11) 2_554 ?
W6 O10 1.876(10) . ?
W6 O20 1.883(4) . ?
W6 O16 1.914(12) . ?
W6 O13 1.918(9) . ?
W6 O21 2.338(10) . ?
W7 O11 1.705(10) . ?
W7 O3 1.872(9) . ?
W7 O19 1.896(4) . ?
W7 O13 1.898(10) . ?
W7 O9 1.908(11) . ?
W7 O21 2.378(10) . ?
Co1 O5 2.034(12) . ?
Co1 O22 2.077(11) . ?
Co1 O24 2.105(11) . ?
Co1 N2 2.111(18) 6_654 ?
Co1 N4 2.153(19) . ?
B1 O21 1.535(17) . ?
B1 O21 1.535(17) 8_565 ?
B1 O18 1.51(3) . ?
B1 O17 1.56(3) . ?
O1 W2 1.904(7) 8_565 ?
O4 W5 1.919(7) 8_565 ?
O24 W5 1.693(11) 2_554 ?
O5 W6 1.693(11) 2 ?
O17 W5 2.316(10) 8_565 ?
O18 W2 2.367(10) 8_565 ?
O19 W7 1.896(4) 8_565 ?
O20 W6 1.883(4) 8_565 ?
C1 C10 1.32(2) 5_654 ?
C1 C5 1.35(2) . ?
C1 N3 1.452(19) . ?
C2 C3 1.40(3) . ?
C2 C4 1.38(3) . ?
C2 N5 1.42(2) . ?
C3 C13 1.42(3) . ?
C4 C14 1.45(3) . ?
C5 C10 1.37(2) . ?
C6 N5 1.28(3) . ?
C6 C11 1.40(3) . ?
C7 N6 1.33(2) . ?
C7 N3 1.30(2) . ?
C8 C9 1.37(2) . ?
C8 N3 1.36(2) . ?
C9 N6 1.38(2) . ?
C10 C1 1.32(2) 5_654 ?
C11 N4 1.39(3) . ?
C12 N5 1.36(2) . ?
C12 N4 1.44(2) . ?
C13 C15 1.32(3) . ?
C14 C15 1.37(3) . ?
C15 N1 1.41(2) . ?
C16 N1 1.36(2) . ?
C16 N2 1.39(3) . ?
C17 C18 1.39(3) . ?
C17 N1 1.41(2) . ?
N2 C18 1.32(2) . ?
N2 Co1 2.111(18) 6_554 ?

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
O23 W1 O12 100.3(5) . . ?
O23 W1 O12 100.3(5) . 8_565 ?
O12 W1 O12 90.0(6) . 8_565 ?
O23 W1 O10 99.3(5) . 8_565 ?
O12 W1 O10 160.3(4) . 8_565 ?
O12 W1 O10 88.8(4) 8_565 8_565 ?
O23 W1 O10 99.3(5) . . ?
O12 W1 O10 88.8(4) . . ?
O12 W1 O10 160.3(4) 8_565 . ?
O10 W1 O10 85.8(6) 8_565 . ?
O23 W1 O18 174.2(6) . . ?
O12 W1 O18 75.7(4) . . ?
O12 W1 O18 75.7(4) 8_565 . ?
O10 W1 O18 84.9(4) 8_565 . ?
O10 W1 O18 84.9(4) . . ?
O15 W2 O7 101.5(5) . . ?
O15 W2 O1 99.2(5) . . ?
O7 W2 O1 91.2(5) . . ?
O15 W2 O2 101.2(5) . . ?
O7 W2 O2 87.1(4) . . ?
O1 W2 O2 159.5(5) . . ?
O15 W2 O12 98.4(5) . . ?
O7 W2 O12 159.9(4) . . ?
O1 W2 O12 88.3(5) . . ?
O2 W2 O12 86.5(4) . . ?
O15 W2 O18 171.9(5) . . ?
O7 W2 O18 84.9(4) . . ?
O1 W2 O18 75.6(4) . . ?
O2 W2 O18 84.0(4) . . ?
O12 W2 O18 75.5(4) . . ?
O6 W3 O8 98.8(5) . . ?
O6 W3 O8 98.8(5) . 8_565 ?
O8 W3 O8 87.4(6) . 8_565 ?
O6 W3 O3 101.1(5) . . ?
O8 W3 O3 88.4(4) . . ?
O8 W3 O3 160.1(4) 8_565 . ?
O6 W3 O3 101.1(5) . 8_565 ?
O8 W3 O3 160.1(4) . 8_565 ?
O8 W3 O3 88.4(4) 8_565 8_565 ?
O3 W3 O3 89.0(6) . 8_565 ?
O6 W3 O17 169.8(7) . . ?
O8 W3 O17 74.0(4) . . ?
O8 W3 O17 74.0(4) 8_565 . ?
O3 W3 O17 86.1(4) . . ?
O3 W3 O17 86.1(4) 8_565 . ?
O22 W4 O14 100.9(5) . . ?
O22 W4 O2 100.4(5) . . ?
O14 W4 O2 87.6(4) . . ?
O22 W4 O16 97.4(5) . . ?
O14 W4 O16 161.7(5) . . ?
O2 W4 O16 88.8(4) . . ?
O22 W4 O9 98.4(5) . . ?
O14 W4 O9 89.4(4) . . ?
O2 W4 O9 161.2(4) . . ?
O16 W4 O9 88.2(4) . . ?
O22 W4 O21 171.2(5) . . ?
O14 W4 O21 86.0(4) . . ?
O2 W4 O21 85.3(4) . . ?
O16 W4 O21 75.9(4) . . ?
O9 W4 O21 76.0(4) . . ?
O24 W5 O7 100.6(5) 2 . ?
O24 W5 O14 100.7(5) 2 . ?
O7 W5 O14 86.4(4) . . ?
O24 W5 O8 98.0(5) 2 . ?
O7 W5 O8 161.4(4) . . ?
O14 W5 O8 90.0(4) . . ?
O24 W5 O4 97.0(5) 2 . ?
O7 W5 O4 89.4(5) . . ?
O14 W5 O4 162.3(5) . . ?
O8 W5 O4 88.5(5) . . ?
O24 W5 O17 169.8(5) 2 . ?
O7 W5 O17 86.6(4) . . ?
O14 W5 O17 86.8(4) . . ?
O8 W5 O17 74.9(4) . . ?
O4 W5 O17 75.8(4) . . ?
O5 W6 O10 100.2(5) 2_554 . ?
O5 W6 O20 100.5(7) 2_554 . ?
O10 W6 O20 87.2(5) . . ?
O5 W6 O16 97.8(6) 2_554 . ?
O10 W6 O16 89.1(4) . . ?
O20 W6 O16 161.6(5) . . ?
O5 W6 O13 99.0(5) 2_554 . ?
O10 W6 O13 160.8(4) . . ?
O20 W6 O13 89.2(5) . . ?
O16 W6 O13 88.4(4) . . ?
O5 W6 O21 171.2(5) 2_554 . ?
O10 W6 O21 85.2(4) . . ?
O20 W6 O21 86.6(5) . . ?
O16 W6 O21 75.2(4) . . ?
O13 W6 O21 75.8(4) . . ?
O11 W7 O3 100.5(5) . . ?
O11 W7 O19 100.5(6) . . ?
O3 W7 O19 88.5(5) . . ?
O11 W7 O13 98.7(5) . . ?
O3 W7 O13 160.8(4) . . ?
O19 W7 O13 88.7(5) . . ?
O11 W7 O9 98.4(5) . . ?
O3 W7 O9 87.8(5) . . ?
O19 W7 O9 161.1(5) . . ?
O13 W7 O9 88.7(5) . . ?
O11 W7 O21 170.9(4) . . ?
O3 W7 O21 85.7(4) . . ?
O19 W7 O21 86.2(5) . . ?
O13 W7 O21 75.2(4) . . ?
O9 W7 O21 75.1(4) . . ?
O5 Co1 O22 96.1(5) . . ?
O5 Co1 O24 165.4(6) . . ?
O22 Co1 O24 98.2(5) . . ?
O5 Co1 N2 89.9(6) . 6_654 ?
O22 Co1 N2 84.4(6) . 6_654 ?
O24 Co1 N2 88.5(6) . 6_654 ?
O5 Co1 N4 91.5(6) . . ?
O22 Co1 N4 88.1(6) . . ?
O24 Co1 N4 92.0(5) . . ?
N2 Co1 N4 172.5(7) 6_654 . ?
O21 B1 O21 110.4(17) . 8_565 ?
O21 B1 O18 109.5(11) . . ?
O21 B1 O18 109.5(11) 8_565 . ?
O21 B1 O17 109.4(11) . . ?
O21 B1 O17 109.4(11) 8_565 . ?
O18 B1 O17 108.7(17) . . ?
W2 O1 W2 120.4(7) . 8_565 ?
W4 O2 W2 147.5(6) . . ?
W7 O3 W3 146.7(6) . . ?
W5 O4 W5 117.9(7) . 8_565 ?
W5 O24 Co1 146.0(7) 2_554 . ?
W6 O5 Co1 166.3(8) 2 . ?
W5 O7 W2 149.4(6) . . ?
W3 O8 W5 120.9(5) . . ?
W7 O9 W4 119.2(5) . . ?
W6 O10 W1 149.1(6) . . ?
W1 O12 W2 119.8(5) . . ?
W7 O13 W6 120.0(5) . . ?
W5 O14 W4 148.5(6) . . ?
W4 O16 W6 119.1(5) . . ?
B1 O17 W5 125.3(6) . . ?
B1 O17 W5 125.3(6) . 8_565 ?
W5 O17 W5 90.5(5) . 8_565 ?
B1 O17 W3 124.7(11) . . ?
W5 O17 W3 90.1(4) . . ?
W5 O17 W3 90.1(4) 8_565 . ?
B1 O18 W1 125.5(13) . . ?
B1 O18 W2 126.5(7) . . ?
W1 O18 W2 88.8(4) . . ?
B1 O18 W2 126.5(7) . 8_565 ?
W1 O18 W2 88.8(4) . 8_565 ?
W2 O18 W2 88.5(5) . 8_565 ?
W7 O19 W7 147.9(9) . 8_565 ?
W6 O20 W6 148.0(8) . 8_565 ?
B1 O21 W4 126.2(9) . . ?
B1 O21 W6 125.4(11) . . ?
W4 O21 W6 89.8(3) . . ?
B1 O21 W7 125.1(10) . . ?
W4 O21 W7 89.8(3) . . ?
W6 O21 W7 89.0(3) . . ?
W4 O22 Co1 166.4(7) . . ?
C10 C1 C5 120.3(15) 5_654 . ?
C10 C1 N3 120.5(14) 5_654 . ?
C5 C1 N3 119.2(13) . . ?
C3 C2 C4 121.6(18) . . ?
C3 C2 N5 119.0(17) . . ?
C4 C2 N5 119.3(16) . . ?
C2 C3 C13 117(2) . . ?
C2 C4 C14 118.3(16) . . ?
C1 C5 C10 116.9(15) . . ?
N5 C6 C11 108(2) . . ?
N6 C7 N3 109.9(14) . . ?
C9 C8 N3 107.9(15) . . ?
C8 C9 N6 105.2(14) . . ?
C1 C10 C5 122.6(18) 5_654 . ?
C6 C11 N4 111(2) . . ?
N5 C12 N4 109.5(15) . . ?
C15 C13 C3 121(2) . . ?
C15 C14 C4 118.6(17) . . ?
C13 C15 C14 122.4(19) . . ?
C13 C15 N1 119.1(18) . . ?
C14 C15 N1 118.4(17) . . ?
N1 C16 N2 111.8(19) . . ?
C18 C17 N1 103.1(17) . . ?
C18 N2 C16 102.9(18) . . ?
C18 N2 Co1 127.1(15) . 6_554 ?
C16 N2 Co1 130.0(14) . 6_554 ?
C16 N1 C17 106.8(16) . . ?
C16 N1 C15 129.6(17) . . ?
C17 N1 C15 123.2(15) . . ?
N2 C18 C17 115(2) . . ?
C7 N3 C8 108.5(13) . . ?
C7 N3 C1 127.3(13) . . ?
C8 N3 C1 124.1(13) . . ?
C11 N4 C12 101.4(17) . . ?
C11 N4 Co1 130.9(14) . . ?
C12 N4 Co1 127.2(12) . . ?
C6 N5 C12 110.2(18) . . ?
C6 N5 C2 125.7(18) . . ?
C12 N5 C2 124.2(15) . . ?
C7 N6 C9 108.4(14) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         5.550
_refine_diff_density_min         -4.697
_refine_diff_density_rms         0.434
####################################################################### 
# 
# 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_compound_4
_database_code_depnum_ccdc_archive 'CCDC 1474353'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-06-28 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 H38 Co2 N12 O42 W12'
_chemical_formula_weight         3630.65

