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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 1417285'
_audit_update_record             
;
2015-11-27 deposited with the CCDC.
2015-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 Cu2 N4 O21 P2 W5,2H2O'
_chemical_formula_sum            'C32 H30 Cu2 N4 O23 P2 W5'
_chemical_formula_weight         1946.87

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   19.0050(11)
_cell_length_b                   42.763(2)
_cell_length_c                   10.6834(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8682.6(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5641
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      26.72

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.979
_exptl_crystal_F_000             7136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.064
_exptl_absorpt_coefficient_mu    14.318
_shelx_estimated_absorpt_T_min   0.362
_shelx_estimated_absorpt_T_max   0.461
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3622
_exptl_absorpt_correction_T_max  0.4610
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10739
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.905
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        24.995
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3340
_reflns_number_gt                3305
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'SMART (Bruker, 2005)'
_computing_cell_refinement       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997a)'
_computing_publication_material  SHELXTL
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0340P)²+117.5924P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.000014(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.489(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3340
_refine_ls_number_parameters     316
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0625
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.2500 0.2500 -0.70074(6) 0.01241(16) Uani 1 2 d S T P . .
W2 W 0.33539(2) 0.23008(2) -0.21392(4) 0.01250(13) Uani 1 1 d . . . . .
W3 W 0.36707(2) 0.21141(2) -0.51812(5) 0.01432(14) Uani 1 1 d . . . . .
Cu1 Cu 0.41465(8) 0.25696(3) 0.07350(15) 0.0181(3) Uani 1 1 d . . . . .
P1 P 0.19424(15) 0.21475(6) -0.4258(3) 0.0114(6) Uani 1 1 d . . . . .
O1 O 0.2500 0.2500 -0.1670(11) 0.014(2) Uani 1 2 d S T P . .
O2 O 0.3926(4) 0.2450(2) -0.0993(9) 0.0175(19) Uani 1 1 d . . . . .
O3 O 0.2965(4) 0.21260(18) -0.6468(9) 0.0186(19) Uani 1 1 d . . . . .
O4 O 0.3796(5) 0.1718(2) -0.5248(11) 0.026(2) Uani 1 1 d . . . . .
O5 O 0.4416(5) 0.2266(2) -0.5900(10) 0.026(2) Uani 1 1 d . . . . .
O6 O 0.3154(4) 0.1940(2) -0.1564(9) 0.022(2) Uani 1 1 d . . . . .
O7 O 0.1870(5) 0.2349(2) -0.8035(9) 0.021(2) Uani 1 1 d . . . . .
O8 O 0.3996(4) 0.2188(2) -0.3451(8) 0.0137(18) Uani 1 1 d . . . . .
O9 O 0.2752(4) 0.21521(19) -0.3926(9) 0.0145(17) Uani 1 1 d . . . . .
O10 O 0.3465(4) 0.27574(19) -0.3119(8) 0.0147(18) Uani 1 1 d . U . . .
O11 O 0.1792(4) 0.2367(2) -0.5362(9) 0.0151(17) Uani 1 1 d . . . . .
N1 N 0.4005(5) 0.3022(2) 0.0303(12) 0.018(2) Uani 1 1 d . . . . .
N2 N 0.3361(5) 0.4606(2) -0.1334(11) 0.020(2) Uani 1 1 d . . . . .
C1 C 0.1714(6) 0.1761(3) -0.4702(14) 0.019(3) Uani 1 1 d . . . . .
C2 C 0.1895(11) 0.1517(3) -0.3912(18) 0.048(5) Uani 1 1 d . . . . .
H2A H 0.2150 0.1555 -0.3186 0.057 Uiso 1 1 calc R U . . .
C3 C 0.1690(12) 0.1214(4) -0.422(2) 0.060(5) Uani 1 1 d . U . . .
H3A H 0.1787 0.1051 -0.3669 0.072 Uiso 1 1 calc R U . . .
