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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1048166'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H18 Cl2 N4 O5 Zn'
_chemical_formula_weight         542.66

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'
Cl Cl 0.1484 0.1585 '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'
Zn Zn 0.2839 1.4301 '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, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   14.5366(10)
_cell_length_b                   18.2023(12)
_cell_length_c                   8.0806(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2138.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5704
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3592
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5704
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         26.37
_reflns_number_total             2251
_reflns_number_gt                1409
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1a (Brandenburg, 2005)'
_computing_publication_material  'PLATON (Spek, 2009)'

_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)+(0.0619P)²+8.5080P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2251
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0758
_refine_ls_wR_factor_ref         0.1961
_refine_ls_wR_factor_gt          0.1744
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.12860(8) 0.7500 0.06494(15) 0.0633(4) Uani 1 2 d S . .
Cl1 Cl 0.11973(16) 0.7500 -0.2166(3) 0.0643(6) Uani 1 2 d S . .
Cl2 Cl 0.00137(18) 0.7500 0.2256(3) 0.0715(7) Uani 1 2 d S . .
O1 O 0.2174(3) 0.6726(3) 0.1239(7) 0.0758(14) Uani 1 1 d . . .
O2 O 0.1269(3) 0.5795(3) 0.0546(7) 0.0803(15) Uani 1 1 d . . .
O101 O 0.2558(8) 0.7500 0.4556(13) 0.143(4) Uani 1 2 d S . .
H10A H 0.3126 0.7500 0.4278 0.171 Uiso 1 2 d S . .
H10B H 0.2268 0.7500 0.3639 0.171 Uiso 1 2 d S . .
N1 N 0.5938(4) 0.3160(3) 0.1651(8) 0.0641(14) Uani 1 1 d . . .
N2 N 0.5036(4) 0.4086(3) 0.1902(7) 0.0632(14) Uani 1 1 d . . .
C1 C 0.5604(6) 0.4088(5) 0.3248(11) 0.092(3) Uani 1 1 d . . .
H1A H 0.5601 0.4423 0.4117 0.111 Uiso 1 1 calc R . .
C2 C 0.6163(6) 0.3514(5) 0.3067(11) 0.090(3) Uani 1 1 d . . .
H2A H 0.6630 0.3380 0.3793 0.108 Uiso 1 1 calc R . .
C3 C 0.4293(5) 0.4601(4) 0.1622(8) 0.0618(16) Uani 1 1 d . . .
C4 C 0.2815(5) 0.4847(4) 0.0527(10) 0.075(2) Uani 1 1 d . . .
H4A H 0.2304 0.4699 -0.0080 0.090 Uiso 1 1 calc R . .
C5 C 0.3531(5) 0.4362(4) 0.0744(10) 0.074(2) Uani 1 1 d . . .
H5A H 0.3504 0.3889 0.0315 0.088 Uiso 1 1 calc R . .
C6 C 0.5251(5) 0.3516(4) 0.0963(9) 0.0627(17) Uani 1 1 d . . .
H6A H 0.4963 0.3388 -0.0023 0.075 Uiso 1 1 calc R . .
C7 C 0.2833(5) 0.5542(4) 0.1180(9) 0.0633(17) Uani 1 1 d . . .
C8 C 0.4350(5) 0.5292(4) 0.2237(9) 0.0645(17) Uani 1 1 d . . .
H8A H 0.4874 0.5446 0.2800 0.077 Uiso 1 1 calc R . .
C9 C 0.3624(5) 0.5763(4) 0.2017(8) 0.0616(17) Uani 1 1 d . . .
H9A H 0.3659 0.6238 0.2434 0.074 Uiso 1 1 calc R . .
C10 C 0.6372(7) 0.2500 0.1012(14) 0.067(3) Uani 1 2 d S . .
H10C H 0.7018 0.2500 0.1316 0.080 Uiso 1 2 calc SR . .
H10D H 0.6334 0.2500 -0.0187 0.080 Uiso 1 2 calc SR . .
C11 C 0.2005(5) 0.6055(4) 0.0958(9) 0.0651(17) 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
Zn1 O1 1.970(5) 7_575 ?
Zn1 O1 1.970(5) . ?
Zn1 Cl2 2.260(3) . ?
Zn1 Cl1 2.279(3) . ?
O1 C11 1.266(8) . ?
O2 C11 1.216(8) . ?
N1 C6 1.314(8) . ?
N1 C2 1.353(10) . ?
N1 C10 1.452(8) . ?
N2 C6 1.323(8) . ?
N2 C1 1.366(9) . ?
N2 C3 1.448(8) . ?
C1 C2 1.330(10) . ?
C3 C8 1.356(9) . ?
C3 C5 1.386(10) . ?
C4 C7 1.371(10) . ?
C4 C5 1.375(10) . ?
C7 C9 1.393(9) . ?
C7 C11 1.534(10) . ?
C8 C9 1.371(9) . ?
C10 N1 1.452(8) 7_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
O1 Zn1 O1 91.3(3) 7_575 . ?
O1 Zn1 Cl2 113.43(17) 7_575 . ?
O1 Zn1 Cl2 113.43(17) . . ?
O1 Zn1 Cl1 106.18(17) 7_575 . ?
O1 Zn1 Cl1 106.18(17) . . ?
Cl2 Zn1 Cl1 121.81(11) . . ?
C11 O1 Zn1 121.2(5) . . ?
C6 N1 C2 107.9(6) . . ?
C6 N1 C10 126.0(7) . . ?
C2 N1 C10 126.2(7) . . ?
C6 N2 C1 108.4(6) . . ?
C6 N2 C3 126.5(6) . . ?
C1 N2 C3 125.0(6) . . ?
C2 C1 N2 106.3(7) . . ?
C1 C2 N1 108.6(7) . . ?
C8 C3 C5 121.8(7) . . ?
C8 C3 N2 119.9(6) . . ?
C5 C3 N2 118.3(6) . . ?
C7 C4 C5 121.9(7) . . ?
C4 C5 C3 118.0(7) . . ?
N1 C6 N2 108.9(6) . . ?
C4 C7 C9 118.0(7) . . ?
C4 C7 C11 120.1(7) . . ?
C9 C7 C11 121.9(6) . . ?
C3 C8 C9 119.0(7) . . ?
C8 C9 C7 121.2(7) . . ?
N1 C10 N1 111.7(8) . 7_565 ?
O2 C11 O1 126.5(7) . . ?
O2 C11 C7 119.1(7) . . ?
O1 C11 C7 114.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.120
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1048168'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 N8 O48 P W12 Zn'
_chemical_formula_weight         3719.30

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   21.205(2)
_cell_length_b                   30.853(2)
_cell_length_c                   19.6747(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.033(8)
_cell_angle_gamma                90.00
_cell_volume                     12675.0(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24730
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.06

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6628
_exptl_absorpt_coefficient_mu    11.099
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_T_max  0.368
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3592
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24730
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.06
_reflns_number_total             11217
_reflns_number_gt                4402
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1a (Brandenburg, 2005)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          SQUEEZE

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.004 -0.003 -0.011 6769 1284 ' '
_platon_squeeze_details          
;
About one [(CH₃)₂NH₂]⁺, eight DMF and fourteen water lattice 
guests were removed from the formula unit by the SQUEEZE process.
;

_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)+(0.0686P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11217
_refine_ls_number_parameters     514
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0848
_refine_ls_wR_factor_ref         0.2220
_refine_ls_wR_factor_gt          0.2025
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.37880(5) 0.12963(3) 0.31619(6) 0.1004(4) Uani 1 1 d . . .
W2 W 0.37809(6) 0.24507(4) 0.31518(6) 0.1045(4) Uani 1 1 d . . .
W3 W 0.61972(6) 0.24537(3) 0.36507(6) 0.1030(4) Uani 1 1 d . . .
W4 W 0.49760(6) 0.18750(4) 0.42998(5) 0.1021(4) Uani 1 1 d . . .
W5 W 0.61915(6) 0.12980(4) 0.36385(7) 0.1125(4) Uani 1 1 d . . .
W6 W 0.5000 0.30301(4) 0.2500 0.1018(5) Uani 1 2 d S . .
W7 W 0.5000 0.07156(4) 0.2500 0.1053(5) Uani 1 2 d S . .
P1 P 0.5000 0.18707(19) 0.2500 0.0497(13) Uani 1 2 d SD . .
Zn1 Zn 0.5000 -0.17898(9) 0.2500 0.0690(8) Uani 1 2 d S . .
O1 O 0.4559(10) 0.1491(6) 0.2464(14) 0.086(8) Uani 0.50 1 d PD . .
O2 O 0.4564(8) 0.1845(6) 0.3023(8) 0.063(6) Uani 0.50 1 d PD . .
O3 O 0.4358(8) 0.2899(5) 0.1713(8) 0.108(5) Uani 1 1 d . . .
O4 O 0.5578(10) 0.1463(6) 0.4197(14) 0.165(9) Uani 1 1 d . . .
O5 O 0.5000 0.3588(8) 0.2500 0.148(10) Uani 1 2 d S . .
O6 O 0.3207(10) 0.0994(7) 0.3484(11) 0.155(8) Uani 1 1 d . . .
O7 O 0.6754(9) 0.1003(6) 0.4195(9) 0.128(6) Uani 1 1 d . . .
O8 O 0.5620(12) 0.2328(6) 0.4218(12) 0.158(8) Uani 1 1 d . . .
O9 O 0.3474(9) 0.1883(7) 0.3138(8) 0.135(7) Uani 1 1 d . . .
O10 O 0.4333(10) 0.2289(6) 0.3970(10) 0.138(6) Uani 1 1 d U . .
O11 O 0.6505(10) 0.1863(7) 0.3753(11) 0.153(7) Uani 1 1 d U . .
O12 O 0.4389(10) 0.0855(6) 0.1711(11) 0.142(7) Uani 1 1 d U . .
O13 O 0.4426(11) 0.0857(5) 0.3001(11) 0.160(10) Uani 1 1 d . . .
O14 O 0.4342(9) 0.2912(7) 0.3073(10) 0.144(7) Uani 1 1 d . . .
O15 O 0.6780(9) 0.2724(5) 0.4217(10) 0.127(6) Uani 1 1 d . . .
O16 O 0.4349(8) 0.1452(5) 0.3995(8) 0.112(5) Uani 1 1 d . . .
O17 O 0.3473(8) 0.1268(5) 0.2224(9) 0.110(5) Uani 1 1 d . . .
O18 O 0.6507(9) 0.2459(7) 0.2836(11) 0.141(7) Uani 1 1 d . . .
O19 O 0.4989(8) 0.1874(5) 0.5123(10) 0.120(5) Uani 1 1 d . . .
O20 O 0.3231(10) 0.2709(6) 0.3424(10) 0.139(7) Uani 1 1 d . . .
O21 O 0.4594(10) 0.2273(5) 0.2437(12) 0.075(7) Uani 0.50 1 d PDU . .
O22 O 0.4577(11) 0.1875(9) 0.1806(8) 0.089(8) Uani 0.50 1 d PDU . .
O23 O 0.5000 0.0187(8) 0.2500 0.125(8) Uani 1 2 d SU . .
O24 O 0.9629(7) -0.6432(4) 0.3164(6) 0.075(3) Uani 1 1 d . . .
O25 O 0.9061(7) -0.6008(4) 0.2361(7) 0.087(4) Uani 1 1 d . . .
O26 O 0.5011(10) -0.2497(9) 0.3404(14) 0.204(11) Uani 1 1 d DU . .
O27 O 0.5735(9) -0.2081(6) 0.3099(9) 0.128(6) Uani 1 1 d DU . .
N1 N 0.9086(7) -0.4868(4) 0.5081(7) 0.062(4) Uani 1 1 d . . .
N2 N 0.9101(7) -0.4253(4) 0.5617(8) 0.061(4) Uani 1 1 d . . .
N3 N 0.8444(7) -0.3606(5) 0.5656(8) 0.066(4) Uani 1 1 d . . .
N4 N 0.7567(7) -0.3287(5) 0.5172(7) 0.070(4) Uani 1 1 d . . .
C1 C 0.9311(10) -0.6100(6) 0.2968(9) 0.068(5) Uani 1 1 d . . .
C2 C 0.9188(9) -0.5774(5) 0.3528(9) 0.063(5) Uani 1 1 d . . .
C3 C 0.9034(13) -0.5358(7) 0.3368(10) 0.102(8) Uani 1 1 d . . .
H3A H 0.8966 -0.5267 0.2910 0.123 Uiso 1 1 calc R . .
C4 C 0.8980(13) -0.5071(6) 0.3885(11) 0.097(7) Uani 1 1 d . . .
H4A H 0.8852 -0.4790 0.3757 0.116 Uiso 1 1 calc R . .
C5 C 0.9093(10) -0.5160(6) 0.4536(8) 0.068(5) Uani 1 1 d . . .
C6 C 0.9283(8) -0.5590(8) 0.4715(10) 0.081(6) Uani 1 1 d . . .
H6A H 0.9385 -0.5675 0.5175 0.097 Uiso 1 1 calc R . .
C7 C 0.9312(9) -0.5888(6) 0.4177(10) 0.067(5) Uani 1 1 d . . .
H7A H 0.9423 -0.6174 0.4288 0.081 Uiso 1 1 calc R . .
C8 C 0.9104(8) -0.4437(6) 0.5016(9) 0.068(5) Uani 1 1 d . . .
H8A H 0.9117 -0.4290 0.4606 0.081 Uiso 1 1 calc R . .
C9 C 0.9119(12) -0.4933(7) 0.5764(13) 0.102(8) Uani 1 1 d . . .
H9A H 0.9150 -0.5204 0.5974 0.122 Uiso 1 1 calc R . .
C10 C 0.9100(11) -0.4554(6) 0.6106(10) 0.084(6) Uani 1 1 d . . .
H10A H 0.9090 -0.4512 0.6572 0.101 Uiso 1 1 calc R . .
C11 C 0.9118(10) -0.3801(7) 0.5736(11) 0.083(6) Uani 1 1 d . . .
H11A H 0.9350 -0.3662 0.5414 0.100 Uiso 1 1 calc R . .
H11B H 0.9346 -0.3744 0.6199 0.100 Uiso 1 1 calc R . .
C12 C 0.8153(10) -0.3400(5) 0.5072(9) 0.067(5) Uani 1 1 d . . .
H12A H 0.8329 -0.3347 0.4679 0.080 Uiso 1 1 calc R . .
C13 C 0.8026(11) -0.3611(7) 0.6099(10) 0.082(6) Uani 1 1 d . . .
H13A H 0.8104 -0.3721 0.6546 0.098 Uiso 1 1 calc R . .
C14 C 0.7499(12) -0.3436(7) 0.5799(12) 0.096(7) Uani 1 1 d . . .
H14A H 0.7127 -0.3416 0.5987 0.116 Uiso 1 1 calc R . .
C15 C 0.7139(7) -0.3058(5) 0.4701(8) 0.072(5) Uani 1 1 d GU . .
C16 C 0.6548(9) -0.2952(6) 0.4871(8) 0.133(9) Uani 1 1 d GU . .
H16A H 0.6447 -0.3043 0.5289 0.159 Uiso 1 1 calc R . .
C17 C 0.6110(7) -0.2710(6) 0.4416(11) 0.159(12) Uani 1 1 d GU . .
H17A H 0.5715 -0.2639 0.4530 0.191 Uiso 1 1 calc R . .
C18 C 0.6262(9) -0.2574(5) 0.3790(9) 0.102(7) Uani 1 1 d GDU . .
C19 C 0.6853(10) -0.2680(6) 0.3620(7) 0.141(10) Uani 1 1 d GU . .
H19A H 0.6954 -0.2590 0.3202 0.170 Uiso 1 1 calc R . .
C20 C 0.7291(7) -0.2922(6) 0.4075(9) 0.179(14) Uani 1 1 d GU . .
H20A H 0.7686 -0.2993 0.3961 0.215 Uiso 1 1 calc R . .
C21 C 0.5627(9) -0.2410(10) 0.3419(19) 0.195(17) Uani 1 1 d DU . .