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'
Co Co 0.3494 0.9721 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '

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

_cell_length_a                   26.548(5)
_cell_length_b                   20.076(5)
_cell_length_c                   12.964(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6910(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7836
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      27.33

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6368
_exptl_absorpt_coefficient_mu    20.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.001
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems. These atoms are as follows: O19. These restraint refinement leads to a relatively high restraint value 6. 
In the final refinement, the H atoms on coordination water molecules cannot be found from the residual peaks and directly included into the final molecular formula. Some free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. The SQUEEZE program indicates that there are at least one solvent water molecule in the crystal structure. These molecule were directly included in the final molecular formula based on the elemental analysis, and SQUEEZE analysis.  
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46716
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         27.44
_reflns_number_total             8119
_reflns_number_gt                6234
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0753P)²+301.7716P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8119
_refine_ls_number_parameters     475
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1613
_refine_ls_wR_factor_gt          0.1470
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.036 0.250 0.095 210.5 51.8
2 -0.036 0.750 -0.095 210.5 50.9
3 0.536 0.250 0.405 210.5 50.6
4 0.629 0.750 0.250 18.0 1.2
5 0.129 0.750 0.250 18.0 0.6
6 0.464 0.750 0.595 210.5 50.9
7 0.871 0.250 0.750 18.0 1.9
8 0.371 0.250 0.749 17.9 1.2

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
Co1 Co 0.74075(12) 0.10694(17) 0.5966(2) 0.0523(8) Uani 1 1 d . . .
W1 W 0.84708(2) 0.16718(3) 0.01567(5) 0.02181(15) Uani 1 1 d . . .
W2 W 0.84766(3) 0.2500 0.23956(7) 0.0252(2) Uani 1 2 d S . .
W3 W 0.63104(3) 0.2500 -0.06551(7) 0.0220(2) Uani 1 2 d S . .
W4 W 0.73305(2) 0.07704(3) 0.10493(5) 0.02578(16) Uani 1 1 d . . .
W5 W 0.73107(3) 0.16945(3) -0.14064(5) 0.02489(16) Uani 1 1 d . . .
W6 W 0.63182(2) 0.15782(3) 0.18144(5) 0.02477(16) Uani 1 1 d . . .
W7 W 0.73380(3) 0.15814(5) 0.32371(6) 0.0380(2) Uani 1 1 d . . .
N1 N 0.6616(6) 0.0811(8) 0.5876(12) 0.038(4) Uani 1 1 d . . .
O1 O 0.7457(5) 0.0749(7) 0.2483(10) 0.039(3) Uani 1 1 d . . .
O2 O 0.8002(4) 0.1075(5) 0.0842(9) 0.024(2) Uani 1 1 d . . .
O3 O 0.8005(4) 0.3153(6) 0.2890(8) 0.028(3) Uani 1 1 d . . .
O4 O 0.6624(4) 0.1415(6) 0.3145(8) 0.028(3) Uani 1 1 d . . .
O5 O 0.8773(5) 0.2500 -0.0269(12) 0.022(3) Uani 1 2 d S . .
O6 O 0.8761(4) 0.1826(5) 0.1511(9) 0.027(2) Uani 1 1 d . . .
O7 O 0.6592(4) 0.1821(5) -0.1541(8) 0.024(2) Uani 1 1 d . . .
O8 O 0.7214(7) 0.2500 0.3493(13) 0.039(5) Uani 1 2 d S . .
O9 O 0.6617(4) 0.0752(6) 0.1329(10) 0.030(3) Uani 1 1 d . . .
O10 O 0.8901(4) 0.1129(5) -0.0331(10) 0.031(3) Uani 1 1 d . . .
O11 O 0.5707(6) 0.2500 -0.1144(13) 0.033(4) Uani 1 2 d S . .
O12 O 0.8017(5) 0.2500 0.0891(11) 0.022(3) Uani 1 2 d S . .
O13 O 0.7138(5) 0.2500 -0.0352(11) 0.017(3) Uani 1 2 d S . .
O14 O 0.7142(4) 0.1783(6) 0.1610(8) 0.026(2) Uani 1 1 d . . .
O15 O 0.7989(4) 0.1722(5) -0.0926(8) 0.023(2) Uani 1 1 d . . .
O16 O 0.7432(5) 0.1278(9) 0.4454(10) 0.056(4) Uani 1 1 d . . .
O17 O 0.7196(4) 0.1085(5) -0.0307(9) 0.025(2) Uani 1 1 d . . .
O18 O 0.7437(5) 0.2500 -0.2209(11) 0.021(3) Uani 1 2 d SU . .
O20 O 0.5728(4) 0.1285(7) 0.2089(10) 0.037(3) Uani 1 1 d . . .
O21 O 0.6251(6) 0.2500 0.2139(12) 0.028(4) Uani 1 2 d S . .
O22 O 0.8911(6) 0.2500 0.3384(13) 0.037(4) Uani 1 2 d S . .
O23 O 0.6239(4) 0.1848(6) 0.0409(8) 0.026(2) Uani 1 1 d . . .
O24 O 0.7415(4) -0.0071(5) 0.0845(10) 0.030(3) Uani 1 1 d . . .
C1 C 0.6385(9) 0.0355(10) 0.5231(16) 0.046(5) Uani 1 1 d . . .
H1A H 0.6546 0.0120 0.4707 0.055 Uiso 1 1 calc R . .
N5 N 0.5803(6) 0.0724(8) 0.6286(12) 0.037(4) Uani 1 1 d . . .
C9 C 0.5342(7) 0.0834(10) 0.6819(15) 0.039(4) Uani 1 1 d . . .
C5 C 0.4528(7) 0.0444(10) 0.7383(17) 0.044(5) Uani 1 1 d . . .
H5A H 0.4279 0.0119 0.7403 0.053 Uiso 1 1 calc R . .
C10 C 0.4980(8) 0.0331(10) 0.6854(17) 0.046(5) Uani 1 1 d . . .
H10F H 0.5038 -0.0075 0.6530 0.055 Uiso 1 1 calc R . .
C11 C 0.4459(7) 0.1041(8) 0.7871(15) 0.034(4) Uani 1 1 d . . .
C12 C 0.6259(8) 0.0999(10) 0.6530(16) 0.045(5) Uani 1 1 d . . .
H12A H 0.6313 0.1283 0.7086 0.053 Uiso 1 1 calc R . .
C13 C 0.4805(10) 0.1522(11) 0.784(2) 0.071(8) Uani 1 1 d . . .
H13A H 0.4741 0.1929 0.8152 0.085 Uiso 1 1 calc R . .
C14 C 0.5273(8) 0.1417(11) 0.731(2) 0.062(8) Uani 1 1 d . . .
H14A H 0.5522 0.1742 0.7318 0.075 Uiso 1 1 calc R . .
C15 C 0.5899(10) 0.0301(12) 0.5470(18) 0.057(6) Uani 1 1 d . . .
H15A H 0.5665 0.0026 0.5145 0.069 Uiso 1 1 calc R . .
N6 N 0.4011(6) 0.1186(8) 0.8445(13) 0.039(4) Uani 1 1 d . . .
C18 C 0.3482(9) 0.1568(12) 0.9622(16) 0.055(6) Uani 1 1 d . . .
H18A H 0.3355 0.1786 1.0199 0.066 Uiso 1 1 calc R . .
C17 C 0.3982(8) 0.1572(11) 0.9344(16) 0.046(5) Uani 1 1 d . . .
H17A H 0.4245 0.1786 0.9681 0.056 Uiso 1 1 calc R . .
N101 N 0.5886(5) -0.0169(8) 0.8870(11) 0.029(3) Uani 1 1 d . . .
N102 N 0.6427(6) -0.0540(9) 0.7758(14) 0.045(4) Uani 1 1 d . . .
C104 C 0.6319(6) 0.0163(9) 0.9032(16) 0.037(4) Uani 1 1 d . . .
H10A H 0.6371 0.0492 0.9527 0.045 Uiso 1 1 calc R . .
C103 C 0.5425(6) -0.0080(8) 0.9451(14) 0.029(4) Uani 1 1 d . . .
C102 C 0.5963(6) -0.0612(10) 0.8119(16) 0.037(5) Uani 1 1 d . . .
H10B H 0.5729 -0.0922 0.7887 0.045 Uiso 1 1 calc R . .
C105 C 0.6669(7) -0.0066(10) 0.8342(18) 0.045(5) Uani 1 1 d . . .
H10C H 0.7003 0.0071 0.8281 0.054 Uiso 1 1 calc R . .
C101 C 0.5348(7) 0.0502(10) 0.9938(17) 0.042(5) Uani 1 1 d . . .
H10D H 0.5587 0.0841 0.9900 0.050 Uiso 1 1 calc R . .
C100 C 0.4917(7) 0.0591(11) 1.0487(18) 0.049(5) Uani 1 1 d . . .
H10E H 0.4855 0.0993 1.0818 0.058 Uiso 1 1 calc R . .
N4 N 0.3198(7) 0.1208(9) 0.8957(13) 0.045(4) Uani 1 1 d . . .
C16 C 0.3530(9) 0.0989(13) 0.8236(18) 0.057(6) Uani 1 1 d . . .
H16A H 0.3439 0.0734 0.7667 0.068 Uiso 1 1 calc R . .
O19 O 0.7372(4) 0.1148(6) -0.2442(8) 0.028(3) 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
Co1 O16 2.005(13) . ?
Co1 O24 2.066(11) 2_655 ?
Co1 O19 2.073(11) 1_556 ?
Co1 N4 2.119(17) 6_657 ?
Co1 N1 2.167(16) . ?
W1 O10 1.700(11) . ?
W1 O15 1.901(11) . ?
W1 O5 1.926(8) . ?
W1 O6 1.942(12) . ?
W1 O2 1.942(10) . ?
W1 O12 2.263(9) . ?
W2 O22 1.723(16) . ?
W2 O3 1.922(11) 8_565 ?
W2 O3 1.922(11) . ?
W2 O6 1.927(12) . ?
W2 O6 1.927(12) 8_565 ?
W2 O12 2.301(14) . ?
W3 O11 1.723(15) . ?
W3 O23 1.911(11) . ?
W3 O23 1.911(11) 8_565 ?
W3 O7 1.933(11) . ?
W3 O7 1.933(11) 8_565 ?
W3 O13 2.231(14) . ?
W4 O24 1.724(11) . ?
W4 O1 1.889(13) . ?
W4 O17 1.902(11) . ?
W4 O2 1.905(10) . ?
W4 O9 1.930(11) . ?
W4 O14 2.216(12) . ?
W5 O19 1.741(11) . ?
W5 O17 1.903(11) . ?
W5 O15 1.907(11) . ?
W5 O7 1.933(11) . ?
W5 O18 1.952(8) . ?
W5 O13 2.167(9) . ?
W5 W5 3.2341(15) 8_565 ?
W6 O20 1.711(11) . ?
W6 O21 1.906(4) . ?
W6 O23 1.912(11) . ?
W6 O4 1.935(11) . ?
W6 O9 1.942(12) . ?
W6 O14 2.241(11) . ?
W7 O16 1.709(13) . ?
W7 O8 1.903(4) . ?
W7 O3 1.904(11) 8_565 ?
W7 O4 1.929(11) . ?
W7 O1 1.961(14) . ?
W7 O14 2.210(11) . ?
N1 C12 1.33(3) . ?
N1 C1 1.38(2) . ?
O3 W7 1.904(11) 8_565 ?
O5 W1 1.926(8) 8_565 ?
O8 W7 1.903(4) 8_565 ?
O12 W1 2.263(10) 8_565 ?
O13 W5 2.167(9) 8_565 ?
O18 W5 1.952(8) 8_565 ?
O21 W6 1.906(4) 8_565 ?
O24 Co1 2.066(11) 2_654 ?
C1 C15 1.33(3) . ?
N5 C12 1.37(2) . ?
N5 C15 1.38(2) . ?
N5 C9 1.42(2) . ?
C9 C14 1.35(3) . ?
C9 C10 1.40(3) . ?
C5 C11 1.37(3) . ?
C5 C10 1.40(3) . ?
C11 C13 1.33(3) . ?
C11 N6 1.43(2) . ?
C13 C14 1.43(3) . ?
N6 C16 1.36(3) . ?
N6 C17 1.40(2) . ?
C18 N4 1.36(3) . ?
C18 C17 1.37(3) . ?
N101 C102 1.33(2) . ?
N101 C104 1.35(2) . ?
N101 C103 1.45(2) . ?
N102 C102 1.33(2) . ?
N102 C105 1.38(2) . ?
C104 C105 1.37(3) . ?
C103 C101 1.34(2) . ?
C103 C100 1.37(2) 5_657 ?
C101 C100 1.36(3) . ?
C100 C103 1.37(2) 5_657 ?
N4 C16 1.36(3) . ?
N4 Co1 2.119(17) 6_557 ?
O19 Co1 2.073(11) 1_554 ?