C4 C 0.1354(11) 0.1155(4) -0.530(2) 0.053(5) Uani 1 1 d . U . . .
H4A H 0.1232 0.0951 -0.5507 0.064 Uiso 1 1 calc R U . . .
C5 C 0.1192(13) 0.1393(5) -0.609(2) 0.068(7) Uani 1 1 d . . . . .
H5A H 0.0961 0.1350 -0.6835 0.082 Uiso 1 1 calc R U . . .
C6 C 0.1368(10) 0.1698(4) -0.5788(17) 0.047(5) Uani 1 1 d . . . . .
H6A H 0.1250 0.1860 -0.6330 0.057 Uiso 1 1 calc R U . . .
C7 C 0.3395(7) 0.3107(3) -0.0240(15) 0.027(3) Uani 1 1 d . . . . .
H7A H 0.3073 0.2950 -0.0437 0.032 Uiso 1 1 calc R U . . .
C8 C 0.3222(6) 0.3410(3) -0.0520(13) 0.021(3) Uani 1 1 d . . . . .
H8A H 0.2786 0.3456 -0.0870 0.025 Uiso 1 1 calc R U . . .
C9 C 0.3701(7) 0.3650(3) -0.0280(15) 0.022(3) Uani 1 1 d . . . . .
C10 C 0.4314(7) 0.3567(3) 0.0324(16) 0.027(3) Uani 1 1 d . . . . .
H10A H 0.4634 0.3721 0.0553 0.032 Uiso 1 1 calc R U . . .
C11 C 0.4464(6) 0.3255(3) 0.0597(14) 0.023(3) Uani 1 1 d . . . . .
H11A H 0.4886 0.3205 0.0989 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2809(7) 0.4425(3) -0.0940(14) 0.028(3) Uani 1 1 d . . . . .
H12A H 0.2364 0.4515 -0.0902 0.034 Uiso 1 1 calc R U . . .
C13 C 0.2881(7) 0.4121(3) -0.0601(14) 0.028(3) Uani 1 1 d . . . . .
H13A H 0.2492 0.4006 -0.0342 0.033 Uiso 1 1 calc R U . . .
C14 C 0.3552(7) 0.3982(3) -0.0649(13) 0.020(3) Uani 1 1 d . . . . .
C15 C 0.4110(7) 0.4169(3) -0.1069(13) 0.022(3) Uani 1 1 d . . . . .
H15A H 0.4561 0.4086 -0.1120 0.027 Uiso 1 1 calc R U . . .
C16 C 0.3989(7) 0.4470(3) -0.1401(13) 0.021(3) Uani 1 1 d . . . . .
H16A H 0.4366 0.4588 -0.1691 0.026 Uiso 1 1 calc R U . . .
O1W O 0.4687(4) 0.2678(2) 0.2240(10) 0.0217(19) Uani 1 1 d D . . . .
H1WA H 0.462(7) 0.258(3) 0.293(7) 0.026 Uiso 1 1 d D U . . .
H1WB H 0.510(3) 0.270(3) 0.196(14) 0.026 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O7 1.747(9) 14 ?
W1 O7 1.747(9) . ?
W1 O3 1.915(8) . ?
W1 O3 1.916(8) 14 ?
W1 O11 2.286(9) . ?
W1 O11 2.286(9) 14 ?
W2 O6 1.705(9) . ?
W2 O2 1.758(9) . ?
W2 O1 1.900(3) . ?
W2 O8 1.920(9) . ?
W2 O10 2.225(8) . ?
W2 O9 2.314(9) . ?
W3 O4 1.712(9) . ?
W3 O5 1.736(9) . ?
W3 O3 1.922(10) . ?
W3 O8 1.975(9) . ?
W3 O9 2.208(8) . ?
W3 O11 2.395(8) 14 ?
Cu1 O2 1.961(9) . ?
Cu1 O1W 1.963(10) . ?
Cu1 N1 2.008(10) . ?
Cu1 N2 2.035(10) 16_545 