_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 1.75(2) . ?
W1 O17 1.851(17) . ?
W1 O16 1.911(16) . ?
W1 O9 1.926(19) . ?
W1 O13 1.98(2) . ?
W1 O1 2.39(2) . ?
W1 O2 2.410(15) . ?
W2 O20 1.58(2) . ?
W2 O9 1.87(2) . ?
W2 O14 1.88(2) . ?
W2 O10 1.88(2) . ?
W2 O18 1.93(2) 2_655 ?
W2 O21 2.47(2) . ?
W3 O15 1.729(18) . ?
W3 O8 1.84(2) . ?
W3 O18 1.84(2) . ?
W3 O3 1.870(16) 2_655 ?
W3 O11 1.93(2) . ?
W3 O22 2.49(2) 2_655 ?
W4 O19 1.615(19) . ?
W4 O4 1.84(2) . ?
W4 O16 1.885(18) . ?
W4 O10 1.90(2) . ?
W4 O8 1.98(2) . ?
W4 O2 2.513(17) . ?
W4 O22 2.52(2) 2_655 ?
W5 O7 1.731(17) . ?
W5 O11 1.87(2) . ?
W5 O12 1.887(19) 2_655 ?
W5 O4 1.91(2) . ?
W5 O17 1.954(18) 2_655 ?
W5 O22 2.47(2) 2_655 ?
W5 O1 2.53(2) 2_655 ?
W6 O5 1.72(3) . ?
W6 O3 1.918(16) . ?
W6 O3 1.918(16) 2_655 ?
W6 O14 1.97(2) 2_655 ?
W6 O14 1.97(2) . ?
W6 O21 2.49(2) . ?
W6 O21 2.49(2) 2_655 ?
W7 O23 1.63(3) . ?
W7 O13 1.75(3) . ?
W7 O13 1.75(3) 2_655 ?
W7 O12 1.890(19) . ?
W7 O12 1.89(2) 2_655 ?
P1 O1 1.492(10) . ?
P1 O1 1.492(10) 2_655 ?
P1 O22 1.496(10) . ?
P1 O22 1.496(10) 2_655 ?
P1 O2 1.500(10) 2_655 ?
P1 O2 1.500(10) . ?
P1 O21 1.504(10) . ?
P1 O21 1.504(10) 2_655 ?
Zn1 O24 1.975(13) 4_655 ?
Zn1 O24 1.975(13) 3_455 ?
Zn1 O27 1.996(17) 2_655 ?
Zn1 O27 1.996(17) . ?
O1 O2 1.55(3) . ?
O1 O22 1.76(3) . ?
O1 W5 2.53(2) 2_655 ?
O2 O21 1.76(3) . ?
O2 O22 1.79(3) 2_655 ?
O3 W3 1.870(16) 2_655 ?
O12 W5 1.887(19) 2_655 ?
O17 W5 1.954(18) 2_655 ?
O18 W2 1.93(2) 2_655 ?
O21 O21 1.70(4) 2_655 ?
O21 O22 1.74(3) . ?
O22 O2 1.79(3) 2_655 ?
O22 W5 2.47(2) 2_655 ?
O22 W3 2.49(2) 2_655 ?
O22 W4 2.52(2) 2_655 ?
O24 C1 1.25(2) . ?
O24 Zn1 1.975(13) 3_545 ?
O25 C1 1.25(2) . ?
O26 C21 1.329(10) . ?
O27 C21 1.236(10) . ?
N1 C8 1.34(2) . ?
N1 C9 1.35(3) . ?
N1 C5 1.40(2) . ?
N2 C8 1.31(2) . ?
N2 C10 1.34(2) . ?
N2 C11 1.41(2) . ?
N3 C13 1.35(2) . ?
N3 C12 1.36(2) . ?
N3 C11 1.53(2) . ?
N4 C12 1.34(2) . ?
N4 C14 1.35(3) . ?
N4 C15 1.375(18) . ?
C1 C2 1.55(3) . ?
C2 C7 1.31(2) . ?
C2 C3 1.35(2) . ?
C3 C4 1.37(3) . ?
C4 C5 1.29(2) . ?
C5 C6 1.41(3) . ?
C6 C7 1.41(3) . ?
C9 C10 1.35(3) . ?
C13 C14 1.29(3) . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 C21 1.505(10) . ?
C19 C20 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O17 100.4(9) . . ?
O6 W1 O16 101.3(9) . . ?
O17 W1 O16 158.3(8) . . ?
O6 W1 O9 104.3(10) . . ?
O17 W1 O9 87.6(6) . . ?
O16 W1 O9 86.9(7) . . ?
O6 W1 O13 103.8(10) . . ?
O17 W1 O13 86.9(7) . . ?
O16 W1 O13 88.2(7) . . ?
O9 W1 O13 151.9(10) . . ?
O6 W1 O1 159.8(10) . . ?
O17 W1 O1 66.6(7) . . ?
O16 W1 O1 92.5(7) . . ?
O9 W1 O1 91.0(8) . . ?
O13 W1 O1 61.6(9) . . ?
O6 W1 O2 162.4(9) . . ?
O17 W1 O2 93.2(7) . . ?
O16 W1 O2 65.5(7) . . ?
O9 W1 O2 65.0(8) . . ?
O13 W1 O2 87.9(8) . . ?
O1 W1 O2 37.7(6) . . ?
O20 W2 O9 101.7(9) . . ?
O20 W2 O14 99.2(9) . . ?
O9 W2 O14 159.0(9) . . ?
O20 W2 O10 103.2(9) . . ?
O9 W2 O10 85.8(7) . . ?
O14 W2 O10 87.9(8) . . ?
O20 W2 O18 102.2(9) . 2_655 ?
O9 W2 O18 87.1(7) . 2_655 ?
O14 W2 O18 90.1(8) . 2_655 ?
O10 W2 O18 154.5(9) . 2_655 ?
O20 W2 O21 159.1(7) . . ?
O9 W2 O21 93.4(7) . . ?
O14 W2 O21 66.8(8) . . ?
O10 W2 O21 92.1(8) . . ?
O18 W2 O21 63.9(8) 2_655 . ?
O15 W3 O8 100.8(10) . . ?
O15 W3 O18 103.6(9) . . ?
O8 W3 O18 155.6(10) . . ?
O15 W3 O3 103.0(7) . 2_655 ?
O8 W3 O3 86.9(8) . 2_655 ?
O18 W3 O3 87.6(8) . 2_655 ?
O15 W3 O11 101.3(8) . . ?
O8 W3 O11 89.2(9) . . ?
O18 W3 O11 86.2(9) . . ?
O3 W3 O11 155.7(8) 2_655 . ?
O15 W3 O22 158.9(7) . 2_655 ?
O8 W3 O22 66.4(9) . 2_655 ?
O18 W3 O22 90.3(8) . 2_655 ?
O3 W3 O22 93.3(7) 2_655 2_655 ?
O11 W3 O22 63.3(9) . 2_655 ?
O19 W4 O4 102.6(10) . . ?
O19 W4 O16 101.9(7) . . ?
O4 W4 O16 87.2(8) . . ?
O19 W4 O10 103.3(9) . . ?
O4 W4 O10 154.1(10) . . ?
O16 W4 O10 86.1(7) . . ?
O19 W4 O8 101.0(9) . . ?
O4 W4 O8 88.7(9) . . ?
O16 W4 O8 157.0(8) . . ?
O10 W4 O8 87.8(9) . . ?
O19 W4 O2 160.9(7) . . ?
O4 W4 O2 89.5(9) . . ?
O16 W4 O2 63.5(6) . . ?
O10 W4 O2 65.1(7) . . ?
O8 W4 O2 93.9(7) . . ?
O19 W4 O22 157.3(7) . 2_655 ?
O4 W4 O22 62.1(9) . 2_655 ?
O16 W4 O22 94.3(7) . 2_655 ?
O10 W4 O22 93.5(8) . 2_655 ?
O8 W4 O22 64.0(9) . 2_655 ?
O2 W4 O22 41.8(5) . 2_655 ?
O7 W5 O11 102.9(9) . . ?
O7 W5 O12 100.6(9) . 2_655 ?
O11 W5 O12 156.5(9) . 2_655 ?
O7 W5 O4 103.8(9) . . ?
O11 W5 O4 86.9(9) . . ?
O12 W5 O4 86.3(10) 2_655 . ?
O7 W5 O17 102.1(8) . 2_655 ?
O11 W5 O17 88.5(8) . 2_655 ?
O12 W5 O17 87.8(8) 2_655 2_655 ?
O4 W5 O17 154.0(8) . 2_655 ?
O7 W5 O22 160.6(8) . 2_655 ?
O11 W5 O22 64.5(9) . 2_655 ?
O12 W5 O22 92.5(8) 2_655 2_655 ?
O4 W5 O22 62.5(8) . 2_655 ?
O17 W5 O22 92.5(7) 2_655 2_655 ?
O7 W5 O1 158.2(7) . 2_655 ?
O11 W5 O1 92.4(8) . 2_655 ?
O12 W5 O1 65.5(8) 2_655 2_655 ?
O4 W5 O1 92.3(9) . 2_655 ?
O17 W5 O1 62.3(7) 2_655 2_655 ?
O22 W5 O1 41.2(5) 2_655 2_655 ?
O5 W6 O3 102.2(5) . . ?
O5 W6 O3 102.2(5) . 2_655 ?
O3 W6 O3 155.7(10) . 2_655 ?
O5 W6 O14 100.6(6) . 2_655 ?
O3 W6 O14 88.4(7) . 2_655 ?
O3 W6 O14 87.1(7) 2_655 2_655 ?
O5 W6 O14 100.6(6) . . ?
O3 W6 O14 87.1(7) . . ?
O3 W6 O14 88.4(7) 2_655 . ?
O14 W6 O14 158.7(13) 2_655 . ?
O5 W6 O21 160.0(4) . . ?
O3 W6 O21 64.6(7) . . ?
O3 W6 O21 91.9(7) 2_655 . ?
O14 W6 O21 94.1(8) 2_655 . ?
O14 W6 O21 65.3(8) . . ?
O5 W6 O21 160.0(4) . 2_655 ?
O3 W6 O21 91.9(7) . 2_655 ?
O3 W6 O21 64.6(7) 2_655 2_655 ?
O14 W6 O21 65.3(8) 2_655 2_655 ?
O14 W6 O21 94.1(8) . 2_655 ?
O21 W6 O21 39.9(8) . 2_655 ?
O23 W7 O13 104.5(6) . . ?
O23 W7 O13 104.5(6) . 2_655 ?
O13 W7 O13 151.1(12) . 2_655 ?
O23 W7 O12 103.1(6) . . ?
O13 W7 O12 87.8(8) . . ?
O13 W7 O12 85.7(9) 2_655 . ?
O23 W7 O12 103.1(6) . 2_655 ?
O13 W7 O12 85.7(9) . 2_655 ?
O13 W7 O12 87.8(8) 2_655 2_655 ?
O12 W7 O12 153.7(12) . 2_655 ?
O1 P1 O1 77(2) . 2_655 ?
O1 P1 O22 72.1(14) . . ?
O1 P1 O22 108.7(14) 2_655 . ?
O1 P1 O22 108.7(14) . 2_655 ?
O1 P1 O22 72.1(14) 2_655 2_655 ?
O22 P1 O22 179(2) . 2_655 ?
O1 P1 O2 112.5(14) . 2_655 ?
O1 P1 O2 62.3(13) 2_655 2_655 ?
O22 P1 O2 73.6(13) . 2_655 ?
O22 P1 O2 106.5(13) 2_655 2_655 ?
O1 P1 O2 62.3(13) . . ?
O1 P1 O2 112.5(14) 2_655 . ?
O22 P1 O2 106.5(13) . . ?
O22 P1 O2 73.6(13) 2_655 . ?
O2 P1 O2 174.0(14) 2_655 . ?
O1 P1 O21 107.4(13) . . ?
O1 P1 O21 175.4(15) 2_655 . ?
O22 P1 O21 71.0(14) . . ?
O22 P1 O21 108.2(14) 2_655 . ?
O2 P1 O21 113.5(12) 2_655 . ?
O2 P1 O21 71.8(12) . . ?
O1 P1 O21 175.4(15) . 2_655 ?
O1 P1 O21 107.4(13) 2_655 2_655 ?
O22 P1 O21 108.2(14) . 2_655 ?
O22 P1 O21 71.0(14) 2_655 2_655 ?
O2 P1 O21 71.8(12) 2_655 2_655 ?
O2 P1 O21 113.5(12) . 2_655 ?
O21 P1 O21 68.7(19) . 2_655 ?
O24 Zn1 O24 112.1(8) 4_655 3_455 ?
O24 Zn1 O27 102.8(7) 4_655 2_655 ?
O24 Zn1 O27 106.4(7) 3_455 2_655 ?
O24 Zn1 O27 106.4(7) 4_655 . ?
O24 Zn1 O27 102.8(7) 3_455 . ?
O27 Zn1 O27 126.5(10) 2_655 . ?
P1 O1 O2 59.1(8) . . ?
P1 O1 O22 54.1(8) . . ?
O2 O1 O22 92.9(13) . . ?
P1 O1 W1 131.0(16) . . ?
O2 O1 W1 72.0(12) . . ?
O22 O1 W1 134.2(16) . . ?
P1 O1 W5 121.4(12) . 2_655 ?
O2 O1 W5 134.5(15) . 2_655 ?
O22 O1 W5 67.6(9) . 2_655 ?
W1 O1 W5 92.4(5) . 2_655 ?
P1 O2 O1 58.6(8) . . ?
P1 O2 O21 54.2(7) . . ?
O1 O2 O21 93.4(12) . . ?
P1 O2 O22 53.1(8) . 2_655 ?
O1 O2 O22 92.8(13) . 2_655 ?
O21 O2 O22 86.2(12) . 2_655 ?
P1 O2 W1 129.0(9) . . ?
O1 O2 W1 70.4(9) . . ?
O21 O2 W1 134.7(13) . . ?
O22 O2 W1 134.8(13) 2_655 . ?
P1 O2 W4 122.4(11) . . ?
O1 O2 W4 133.9(13) . . ?
O21 O2 W4 125.6(11) . . ?
O22 O2 W4 69.3(9) 2_655 . ?
W1 O2 W4 92.2(4) . . ?
W3 O3 W6 140.8(9) 2_655 . ?
W4 O4 W5 143.3(12) . . ?
W3 O8 W4 137.8(12) . . ?
W2 O9 W1 139.8(11) . . ?
W2 O10 W4 140.6(11) . . ?
W5 O11 W3 139.5(12) . . ?
W5 O12 W7 140.7(11) 2_655 . ?
W7 O13 W1 145.4(12) . . ?
W2 O14 W6 135.0(11) . . ?
W4 O16 W1 138.3(9) . . ?
W1 O17 W5 137.8(10) . 2_655 ?
W3 O18 W2 141.2(11) . 2_655 ?
P1 O21 O21 55.6(9) . 2_655 ?
P1 O21 O22 54.3(8) . . ?
O21 O21 O22 89.9(16) 2_655 . ?
P1 O21 O2 54.0(7) . . ?
O21 O21 O2 93.2(14) 2_655 . ?
O22 O21 O2 86.5(12) . . ?
P1 O21 W2 125.7(13) . . ?
O21 O21 W2 135.1(19) 2_655 . ?
O22 O21 W2 129.3(15) . . ?
O2 O21 W2 71.7(10) . . ?
P1 O21 W6 125.7(13) . . ?
O21 O21 W6 70.0(4) 2_655 . ?
O22 O21 W6 131.5(16) . . ?
O2 O21 W6 136.3(13) . . ?
W2 O21 W6 91.9(5) . . ?
P1 O22 O21 54.7(8) . . ?
P1 O22 O1 53.8(8) . . ?
O21 O22 O1 87.2(14) . . ?
P1 O22 O2 53.3(7) . 2_655 ?
O21 O22 O2 90.5(12) . 2_655 ?
O1 O22 O2 88.9(12) . 2_655 ?
P1 O22 W5 124.8(14) . 2_655 ?
O21 O22 W5 133.7(17) . 2_655 ?
O1 O22 W5 71.2(11) . 2_655 ?
O2 O22 W5 128.0(15) 2_655 2_655 ?
P1 O22 W3 126.0(14) . 2_655 ?
O21 O22 W3 71.4(10) . 2_655 ?
O1 O22 W3 130.7(17) . 2_655 ?
O2 O22 W3 133.5(15) 2_655 2_655 ?
W5 O22 W3 92.0(6) 2_655 2_655 ?
P1 O22 W4 122.1(14) . 2_655 ?
O21 O22 W4 130.6(16) . 2_655 ?
O1 O22 W4 134.1(17) . 2_655 ?
O2 O22 W4 68.9(10) 2_655 2_655 ?
W5 O22 W4 91.1(6) 2_655 2_655 ?
W3 O22 W4 90.6(6) 2_655 2_655 ?
C1 O24 Zn1 120.7(12) . 3_545 ?
C21 O27 Zn1 118.4(14) . . ?
C8 N1 C9 104.3(15) . . ?
C8 N1 C5 124.1(15) . . ?
C9 N1 C5 131.3(16) . . ?
C8 N2 C10 110.4(15) . . ?
C8 N2 C11 125.0(16) . . ?
C10 N2 C11 124.6(17) . . ?
C13 N3 C12 107.4(17) . . ?
C13 N3 C11 129.4(16) . . ?
C12 N3 C11 123.2(17) . . ?
C12 N4 C14 107.2(16) . . ?
C12 N4 C15 123.8(16) . . ?
C14 N4 C15 128.9(17) . . ?
O24 C1 O25 126.6(18) . . ?
O24 C1 C2 117.6(15) . . ?
O25 C1 C2 115.9(18) . . ?
C7 C2 C3 119.1(17) . . ?
C7 C2 C1 119.3(16) . . ?
C3 C2 C1 121.1(17) . . ?
C2 C3 C4 119.3(18) . . ?
C5 C4 C3 125.2(19) . . ?
C4 C5 N1 126.7(17) . . ?
C4 C5 C6 116.2(19) . . ?
N1 C5 C6 116.9(15) . . ?
C7 C6 C5 118.2(16) . . ?
C2 C7 C6 121.9(17) . . ?
N2 C8 N1 109.8(16) . . ?
N1 C9 C10 111.3(18) . . ?
N2 C10 C9 103.9(18) . . ?
N2 C11 N3 112.0(15) . . ?
N4 C12 N3 107.0(18) . . ?
C14 C13 N3 108.3(18) . . ?
C13 C14 N4 110(2) . . ?
N4 C15 C16 118.4(14) . . ?
N4 C15 C20 121.6(14) . . ?
C16 C15 C20 120.0 . . ?
C17 C16 C15 120.0 . . ?
C16 C17 C18 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 C21 101.8(19) . . ?
C19 C18 C21 137(2) . . ?
C20 C19 C18 120.0 . . ?
C19 C20 C15 120.0 . . ?
O27 C21 O26 115(2) . . ?
O27 C21 C18 107.1(16) . . ?
O26 C21 C18 137(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.299
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1048169'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 N8 O48 Si W12 Zn'
_chemical_formula_weight         3716.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   21.826(18)
_cell_length_b                   30.504(16)
_cell_length_c                   19.495(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.29(3)
_cell_angle_gamma                90.00
_cell_volume                     12771(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    38793
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      25.06