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
O16 Co1 O24 97.0(7) . 2_655 ?
O16 Co1 O19 163.6(7) . 1_556 ?
O24 Co1 O19 99.2(5) 2_655 1_556 ?
O16 Co1 N4 89.3(6) . 6_657 ?
O24 Co1 N4 84.5(6) 2_655 6_657 ?
O19 Co1 N4 89.3(6) 1_556 6_657 ?
O16 Co1 N1 91.6(6) . . ?
O24 Co1 N1 89.1(5) 2_655 . ?
O19 Co1 N1 91.6(5) 1_556 . ?
N4 Co1 N1 173.7(7) 6_657 . ?
O10 W1 O15 102.2(5) . . ?
O10 W1 O5 99.7(5) . . ?
O15 W1 O5 91.3(5) . . ?
O10 W1 O6 99.9(6) . . ?
O15 W1 O6 157.7(5) . . ?
O5 W1 O6 87.5(6) . . ?
O10 W1 O2 101.8(5) . . ?
O15 W1 O2 86.6(4) . . ?
O5 W1 O2 158.4(5) . . ?
O6 W1 O2 86.5(5) . . ?
O10 W1 O12 170.0(5) . . ?
O15 W1 O12 85.0(5) . . ?
O5 W1 O12 73.0(5) . . ?
O6 W1 O12 73.3(5) . . ?
O2 W1 O12 85.4(4) . . ?
O22 W2 O3 100.8(5) . 8_565 ?
O22 W2 O3 100.8(5) . . ?
O3 W2 O3 86.0(7) 8_565 . ?
O22 W2 O6 100.4(5) . . ?
O3 W2 O6 88.6(5) 8_565 . ?
O3 W2 O6 158.7(5) . . ?
O22 W2 O6 100.4(5) . 8_565 ?
O3 W2 O6 158.7(5) 8_565 8_565 ?
O3 W2 O6 88.6(5) . 8_565 ?
O6 W2 O6 89.1(6) . 8_565 ?
O22 W2 O12 170.0(7) . . ?
O3 W2 O12 86.4(4) 8_565 . ?
O3 W2 O12 86.4(4) . . ?
O6 W2 O12 72.7(4) . . ?
O6 W2 O12 72.7(4) 8_565 . ?
O11 W3 O23 100.0(5) . . ?
O11 W3 O23 100.0(5) . 8_565 ?
O23 W3 O23 86.5(7) . 8_565 ?
O11 W3 O7 98.1(5) . . ?
O23 W3 O7 89.1(5) . . ?
O23 W3 O7 161.9(5) 8_565 . ?
O11 W3 O7 98.1(5) . 8_565 ?
O23 W3 O7 161.9(5) . 8_565 ?
O23 W3 O7 89.1(5) 8_565 8_565 ?
O7 W3 O7 89.7(6) . 8_565 ?
O11 W3 O13 168.6(7) . . ?
O23 W3 O13 88.3(4) . . ?
O23 W3 O13 88.3(4) 8_565 . ?
O7 W3 O13 74.0(4) . . ?
O7 W3 O13 74.0(4) 8_565 . ?
O24 W4 O1 96.1(6) . . ?
O24 W4 O17 102.0(5) . . ?
O1 W4 O17 161.8(5) . . ?
O24 W4 O2 99.9(5) . . ?
O1 W4 O2 88.8(5) . . ?
O17 W4 O2 86.5(5) . . ?
O24 W4 O9 97.9(5) . . ?
O1 W4 O9 89.4(5) . . ?
O17 W4 O9 89.8(5) . . ?
O2 W4 O9 162.2(5) . . ?
O24 W4 O14 168.0(5) . . ?
O1 W4 O14 74.8(5) . . ?
O17 W4 O14 87.5(4) . . ?
O2 W4 O14 87.9(4) . . ?
O9 W4 O14 74.6(5) . . ?
O19 W5 O17 100.8(5) . . ?
O19 W5 O15 100.5(5) . . ?
O17 W5 O15 85.7(4) . . ?
O19 W5 O7 96.0(5) . . ?
O17 W5 O7 89.7(4) . . ?
O15 W5 O7 163.4(4) . . ?
O19 W5 O18 95.4(5) . . ?
O17 W5 O18 163.6(5) . . ?
O15 W5 O18 89.2(5) . . ?
O7 W5 O18 90.8(5) . . ?
O19 W5 O13 167.5(5) . . ?
O17 W5 O13 88.5(4) . . ?
O15 W5 O13 88.4(5) . . ?
O7 W5 O13 75.5(5) . . ?
O18 W5 O13 75.8(4) . . ?
O19 W5 W5 129.1(4) . 8_565 ?
O17 W5 W5 130.0(3) . 8_565 ?
O15 W5 W5 88.3(3) . 8_565 ?
O7 W5 W5 82.5(3) . 8_565 ?
O18 W5 W5 34.1(3) . 8_565 ?
O13 W5 W5 41.7(3) . 8_565 ?
O20 W6 O21 101.7(6) . . ?
O20 W6 O23 101.3(5) . . ?
O21 W6 O23 85.7(6) . . ?
O20 W6 O4 98.0(6) . . ?
O21 W6 O4 90.4(6) . . ?
O23 W6 O4 160.7(5) . . ?
O20 W6 O9 98.4(6) . . ?
O21 W6 O9 159.8(6) . . ?
O23 W6 O9 88.7(5) . . ?
O4 W6 O9 88.5(5) . . ?
O20 W6 O14 168.8(5) . . ?
O21 W6 O14 86.6(5) . . ?
O23 W6 O14 86.7(4) . . ?
O4 W6 O14 74.2(4) . . ?
O9 W6 O14 73.7(4) . . ?
O16 W7 O8 102.1(8) . . ?
O16 W7 O3 100.5(5) . 8_565 ?
O8 W7 O3 86.0(6) . 8_565 ?
O16 W7 O4 98.0(6) . . ?
O8 W7 O4 90.5(6) . . ?
O3 W7 O4 161.5(4) 8_565 . ?
O16 W7 O1 97.7(8) . . ?
O8 W7 O1 160.1(6) . . ?
O3 W7 O1 88.4(5) 8_565 . ?
O4 W7 O1 88.8(5) . . ?
O16 W7 O14 168.6(7) . . ?
O8 W7 O14 87.0(6) . . ?
O3 W7 O14 86.7(4) 8_565 . ?
O4 W7 O14 75.0(4) . . ?
O1 W7 O14 73.6(5) . . ?
C12 N1 C1 105.0(17) . . ?
C12 N1 Co1 126.1(13) . . ?
C1 N1 Co1 128.4(13) . . ?
W4 O1 W7 116.3(7) . . ?
W4 O2 W1 149.6(6) . . ?
W7 O3 W2 151.2(7) 8_565 . ?
W7 O4 W6 116.0(5) . . ?
W1 O5 W1 119.3(8) . 8_565 ?
W2 O6 W1 119.7(6) . . ?
W5 O7 W3 114.8(5) . . ?
W7 O8 W7 151.5(10) . 8_565 ?
W4 O9 W6 116.4(6) . . ?
W1 O12 W1 94.6(5) . 8_565 ?
W1 O12 W2 94.3(5) . . ?
W1 O12 W2 94.3(5) 8_565 . ?
W5 O13 W5 96.5(5) . 8_565 ?
W5 O13 W3 95.6(4) . . ?
W5 O13 W3 95.6(4) 8_565 . ?
W7 O14 W4 95.3(4) . . ?
W7 O14 W6 94.8(4) . . ?
W4 O14 W6 95.2(4) . . ?
W1 O15 W5 151.0(6) . . ?
W7 O16 Co1 166.4(10) . . ?
W4 O17 W5 151.2(6) . . ?
W5 O18 W5 111.9(7) . 8_565 ?
W6 O21 W6 152.3(9) . 8_565 ?
W6 O23 W3 150.6(7) . . ?
W4 O24 Co1 165.7(8) . 2_654 ?
C15 C1 N1 110.1(17) . . ?
C12 N5 C15 105.3(17) . . ?
C12 N5 C9 125.8(16) . . ?
C15 N5 C9 128.8(17) . . ?
C14 C9 C10 121.2(18) . . ?
C14 C9 N5 119.0(17) . . ?
C10 C9 N5 119.8(17) . . ?
C11 C5 C10 118.9(18) . . ?
C9 C10 C5 119.3(18) . . ?
C13 C11 C5 121.8(19) . . ?
C13 C11 N6 116.3(17) . . ?
C5 C11 N6 121.9(16) . . ?
N1 C12 N5 111.6(17) . . ?
C11 C13 C14 121(2) . . ?
C9 C14 C13 118.2(19) . . ?
C1 C15 N5 107.8(19) . . ?
C16 N6 C17 105.9(17) . . ?
C16 N6 C11 128.0(17) . . ?
C17 N6 C11 126.1(16) . . ?
N4 C18 C17 112.0(18) . . ?
C18 C17 N6 105.5(17) . . ?
C102 N101 C104 108.3(13) . . ?
C102 N101 C103 126.3(14) . . ?
C104 N101 C103 125.4(15) . . ?
C102 N102 C105 108.4(15) . . ?
N101 C104 C105 108.1(16) . . ?
C101 C103 C100 121.4(17) . 5_657 ?
C101 C103 N101 118.7(16) . . ?
C100 C103 N101 119.8(16) 5_657 . ?
N102 C102 N101 109.1(15) . . ?
C104 C105 N102 105.9(15) . . ?
C103 C101 C100 119.2(18) . . ?
C101 C100 C103 119.4(19) . 5_657 ?
C18 N4 C16 104.5(17) . . ?
C18 N4 Co1 126.3(14) . 6_557 ?
C16 N4 Co1 129.2(14) . 6_557 ?
N4 C16 N6 112.1(18) . . ?
W5 O19 Co1 145.1(7) . 1_554 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         7.400
_refine_diff_density_min         -4.409
_refine_diff_density_rms         0.454
####################################################################### 
# 
# 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_compound_5
_database_code_depnum_ccdc_archive 'CCDC 1474354'
_audit_update_record             
;
2016-04-15 deposited with the CCDC.
2016-06-28 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 H34 B Cu N12 O42 W12'
_chemical_formula_weight         3587.15

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   11.2301(6)
_cell_length_b                   12.9434(7)
_cell_length_c                   13.2453(8)
_cell_angle_alpha                96.4550(10)
_cell_angle_beta                 113.4620(10)
_cell_angle_gamma                104.4270(10)
_cell_volume                     1661.18(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3573
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.19

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1572
_exptl_absorpt_coefficient_mu    21.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems. These atoms are as follows: O4 O14 O16 O3O21 O10 O12 O13 C17 C18 O1 C1 B1O O20 O19. The command 'delu' was used to solve the non-H atoms with 'Large Hirshfeld Difference...' problems. These atoms are as follows: O18 B1. These restraint refinement leads to a relatively high restraint value 91. 
In the final refinement, the H atoms on coordination water molecules cannot be found from the residual peaks and directly included into the final molecular formula. Some free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. 
The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. The SQUEEZE program indicates that there are at least two solvent water molecules in the crystal structure. These molecules were directly included in the final molecular formula based on the elemental analysis, and SQUEEZE analysis. 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12240
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         28.30
_reflns_number_total             8248
_reflns_number_gt                6691
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0419P)²+84.9558P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8158
_refine_ls_number_parameters     481
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.155
_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 1.04324(7) 0.78071(5) 0.53716(6) 0.02357(16) Uani 1 1 d . . .
W2 W 0.96817(7) 0.62385(6) 0.27320(7) 0.02908(17) Uani 1 1 d . . .
W3 W 0.67865(7) 0.44304(6) 0.27105(7) 0.0361(2) Uani 1 1 d . . .
W4 W 1.28963(7) 0.68186(5) 0.50370(6) 0.02664(17) Uani 1 1 d . . .
W5 W 1.07526(7) 0.65680(6) 0.76258(6) 0.03048(18) Uani 1 1 d . . .
W6 W 0.75345(7) 0.59896(6) 0.53293(6) 0.02975(17) Uani 1 1 d . . .
Cu1 Cu 0.5000 1.0000 0.5000 0.0475(10) Uani 1 2 d S . .
C1 C 0.276(2) 0.5565(19) 0.064(2) 0.050(5) Uani 1 1 d U . .
H1A H 0.2610 0.5623 -0.0096 0.060 Uiso 1 1 calc R . .
C2 C 0.3167(18) 0.8779(15) 0.2659(15) 0.031(4) Uani 1 1 d . . .
H2A H 0.2524 0.8336 0.2836 0.038 Uiso 1 1 calc R . .
C3 C 0.3105(18) 0.8725(15) 0.1595(16) 0.032(4) Uani 1 1 d . . .
H3A H 0.2429 0.8239 0.0921 0.039 Uiso 1 1 calc R . .
C4 C 0.4649(18) 0.9777(14) 0.0862(13) 0.028(4) Uani 1 1 d . . .
C5 C 0.4969(18) 1.0015(14) 0.2827(13) 0.029(4) Uani 1 1 d . . .
H5A H 0.5810 1.0572 0.3146 0.035 Uiso 1 1 calc R . .
C6 C 0.5394(19) 1.0838(14) 0.0936(13) 0.028(4) Uani 1 1 d . . .
H6 H 0.5644 1.1405 0.1553 0.034 Uiso 1 1 calc R . .
C7 C 0.4240(17) 0.8960(14) -0.0078(13) 0.026(4) Uani 1 1 d . . .
H7 H 0.3706 0.8258 -0.0139 0.031 Uiso 1 1 calc R . .
C8 C 0.5180(18) 0.6854(16) 0.1731(15) 0.032(4) Uani 1 1 d . . .
C9 C 0.5956(19) 0.7718(16) 0.2661(15) 0.033(4) Uani 1 1 d . . .
H9A H 0.5700 0.7809 0.3244 0.040 Uiso 1 1 calc R . .
C10 C 0.551(2) 0.6696(15) 0.0836(15) 0.034(4) Uani 1 1 d . . .
H10A H 0.4978 0.6095 0.0221 0.041 Uiso 1 1 calc R . .
C11 C 0.188(3) 0.492(3) 0.098(2) 0.074(8) Uani 1 1 d . . .
H11A H 0.1013 0.4430 0.0489 0.089 Uiso 1 1 calc R . .
C12 C 0.3739(19) 0.5776(19) 0.2488(17) 0.042(5) Uani 1 1 d . . .
H12A H 0.4393 0.5984 0.3241 0.050 Uiso 1 1 calc R . .
C13 C 0.710(2) 0.8437(18) 0.2720(18) 0.043(5) Uani 1 1 d . . .
H13A H 0.7661 0.9004 0.3364 0.052 Uiso 1 1 calc R . .
C14 C 0.743(2) 0.8327(17) 0.1814(18) 0.040(5) Uani 1 1 d . . .
C15 C 0.664(2) 0.7436(16) 0.0875(17) 0.038(5) Uani 1 1 d . . .
H15A H 0.6879 0.7350 0.0282 0.046 Uiso 1 1 calc R . .
C16 C 0.986(2) 0.9507(16) 0.2719(17) 0.039(5) Uani 1 1 d . . .
H16A H 1.0140 0.9299 0.3405 0.047 Uiso 1 1 calc R . .
C17 C 0.989(3) 1.032(3) 0.136(3) 0.075(8) Uani 1 1 d U . .
H17A H 1.0209 1.0784 0.0965 0.090 Uiso 1 1 calc R . .
C18 C 0.863(3) 0.961(3) 0.098(3) 0.079(8) Uani 1 1 d U . .
H18A H 0.7900 0.9470 0.0264 0.095 Uiso 1 1 calc R . .
N1 N 0.4337(17) 0.9594(12) 0.3408(11) 0.033(4) Uani 1 1 d . . .
N2 N 0.4260(14) 0.9547(11) 0.1733(11) 0.025(3) Uani 1 1 d . . .
N3 N 0.3923(15) 0.6109(13) 0.1642(13) 0.032(3) Uani 1 1 d . . .
N4 N 0.8613(18) 0.9112(15) 0.1863(16) 0.043(4) Uani 1 1 d . . .
N5 N 1.0624(19) 1.0233(16) 0.2437(19) 0.055(5) Uani 1 1 d . . .
N6 N 0.2439(18) 0.5082(18) 0.2079(16) 0.055(5) Uani 1 1 d . . .
B1 B 1.0000 0.5000 0.5000 0.015(4) Uani 1 2 d SU . .
O1 O 0.5226(14) 0.4175(11) 0.1627(11) 0.036(3) Uani 1 1 d U . .
O2 O 0.6360(16) 0.6481(14) 0.5505(16) 0.055(4) Uani 1 1 d . . .
O3 O 0.664(2) 0.5484(17) 0.3742(18) 0.077(6) Uani 1 1 d U . .
O4 O 0.8799(17) 0.6284(14) 0.6851(14) 0.055(4) Uani 1 1 d U . .
O5 O 0.8589(15) 0.7249(17) 0.5181(13) 0.067(6) Uani 1 1 d . . .
O6 O 1.0626(15) 0.9157(11) 0.5541(15) 0.057(5) Uani 1 1 d . . .
O7 O 0.9741(15) 0.7414(16) 0.3786(12) 0.058(5) Uani 1 1 d . . .
O8 O 0.633(3) 0.3341(13) 0.3450(13) 0.088(8) Uani 1 1 d . . .
O9 O 1.2189(15) 0.7830(15) 0.5550(12) 0.052(4) Uani 1 1 d . . .
O10 O 1.311(2) 0.5491(16) 0.4523(17) 0.072(5) Uani 1 1 d U . .
O11 O 1.4291(14) 0.7727(12) 0.5040(13) 0.049(4) Uani 1 1 d . . .
O12 O 0.780(2) 0.5615(17) 0.2319(18) 0.079(6) Uani 1 1 d U . .
O13 O 1.1629(15) 0.6652(12) 0.3557(13) 0.044(3) Uani 1 1 d U . .
O14 O 1.253(2) 0.6517(16) 0.7962(17) 0.068(5) Uani 1 1 d U . .
O15 O 1.1067(13) 0.7280(12) 0.8909(10) 0.038(3) Uani 1 1 d . . .
O16 O 1.1034(18) 0.7683(14) 0.6910(15) 0.057(4) Uani 1 1 d U . .
O17 O 0.9586(15) 0.6862(13) 0.1682(12) 0.045(4) Uani 1 1 d . . .
O19 O 1.0535(18) 0.6015(14) 0.4730(15) 0.010(3) Uani 0.50 1 d PU . .
O20 O 0.929(2) 0.4884(16) 0.3672(17) 0.017(4) Uani 0.50 1 d PU . .
O21 O 0.965(2) 0.4856(17) 0.2072(18) 0.077(6) Uani 1 1 d U . .
O18 O 1.022(2) 0.4021(16) 0.4462(18) 0.018(4) Uani 0.50 1 d PU . .
O22 O 0.843(2) 0.4726(17) 0.468(2) 0.023(5) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O6 1.684(13) . ?
W1 O7 1.880(15) . ?
W1 O9 1.883(14) . ?
W1 O16 1.914(17) . ?
W1 O5 1.915(14) . ?
W1 O18 2.359(19) 2_766 ?
W1 O19 2.426(18) . ?
W2 O17 1.666(14) . ?
W2 O12 1.89(2) . ?
W2 O21 1.89(2) . ?
W2 O13 1.910(15) . ?
W2 O7 1.915(16) . ?
W2 O20 2.32(2) . ?
W2 O19 2.509(18) . ?
W3 O1 1.686(14) . ?
W3 O8 1.886(19) . ?
W3 O3 1.91(2) . ?
W3 O14 1.914(19) 2_766 ?
W3 O12 1.92(2) . ?
W3 O22 2.44(2) . ?
W3 O20 2.45(2) . ?
W4 O11 1.707(13) . ?
W4 O13 1.856(15) . ?
W4 O10 1.88(2) . ?
W4 O9 1.886(15) . ?
W4 O8 1.900(16) 2_766 ?
W4 O22 2.34(2) 2_766 ?
W4 O19 2.439(18) . ?
W5 O15 1.695(12) . ?
W5 O16 1.844(17) . ?
W5 O14 1.881(19) . ?
W5 O21 1.91(2) 2_766 ?
W5 O4 1.929(17) . ?
W5 O20 2.38(2) 2_766 ?
W5 O18 2.48(2) 2_766 ?
W6 O2 1.681(14) . ?
W6 O5 1.842(17) . ?
W6 O4 1.872(17) . ?
W6 O3 1.88(2) . ?
W6 O10 1.93(2) 2_766 ?
W6 O22 2.37(2) . ?
W6 O18 2.43(2) 2_766 ?
Cu1 N1 1.893(13) . ?
Cu1 N1 1.893(13) 2_676 ?
C1 C11 1.38(4) . ?
C1 N3 1.39(3) . ?
C2 N1 1.36(2) . ?
C2 C3 1.38(2) . ?
C3 N2 1.39(2) . ?
C4 C7 1.37(2) . ?
C4 C6 1.39(2) . ?
C4 N2 1.42(2) . ?
C5 N1 1.32(2) . ?
C5 N2 1.32(2) . ?
C6 C7 1.38(2) 2_675 ?
C7 C6 1.38(2) 2_675 ?
C8 C9 1.37(2) . ?
C8 C10 1.39(3) . ?
C8 N3 1.45(2) . ?
C9 C13 1.35(3) . ?
C10 C15 1.36(3) . ?
C11 N6 1.31(3) . ?
C12 N3 1.32(2) . ?
C12 N6 1.36(3) . ?
C13 C14 1.40(3) . ?
C14 C15 1.40(3) . ?
C14 N4 1.43(2) . ?
C16 N4 1.33(3) . ?
C16 N5 1.30(3) . ?
C17 C18 1.34(4) . ?
C17 N5 1.37(4) . ?
C18 N4 1.40(4) . ?
B1 O19 1.449(18) . ?
B1 O19 1.449(18) 2_766 ?
B1 O18 1.504(19) . ?
B1 O18 1.504(19) 2_766 ?
B1 O20 1.59(2) . ?
B1 O20 1.59(2) 2_766 ?
B1 O22 1.57(2) 2_766 ?
B1 O22 1.57(2) . ?
O8 W4 1.900(16) 2_766 ?