_exptl_crystal_description       needle
_exptl_crystal_colour            'light grey'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6624
_exptl_absorpt_coefficient_mu    11.012
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3592
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38815
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         25.06
_reflns_number_total             11297
_reflns_number_gt                4376
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1a (Brandenburg, 2005)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          SQUEEZE

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.005 -0.001 -0.016 6900 1251 ' '
_platon_squeeze_details          
;
About two [(CH₃)₂NH₂]⁺, seven DMF and thirteen water lattice 
guests were removed from the formula unit by the SQUEEZE process.
;

_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)+(0.0567P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11297
_refine_ls_number_parameters     490
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.0939
_refine_ls_wR_factor_ref         0.2386
_refine_ls_wR_factor_gt          0.2163
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.38218(6) 0.13286(3) 0.31348(5) 0.1235(4) Uani 1 1 d . . .
W2 W 0.38150(6) 0.24870(4) 0.31364(6) 0.1381(5) Uani 1 1 d . . .
W3 W 0.61503(7) 0.24870(3) 0.36601(5) 0.1267(4) Uani 1 1 d . . .
W4 W 0.49661(6) 0.19095(3) 0.42919(5) 0.1207(4) Uani 1 1 d . . .
W5 W 0.61338(7) 0.13372(4) 0.36623(6) 0.1492(5) Uani 1 1 d . . .
W6 W 0.5000 0.30596(5) 0.2500 0.1548(7) Uani 1 2 d S . .
W7 W 0.5000 0.07497(4) 0.2500 0.1553(8) Uani 1 2 d S . .
Si1 Si 0.5000 0.19090(18) 0.2500 0.0727(19) Uani 1 2 d SD . .
Zn1 Zn 0.5000 -0.18160(9) 0.2500 0.0856(9) Uani 1 2 d S . .
O1 O 0.4549(11) 0.1527(7) 0.2458(15) 0.118(9) Uani 0.50 1 d PDU . .
O2 O 0.4598(10) 0.1883(5) 0.3052(10) 0.087(7) Uani 0.50 1 d PD . .
O3 O 0.4380(9) 0.2935(6) 0.1654(9) 0.155(6) Uani 1 1 d U . .
O4 O 0.5583(8) 0.1481(6) 0.4256(10) 0.159(7) Uani 1 1 d . . .
O5 O 0.5000 0.3631(7) 0.2500 0.129(7) Uani 1 2 d S . .
O6 O 0.3252(15) 0.1043(10) 0.3457(15) 0.247(8) Uani 1 1 d U . .
O7 O 0.6679(9) 0.1050(5) 0.4220(7) 0.139(6) Uani 1 1 d . . .
O8 O 0.5591(8) 0.2353(5) 0.4246(9) 0.137(6) Uani 1 1 d . . .
O9 O 0.3531(9) 0.1910(8) 0.3123(8) 0.177(9) Uani 1 1 d . . .
O10 O 0.4315(9) 0.2342(6) 0.3972(10) 0.160(6) Uani 1 1 d U . .
O11 O 0.6464(8) 0.1908(6) 0.3812(11) 0.155(6) Uani 1 1 d . . .
O12 O 0.4385(12) 0.0861(8) 0.1734(10) 0.207(10) Uani 1 1 d . . .
O13 O 0.4373(10) 0.0876(6) 0.3031(9) 0.166(6) Uani 1 1 d U . .
O14 O 0.4385(12) 0.2955(7) 0.3031(8) 0.188(9) Uani 1 1 d . . .
O15 O 0.6705(9) 0.2742(6) 0.4162(9) 0.147(6) Uani 1 1 d . . .
O16 O 0.4385(10) 0.1496(7) 0.3968(8) 0.159(7) Uani 1 1 d . . .
O17 O 0.3546(13) 0.1306(6) 0.2172(9) 0.193(10) Uani 1 1 d . . .
O18 O 0.6500(11) 0.2502(7) 0.2856(11) 0.187(8) Uani 1 1 d . . .
O19 O 0.4951(11) 0.1918(5) 0.5138(9) 0.170(8) Uani 1 1 d . . .
O20 O 0.3241(8) 0.2745(4) 0.3415(7) 0.118(5) Uani 1 1 d . . .
O21 O 0.4556(11) 0.2293(7) 0.2375(14) 0.115(9) Uani 0.50 1 d PDU . .
O22 O 0.4626(11) 0.1931(8) 0.1780(7) 0.098(7) Uani 0.50 1 d PDU . .
O23 O 0.5000 0.0218(9) 0.2500 0.152(9) Uani 1 2 d S . .
O24 O 0.9641(6) -0.6445(4) 0.3154(6) 0.094(4) Uani 1 1 d U . .
O25 O 0.9081(7) -0.6027(4) 0.2343(6) 0.100(4) Uani 1 1 d . . .
O26 O 0.5554(9) -0.2114(6) 0.3221(9) 0.156(5) Uani 1 1 d D . .
O27 O 0.6092(14) -0.2408(10) 0.2425(12) 0.247(8) Uani 1 1 d DU . .
N1 N 0.9115(8) -0.4848(4) 0.5068(6) 0.086(4) Uani 1 1 d . . .
N2 N 0.9116(7) -0.4243(4) 0.5595(7) 0.083(4) Uani 1 1 d . . .
N3 N 0.8492(7) -0.3578(5) 0.5622(8) 0.078(4) Uani 1 1 d . . .
N4 N 0.7646(7) -0.3274(5) 0.5108(8) 0.080(4) Uani 1 1 d . . .
C1 C 0.9320(9) -0.6119(6) 0.2915(10) 0.082(5) Uani 1 1 d U . .
C2 C 0.9207(6) -0.5794(3) 0.3502(4) 0.073(5) Uani 1 1 d G . .
C3 C 0.9041(7) -0.5364(4) 0.3316(4) 0.106(7) Uani 1 1 d G . .
H3A H 0.8958 -0.5284 0.2848 0.128 Uiso 1 1 calc R . .
C4 C 0.8998(7) -0.5055(3) 0.3829(5) 0.108(7) Uani 1 1 d G . .
H4A H 0.8887 -0.4768 0.3705 0.130 Uiso 1 1 calc R . .
C5 C 0.9123(7) -0.5175(3) 0.4528(5) 0.080(5) Uani 1 1 d G . .
C6 C 0.9289(7) -0.5604(3) 0.4714(4) 0.098(6) Uani 1 1 d G . .
H6A H 0.9373 -0.5685 0.5181 0.118 Uiso 1 1 calc R . .
C7 C 0.9332(6) -0.5914(3) 0.4201(5) 0.098(6) Uani 1 1 d G . .
H7A H 0.9443 -0.6201 0.4325 0.118 Uiso 1 1 calc R . .
C8 C 0.9109(9) -0.4438(6) 0.5002(10) 0.094(6) Uani 1 1 d . . .
H8A H 0.9101 -0.4292 0.4582 0.112 Uiso 1 1 calc R . .
C9 C 0.9102(11) -0.4926(8) 0.5730(12) 0.120(7) Uani 1 1 d U . .
H9A H 0.9073 -0.5205 0.5914 0.144 Uiso 1 1 calc R . .
C10 C 0.9136(11) -0.4567(6) 0.6098(8) 0.102(7) Uani 1 1 d . . .
H10A H 0.9166 -0.4536 0.6577 0.123 Uiso 1 1 calc R . .
C11 C 0.9129(10) -0.3782(6) 0.5725(10) 0.097(6) Uani 1 1 d U . .
H11A H 0.9371 -0.3641 0.5416 0.116 Uiso 1 1 calc R . .
H11B H 0.9338 -0.3730 0.6201 0.116 Uiso 1 1 calc R . .
C12 C 0.8187(12) -0.3397(6) 0.5067(10) 0.089(6) Uani 1 1 d . . .
H12A H 0.8356 -0.3360 0.4665 0.107 Uiso 1 1 calc R . .
C13 C 0.8142(11) -0.3568(6) 0.6097(11) 0.097(6) Uani 1 1 d . . .
H13A H 0.8243 -0.3686 0.6542 0.117 Uiso 1 1 calc R . .
C14 C 0.7619(13) -0.3361(9) 0.5839(13) 0.132(8) Uani 1 1 d U . .
H14A H 0.7300 -0.3285 0.6076 0.159 Uiso 1 1 calc R . .
C15 C 0.7195(7) -0.3040(5) 0.4654(7) 0.109(7) Uani 1 1 d G . .
C16 C 0.6657(8) -0.2851(5) 0.4809(6) 0.147(12) Uani 1 1 d G . .
H16A H 0.6565 -0.2876 0.5256 0.176 Uiso 1 1 calc R . .
C17 C 0.6254(7) -0.2625(5) 0.4297(8) 0.107(6) Uani 1 1 d GU . .
H17A H 0.5894 -0.2498 0.4401 0.129 Uiso 1 1 calc R . .
C18 C 0.6390(8) -0.2587(5) 0.3630(7) 0.141(8) Uani 1 1 d GDU . .
C19 C 0.6929(9) -0.2775(6) 0.3475(6) 0.139(8) Uani 1 1 d GU . .
H19A H 0.7020 -0.2750 0.3028 0.167 Uiso 1 1 calc R . .
C20 C 0.7332(7) -0.3002(5) 0.3987(8) 0.153(9) Uani 1 1 d GU . .
H20A H 0.7692 -0.3128 0.3883 0.184 Uiso 1 1 calc R . .
C21 C 0.5992(11) -0.2350(9) 0.3030(10) 0.156(5) Uani 1 1 d DU . .