O10 W6 1.93(2) 2_766 ?
O14 W3 1.914(19) 2_766 ?
O19 O18 1.60(3) 2_766 ?
O19 O22 1.70(3) 2_766 ?
O19 O20 1.74(3) . ?
O20 W5 2.38(2) 2_766 ?
O21 W5 1.91(2) 2_766 ?
O18 O19 1.60(3) 2_766 ?
O18 W1 2.359(19) 2_766 ?
O18 W6 2.43(2) 2_766 ?
O18 W5 2.48(2) 2_766 ?
O22 O19 1.70(3) 2_766 ?
O22 W4 2.34(2) 2_766 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O7 98.9(9) . . ?
O6 W1 O9 100.4(8) . . ?
O7 W1 O9 90.7(6) . . ?
O6 W1 O16 100.6(8) . . ?
O7 W1 O16 160.5(8) . . ?
O9 W1 O16 86.5(7) . . ?
O6 W1 O5 99.9(9) . . ?
O7 W1 O5 88.3(7) . . ?
O9 W1 O5 159.6(9) . . ?
O16 W1 O5 87.7(7) . . ?
O6 W1 O18 160.1(8) . 2_766 ?
O7 W1 O18 94.3(8) . 2_766 ?
O9 W1 O18 94.3(8) . 2_766 ?
O16 W1 O18 66.7(7) . 2_766 ?
O5 W1 O18 65.5(8) . 2_766 ?
O6 W1 O19 160.7(8) . . ?
O7 W1 O19 68.4(7) . . ?
O9 W1 O19 66.6(7) . . ?
O16 W1 O19 92.9(7) . . ?
O5 W1 O19 94.3(8) . . ?
O18 W1 O19 39.2(6) 2_766 . ?
O17 W2 O12 99.8(8) . . ?
O17 W2 O21 99.6(8) . . ?
O12 W2 O21 88.2(9) . . ?
O17 W2 O13 99.1(7) . . ?
O12 W2 O13 161.1(8) . . ?
O21 W2 O13 89.4(8) . . ?
O17 W2 O7 98.8(8) . . ?
O12 W2 O7 88.5(8) . . ?
O21 W2 O7 161.6(9) . . ?
O13 W2 O7 87.9(6) . . ?
O17 W2 O20 160.5(8) . . ?
O12 W2 O20 68.3(8) . . ?
O21 W2 O20 65.8(8) . . ?
O13 W2 O20 93.7(7) . . ?
O7 W2 O20 96.3(8) . . ?
O17 W2 O19 157.4(7) . . ?
O12 W2 O19 96.5(8) . . ?
O21 W2 O19 96.4(8) . . ?
O13 W2 O19 65.1(6) . . ?
O7 W2 O19 66.0(7) . . ?
O20 W2 O19 42.0(6) . . ?
O1 W3 O8 99.1(8) . . ?
O1 W3 O3 97.3(8) . . ?
O8 W3 O3 89.6(8) . . ?
O1 W3 O14 99.8(7) . 2_766 ?
O8 W3 O14 88.6(8) . 2_766 ?
O3 W3 O14 162.8(9) . 2_766 ?
O1 W3 O12 98.4(8) . . ?
O8 W3 O12 162.5(10) . . ?
O3 W3 O12 89.0(9) . . ?
O14 W3 O12 87.6(9) 2_766 . ?
O1 W3 O22 155.9(7) . . ?
O8 W3 O22 64.9(8) . . ?
O3 W3 O22 66.2(8) . . ?
O14 W3 O22 97.7(8) 2_766 . ?
O12 W3 O22 98.7(8) . . ?
O1 W3 O20 157.5(7) . . ?
O8 W3 O20 98.0(9) . . ?
O3 W3 O20 97.2(8) . . ?
O14 W3 O20 66.2(7) 2_766 . ?
O12 W3 O20 64.8(8) . . ?
O22 W3 O20 46.6(7) . . ?
O11 W4 O13 99.2(7) . . ?
O11 W4 O10 99.5(8) . . ?
O13 W4 O10 87.1(8) . . ?
O11 W4 O9 98.8(8) . . ?
O13 W4 O9 89.9(6) . . ?
O10 W4 O9 161.7(8) . . ?
O11 W4 O8 100.1(10) . 2_766 ?
O13 W4 O8 160.7(9) . 2_766 ?
O10 W4 O8 90.1(8) . 2_766 ?
O9 W4 O8 86.8(7) . 2_766 ?
O11 W4 O22 159.6(8) . 2_766 ?
O13 W4 O22 94.6(7) . 2_766 ?
O10 W4 O22 66.1(8) . 2_766 ?
O9 W4 O22 96.1(8) . 2_766 ?
O8 W4 O22 66.9(9) 2_766 2_766 ?
O11 W4 O19 158.9(7) . . ?
O13 W4 O19 67.3(6) . . ?
O10 W4 O19 96.1(7) . . ?
O9 W4 O19 66.2(7) . . ?
O8 W4 O19 94.0(9) 2_766 . ?
O22 W4 O19 41.5(7) 2_766 . ?
O15 W5 O16 101.6(7) . . ?
O15 W5 O14 99.0(8) . . ?
O16 W5 O14 89.7(8) . . ?
O15 W5 O21 96.2(8) . 2_766 ?
O16 W5 O21 162.2(8) . 2_766 ?
O14 W5 O21 87.3(9) . 2_766 ?
O15 W5 O4 99.1(7) . . ?
O16 W5 O4 90.1(7) . . ?
O14 W5 O4 161.6(8) . . ?
O21 W5 O4 87.2(8) 2_766 . ?
O15 W5 O20 156.1(7) . 2_766 ?
O16 W5 O20 98.6(7) . 2_766 ?
O14 W5 O20 68.3(8) . 2_766 ?
O21 W5 O20 64.1(8) 2_766 2_766 ?
O4 W5 O20 93.6(7) . 2_766 ?
O15 W5 O18 158.9(7) . 2_766 ?
O16 W5 O18 64.9(7) . 2_766 ?
O14 W5 O18 97.2(8) . 2_766 ?
O21 W5 O18 98.0(8) 2_766 2_766 ?
O4 W5 O18 66.2(7) . 2_766 ?
O20 W5 O18 44.6(7) 2_766 2_766 ?
O2 W6 O5 98.6(9) . . ?
O2 W6 O4 98.9(8) . . ?
O5 W6 O4 89.7(7) . . ?
O2 W6 O3 98.7(9) . . ?
O5 W6 O3 89.4(8) . . ?
O4 W6 O3 162.3(8) . . ?
O2 W6 O10 99.3(8) . 2_766 ?
O5 W6 O10 161.9(9) . 2_766 ?
O4 W6 O10 85.6(8) . 2_766 ?
O3 W6 O10 89.9(9) . 2_766 ?
O2 W6 O22 158.4(8) . . ?
O5 W6 O22 98.3(8) . . ?
O4 W6 O22 94.5(8) . . ?
O3 W6 O22 68.1(9) . . ?
O10 W6 O22 64.8(8) 2_766 . ?
O2 W6 O18 157.9(8) . 2_766 ?
O5 W6 O18 64.8(8) . 2_766 ?
O4 W6 O18 67.9(7) . 2_766 ?
O3 W6 O18 95.9(8) . 2_766 ?
O10 W6 O18 97.3(7) 2_766 2_766 ?
O22 W6 O18 43.8(7) . 2_766 ?
N1 Cu1 N1 180.000(6) . 2_676 ?
C11 C1 N3 104(2) . . ?
N1 C2 C3 108.1(14) . . ?
C2 C3 N2 105.8(15) . . ?
C7 C4 C6 119.7(15) . . ?
C7 C4 N2 120.2(15) . . ?
C6 C4 N2 120.1(15) . . ?
N1 C5 N2 111.5(14) . . ?
C7 C6 C4 119.0(15) 2_675 . ?
C4 C7 C6 121.3(16) . 2_675 ?
C9 C8 C10 122.4(18) . . ?
C9 C8 N3 119.2(17) . . ?
C10 C8 N3 118.3(17) . . ?
C8 C9 C13 119.0(18) . . ?
C15 C10 C8 118.8(17) . . ?
N6 C11 C1 110(2) . . ?
N3 C12 N6 108.7(18) . . ?
C9 C13 C14 120.0(18) . . ?
C13 C14 C15 120.2(18) . . ?
C13 C14 N4 120(2) . . ?
C15 C14 N4 120.0(19) . . ?
C10 C15 C14 119.4(18) . . ?
N4 C16 N5 108.4(19) . . ?
C18 C17 N5 106(3) . . ?
C17 C18 N4 107(3) . . ?
C5 N1 C2 107.3(13) . . ?
C5 N1 Cu1 125.7(12) . . ?
C2 N1 Cu1 126.9(12) . . ?
C5 N2 C3 107.3(13) . . ?
C5 N2 C4 126.8(14) . . ?
C3 N2 C4 125.8(14) . . ?
C12 N3 C1 109.2(17) . . ?
C12 N3 C8 125.6(16) . . ?
C1 N3 C8 125.0(17) . . ?
C16 N4 C18 108(2) . . ?
C16 N4 C14 127.7(18) . . ?
C18 N4 C14 124(2) . . ?
C16 N5 C17 111(2) . . ?
C11 N6 C12 108(2) . . ?
O19 B1 O19 180.000(4) . 2_766 ?
O19 B1 O18 114.2(10) . . ?
O19 B1 O18 65.8(10) 2_766 . ?
O19 B1 O18 65.8(10) . 2_766 ?
O19 B1 O18 114.2(10) 2_766 2_766 ?
O18 B1 O18 180.0(17) . 2_766 ?
O19 B1 O20 69.7(10) . . ?
O19 B1 O20 110.3(10) 2_766 . ?
O18 B1 O20 73.3(11) . . ?
O18 B1 O20 106.7(11) 2_766 . ?
O19 B1 O20 110.3(10) . 2_766 ?
O19 B1 O20 69.7(10) 2_766 2_766 ?
O18 B1 O20 106.7(11) . 2_766 ?
O18 B1 O20 73.3(11) 2_766 2_766 ?
O20 B1 O20 180.000(7) . 2_766 ?
O19 B1 O22 68.2(11) . 2_766 ?
O19 B1 O22 111.8(10) 2_766 2_766 ?
O18 B1 O22 71.2(11) . 2_766 ?
O18 B1 O22 108.8(11) 2_766 2_766 ?
O20 B1 O22 104.5(11) . 2_766 ?
O20 B1 O22 75.5(11) 2_766 2_766 ?
O19 B1 O22 111.8(10) . . ?
O19 B1 O22 68.2(11) 2_766 . ?
O18 B1 O22 108.8(11) . . ?
O18 B1 O22 71.2(11) 2_766 . ?
O20 B1 O22 75.5(11) . . ?
O20 B1 O22 104.5(11) 2_766 . ?
O22 B1 O22 180.000(3) 2_766 . ?
W6 O3 W3 133.1(12) . . ?
W6 O4 W5 134.2(9) . . ?
W6 O5 W1 136.0(12) . . ?
W1 O7 W2 134.6(10) . . ?
W3 O8 W4 134.3(12) . 2_766 ?
W1 O9 W4 134.8(10) . . ?
W4 O10 W6 132.6(11) . 2_766 ?
W2 O12 W3 132.8(12) . . ?
W4 O13 W2 137.0(8) . . ?
W5 O14 W3 133.3(11) . 2_766 ?
W5 O16 W1 135.8(10) . . ?
B1 O19 O18 58.8(9) . 2_766 ?
B1 O19 O22 59.3(10) . 2_766 ?
O18 O19 O22 98.5(14) 2_766 2_766 ?
B1 O19 O20 58.8(9) . . ?
O18 O19 O20 95.7(14) 2_766 . ?
O22 O19 O20 93.2(13) 2_766 . ?
B1 O19 W1 126.9(10) . . ?
O18 O19 W1 68.2(9) 2_766 . ?
O22 O19 W1 134.1(12) 2_766 . ?
O20 O19 W1 130.6(12) . . ?
B1 O19 W4 125.5(10) . . ?
O18 O19 W4 134.0(13) 2_766 . ?
O22 O19 W4 66.1(9) 2_766 . ?
O20 O19 W4 126.8(11) . . ?
W1 O19 W4 91.3(6) . . ?
B1 O19 W2 121.9(10) . . ?
O18 O19 W2 128.7(12) 2_766 . ?
O22 O19 W2 126.9(12) 2_766 . ?
O20 O19 W2 63.1(9) . . ?
W1 O19 W2 90.4(6) . . ?
W4 O19 W2 90.1(6) . . ?
B1 O20 O19 51.4(9) . . ?
B1 O20 W2 126.3(11) . . ?
O19 O20 W2 74.9(9) . . ?
B1 O20 W5 121.7(11) . 2_766 ?
O19 O20 W5 136.2(12) . 2_766 ?
W2 O20 W5 96.1(7) . 2_766 ?
B1 O20 W3 118.3(10) . . ?
O19 O20 W3 130.5(12) . . ?
W2 O20 W3 94.0(7) . . ?
W5 O20 W3 92.3(7) 2_766 . ?
W2 O21 W5 133.7(12) . 2_766 ?
B1 O18 O19 55.5(9) . 2_766 ?
B1 O18 W1 128.1(11) . 2_766 ?
O19 O18 W1 72.6(9) 2_766 2_766 ?
B1 O18 W6 122.4(12) . 2_766 ?
O19 O18 W6 135.6(14) 2_766 2_766 ?
W1 O18 W6 93.3(7) 2_766 2_766 ?
B1 O18 W5 120.3(11) . 2_766 ?
O19 O18 W5 130.3(13) 2_766 2_766 ?
W1 O18 W5 92.1(7) 2_766 2_766 ?
W6 O18 W5 91.0(6) 2_766 2_766 ?
B1 O22 O19 52.5(9) . 2_766 ?
B1 O22 W4 124.8(12) . 2_766 ?
O19 O22 W4 72.4(9) 2_766 2_766 ?
B1 O22 W6 122.6(12) . . ?
O19 O22 W6 136.6(14) 2_766 . ?
W4 O22 W6 95.8(8) 2_766 . ?
B1 O22 W3 119.6(12) . . ?
O19 O22 W3 129.1(13) 2_766 . ?
W4 O22 W3 93.6(8) 2_766 . ?
W6 O22 W3 92.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         5.550
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.396
####################################################################### 
# 
# 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_zcy
_database_code_depnum_ccdc_archive 'CCDC 1474355'
_audit_update_record             
;
2016-06-23 deposited with the CCDC.
2016-06-28 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 H41 Ag2 B N12 O42 W12'
_chemical_formula_weight         3746.15

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'
B B 0.0013 0.0007 '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'
Ag Ag -0.8971 1.1015 '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           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '

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

_cell_length_a                   26.664(5)
_cell_length_b                   20.022(5)
_cell_length_c                   12.937(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6907(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5410
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      24.96

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6580.0
_exptl_absorpt_coefficient_mu    20.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_T_max  0.006
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
 During the refinement, the restraint command 'ISOR' is used to refine the non-H atoms with ADP problems.
 These atoms are as follows: O12 C17 C1 O14 C8 O13 O3 Ow3 C14 C5 O4 O3 B1 C15 O21 O24 C2 C6 N4 N1 C12 C16 and C4. 
The command 'delu' was used to solve the non-H atoms with 'Large Hirshfeld Difference...' problems. 
These atoms are as follows: Ag1 N4 C9 N5 C11 W7 O1 W4 O20 N1 C8. 
These restraint refinement leads to a relatively high restraint value 133. 
In the previous version, even after a 15-cycle refinement run, the refinement had not fully converged. 
There is a major problem with the anisotropic vibration parameters for the B1 atom. 
The reason for the problem may be that the atomic mass of B atom is small, which may probably result in the B with an NDP problem. 
Therefore, in this version, the B atom in the refinement with unit-occupancy and a fixed (not refined) Uiso value of 0.02. Consequently, with this change a 15-cycle refinement run will give complete convergence positions, which is featureless, and should be due to the "series termination errors". 
In the final refinement, the H atoms on coordination water molecules cannot be found from the residual peaks and directly included into the final molecular formula. Some free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. The SQUEEZE program indicates that there are at least one solvent water molecule in the crystal structure. This one molecule was directly included in the final molecular formula based on the elemental analysis, and SQUEEZE analysis. 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35719
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         24.75
_reflns_number_total             6105
_reflns_number_gt                4119
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1344P)²+604.9061P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6011
_refine_ls_number_parameters     483
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.1995
_refine_ls_wR_factor_gt          0.1760
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_restrained_S_all      0.826
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.032 0.250 -0.045 191.8 56.1
2 0.032 0.750 0.045 192.6 57.0
3 0.126 0.250 0.244 22.3 2.9
4 0.532 0.750 0.455 192.4 53.6
5 0.622 0.250 0.260 23.1 3.4
6 0.467 0.250 0.546 190.9 57.3
7 0.374 0.750 0.744 21.7 4.0
8 0.874 0.750 0.756 21.4 3.8