_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 1.73(3) . ?
W1 O13 1.87(2) . ?
W1 O17 1.868(17) . ?
W1 O9 1.88(2) . ?
W1 O16 1.922(19) . ?
W1 O1 2.32(2) . ?
W1 O2 2.420(17) . ?
W2 O20 1.652(16) . ?
W2 O10 1.845(19) . ?
W2 O9 1.86(2) . ?
W2 O14 1.93(2) . ?
W2 O18 1.93(2) 2_655 ?
W2 O21 2.46(3) . ?
W3 O15 1.613(17) . ?
W3 O3 1.825(18) 2_655 ?
W3 O8 1.860(19) . ?
W3 O18 1.86(2) . ?
W3 O11 1.899(17) . ?
W3 O21 2.38(2) 2_655 ?
W3 O22 2.44(2) 2_655 ?
W4 O19 1.657(19) . ?
W4 O16 1.82(2) . ?
W4 O4 1.89(2) . ?
W4 O8 1.936(17) . ?
W4 O10 1.96(2) . ?
W4 O2 2.41(2) . ?
W4 O22 2.41(2) 2_655 ?
W5 O7 1.704(16) . ?
W5 O4 1.86(2) . ?
W5 O17 1.88(2) 2_655 ?
W5 O11 1.887(19) . ?
W5 O12 1.92(2) 2_655 ?
W5 O1 2.48(2) 2_655 ?
W5 O22 2.50(2) 2_655 ?
W6 O5 1.74(2) . ?
W6 O14 1.86(2) 2_655 ?
W6 O14 1.86(2) . ?
W6 O3 1.974(17) . ?
W6 O3 1.974(17) 2_655 ?
W6 O21 2.53(3) 2_655 ?
W6 O21 2.53(3) . ?
W7 O23 1.62(3) . ?
W7 O12 1.85(2) 2_655 ?
W7 O12 1.85(2) . ?
W7 O13 1.90(2) . ?
W7 O13 1.90(2) 2_655 ?
Si1 O22 1.495(10) . ?
Si1 O22 1.495(10) 2_655 ?
Si1 O2 1.507(10) . ?
Si1 O2 1.507(10) 2_655 ?
Si1 O21 1.511(10) . ?
Si1 O21 1.511(10) 2_655 ?
Si1 O1 1.517(10) 2_655 ?
Si1 O1 1.517(10) . ?
Zn1 O26 1.911(18) 2_655 ?
Zn1 O26 1.911(18) . ?
Zn1 O24 1.969(12) 3_455 ?
Zn1 O24 1.969(12) 4_655 ?
O1 O2 1.58(3) . ?
O1 W5 2.48(2) 2_655 ?
O2 O22 1.67(3) 2_655 ?
O2 O21 1.81(3) . ?
O3 W3 1.825(18) 2_655 ?
O12 W5 1.92(2) 2_655 ?
O17 W5 1.88(2) 2_655 ?
O18 W2 1.93(2) 2_655 ?
O21 O22 1.63(3) . ?
O21 W3 2.38(2) 2_655 ?
O22 O2 1.67(3) 2_655 ?
O22 W4 2.41(2) 2_655 ?
O22 W3 2.44(2) 2_655 ?
O22 W5 2.50(2) 2_655 ?
O24 C1 1.26(2) . ?
O24 Zn1 1.969(12) 3_545 ?
O25 C1 1.178(19) . ?
O26 C21 1.303(10) . ?
O27 C21 1.250(10) . ?
N1 C8 1.26(2) . ?
N1 C9 1.32(3) . ?
N1 C5 1.452(15) . ?
N2 C8 1.30(2) . ?
N2 C10 1.39(2) . ?
N2 C11 1.43(2) . ?
N3 C12 1.29(2) . ?
N3 C13 1.30(2) . ?
N3 C11 1.50(2) . ?
N4 C12 1.26(2) . ?
N4 C15 1.396(17) . ?
N4 C14 1.46(3) . ?
C1 C2 1.567(19) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C9 C10 1.30(3) . ?
C13 C14 1.32(3) . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 C21 1.512(10) . ?
C19 C20 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O13 100.7(13) . . ?
O6 W1 O17 102.9(13) . . ?
O13 W1 O17 87.8(7) . . ?
O6 W1 O9 102.5(12) . . ?
O13 W1 O9 156.7(10) . . ?
O17 W1 O9 88.6(6) . . ?
O6 W1 O16 102.7(11) . . ?
O13 W1 O16 87.7(7) . . ?
O17 W1 O16 154.4(11) . . ?
O9 W1 O16 85.6(7) . . ?
O6 W1 O1 161.8(12) . . ?
O13 W1 O1 67.1(10) . . ?
O17 W1 O1 64.5(10) . . ?
O9 W1 O1 90.6(9) . . ?
O16 W1 O1 90.7(8) . . ?
O6 W1 O2 159.3(11) . . ?
O13 W1 O2 92.1(8) . . ?
O17 W1 O2 93.6(10) . . ?
O9 W1 O2 65.1(7) . . ?
O16 W1 O2 61.4(8) . . ?
O1 W1 O2 38.8(6) . . ?
O20 W2 O10 100.8(8) . . ?
O20 W2 O9 100.6(8) . . ?
O10 W2 O9 86.0(8) . . ?
O20 W2 O14 102.9(9) . . ?
O10 W2 O14 88.8(9) . . ?
O9 W2 O14 156.5(10) . . ?
O20 W2 O18 99.4(9) . 2_655 ?
O10 W2 O18 159.5(10) . 2_655 ?
O9 W2 O18 87.2(8) . 2_655 ?
O14 W2 O18 89.8(7) . 2_655 ?
O20 W2 O21 159.1(6) . . ?
O10 W2 O21 97.2(8) . . ?
O9 W2 O21 91.0(8) . . ?
O14 W2 O21 66.9(9) . . ?
O18 W2 O21 63.6(9) 2_655 . ?
O15 W3 O3 101.8(9) . 2_655 ?
O15 W3 O8 103.7(8) . . ?
O3 W3 O8 85.6(7) 2_655 . ?
O15 W3 O18 97.0(10) . . ?
O3 W3 O18 91.7(8) 2_655 . ?
O8 W3 O18 159.2(10) . . ?
O15 W3 O11 98.2(9) . . ?
O3 W3 O11 159.9(9) 2_655 . ?
O8 W3 O11 87.6(7) . . ?
O18 W3 O11 88.0(8) . . ?
O15 W3 O21 159.1(8) . 2_655 ?
O3 W3 O21 68.1(9) 2_655 2_655 ?
O8 W3 O21 94.0(8) . 2_655 ?
O18 W3 O21 66.0(10) . 2_655 ?
O11 W3 O21 93.5(9) . 2_655 ?
O15 W3 O22 161.1(7) . 2_655 ?
O3 W3 O22 92.5(8) 2_655 2_655 ?
O8 W3 O22 64.7(8) . 2_655 ?
O18 W3 O22 94.8(10) . 2_655 ?
O11 W3 O22 67.5(8) . 2_655 ?
O21 W3 O22 39.4(6) 2_655 2_655 ?
O19 W4 O16 102.7(8) . . ?
O19 W4 O4 100.9(10) . . ?
O16 W4 O4 88.0(8) . . ?
O19 W4 O8 100.1(8) . . ?
O16 W4 O8 157.2(7) . . ?
O4 W4 O8 88.2(7) . . ?
O19 W4 O10 99.5(10) . . ?
O16 W4 O10 86.4(7) . . ?
O4 W4 O10 159.5(8) . . ?
O8 W4 O10 89.5(7) . . ?
O19 W4 O2 159.7(9) . . ?
O16 W4 O2 62.7(6) . . ?
O4 W4 O2 93.0(7) . . ?
O8 W4 O2 95.1(6) . . ?
O10 W4 O2 67.0(7) . . ?
O19 W4 O22 159.7(9) . 2_655 ?
O16 W4 O22 93.5(7) . 2_655 ?
O4 W4 O22 67.1(8) . 2_655 ?
O8 W4 O22 64.5(7) . 2_655 ?
O10 W4 O22 93.7(8) . 2_655 ?
O2 W4 O22 40.6(6) . 2_655 ?
O7 W5 O4 100.4(8) . . ?
O7 W5 O17 101.5(10) . 2_655 ?
O4 W5 O17 158.1(10) . 2_655 ?
O7 W5 O11 99.9(8) . . ?
O4 W5 O11 87.6(8) . . ?
O17 W5 O11 89.4(7) 2_655 . ?
O7 W5 O12 99.3(9) . 2_655 ?
O4 W5 O12 91.7(10) . 2_655 ?
O17 W5 O12 84.1(8) 2_655 2_655 ?
O11 W5 O12 160.6(9) . 2_655 ?
O7 W5 O1 157.3(7) . 2_655 ?
O4 W5 O1 98.0(8) . 2_655 ?
O17 W5 O1 60.7(10) 2_655 2_655 ?
O11 W5 O1 94.2(8) . 2_655 ?
O12 W5 O1 66.7(8) 2_655 2_655 ?
O7 W5 O22 159.4(6) . 2_655 ?
O4 W5 O22 65.3(8) . 2_655 ?
O17 W5 O22 93.7(9) 2_655 2_655 ?
O11 W5 O22 66.2(7) . 2_655 ?
O12 W5 O22 95.9(9) 2_655 2_655 ?
O1 W5 O22 43.2(5) 2_655 2_655 ?
O5 W6 O14 99.8(7) . 2_655 ?
O5 W6 O14 99.8(7) . . ?
O14 W6 O14 160.3(14) 2_655 . ?
O5 W6 O3 101.1(6) . . ?
O14 W6 O3 87.5(9) 2_655 . ?
O14 W6 O3 88.7(8) . . ?
O5 W6 O3 101.1(6) . 2_655 ?
O14 W6 O3 88.7(8) 2_655 2_655 ?
O14 W6 O3 87.5(9) . 2_655 ?
O3 W6 O3 157.9(12) . 2_655 ?
O5 W6 O21 157.8(4) . 2_655 ?
O14 W6 O21 66.0(8) 2_655 2_655 ?
O14 W6 O21 95.2(9) . 2_655 ?
O3 W6 O21 95.6(7) . 2_655 ?
O3 W6 O21 63.1(8) 2_655 2_655 ?
O5 W6 O21 157.8(4) . . ?
O14 W6 O21 95.2(9) 2_655 . ?
O14 W6 O21 66.0(8) . . ?
O3 W6 O21 63.1(8) . . ?
O3 W6 O21 95.6(7) 2_655 . ?
O21 W6 O21 44.5(8) 2_655 . ?
O23 W7 O12 100.5(7) . 2_655 ?
O23 W7 O12 100.5(7) . . ?
O12 W7 O12 159.0(15) 2_655 . ?
O23 W7 O13 101.7(6) . . ?
O12 W7 O13 90.7(10) 2_655 . ?
O12 W7 O13 85.0(9) . . ?
O23 W7 O13 101.7(6) . 2_655 ?
O12 W7 O13 85.0(9) 2_655 2_655 ?
O12 W7 O13 90.7(10) . 2_655 ?
O13 W7 O13 156.6(12) . 2_655 ?
O22 Si1 O22 174.8(19) . 2_655 ?
O22 Si1 O2 112.5(14) . . ?
O22 Si1 O2 67.8(14) 2_655 . ?
O22 Si1 O2 67.8(14) . 2_655 ?
O22 Si1 O2 112.5(14) 2_655 2_655 ?
O2 Si1 O2 174.0(13) . 2_655 ?
O22 Si1 O21 65.6(14) . . ?
O22 Si1 O21 110.1(15) 2_655 . ?
O2 Si1 O21 73.6(13) . . ?
O2 Si1 O21 111.3(14) 2_655 . ?
O22 Si1 O21 110.1(15) . 2_655 ?
O22 Si1 O21 65.6(14) 2_655 2_655 ?
O2 Si1 O21 111.3(14) . 2_655 ?
O2 Si1 O21 73.6(13) 2_655 2_655 ?
O21 Si1 O21 79(2) . 2_655 ?
O22 Si1 O1 109.0(15) . 2_655 ?
O22 Si1 O1 75.2(14) 2_655 2_655 ?
O2 Si1 O1 112.1(14) . 2_655 ?
O2 Si1 O1 62.8(13) 2_655 2_655 ?
O21 Si1 O1 173.7(14) . 2_655 ?
O21 Si1 O1 101.2(16) 2_655 2_655 ?
O22 Si1 O1 75.2(14) . . ?
O22 Si1 O1 109.0(15) 2_655 . ?
O2 Si1 O1 62.8(13) . . ?
O2 Si1 O1 112.1(14) 2_655 . ?
O21 Si1 O1 101.2(16) . . ?
O21 Si1 O1 173.7(14) 2_655 . ?
O1 Si1 O1 80(2) 2_655 . ?
O26 Zn1 O26 123.3(12) 2_655 . ?
O26 Zn1 O24 118.5(7) 2_655 3_455 ?
O26 Zn1 O24 94.0(7) . 3_455 ?
O26 Zn1 O24 94.0(7) 2_655 4_655 ?
O26 Zn1 O24 118.5(7) . 4_655 ?
O24 Zn1 O24 109.8(8) 3_455 4_655 ?
Si1 O1 O2 58.3(8) . . ?
Si1 O1 W1 132.4(17) . . ?
O2 O1 W1 74.1(12) . . ?
Si1 O1 W5 120.5(14) . 2_655 ?
O2 O1 W5 139.3(18) . 2_655 ?
W1 O1 W5 94.3(6) . 2_655 ?
Si1 O2 O1 58.9(8) . . ?
Si1 O2 O22 55.8(8) . 2_655 ?
O1 O2 O22 97.9(13) . 2_655 ?
Si1 O2 O21 53.3(8) . . ?
O1 O2 O21 87.2(14) . . ?
O22 O2 O21 90.0(13) 2_655 . ?
Si1 O2 W4 125.6(13) . . ?
O1 O2 W4 136.6(14) . . ?
O22 O2 W4 69.9(10) 2_655 . ?
O21 O2 W4 132.4(13) . . ?
Si1 O2 W1 126.0(10) . . ?
O1 O2 W1 67.1(10) . . ?
O22 O2 W1 138.1(13) 2_655 . ?
O21 O2 W1 126.0(15) . . ?
W4 O2 W1 93.9(4) . . ?
W3 O3 W6 136.3(11) 2_655 . ?
W5 O4 W4 136.9(9) . . ?
W3 O8 W4 136.6(9) . . ?
W2 O9 W1 141.1(11) . . ?
W2 O10 W4 136.4(10) . . ?
W5 O11 W3 135.8(10) . . ?
W7 O12 W5 138.9(11) . 2_655 ?
W1 O13 W7 138.7(12) . . ?
W6 O14 W2 136.7(11) . . ?
W4 O16 W1 141.1(10) . . ?
W1 O17 W5 139.7(16) . 2_655 ?
W3 O18 W2 135.7(13) . 2_655 ?
Si1 O21 O22 56.7(8) . . ?
Si1 O21 O2 53.1(7) . . ?
O22 O21 O2 93.1(12) . . ?
Si1 O21 W3 128.9(14) . 2_655 ?
O22 O21 W3 72.2(11) . 2_655 ?
O2 O21 W3 136.9(17) . 2_655 ?
Si1 O21 W2 124.2(15) . . ?
O22 O21 W2 138.6(19) . . ?
O2 O21 W2 71.2(10) . . ?
W3 O21 W2 93.2(6) 2_655 . ?
Si1 O21 W6 118.5(15) . . ?
O22 O21 W6 127.8(19) . . ?
O2 O21 W6 126.9(15) . . ?
W3 O21 W6 91.7(7) 2_655 . ?
W2 O21 W6 90.1(6) . . ?
Si1 O22 O21 57.7(8) . . ?
Si1 O22 O2 56.5(8) . 2_655 ?
O21 O22 O2 98.0(13) . 2_655 ?
Si1 O22 W4 126.0(15) . 2_655 ?
O21 O22 W4 137.0(17) . 2_655 ?
O2 O22 W4 69.5(11) 2_655 2_655 ?
Si1 O22 W3 126.1(14) . 2_655 ?
O21 O22 W3 68.4(10) . 2_655 ?
O2 O22 W3 138.1(14) 2_655 2_655 ?
W4 O22 W3 93.2(5) 2_655 2_655 ?
Si1 O22 W5 120.5(13) . 2_655 ?
O21 O22 W5 126.5(18) . 2_655 ?
O2 O22 W5 126.1(14) 2_655 2_655 ?
W4 O22 W5 90.4(6) 2_655 2_655 ?
W3 O22 W5 90.4(6) 2_655 2_655 ?
C1 O24 Zn1 118.4(11) . 3_545 ?
C21 O26 Zn1 116.9(13) . . ?
C8 N1 C9 106.1(17) . . ?
C8 N1 C5 127.6(14) . . ?
C9 N1 C5 126.2(15) . . ?
C8 N2 C10 107.3(14) . . ?
C8 N2 C11 127.2(16) . . ?
C10 N2 C11 125.4(14) . . ?
C12 N3 C13 107.8(17) . . ?
C12 N3 C11 128.0(19) . . ?
C13 N3 C11 124.1(16) . . ?
C12 N4 C15 132.6(18) . . ?
C12 N4 C14 102.1(17) . . ?
C15 N4 C14 124.4(19) . . ?
O25 C1 O24 131.5(18) . . ?
O25 C1 C2 116.1(17) . . ?
O24 C1 C2 112.3(15) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 118.3(10) . . ?
C7 C2 C1 121.3(10) . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 N1 120.3(8) . . ?
C6 C5 N1 119.6(8) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C2 120.0 . . ?
N1 C8 N2 111.5(17) . . ?
C10 C9 N1 112(2) . . ?
C9 C10 N2 102.6(16) . . ?
N2 C11 N3 113.2(15) . . ?
N4 C12 N3 115(2) . . ?
N3 C13 C14 108.6(19) . . ?
C13 C14 N4 106(2) . . ?
C16 C15 C20 120.0 . . ?
C16 C15 N4 127.0(13) . . ?
C20 C15 N4 113.0(13) . . ?
C15 C16 C17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 C21 115.0(14) . . ?
C17 C18 C21 125.0(14) . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C15 120.0 . . ?
O27 C21 O26 128(2) . . ?
O27 C21 C18 119(2) . . ?
O26 C21 C18 113.2(18) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.267
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1048170'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 B N8 O48 W12 Zn'
_chemical_formula_weight         3699.14