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 0.15469(5) 0.2500 -0.25235(12) 0.0275(3) Uani 1 2 d S . .
W2 W 0.15487(4) 0.16719(4) -0.03067(8) 0.0265(3) Uani 1 1 d . . .
W3 W 0.36799(5) 0.2500 0.05493(11) 0.0270(3) Uani 1 2 d S . .
W4 W 0.26672(4) 0.16822(5) 0.12835(8) 0.0312(3) Uani 1 1 d U . .
W5 W 0.26635(4) 0.07766(5) -0.11409(9) 0.0308(3) Uani 1 1 d . . .
W6 W 0.36799(4) 0.15892(5) -0.18838(8) 0.0272(3) Uani 1 1 d . . .
W7 W 0.26645(4) 0.15955(5) -0.33397(9) 0.0339(3) Uani 1 1 d U . .
Ag1 Ag 0.25710(17) 0.1059(2) 0.3908(3) 0.1067(13) Uani 1 1 d U . .
O2 O 0.2075(7) 0.2500 -0.1054(18) 0.025(5) Uani 1 2 d S . .
O3 O 0.2818(5) 0.1884(7) -0.1589(12) 0.020(3) Uani 1 1 d U . .
O4 O 0.2564(7) 0.0781(9) -0.2563(16) 0.043(5) Uani 1 1 d U . .
O5 O 0.4260(6) 0.1286(9) -0.2174(13) 0.033(4) Uani 1 1 d . . .
O6 O 0.3763(8) 0.2500 -0.2244(17) 0.025(5) Uani 1 2 d S . .
O7 O 0.3782(5) 0.1838(7) -0.0468(12) 0.022(3) Uani 1 1 d . . .
O8 O 0.4273(9) 0.2500 0.1119(19) 0.037(6) Uani 1 2 d S . .
O9 O 0.3375(6) 0.1845(8) 0.1400(12) 0.024(3) Uani 1 1 d . . .
O10 O 0.2000(6) 0.1714(8) 0.0785(14) 0.031(4) Uani 1 1 d . . .
O11 O 0.1115(6) 0.1131(7) 0.0168(13) 0.033(4) Uani 1 1 d . . .
O12 O 0.1271(7) 0.2500 0.0076(17) 0.021(5) Uani 1 2 d SU . .
O13 O 0.1260(5) 0.1848(7) -0.1647(12) 0.023(3) Uani 1 1 d U . .
O14 O 0.1109(10) 0.2500 -0.346(2) 0.044(7) Uani 1 2 d SU . .
O15 O 0.2006(6) 0.3145(9) -0.3033(13) 0.033(4) Uani 1 1 d . . .
O16 O 0.2797(9) 0.2500 -0.3640(19) 0.031(6) Uani 1 2 d S . .
O17 O 0.3377(6) 0.1460(8) -0.3189(14) 0.033(4) Uani 1 1 d . . .
O18 O 0.3372(6) 0.0787(7) -0.1441(14) 0.030(4) Uani 1 1 d . . .
O19 O 0.2798(7) 0.1057(8) 0.0231(15) 0.041(5) Uani 1 1 d . . .
O20 O 0.2608(6) 0.1162(9) 0.2340(18) 0.048(4) Uani 1 1 d U . .
O21 O 0.2567(9) 0.2500 0.201(2) 0.038(6) Uani 1 2 d SU . .
O22 O 0.2842(9) 0.2500 0.004(2) 0.034(6) Uani 1 2 d S . .
O23 O 0.1989(5) 0.1072(7) -0.0974(13) 0.024(3) Uani 1 1 d . . .
O1 O 0.2589(6) 0.1261(11) -0.4525(16) 0.047(5) Uani 1 1 d U . .
N1 N 0.3354(13) 0.0783(18) 0.394(3) 0.088(7) Uani 1 1 d U . .
N2 N 0.4097(7) 0.9816(10) 0.1107(17) 0.031(5) Uani 1 1 d . . .
N3 N 0.3538(7) 0.9444(12) 0.2155(19) 0.041(6) Uani 1 1 d . . .
N4 N 0.1841(10) 0.1208(14) 0.385(2) 0.059(6) Uani 1 1 d U . .
N5 N 0.4154(10) 0.0705(12) 0.3607(19) 0.048(6) Uani 1 1 d U . .
N6 N 0.0985(9) 0.1187(13) 0.344(2) 0.056(7) Uani 1 1 d . . .
C1 C 0.4651(11) 1.0501(15) 0.001(2) 0.048(7) Uani 1 1 d U . .
H1 H 0.4417 1.0845 0.0044 0.057 Uiso 1 1 calc R . .
C2 C 0.4561(8) 0.9919(11) 0.0528(19) 0.027(5) Uani 1 1 d U . .
C3 C 0.4001(10) 0.9400(12) 0.1856(19) 0.035(6) Uani 1 1 d . . .
H3 H 0.4235 0.9108 0.2141 0.042 Uiso 1 1 calc R . .
C4 C 0.3664(10) 1.0138(15) 0.088(2) 0.046(7) Uani 1 1 d U . .
H4 H 0.3618 1.0449 0.0349 0.055 Uiso 1 1 calc R . .
C5 C 0.5080(12) 1.0583(17) -0.054(3) 0.056(8) Uani 1 1 d U . .
H5 H 0.5133 1.0969 -0.0924 0.068 Uiso 1 1 calc R . .
C6 C 0.3312(10) 0.9928(13) 0.154(2) 0.038(6) Uani 1 1 d U . .
H6 H 0.2982 1.0077 0.1590 0.046 Uiso 1 1 calc R . .
C7 C 0.3703(10) 0.0987(15) 0.332(2) 0.043(7) Uani 1 1 d . . .
H7 H 0.3656 0.1279 0.2774 0.052 Uiso 1 1 calc R . .
C8 C 0.1462(12) 0.0995(16) 0.318(3) 0.056(7) Uani 1 1 d U . .
H8 H 0.1530 0.0740 0.2598 0.067 Uiso 1 1 calc R . .
C9 C 0.1524(13) 0.1567(15) 0.462(3) 0.061(9) Uani 1 1 d U . .
H9 H 0.1656 0.1775 0.5203 0.073 Uiso 1 1 calc R . .
C10 C 0.5011(12) 0.034(2) 0.311(3) 0.084(14) Uani 1 1 d . . .
H10 H 0.4957 -0.0068 0.3439 0.101 Uiso 1 1 calc R . .
C11 C 0.4632(11) 0.0814(16) 0.305(3) 0.055(8) Uani 1 1 d U . .
C12 C 0.4061(11) 0.0355(15) 0.442(2) 0.046(7) Uani 1 1 d U . .
H12 H 0.4296 0.0112 0.4793 0.056 Uiso 1 1 calc R . .
C13 C 0.3581(13) 0.0396(15) 0.463(3) 0.059(9) Uani 1 1 d . . .
H13 H 0.3424 0.0185 0.5187 0.071 Uiso 1 1 calc R . .
C14 C 0.4705(14) 0.1398(19) 0.250(3) 0.068(9) Uani 1 1 d U . .
H14 H 0.4450 0.1712 0.2437 0.081 Uiso 1 1 calc R . .
C15 C 0.5151(17) 0.149(2) 0.208(4) 0.095(13) Uani 1 1 d U . .
H15 H 0.5200 0.1891 0.1721 0.114 Uiso 1 1 calc R . .
C16 C 0.1036(11) 0.1564(13) 0.440(2) 0.041(7) Uani 1 1 d U . .
H16 H 0.0780 0.1761 0.4782 0.049 Uiso 1 1 calc R . .
C17 C 0.0554(11) 0.1054(14) 0.287(2) 0.045(7) Uani 1 1 d U . .
C18 C 0.0460(14) 0.0484(17) 0.233(3) 0.077(12) Uani 1 1 d . . .
H18 H 0.0720 0.0178 0.2250 0.093 Uiso 1 1 calc R . .
B1 B 0.2637(13) 0.2500 -0.104(3) 0.020 Uiso 1 2 d S . .
O24 O 0.2599(6) -0.0079(9) -0.0952(15) 0.037(4) Uani 1 1 d U . .
OW1 O 0.0107(17) 0.2500 0.539(4) 0.131(19) Uani 1 2 d S . .


_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 O14 1.68(3) . ?
W1 O13 1.891(15) 8_565 ?
W1 O13 1.891(15) . ?
W1 O15 1.897(17) 8_565 ?
W1 O15 1.897(17) . ?
W1 O2 2.37(2) . ?
W2 O11 1.700(15) . ?
W2 O10 1.857(16) . ?
W2 O12 1.882(10) . ?
W2 O23 1.888(15) . ?
W2 O13 1.929(15) . ?
W2 O2 2.378(14) . ?
W3 O8 1.75(2) . ?
W3 O7 1.888(14) 8_565 ?
W3 O7 1.888(14) . ?
W3 O9 1.894(14) 8_565 ?
W3 O9 1.894(14) . ?
W3 O22 2.33(2) . ?
W4 O20 1.726(19) . ?
W4 O19 1.882(16) . ?
W4 O10 1.894(15) . ?
W4 O21 1.909(14) . ?
W4 O9 1.923(15) . ?
W4 O22 2.343(19) . ?
W5 O24 1.738(18) . ?
W5 O4 1.86(2) . ?
W5 O19 1.895(18) . ?
W5 O23 1.906(14) . ?
W5 O18 1.929(16) . ?
W5 O3 2.328(14) . ?
W6 O5 1.704(15) . ?
W6 O6 1.895(6) . ?
W6 O17 1.890(17) . ?
W6 O18 1.892(16) . ?
W6 O7 1.917(15) . ?
W6 O3 2.403(14) . ?
W7 O1 1.69(2) . ?
W7 O15 1.874(17) 8_565 ?
W7 O16 1.885(6) . ?
W7 O4 1.933(19) . ?
W7 O17 1.929(15) . ?
W7 O3 2.372(15) . ?
Ag1 N4 1.97(3) . ?
Ag1 O20 2.04(2) . ?
Ag1 O24 2.022(19) 2 ?
Ag1 O1 2.07(2) 1_556 ?
Ag1 N1 2.16(4) . ?
O2 B1 1.50(4) . ?
O2 W2 2.378(14) 8_565 ?
O3 B1 1.50(3) . ?
O6 W6 1.895(6) 8_565 ?
O12 W2 1.882(10) 8_565 ?
O15 W7 1.874(17) 8_565 ?
O16 W7 1.885(6) 8_565 ?
O21 W4 1.909(14) 8_565 ?
O22 B1 1.50(4) . ?
O22 W4 2.343(19) 8_565 ?
O1 Ag1 2.07(2) 1_554 ?
N1 C13 1.33(4) . ?
N1 C7 1.29(4) . ?
N2 C3 1.30(3) . ?
N2 C4 1.36(3) . ?
N2 C2 1.46(3) . ?
N3 C3 1.30(3) . ?
N3 C6 1.39(3) . ?
N4 C8 1.40(4) . ?
N4 C9 1.49(4) . ?
N5 C12 1.29(4) . ?
N5 C7 1.38(4) . ?
N5 C11 1.48(4) . ?
N6 C17 1.39(4) . ?
N6 C8 1.37(4) . ?
N6 C16 1.46(4) . ?
C1 C2 1.36(4) . ?
C1 C5 1.36(4) . ?
C2 C5 1.39(4) 5_675 ?
C4 C6 1.34(4) . ?
C5 C2 1.39(4) 5_675 ?
C9 C16 1.33(4) . ?
C10 C18 1.36(5) 6_656 ?
C10 C11 1.39(4) . ?
C11 C14 1.38(5) . ?
C12 C13 1.31(4) . ?
C14 C15 1.32(5) . ?
C15 C17 1.39(5) 6_656 ?
C17 C15 1.39(5) 6_556 ?
C17 C18 1.37(4) . ?
C18 C10 1.36(5) 6_556 ?
B1 O3 1.50(3) 8_565 ?
O24 Ag1 2.022(19) 2_554 ?