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   20.949(12)
_cell_length_b                   31.1225(14)
_cell_length_c                   19.7567(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.761(15)
_cell_angle_gamma                90.00
_cell_volume                     12695(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18815
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      24.71

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6588
_exptl_absorpt_coefficient_mu    11.069
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_T_max  0.515
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3592
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18815
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         24.71
_reflns_number_total             10464
_reflns_number_gt                3873
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1a (Brandenburg, 2005)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          SQUEEZE

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.004 -0.003 -0.011 6867 1211 ' '
_platon_squeeze_details          
;
About three [(CH₃)₂NH₂]⁺, four DMF and four water lattice 
guests were removed from the formula unit by the SQUEEZE process.
;

_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)+(0.0469P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10464
_refine_ls_number_parameters     484
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.2027
_refine_ls_wR_factor_gt          0.1835
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.38061(6) 0.13044(3) 0.31526(5) 0.1099(4) Uani 1 1 d . . .
W2 W 0.37964(7) 0.24281(4) 0.31502(6) 0.1296(5) Uani 1 1 d . . .
W3 W 0.61828(6) 0.24335(4) 0.36141(6) 0.1233(4) Uani 1 1 d . . .
W4 W 0.49765(6) 0.18720(4) 0.42588(6) 0.1239(4) Uani 1 1 d . . .
W5 W 0.61798(6) 0.13050(4) 0.36059(7) 0.1272(4) Uani 1 1 d . . .
W6 W 0.5000 0.29916(4) 0.2500 0.1133(5) Uani 1 2 d S . .
W7 W 0.5000 0.07367(4) 0.2500 0.1317(6) Uani 1 2 d S . .
B1 B 0.5000 0.1873(5) 0.2500 0.046(6) Uani 1 2 d SD . .
Zn1 Zn 0.5000 -0.17837(10) 0.2500 0.0882(10) Uani 1 2 d S . .
O1 O 0.4583(10) 0.1479(6) 0.2499(12) 0.086(7) Uani 0.50 1 d PDU . .
O2 O 0.4549(9) 0.1848(6) 0.3017(9) 0.072(6) Uani 0.50 1 d PD . .
O3 O 0.4365(9) 0.2860(5) 0.1698(9) 0.143(6) Uani 1 1 d . . .
O4 O 0.5626(13) 0.1466(7) 0.4102(13) 0.206(9) Uani 1 1 d U . .
O5 O 0.5000 0.3502(10) 0.2500 0.184(11) Uani 1 2 d SU . .
O6 O 0.3303(11) 0.1024(7) 0.3481(10) 0.176(7) Uani 1 1 d U . .
O7 O 0.6732(9) 0.1033(5) 0.4137(9) 0.149(6) Uani 1 1 d . . .
O8 O 0.5620(9) 0.2297(5) 0.4177(9) 0.145(6) Uani 1 1 d U . .
O9 O 0.3467(10) 0.1854(7) 0.3131(8) 0.162(7) Uani 1 1 d . . .
O10 O 0.4406(11) 0.2283(5) 0.3989(9) 0.173(8) Uani 1 1 d . . .
O11 O 0.6512(11) 0.1849(6) 0.3734(10) 0.173(7) Uani 1 1 d U . .
O12 O 0.4371(11) 0.0868(6) 0.1701(10) 0.180(8) Uani 1 1 d . . .
O13 O 0.4373(11) 0.0859(5) 0.3042(8) 0.158(7) Uani 1 1 d . . .
O14 O 0.4368(10) 0.2877(6) 0.3034(9) 0.159(7) Uani 1 1 d . . .
O15 O 0.6741(10) 0.2695(5) 0.4125(10) 0.155(7) Uani 1 1 d . . .
O16 O 0.4368(10) 0.1453(5) 0.3994(9) 0.152(7) Uani 1 1 d . . .
O17 O 0.3499(10) 0.1287(5) 0.2212(10) 0.160(7) Uani 1 1 d . . .
O18 O 0.6475(10) 0.2440(6) 0.2827(10) 0.166(7) Uani 1 1 d U . .
O19 O 0.4960(9) 0.1864(5) 0.5062(10) 0.147(6) Uani 1 1 d . . .
O20 O 0.3256(11) 0.2702(4) 0.3454(9) 0.166(8) Uani 1 1 d . . .
O21 O 0.4583(11) 0.2270(6) 0.2437(11) 0.086(7) Uani 0.50 1 d PD . .
O22 O 0.5385(14) 0.1857(9) 0.3220(8) 0.117(9) Uani 0.50 1 d PDU . .
O23 O 0.5000 0.0221(8) 0.2500 0.168(10) Uani 1 2 d S . .
O24 O 0.9612(7) -0.6422(4) 0.3157(6) 0.099(4) Uani 1 1 d . . .
O25 O 0.9064(8) -0.6003(4) 0.2344(7) 0.108(4) Uani 1 1 d . . .
O26 O 0.5067(12) -0.2443(6) 0.3383(10) 0.176(6) Uani 1 1 d U . .
O27 O 0.5736(10) -0.2060(6) 0.3050(10) 0.157(7) Uani 1 1 d U . .
N1 N 0.9064(9) -0.4859(5) 0.5079(9) 0.093(5) Uani 1 1 d . . .
N2 N 0.9055(8) -0.4250(4) 0.5594(10) 0.085(5) Uani 1 1 d . . .
N3 N 0.8420(9) -0.3608(5) 0.5656(10) 0.097(5) Uani 1 1 d . . .
N4 N 0.7551(9) -0.3293(5) 0.5195(9) 0.086(5) Uani 1 1 d . . .
C1 C 0.9307(12) -0.6092(7) 0.2968(13) 0.101(6) Uani 1 1 d U . .
C2 C 0.9203(7) -0.5774(4) 0.3532(6) 0.091(6) Uani 1 1 d G . .
C3 C 0.9029(8) -0.5354(5) 0.3346(5) 0.123(9) Uani 1 1 d G . .
H3A H 0.8956 -0.5274 0.2886 0.148 Uiso 1 1 calc R . .
C4 C 0.8966(8) -0.5052(3) 0.3850(7) 0.108(8) Uani 1 1 d G . .
H4A H 0.8850 -0.4771 0.3726 0.130 Uiso 1 1 calc R . .
C5 C 0.9076(8) -0.5171(4) 0.4538(6) 0.088(6) Uani 1 1 d G . .
C6 C 0.9249(7) -0.5591(4) 0.4723(5) 0.101(7) Uani 1 1 d G . .
H6A H 0.9323 -0.5670 0.5184 0.121 Uiso 1 1 calc R . .
C7 C 0.9313(7) -0.5893(3) 0.4220(7) 0.086(6) Uani 1 1 d G . .
H7A H 0.9429 -0.6174 0.4344 0.103 Uiso 1 1 calc R . .
C8 C 0.9075(10) -0.4453(7) 0.5000(11) 0.091(6) Uani 1 1 d . . .
H8A H 0.9095 -0.4316 0.4586 0.109 Uiso 1 1 calc R . .
C9 C 0.9100(13) -0.4941(7) 0.5769(11) 0.110(8) Uani 1 1 d . . .
H9A H 0.9152 -0.5210 0.5976 0.133 Uiso 1 1 calc R . .
C10 C 0.9045(13) -0.4562(8) 0.6097(11) 0.119(8) Uani 1 1 d . . .
H10A H 0.9010 -0.4521 0.6556 0.143 Uiso 1 1 calc R . .
C11 C 0.9089(12) -0.3789(7) 0.5731(12) 0.113(7) Uani 1 1 d U . .
H11A H 0.9325 -0.3648 0.5411 0.136 Uiso 1 1 calc R . .
H11B H 0.9319 -0.3737 0.6193 0.136 Uiso 1 1 calc R . .
C12 C 0.8137(13) -0.3391(7) 0.5103(12) 0.106(7) Uani 1 1 d . . .
H12A H 0.8322 -0.3322 0.4721 0.127 Uiso 1 1 calc R . .
C13 C 0.8016(16) -0.3612(8) 0.6112(12) 0.125(9) Uani 1 1 d . . .
H13A H 0.8106 -0.3722 0.6555 0.149 Uiso 1 1 calc R . .
C14 C 0.7488(14) -0.3438(8) 0.5834(12) 0.118(8) Uani 1 1 d . . .
H14A H 0.7118 -0.3414 0.6033 0.142 Uiso 1 1 calc R . .
C15 C 0.7114(10) -0.3029(6) 0.4707(10) 0.158(7) Uani 1 1 d GU . .
C16 C 0.6490(11) -0.2964(6) 0.4836(8) 0.139(9) Uani 1 1 d GU . .
H16A H 0.6369 -0.3074 0.5233 0.166 Uiso 1 1 calc R . .
C17 C 0.6046(8) -0.2733(6) 0.4373(12) 0.158(7) Uani 1 1 d GU . .
H17A H 0.5628 -0.2689 0.4460 0.190 Uiso 1 1 calc R . .
C18 C 0.6226(11) -0.2567(6) 0.3780(10) 0.176(6) Uani 1 1 d GDU . .
C19 C 0.6851(12) -0.2632(7) 0.3650(9) 0.189(9) Uani 1 1 d GU . .
H19A H 0.6971 -0.2521 0.3254 0.227 Uiso 1 1 calc R . .
C20 C 0.7295(9) -0.2863(7) 0.4114(12) 0.189(9) Uani 1 1 d G . .
H20A H 0.7713 -0.2907 0.4027 0.227 Uiso 1 1 calc R . .
C21 C 0.5701(14) -0.2315(9) 0.3346(16) 0.150(11) Uani 1 1 d DU . .


_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 1.59(2) . ?
W1 O9 1.85(2) . ?
W1 O17 1.86(2) . ?
W1 O13 1.862(18) . ?
W1 O16 1.924(17) . ?
W1 O1 2.31(2) . ?
W1 O2 2.345(17) . ?
W2 O20 1.61(2) . ?
W2 O14 1.88(2) . ?
W2 O9 1.91(2) . ?
W2 O18 1.92(2) 2_655 ?
W2 O10 1.97(2) . ?
W2 O21 2.39(2) . ?
W2 O2 2.439(17) . ?
W3 O15 1.628(19) . ?
W3 O18 1.77(2) . ?
W3 O3 1.794(18) 2_655 ?
W3 O8 1.80(2) . ?
W3 O11 1.95(2) . ?
W3 O21 2.45(2) 2_655 ?
W3 O22 2.49(3) . ?
W4 O19 1.594(19) . ?
W4 O10 1.77(2) . ?
W4 O16 1.84(2) . ?
W4 O8 1.915(19) . ?
W4 O4 1.92(3) . ?
W4 O22 2.35(3) . ?
W4 O2 2.467(19) . ?
W5 O7 1.656(17) . ?
W5 O4 1.71(3) . ?
W5 O12 1.82(2) 2_655 ?
W5 O11 1.83(2) . ?
W5 O17 1.85(2) 2_655 ?
W5 O22 2.42(2) . ?
W6 O5 1.59(3) . ?
W6 O14 1.86(2) . ?
W6 O14 1.86(2) 2_655 ?
W6 O3 1.933(19) . ?
W6 O3 1.933(19) 2_655 ?
W6 O21 2.40(2) 2_655 ?
W6 O21 2.40(2) . ?
W7 O23 1.61(3) . ?
W7 O13 1.87(2) . ?
W7 O13 1.87(2) 2_655 ?
W7 O12 1.92(2) 2_655 ?
W7 O12 1.92(2) . ?
W7 O1 2.47(2) . ?
W7 O1 2.47(2) 2_655 ?
B1 O2 1.506(9) . ?
B1 O2 1.506(9) 2_655 ?
B1 O21 1.507(10) . ?
B1 O21 1.507(10) 2_655 ?
B1 O1 1.507(10) . ?
B1 O1 1.507(10) 2_655 ?
B1 O22 1.512(10) 2_655 ?
B1 O22 1.512(10) . ?
Zn1 O27 1.93(2) 2_655 ?
Zn1 O27 1.93(2) . ?
Zn1 O24 1.992(13) 3_455 ?
Zn1 O24 1.992(13) 4_655 ?
O1 O2 1.55(3) . ?
O1 O1 1.75(4) 2_655 ?
O2 O22 1.73(3) . ?
O2 O21 1.75(3) . ?
O3 W3 1.794(18) 2_655 ?
O12 W5 1.82(2) 2_655 ?
O17 W5 1.85(2) 2_655 ?
O18 W2 1.92(2) 2_655 ?
O21 O21 1.72(5) 2_655 ?
O21 W3 2.45(2) 2_655 ?
O24 C1 1.23(2) . ?
O24 Zn1 1.992(13) 3_545 ?
O25 C1 1.28(2) . ?
O26 C21 1.40(3) . ?
O27 C21 1.00(3) . ?
N1 C8 1.27(2) . ?
N1 C9 1.38(2) . ?
N1 C5 1.447(18) . ?
N2 C8 1.34(2) . ?
N2 C10 1.39(2) . ?
N2 C11 1.46(2) . ?
N3 C12 1.34(2) . ?
N3 C13 1.34(3) . ?
N3 C11 1.49(3) . ?
N4 C12 1.31(3) . ?
N4 C14 1.37(2) . ?
N4 C15 1.46(2) . ?
C1 C2 1.53(3) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C9 C10 1.36(3) . ?
C13 C14 1.27(3) . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 C21 1.495(10) . ?
C19 C20 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O9 103.8(10) . . ?
O6 W1 O17 104.5(10) . . ?
O9 W1 O17 86.4(7) . . ?
O6 W1 O13 96.9(10) . . ?
O9 W1 O13 159.3(9) . . ?
O17 W1 O13 88.9(7) . . ?
O6 W1 O16 97.5(10) . . ?
O9 W1 O16 88.5(7) . . ?
O17 W1 O16 158.0(9) . . ?
O13 W1 O16 88.3(7) . . ?
O6 W1 O1 159.6(9) . . ?
O9 W1 O1 94.3(8) . . ?
O17 W1 O1 66.8(8) . . ?
O13 W1 O1 65.5(8) . . ?
O16 W1 O1 92.3(8) . . ?
O6 W1 O2 160.4(8) . . ?
O9 W1 O2 65.8(7) . . ?
O17 W1 O2 91.8(8) . . ?
O13 W1 O2 94.3(8) . . ?
O16 W1 O2 66.7(8) . . ?
O1 W1 O2 38.9(6) . . ?
O20 W2 O14 98.9(9) . . ?
O20 W2 O9 103.1(9) . . ?
O14 W2 O9 158.0(9) . . ?
O20 W2 O18 104.9(9) . 2_655 ?
O14 W2 O18 87.1(8) . 2_655 ?
O9 W2 O18 87.4(7) . 2_655 ?
O20 W2 O10 101.8(9) . . ?
O14 W2 O10 86.5(7) . . ?
O9 W2 O10 89.0(7) . . ?
O18 W2 O10 153.2(9) 2_655 . ?
O20 W2 O21 157.6(7) . . ?
O14 W2 O21 64.2(8) . . ?
O9 W2 O21 94.5(8) . . ?
O18 W2 O21 61.8(8) 2_655 . ?
O10 W2 O21 92.1(8) . . ?
O20 W2 O2 159.8(6) . . ?
O14 W2 O2 95.8(8) . . ?
O9 W2 O2 62.9(8) . . ?
O18 W2 O2 89.5(8) 2_655 . ?
O10 W2 O2 65.3(7) . . ?
O21 W2 O2 42.5(5) . . ?
O15 W3 O18 102.7(9) . . ?
O15 W3 O3 101.1(8) . 2_655 ?
O18 W3 O3 89.2(8) . 2_655 ?
O15 W3 O8 102.2(9) . . ?
O18 W3 O8 155.0(9) . . ?
O3 W3 O8 86.5(8) 2_655 . ?
O15 W3 O11 101.0(9) . . ?
O18 W3 O11 87.1(9) . . ?
O3 W3 O11 157.9(8) 2_655 . ?
O8 W3 O11 87.7(8) . . ?
O15 W3 O21 157.9(7) . 2_655 ?
O18 W3 O21 62.0(9) . 2_655 ?
O3 W3 O21 64.8(8) 2_655 2_655 ?
O8 W3 O21 94.1(8) . 2_655 ?
O11 W3 O21 94.4(8) . 2_655 ?
O15 W3 O22 158.4(7) . . ?
O18 W3 O22 92.7(9) . . ?
O3 W3 O22 94.0(8) 2_655 . ?
O8 W3 O22 63.2(8) . . ?
O11 W3 O22 64.5(9) . . ?
O21 W3 O22 43.7(5) 2_655 . ?
O19 W4 O10 100.6(9) . . ?
O19 W4 O16 98.1(8) . . ?
O10 W4 O16 91.5(8) . . ?
O19 W4 O8 103.2(8) . . ?
O10 W4 O8 85.7(8) . . ?
O16 W4 O8 158.6(8) . . ?
O19 W4 O4 106.6(10) . . ?
O10 W4 O4 152.6(9) . . ?
O16 W4 O4 87.8(9) . . ?
O8 W4 O4 85.0(9) . . ?
O19 W4 O22 160.1(8) . . ?
O10 W4 O22 94.5(9) . . ?
O16 W4 O22 94.3(9) . . ?
O8 W4 O22 64.9(8) . . ?
O4 W4 O22 58.3(9) . . ?
O19 W4 O2 157.6(7) . . ?
O10 W4 O2 67.0(7) . . ?
O16 W4 O2 65.0(7) . . ?
O8 W4 O2 94.5(7) . . ?
O4 W4 O2 88.1(8) . . ?
O22 W4 O2 42.0(6) . . ?
O7 W5 O4 104.7(10) . . ?
O7 W5 O12 99.5(9) . 2_655 ?
O4 W5 O12 87.5(11) . 2_655 ?
O7 W5 O11 100.1(9) . . ?
O4 W5 O11 86.0(10) . . ?
O12 W5 O11 160.3(9) 2_655 . ?
O7 W5 O17 102.7(9) . 2_655 ?
O4 W5 O17 152.6(10) . 2_655 ?
O12 W5 O17 89.4(8) 2_655 2_655 ?
O11 W5 O17 87.9(8) . 2_655 ?
O7 W5 O22 158.4(7) . . ?
O4 W5 O22 58.5(10) . . ?
O12 W5 O22 93.6(9) 2_655 . ?
O11 W5 O22 67.2(10) . . ?
O17 W5 O22 94.5(9) 2_655 . ?
O5 W6 O14 101.0(6) . . ?
O5 W6 O14 101.0(6) . 2_655 ?
O14 W6 O14 158.0(12) . 2_655 ?
O5 W6 O3 102.2(5) . . ?
O14 W6 O3 88.1(7) . . ?
O14 W6 O3 87.2(7) 2_655 . ?
O5 W6 O3 102.2(5) . 2_655 ?
O14 W6 O3 87.2(7) . 2_655 ?
O14 W6 O3 88.1(7) 2_655 2_655 ?
O3 W6 O3 155.5(10) . 2_655 ?
O5 W6 O21 159.0(5) . 2_655 ?
O14 W6 O21 94.5(8) . 2_655 ?
O14 W6 O21 64.2(8) 2_655 2_655 ?
O3 W6 O21 92.2(7) . 2_655 ?
O3 W6 O21 64.3(7) 2_655 2_655 ?
O5 W6 O21 159.0(5) . . ?
O14 W6 O21 64.2(8) . . ?
O14 W6 O21 94.5(8) 2_655 . ?
O3 W6 O21 64.3(7) . . ?
O3 W6 O21 92.2(7) 2_655 . ?
O21 W6 O21 42.0(9) 2_655 . ?
O23 W7 O13 101.8(6) . . ?
O23 W7 O13 101.8(6) . 2_655 ?
O13 W7 O13 156.5(11) . 2_655 ?
O23 W7 O12 102.2(6) . 2_655 ?
O13 W7 O12 86.3(9) . 2_655 ?
O13 W7 O12 88.7(8) 2_655 2_655 ?
O23 W7 O12 102.2(6) . . ?
O13 W7 O12 88.7(8) . . ?
O13 W7 O12 86.3(9) 2_655 . ?
O12 W7 O12 155.5(11) 2_655 . ?
O23 W7 O1 159.3(4) . . ?
O13 W7 O1 61.8(7) . . ?
O13 W7 O1 95.3(7) 2_655 . ?
O12 W7 O1 89.8(8) 2_655 . ?
O12 W7 O1 66.9(7) . . ?
O23 W7 O1 159.3(4) . 2_655 ?
O13 W7 O1 95.3(7) . 2_655 ?
O13 W7 O1 61.8(7) 2_655 2_655 ?
O12 W7 O1 66.9(7) 2_655 2_655 ?
O12 W7 O1 89.8(8) . 2_655 ?
O1 W7 O1 41.5(9) . 2_655 ?
O2 B1 O2 174.1(19) . 2_655 ?
O2 B1 O21 71.1(13) . . ?
O2 B1 O21 114.0(14) 2_655 . ?
O2 B1 O21 114.0(14) . 2_655 ?
O2 B1 O21 71.1(13) 2_655 2_655 ?
O21 B1 O21 70(2) . 2_655 ?
O2 B1 O1 61.9(12) . . ?
O2 B1 O1 112.8(15) 2_655 . ?
O21 B1 O1 109.9(14) . . ?
O21 B1 O1 175.3(13) 2_655 . ?
O2 B1 O1 112.8(15) . 2_655 ?
O2 B1 O1 61.9(12) 2_655 2_655 ?
O21 B1 O1 175.3(13) . 2_655 ?
O21 B1 O1 109.9(14) 2_655 2_655 ?
O1 B1 O1 71(2) . 2_655 ?
O2 B1 O22 109.8(15) . 2_655 ?
O2 B1 O22 69.9(15) 2_655 2_655 ?
O21 B1 O22 74.9(15) . 2_655 ?
O21 B1 O22 108.3(16) 2_655 2_655 ?
O1 B1 O22 75.8(15) . 2_655 ?
O1 B1 O22 101.0(16) 2_655 2_655 ?
O2 B1 O22 69.9(15) . . ?
O2 B1 O22 109.8(15) 2_655 . ?
O21 B1 O22 108.3(16) . . ?
O21 B1 O22 74.9(15) 2_655 . ?
O1 B1 O22 101.0(16) . . ?
O1 B1 O22 75.8(15) 2_655 . ?
O22 B1 O22 176(2) 2_655 . ?
O27 Zn1 O27 127.1(11) 2_655 . ?
O27 Zn1 O24 104.1(8) 2_655 3_455 ?
O27 Zn1 O24 105.1(7) . 3_455 ?
O27 Zn1 O24 105.1(7) 2_655 4_655 ?
O27 Zn1 O24 104.1(8) . 4_655 ?
O24 Zn1 O24 111.2(8) 3_455 4_655 ?
B1 O1 O2 59.0(7) . . ?
B1 O1 O1 54.6(10) . 2_655 ?
O2 O1 O1 99.0(14) . 2_655 ?
B1 O1 W1 130.9(14) . . ?
O2 O1 W1 71.9(11) . . ?
O1 O1 W1 143.0(18) 2_655 . ?
B1 O1 W7 123.8(14) . . ?
O2 O1 W7 138.6(15) . . ?
O1 O1 W7 69.3(4) 2_655 . ?
W1 O1 W7 93.6(6) . . ?
B1 O2 O1 59.1(8) . . ?
B1 O2 O22 55.2(8) . . ?
O1 O2 O22 90.4(13) . . ?
B1 O2 O21 54.5(7) . . ?
O1 O2 O21 96.5(12) . . ?
O22 O2 O21 89.3(13) . . ?
B1 O2 W1 128.3(12) . . ?
O1 O2 W1 69.2(10) . . ?
O22 O2 W1 130.6(13) . . ?
O21 O2 W1 135.9(14) . . ?
B1 O2 W2 121.8(11) . . ?
O1 O2 W2 136.4(14) . . ?
O22 O2 W2 127.6(13) . . ?
O21 O2 W2 67.4(9) . . ?
W1 O2 W2 93.9(5) . . ?
B1 O2 W4 120.6(11) . . ?
O1 O2 W4 129.0(13) . . ?
O22 O2 W4 65.5(10) . . ?
O21 O2 W4 125.4(13) . . ?
W1 O2 W4 92.5(5) . . ?
W2 O2 W4 90.1(5) . . ?
W3 O3 W6 138.6(9) 2_655 . ?
W5 O4 W4 148.3(14) . . ?
W3 O8 W4 139.2(10) . . ?
W1 O9 W2 136.7(11) . . ?
W4 O10 W2 136.8(8) . . ?
W5 O11 W3 136.8(12) . . ?
W5 O12 W7 137.7(9) 2_655 . ?
W1 O13 W7 138.0(11) . . ?
W6 O14 W2 137.7(11) . . ?
W4 O16 W1 135.3(10) . . ?
W5 O17 W1 139.0(12) 2_655 . ?
W3 O18 W2 143.0(13) . 2_655 ?
B1 O21 O21 55.2(11) . 2_655 ?
B1 O21 O2 54.4(7) . . ?
O21 O21 O2 93.3(13) 2_655 . ?
B1 O21 W2 124.5(13) . . ?
O21 O21 W2 134.2(18) 2_655 . ?
O2 O21 W2 70.1(10) . . ?
B1 O21 W6 124.2(15) . . ?
O21 O21 W6 69.0(5) 2_655 . ?
O2 O21 W6 136.1(14) . . ?
W2 O21 W6 93.3(6) . . ?
B1 O21 W3 121.8(11) . 2_655 ?
O21 O21 W3 128.7(19) 2_655 2_655 ?
O2 O21 W3 128.0(15) . 2_655 ?
W2 O21 W3 92.2(7) . 2_655 ?
W6 O21 W3 91.8(6) . 2_655 ?
B1 O22 O2 54.9(8) . . ?
B1 O22 W4 127.2(17) . . ?
O2 O22 W4 72.5(12) . . ?
B1 O22 W5 123.2(16) . . ?
O2 O22 W5 132.5(16) . . ?
W4 O22 W5 94.1(6) . . ?
B1 O22 W3 119.6(16) . . ?
O2 O22 W3 133.2(15) . . ?
W4 O22 W3 92.1(6) . . ?
W5 O22 W3 91.3(8) . . ?
C1 O24 Zn1 121.4(14) . 3_545 ?
C21 O27 Zn1 124(2) . . ?
C8 N1 C9 107.8(17) . . ?
C8 N1 C5 124.9(17) . . ?
C9 N1 C5 127.0(17) . . ?
C8 N2 C10 107.6(16) . . ?
C8 N2 C11 128.3(18) . . ?
C10 N2 C11 124(2) . . ?
C12 N3 C13 108(2) . . ?
C12 N3 C11 123(2) . . ?
C13 N3 C11 128(2) . . ?
C12 N4 C14 106.9(18) . . ?
C12 N4 C15 122(2) . . ?
C14 N4 C15 130(2) . . ?
O24 C1 O25 125(2) . . ?
O24 C1 C2 117(2) . . ?
O25 C1 C2 118(2) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 118.7(13) . . ?
C7 C2 C1 121.3(13) . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 N1 121.6(12) . . ?
C6 C5 N1 118.2(11) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C2 120.0 . . ?
N1 C8 N2 110.9(18) . . ?
C10 C9 N1 108.4(19) . . ?
C9 C10 N2 104.6(19) . . ?
N2 C11 N3 109.6(17) . . ?
N4 C12 N3 108(2) . . ?
C14 C13 N3 108(2) . . ?
C13 C14 N4 109(2) . . ?
C16 C15 C20 120.0 . . ?
C16 C15 N4 117.6(18) . . ?
C20 C15 N4 122.3(18) . . ?
C17 C16 C15 120.0 . . ?
C16 C17 C18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 C21 126(2) . . ?
C17 C18 C21 113(2) . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C15 120.0 . . ?
O27 C21 O26 115(2) . . ?
O27 C21 C18 129(3) . . ?
O26 C21 C18 116(3) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.231
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1048171'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 Co N8 O48 W12 Zn'
_chemical_formula_weight         3747.26