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
O14 W1 O13 98.6(8) . 8_565 ?
O14 W1 O13 98.6(8) . . ?
O13 W1 O13 87.3(9) 8_565 . ?
O14 W1 O15 101.5(8) . 8_565 ?
O13 W1 O15 159.9(7) 8_565 8_565 ?
O13 W1 O15 90.0(7) . 8_565 ?
O14 W1 O15 101.5(8) . . ?
O13 W1 O15 90.0(7) 8_565 . ?
O13 W1 O15 159.9(7) . . ?
O15 W1 O15 85.8(10) 8_565 . ?
O14 W1 O2 172.4(11) . . ?
O13 W1 O2 76.1(6) 8_565 . ?
O13 W1 O2 76.1(6) . . ?
O15 W1 O2 84.0(6) 8_565 . ?
O15 W1 O2 84.0(6) . . ?
O11 W2 O10 101.2(8) . . ?
O11 W2 O12 101.4(7) . . ?
O10 W2 O12 90.9(8) . . ?
O11 W2 O23 100.6(7) . . ?
O10 W2 O23 88.5(7) . . ?
O12 W2 O23 157.7(7) . . ?
O11 W2 O13 99.8(8) . . ?
O10 W2 O13 159.0(7) . . ?
O12 W2 O13 85.3(8) . . ?
O23 W2 O13 87.3(6) . . ?
O11 W2 O2 173.3(8) . . ?
O10 W2 O2 84.0(8) . . ?
O12 W2 O2 74.0(6) . . ?
O23 W2 O2 83.7(6) . . ?
O13 W2 O2 75.1(7) . . ?
O8 W3 O7 99.4(7) . 8_565 ?
O8 W3 O7 99.4(7) . . ?
O7 W3 O7 89.2(10) 8_565 . ?
O8 W3 O9 98.2(8) . 8_565 ?
O7 W3 O9 88.9(7) 8_565 8_565 ?
O7 W3 O9 162.3(6) . 8_565 ?
O8 W3 O9 98.2(8) . . ?
O7 W3 O9 162.3(6) 8_565 . ?
O7 W3 O9 88.9(7) . . ?
O9 W3 O9 87.6(10) 8_565 . ?
O8 W3 O22 171.5(11) . . ?
O7 W3 O22 86.6(6) 8_565 . ?
O7 W3 O22 86.6(6) . . ?
O9 W3 O22 75.7(6) 8_565 . ?
O9 W3 O22 75.7(6) . . ?
O20 W4 O19 100.9(10) . . ?
O20 W4 O10 101.8(8) . . ?
O19 W4 O10 87.1(7) . . ?
O20 W4 O21 96.5(10) . . ?
O19 W4 O21 162.6(9) . . ?
O10 W4 O21 90.5(9) . . ?
O20 W4 O9 97.5(7) . . ?
O19 W4 O9 89.3(7) . . ?
O10 W4 O9 160.7(7) . . ?
O21 W4 O9 87.3(9) . . ?
O20 W4 O22 169.8(9) . . ?
O19 W4 O22 86.0(8) . . ?
O10 W4 O22 85.9(8) . . ?
O21 W4 O22 76.6(8) . . ?
O9 W4 O22 74.9(7) . . ?
O24 W5 O4 97.5(8) . . ?
O24 W5 O19 100.3(8) . . ?
O4 W5 O19 162.2(8) . . ?
O24 W5 O23 101.3(7) . . ?
O4 W5 O23 88.6(7) . . ?
O19 W5 O23 88.9(7) . . ?
O24 W5 O18 97.9(7) . . ?
O4 W5 O18 86.6(8) . . ?
O19 W5 O18 90.0(8) . . ?
O23 W5 O18 160.7(6) . . ?
O24 W5 O3 172.1(7) . . ?
O4 W5 O3 76.9(7) . . ?
O19 W5 O3 85.3(7) . . ?
O23 W5 O3 84.3(6) . . ?
O18 W5 O3 76.5(6) . . ?
O5 W6 O6 100.5(9) . . ?
O5 W6 O17 98.2(8) . . ?
O6 W6 O17 87.8(8) . . ?
O5 W6 O18 99.1(7) . . ?
O6 W6 O18 160.3(8) . . ?
O17 W6 O18 88.3(7) . . ?
O5 W6 O7 100.0(7) . . ?
O6 W6 O7 88.2(8) . . ?
O17 W6 O7 161.8(7) . . ?
O18 W6 O7 89.6(7) . . ?
O5 W6 O3 172.2(7) . . ?
O6 W6 O3 85.1(8) . . ?
O17 W6 O3 76.5(6) . . ?
O18 W6 O3 75.2(6) . . ?
O7 W6 O3 85.5(6) . . ?
O1 W7 O15 101.0(8) . 8_565 ?
O1 W7 O16 102.5(11) . . ?
O15 W7 O16 87.3(8) 8_565 . ?
O1 W7 O4 97.0(10) . . ?
O15 W7 O4 89.7(8) 8_565 . ?
O16 W7 O4 160.5(10) . . ?
O1 W7 O17 98.9(8) . . ?
O15 W7 O17 160.1(8) 8_565 . ?
O16 W7 O17 88.4(8) . . ?
O4 W7 O17 88.0(7) . . ?
O1 W7 O3 170.3(8) . . ?
O15 W7 O3 83.8(6) 8_565 . ?
O16 W7 O3 86.0(8) . . ?
O4 W7 O3 74.5(7) . . ?
O17 W7 O3 76.6(6) . . ?
N4 Ag1 O20 89.9(10) . . ?
N4 Ag1 O24 86.0(10) . 2 ?
O20 Ag1 O24 101.4(8) . 2 ?
N4 Ag1 O1 91.6(10) . 1_556 ?
O20 Ag1 O1 162.4(9) . 1_556 ?
O24 Ag1 O1 96.1(8) 2 1_556 ?
N4 Ag1 N1 173.9(13) . . ?
O20 Ag1 N1 90.0(11) . . ?
O24 Ag1 N1 88.1(11) 2 . ?
O1 Ag1 N1 90.4(11) 1_556 . ?
B1 O2 W1 127.1(19) . . ?
B1 O2 W2 125.9(11) . 8_565 ?
W1 O2 W2 88.6(6) . 8_565 ?
B1 O2 W2 125.9(11) . . ?
W1 O2 W2 88.6(6) . . ?
W2 O2 W2 88.4(7) 8_565 . ?
B1 O3 W5 127.4(14) . . ?
B1 O3 W7 126.4(16) . . ?
W5 O3 W7 88.6(5) . . ?
B1 O3 W6 125.7(15) . . ?
W5 O3 W6 88.6(5) . . ?
W7 O3 W6 87.4(5) . . ?
W5 O4 W7 119.9(10) . . ?
W6 O6 W6 148.4(14) 8_565 . ?
W3 O7 W6 145.9(8) . . ?
W3 O9 W4 119.5(8) . . ?
W2 O10 W4 150.0(11) . . ?
W2 O12 W2 123.5(11) 8_565 . ?
W1 O13 W2 120.2(8) . . ?
W7 O15 W1 150.1(10) 8_565 . ?
W7 O16 W7 147.7(13) 8_565 . ?
W6 O17 W7 119.4(9) . . ?
W6 O18 W5 119.7(7) . . ?
W4 O19 W5 147.1(10) . . ?
W4 O20 Ag1 148.5(12) . . ?
W4 O21 W4 118.1(14) 8_565 . ?
B1 O22 W3 128(2) . . ?
B1 O22 W4 124.6(10) . 8_565 ?
W3 O22 W4 89.7(7) . 8_565 ?
B1 O22 W4 124.6(10) . . ?
W3 O22 W4 89.7(7) . . ?
W4 O22 W4 88.6(9) 8_565 . ?
W2 O23 W5 146.7(8) . . ?
W7 O1 Ag1 166.5(13) . 1_554 ?
C13 N1 C7 106(3) . . ?
C13 N1 Ag1 127(3) . . ?
C7 N1 Ag1 127(3) . . ?
C3 N2 C4 107(2) . . ?
C3 N2 C2 130(2) . . ?
C4 N2 C2 123(2) . . ?
C3 N3 C6 107(2) . . ?
C8 N4 C9 99(2) . . ?
C8 N4 Ag1 133(2) . . ?
C9 N4 Ag1 128(2) . . ?
C12 N5 C7 106(3) . . ?
C12 N5 C11 130(3) . . ?
C7 N5 C11 124(2) . . ?
C17 N6 C8 126(3) . . ?
C17 N6 C16 129(3) . . ?
C8 N6 C16 105(2) . . ?
C2 C1 C5 120(3) . . ?
C1 C2 C5 120(3) . 5_675 ?
C1 C2 N2 121(2) . . ?
C5 C2 N2 118(2) 5_675 . ?
N3 C3 N2 111(2) . . ?
N2 C4 C6 108(3) . . ?
C2 C5 C1 119(3) 5_675 . ?
C4 C6 N3 106(2) . . ?
N1 C7 N5 110(3) . . ?
N6 C8 N4 116(3) . . ?
C16 C9 N4 114(3) . . ?
C18 C10 C11 118(3) 6_656 . ?
C14 C11 C10 121(3) . . ?
C14 C11 N5 120(3) . . ?
C10 C11 N5 120(3) . . ?
N5 C12 C13 109(3) . . ?
N1 C13 C12 110(3) . . ?
C15 C14 C11 117(4) . . ?
C14 C15 C17 126(4) . 6_656 ?
C9 C16 N6 106(3) . . ?
C15 C17 N6 120(3) 6_556 . ?
C15 C17 C18 114(3) 6_556 . ?
N6 C17 C18 126(3) . . ?
C10 C18 C17 124(3) 6_556 . ?
O3 B1 O3 110(3) 8_565 . ?
O3 B1 O22 108.8(17) 8_565 . ?
O3 B1 O22 108.8(17) . . ?
O3 B1 O2 108.5(17) 8_565 . ?
O3 B1 O2 108.5(17) . . ?
O22 B1 O2 112(3) . . ?
W5 O24 Ag1 164.9(11) . 2_554 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        24.75
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         5.550
_refine_diff_density_min         -4.053
_refine_diff_density_rms         0.514