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   21.018(4)
_cell_length_b                   30.814(5)
_cell_length_c                   19.639(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.919(15)
_cell_angle_gamma                90.00
_cell_volume                     12529(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18761
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      23.82

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6676
_exptl_absorpt_coefficient_mu    11.343
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3592
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18761
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.1257
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         23.82
_reflns_number_total             9456
_reflns_number_gt                2949
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1a (Brandenburg, 2005)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          SQUEEZE

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.004 -0.003 -0.011 6684 1449 ' '
_platon_squeeze_details          
;
About four [(CH₃)₂NH₂]⁺, four DMF and seven water lattice 
guests were removed from the formula unit by the SQUEEZE process.
;

_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)+(0.0335P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9456
_refine_ls_number_parameters     466
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.1850
_refine_ls_R_factor_gt           0.0881
_refine_ls_wR_factor_ref         0.2092
_refine_ls_wR_factor_gt          0.1826
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.37882(8) 0.13294(5) 0.31284(7) 0.1267(6) Uani 1 1 d . . .
W2 W 0.37831(8) 0.24563(7) 0.31247(8) 0.1643(8) Uani 1 1 d . . .
W3 W 0.61751(8) 0.24667(6) 0.36447(7) 0.1323(6) Uani 1 1 d . . .
W4 W 0.49507(8) 0.19029(6) 0.42616(6) 0.1337(6) Uani 1 1 d . . .
W5 W 0.61663(9) 0.13324(6) 0.36321(9) 0.1602(7) Uani 1 1 d . . .
W6 W 0.5000 0.30241(7) 0.2500 0.1322(7) Uani 1 2 d S . .
W7 W 0.5000 0.07633(9) 0.2500 0.2027(13) Uani 1 2 d S . .
Co1 Co 0.5000 0.18961(17) 0.2500 0.0899(13) Uani 1 2 d SD . .
Zn1 Zn 1.0000 -0.32017(15) 0.7500 0.0968(13) Uani 1 2 d S . .
O1 O 0.5478(16) 0.1992(11) 0.3414(8) 0.152(10) Uani 0.50 1 d PD . .
O2 O 0.4441(14) 0.1402(8) 0.2448(19) 0.22(2) Uani 0.50 1 d PDU . .
O3 O 0.4361(12) 0.2898(8) 0.1671(11) 0.161(9) Uani 1 1 d . . .
O4 O 0.3459(12) 0.1875(10) 0.3045(12) 0.187(9) Uani 1 1 d U . .
O5 O 0.5000 0.3507(14) 0.2500 0.186(13) Uani 1 2 d SU . .
O6 O 0.3236(12) 0.1071(10) 0.3429(15) 0.210(12) Uani 1 1 d . . .
O7 O 0.6702(13) 0.1080(9) 0.4141(12) 0.177(6) Uani 1 1 d . . .
O8 O 0.5596(14) 0.2309(10) 0.4259(14) 0.193(10) Uani 1 1 d U . .
O9 O 0.3571(14) 0.2470(10) 0.2192(14) 0.206(11) Uani 1 1 d U . .
O10 O 0.4392(15) 0.2302(11) 0.3975(15) 0.208(11) Uani 1 1 d U . .
O11 O 0.6521(13) 0.1874(11) 0.3792(13) 0.202(10) Uani 1 1 d U . .
O12 O 0.5600(17) 0.1494(11) 0.4187(16) 0.249(14) Uani 1 1 d DU . .
O13 O 0.4407(17) 0.0863(12) 0.1756(17) 0.247(13) Uani 1 1 d U . .
O14 O 0.4322(12) 0.2927(8) 0.2991(11) 0.172(8) Uani 1 1 d U . .
O15 O 0.6728(10) 0.2711(8) 0.4138(12) 0.160(8) Uani 1 1 d . . .
O16 O 0.4941(11) 0.1889(8) 0.5082(10) 0.166(8) Uani 1 1 d . . .
O17 O 0.4369(12) 0.1502(10) 0.3927(12) 0.179(10) Uani 1 1 d . . .
O18 O 0.3425(12) 0.1281(9) 0.2215(11) 0.192(11) Uani 1 1 d D . .
O19 O 0.4255(12) 0.0888(8) 0.3120(11) 0.177(6) Uani 1 1 d DU . .
O20 O 0.3234(11) 0.2721(8) 0.3414(9) 0.159(8) Uani 1 1 d . . .
O21 O 0.4447(17) 0.1903(16) 0.3183(17) 0.152(10) Uani 0.50 1 d PDU . .
O22 O 0.5465(15) 0.2435(7) 0.2657(16) 0.115(6) Uani 0.50 1 d PD . .
O23 O 0.5000 0.0254(12) 0.2500 0.174(13) Uani 1 2 d S . .
O24 O 0.5363(11) 0.1449(7) 0.6837(9) 0.115(6) Uani 1 1 d . . .
O25 O 0.5890(10) 0.1023(6) 0.7647(9) 0.123(6) Uani 1 1 d . . .
O26 O 0.9828(16) -0.2547(11) 0.6579(15) 0.224(10) Uani 1 1 d D . .
O27 O 0.9248(14) -0.2921(10) 0.6947(14) 0.203(11) Uani 1 1 d DU . .
N1 N 0.5886(11) -0.0147(8) 0.4922(12) 0.102(7) Uani 1 1 d . . .
N2 N 0.5884(8) -0.0743(7) 0.4421(11) 0.077(5) Uani 1 1 d . . .
N3 N 0.6532(12) -0.1414(7) 0.4358(10) 0.103(7) Uani 1 1 d . . .
N4 N 0.7393(10) -0.1738(7) 0.4830(9) 0.090(6) Uani 1 1 d U . .
C1 C 0.5688(13) 0.1117(12) 0.7048(13) 0.103(10) Uani 1 1 d . . .
C2 C 0.5775(8) 0.0777(6) 0.6490(7) 0.087(7) Uani 1 1 d G . .
C3 C 0.5918(10) 0.0345(6) 0.6655(6) 0.147(14) Uani 1 1 d G . .
H3A H 0.5973 0.0254 0.7113 0.176 Uiso 1 1 calc R . .
C4 C 0.5978(11) 0.0049(5) 0.6135(10) 0.157(14) Uani 1 1 d G . .
H4A H 0.6074 -0.0240 0.6246 0.189 Uiso 1 1 calc R . .
C5 C 0.5896(10) 0.0185(5) 0.5451(8) 0.122(11) Uani 1 1 d G . .
C6 C 0.5753(8) 0.0617(6) 0.5286(6) 0.094(8) Uani 1 1 d G . .
H6A H 0.5698 0.0708 0.4828 0.113 Uiso 1 1 calc R . .
C7 C 0.5692(8) 0.0913(4) 0.5805(8) 0.093(8) Uani 1 1 d G . .
H7A H 0.5597 0.1201 0.5695 0.112 Uiso 1 1 calc R . .
C8 C 0.5893(11) -0.0543(10) 0.5022(12) 0.095(8) Uani 1 1 d D . .
H8A H 0.5903 -0.0679 0.5447 0.114 Uiso 1 1 calc R . .
C9 C 0.5844(15) -0.0060(8) 0.4231(14) 0.114(10) Uani 1 1 d D . .
H9A H 0.5821 0.0213 0.4025 0.137 Uiso 1 1 calc R . .
C10 C 0.5844(13) -0.0427(11) 0.3927(13) 0.107(9) Uani 1 1 d . . .
H10A H 0.5821 -0.0471 0.3455 0.128 Uiso 1 1 calc R . .
C11 C 0.5864(14) -0.1178(11) 0.4274(14) 0.122(11) Uani 1 1 d . . .
H11A H 0.5646 -0.1217 0.3801 0.146 Uiso 1 1 calc R . .
H11B H 0.5605 -0.1320 0.4572 0.146 Uiso 1 1 calc R . .
C12 C 0.6846(12) -0.1598(9) 0.4929(13) 0.101(8) Uani 1 1 d DU . .
H12A H 0.6689 -0.1623 0.5342 0.121 Uiso 1 1 calc R . .
C13 C 0.6909(14) -0.1388(9) 0.3928(13) 0.106(8) Uani 1 1 d U . .
H13A H 0.6802 -0.1272 0.3486 0.127 Uiso 1 1 calc R . .
C14 C 0.7496(14) -0.1555(10) 0.4202(13) 0.120(9) Uani 1 1 d DU . .
H14A H 0.7876 -0.1549 0.4019 0.144 Uiso 1 1 calc R . .
C15 C 0.7715(10) -0.2110(10) 0.5886(14) 0.29(3) Uani 1 1 d G . .
H15A H 0.7304 -0.2074 0.5992 0.344 Uiso 1 1 calc R . .
C16 C 0.7867(10) -0.1927(8) 0.5287(11) 0.112(8) Uani 1 1 d GU . .
C17 C 0.8482(12) -0.1980(8) 0.5129(9) 0.22(2) Uani 1 1 d G . .
H17A H 0.8584 -0.1858 0.4728 0.264 Uiso 1 1 calc R . .
C18 C 0.8945(10) -0.2216(9) 0.5569(13) 0.164(10) Uani 1 1 d G . .
H18A H 0.9356 -0.2252 0.5463 0.197 Uiso 1 1 calc R . .
C19 C 0.8792(13) -0.2399(8) 0.6168(12) 0.164(10) Uani 1 1 d GDU . .
C20 C 0.8178(15) -0.2346(9) 0.6326(12) 0.224(10) Uani 1 1 d G . .
H20A H 0.8076 -0.2468 0.6727 0.269 Uiso 1 1 calc R . .
C21 C 0.9277(15) -0.2680(13) 0.660(2) 0.224(10) Uani 1 1 d DU . .


_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 1.60(2) . ?
W1 O19 1.68(2) . ?
W1 O4 1.82(3) . ?
W1 O18 1.83(2) . ?
W1 O17 1.89(3) . ?
W1 O2 2.09(4) . ?
W1 O21 2.24(5) . ?
W2 O20 1.60(2) . ?
W2 O9 1.81(3) . ?
W2 O14 1.89(2) . ?
W2 O4 1.91(3) . ?
W2 O10 1.98(3) . ?
W2 O21 2.19(4) . ?
W2 O22 2.39(3) 2_655 ?
W3 O15 1.57(2) . ?
W3 O3 1.78(3) 2_655 ?
W3 O9 1.81(3) 2_655 ?
W3 O8 1.92(3) . ?
W3 O11 1.97(3) . ?
W3 O1 2.06(3) . ?
W3 O22 2.24(3) . ?
W4 O16 1.616(19) . ?
W4 O10 1.73(3) . ?
W4 O17 1.78(3) . ?
W4 O8 1.85(3) . ?
W4 O12 1.88(4) . ?
W4 O1 2.17(3) . ?
W4 O21 2.20(4) . ?
W5 O7 1.58(3) . ?
W5 O12 1.82(3) . ?
W5 O11 1.83(3) . ?
W5 O13 1.95(4) 2_655 ?
W5 O18 2.01(2) 2_655 ?
W5 O2 2.29(3) 2_655 ?
W5 O1 2.49(4) . ?
W6 O5 1.49(4) . ?
W6 O14 1.88(2) . ?
W6 O14 1.88(2) 2_655 ?
W6 O3 1.96(3) 2_655 ?
W6 O3 1.96(3) . ?
W6 O22 2.06(3) 2_655 ?
W6 O22 2.06(3) . ?
W7 O23 1.57(4) . ?
W7 O13 1.78(4) 2_655 ?
W7 O13 1.78(4) . ?
W7 O19 2.18(2) . ?
W7 O19 2.18(2) 2_655 ?
W7 O2 2.29(4) . ?
W7 O2 2.29(4) 2_655 ?
Co1 O2 1.914(10) 2_655 ?
Co1 O2 1.914(10) . ?
Co1 O21 1.921(10) . ?
Co1 O21 1.921(10) 2_655 ?
Co1 O1 1.923(10) . ?
Co1 O1 1.923(10) 2_655 ?
Co1 O22 1.924(10) . ?
Co1 O22 1.924(10) 2_655 ?
Zn1 O24 1.945(19) 4_646 ?
Zn1 O24 1.945(19) 3_545 ?
Zn1 O27 1.96(3) 2_756 ?
Zn1 O27 1.96(3) . ?
O2 W5 2.29(3) 2_655 ?
O3 W3 1.78(3) 2_655 ?
O9 W3 1.81(3) 2_655 ?
O13 W5 1.95(4) 2_655 ?
O18 W5 2.01(2) 2_655 ?
O22 W2 2.39(3) 2_655 ?
O24 C1 1.26(3) . ?
O24 Zn1 1.945(19) 3_455 ?
O25 C1 1.21(3) . ?
O26 C21 1.236(10) . ?
O27 C21 1.023(10) . ?
N1 C8 1.24(3) . ?
N1 C9 1.37(3) . ?
N1 C5 1.46(3) . ?
N2 C8 1.33(3) . ?
N2 C10 1.37(3) . ?
N2 C11 1.37(3) . ?
N3 C13 1.26(3) . ?
N3 C12 1.33(3) . ?
N3 C11 1.56(4) . ?
N4 C12 1.27(3) . ?
N4 C16 1.35(2) . ?
N4 C14 1.41(3) . ?
C1 C2 1.55(3) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C9 C10 1.28(3) . ?
C13 C14 1.36(3) . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C19 C21 1.482(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O19 93.6(14) . . ?
O6 W1 O4 101.8(14) . . ?
O19 W1 O4 164.6(11) . . ?
O6 W1 O18 96.6(13) . . ?
O19 W1 O18 94.0(11) . . ?
O4 W1 O18 84.2(11) . . ?
O6 W1 O17 103.8(13) . . ?
O19 W1 O17 86.7(11) . . ?
O4 W1 O17 89.8(11) . . ?
O18 W1 O17 159.5(12) . . ?
O6 W1 O2 152.7(14) . . ?
O19 W1 O2 68.4(9) . . ?
O4 W1 O2 97.2(12) . . ?
O18 W1 O2 65.8(8) . . ?
O17 W1 O2 95.7(11) . . ?
O6 W1 O21 149.0(13) . . ?
O19 W1 O21 106.4(13) . . ?
O4 W1 O21 59.7(13) . . ?
O18 W1 O21 105.2(12) . . ?
O17 W1 O21 55.4(13) . . ?
O2 W1 O21 58.4(9) . . ?
O20 W2 O9 106.3(12) . . ?
O20 W2 O14 98.3(12) . . ?
O9 W2 O14 83.7(11) . . ?
O20 W2 O4 103.8(12) . . ?
O9 W2 O4 85.2(12) . . ?
O14 W2 O4 157.3(10) . . ?
O20 W2 O10 102.9(11) . . ?
O9 W2 O10 150.6(13) . . ?
O14 W2 O10 89.2(12) . . ?
O4 W2 O10 90.8(12) . . ?
O20 W2 O21 150.6(10) . . ?
O9 W2 O21 96.6(13) . . ?
O14 W2 O21 102.3(13) . . ?
O4 W2 O21 59.4(14) . . ?
O10 W2 O21 57.1(13) . . ?
O20 W2 O22 147.4(9) . 2_655 ?
O9 W2 O22 54.8(11) . 2_655 ?
O14 W2 O22 56.7(10) . 2_655 ?
O4 W2 O22 100.8(10) . 2_655 ?
O10 W2 O22 97.6(10) . 2_655 ?
O21 W2 O22 61.7(7) . 2_655 ?
O15 W3 O3 102.2(13) . 2_655 ?
O15 W3 O9 104.7(12) . 2_655 ?
O3 W3 O9 87.0(11) 2_655 2_655 ?
O15 W3 O8 102.5(12) . . ?
O3 W3 O8 88.6(10) 2_655 . ?
O9 W3 O8 152.8(13) 2_655 . ?
O15 W3 O11 98.1(13) . . ?
O3 W3 O11 159.7(12) 2_655 . ?
O9 W3 O11 88.8(12) 2_655 . ?
O8 W3 O11 86.1(11) . . ?
O15 W3 O1 153.7(10) . . ?
O3 W3 O1 94.0(13) 2_655 . ?
O9 W3 O1 96.6(12) 2_655 . ?
O8 W3 O1 57.0(12) . . ?
O11 W3 O1 66.7(13) . . ?
O15 W3 O22 150.2(10) . . ?
O3 W3 O22 56.2(10) 2_655 . ?
O9 W3 O22 58.1(12) 2_655 . ?
O8 W3 O22 97.7(11) . . ?
O11 W3 O22 105.1(11) . . ?
O1 W3 O22 55.7(7) . . ?
O16 W4 O10 102.6(13) . . ?
O16 W4 O17 102.9(11) . . ?
O10 W4 O17 89.3(12) . . ?
O16 W4 O8 99.0(12) . . ?
O10 W4 O8 88.5(14) . . ?
O17 W4 O8 157.9(11) . . ?
O16 W4 O12 101.2(13) . . ?
O10 W4 O12 156.0(13) . . ?
O17 W4 O12 88.2(14) . . ?
O8 W4 O12 85.0(13) . . ?
O16 W4 O1 149.8(9) . . ?
O10 W4 O1 94.0(13) . . ?
O17 W4 O1 102.4(9) . . ?
O8 W4 O1 55.9(10) . . ?
O12 W4 O1 63.4(8) . . ?
O16 W4 O21 150.9(10) . . ?
O10 W4 O21 59.9(14) . . ?
O17 W4 O21 57.2(14) . . ?
O8 W4 O21 103.3(13) . . ?
O12 W4 O21 99.3(14) . . ?
O1 W4 O21 59.1(8) . . ?
O7 W5 O12 103.0(12) . . ?
O7 W5 O11 96.6(13) . . ?
O12 W5 O11 86.4(14) . . ?
O7 W5 O13 101.9(15) . 2_655 ?
O12 W5 O13 90.7(15) . 2_655 ?
O11 W5 O13 161.4(14) . 2_655 ?
O7 W5 O18 97.2(11) . 2_655 ?
O12 W5 O18 159.7(12) . 2_655 ?
O11 W5 O18 89.7(10) . 2_655 ?
O13 W5 O18 86.6(11) 2_655 2_655 ?
O7 W5 O2 149.0(9) . 2_655 ?
O12 W5 O2 102.3(12) . 2_655 ?
O11 W5 O2 102.6(12) . 2_655 ?
O13 W5 O2 60.0(13) 2_655 2_655 ?
O18 W5 O2 59.3(7) 2_655 2_655 ?
O7 W5 O1 147.5(9) . . ?
O12 W5 O1 57.2(9) . . ?
O11 W5 O1 59.5(11) . . ?
O13 W5 O1 103.7(12) 2_655 . ?
O18 W5 O1 104.0(10) 2_655 . ?
O2 W5 O1 63.2(5) 2_655 . ?
O5 W6 O14 99.2(8) . . ?
O5 W6 O14 99.2(8) . 2_655 ?
O14 W6 O14 161.7(16) . 2_655 ?
O5 W6 O3 101.4(7) . 2_655 ?
O14 W6 O3 90.8(9) . 2_655 ?
O14 W6 O3 85.6(9) 2_655 2_655 ?
O5 W6 O3 101.4(7) . . ?
O14 W6 O3 85.6(9) . . ?
O14 W6 O3 90.8(9) 2_655 . ?
O3 W6 O3 157.2(14) 2_655 . ?
O5 W6 O22 151.8(6) . 2_655 ?
O14 W6 O22 63.5(11) . 2_655 ?
O14 W6 O22 99.5(11) 2_655 2_655 ?
O3 W6 O22 100.9(10) 2_655 2_655 ?
O3 W6 O22 57.5(10) . 2_655 ?
O5 W6 O22 151.8(6) . . ?
O14 W6 O22 99.5(11) . . ?
O14 W6 O22 63.5(11) 2_655 . ?
O3 W6 O22 57.5(10) 2_655 . ?
O3 W6 O22 100.9(10) . . ?
O22 W6 O22 56.4(12) 2_655 . ?
O23 W7 O13 99.9(12) . 2_655 ?
O23 W7 O13 99.9(12) . . ?
O13 W7 O13 160(2) 2_655 . ?
O23 W7 O19 100.2(6) . . ?
O13 W7 O19 88.8(12) 2_655 . ?
O13 W7 O19 87.7(12) . . ?
O23 W7 O19 100.2(6) . 2_655 ?
O13 W7 O19 87.7(12) 2_655 2_655 ?
O13 W7 O19 88.8(12) . 2_655 ?
O19 W7 O19 159.6(13) . 2_655 ?
O23 W7 O2 149.5(4) . . ?
O13 W7 O2 99.8(14) 2_655 . ?
O13 W7 O2 62.1(13) . . ?
O19 W7 O2 57.2(7) . . ?
O19 W7 O2 103.7(12) 2_655 . ?
O23 W7 O2 149.5(4) . 2_655 ?
O13 W7 O2 62.1(13) 2_655 2_655 ?
O13 W7 O2 99.8(14) . 2_655 ?
O19 W7 O2 103.7(12) . 2_655 ?
O19 W7 O2 57.2(7) 2_655 2_655 ?
O2 W7 O2 61.1(8) . 2_655 ?
O2 Co1 O2 75(2) 2_655 . ?
O2 Co1 O21 114(2) 2_655 . ?
O2 Co1 O21 66.8(19) . . ?
O2 Co1 O21 66.8(19) 2_655 2_655 ?
O2 Co1 O21 114(2) . 2_655 ?
O21 Co1 O21 179(3) . 2_655 ?
O2 Co1 O1 81.7(15) 2_655 . ?
O2 Co1 O1 112.9(14) . . ?
O21 Co1 O1 68.2(17) . . ?
O21 Co1 O1 111.6(17) 2_655 . ?
O2 Co1 O1 112.9(14) 2_655 2_655 ?
O2 Co1 O1 81.7(15) . 2_655 ?
O21 Co1 O1 111.6(17) . 2_655 ?
O21 Co1 O1 68.2(17) 2_655 2_655 ?
O1 Co1 O1 162(2) . 2_655 ?
O2 Co1 O22 112.8(15) 2_655 . ?
O2 Co1 O22 169.9(16) . . ?
O21 Co1 O22 103.3(18) . . ?
O21 Co1 O22 75.6(17) 2_655 . ?
O1 Co1 O22 63.1(14) . . ?
O1 Co1 O22 100.8(15) 2_655 . ?
O2 Co1 O22 169.9(16) 2_655 2_655 ?
O2 Co1 O22 112.8(15) . 2_655 ?
O21 Co1 O22 75.6(17) . 2_655 ?
O21 Co1 O22 103.3(18) 2_655 2_655 ?
O1 Co1 O22 100.8(15) . 2_655 ?
O1 Co1 O22 63.1(14) 2_655 2_655 ?
O22 Co1 O22 61(2) . 2_655 ?
O24 Zn1 O24 112.7(12) 4_646 3_545 ?
O24 Zn1 O27 104.2(11) 4_646 2_756 ?
O24 Zn1 O27 104.1(10) 3_545 2_756 ?
O24 Zn1 O27 104.1(10) 4_646 . ?
O24 Zn1 O27 104.2(11) 3_545 . ?
O27 Zn1 O27 127.6(17) 2_756 . ?
Co1 O1 W3 123.4(15) . . ?
Co1 O1 W4 116.3(15) . . ?
W3 O1 W4 111.0(9) . . ?
Co1 O1 W5 103.3(13) . . ?
W3 O1 W5 99.9(13) . . ?
W4 O1 W5 97.1(10) . . ?
Co1 O2 W1 121(2) . . ?
Co1 O2 W7 112.1(15) . . ?
W1 O2 W7 105.6(9) . . ?
Co1 O2 W5 111.3(13) . 2_655 ?
W1 O2 W5 105.1(11) . 2_655 ?
W7 O2 W5 99.2(14) . 2_655 ?
W3 O3 W6 137.4(13) 2_655 . ?
W1 O4 W2 137.3(15) . . ?
W4 O8 W3 136.0(16) . . ?
W2 O9 W3 149.1(18) . 2_655 ?
W4 O10 W2 138.6(17) . . ?
W5 O11 W3 133.7(16) . . ?
W5 O12 W4 142.0(16) . . ?
W7 O13 W5 138.3(19) . 2_655 ?
W6 O14 W2 136.2(14) . . ?
W4 O17 W1 143.6(16) . . ?
W1 O18 W5 129.8(13) . 2_655 ?
W1 O19 W7 128.8(12) . . ?
Co1 O21 W2 115(2) . . ?
Co1 O21 W4 115.1(18) . . ?
W2 O21 W4 104.3(15) . . ?
Co1 O21 W1 114(2) . . ?
W2 O21 W1 103.2(13) . . ?
W4 O21 W1 103.8(15) . . ?
Co1 O22 W6 121.4(16) . . ?
Co1 O22 W3 114.9(14) . . ?
W6 O22 W3 108.6(9) . . ?
Co1 O22 W2 107.2(12) . 2_655 ?
W6 O22 W2 103.2(10) . 2_655 ?
W3 O22 W2 98.0(11) . 2_655 ?
C1 O24 Zn1 118.8(17) . 3_455 ?
C21 O27 Zn1 124(3) . . ?
C8 N1 C9 110(2) . . ?
C8 N1 C5 126(2) . . ?
C9 N1 C5 124(2) . . ?
C8 N2 C10 107(2) . . ?
C8 N2 C11 129(2) . . ?
C10 N2 C11 123(3) . . ?
C13 N3 C12 108(3) . . ?
C13 N3 C11 124(2) . . ?
C12 N3 C11 126.6(19) . . ?
C12 N4 C16 129(2) . . ?
C12 N4 C14 106.1(19) . . ?
C16 N4 C14 123(2) . . ?
O25 C1 O24 126(3) . . ?
O25 C1 C2 117(3) . . ?
O24 C1 C2 116(2) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 122.0(18) . . ?
C7 C2 C1 118.0(18) . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 N1 122.1(16) . . ?
C4 C5 N1 117.5(16) . . ?
C5 C6 C7 120.0 . . ?
C6 C7 C2 120.0 . . ?
N1 C8 N2 109(2) . . ?
C10 C9 N1 106.4(19) . . ?
C9 C10 N2 108(2) . . ?
N2 C11 N3 116(2) . . ?
N4 C12 N3 110(2) . . ?
N3 C13 C14 110(2) . . ?
C13 C14 N4 103.5(18) . . ?
C16 C15 C20 120.0 . . ?
N4 C16 C15 119.1(19) . . ?
N4 C16 C17 120.6(19) . . ?
C15 C16 C17 120.0 . . ?
C16 C17 C18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 C21 121(2) . . ?
C18 C19 C21 119(2) . . ?
C19 C20 C15 120.0 . . ?
O27 C21 O26 115(3) . . ?
O27 C21 C19 134(4) . . ?
O26 C21 C19 110(3) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        23.82
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.205
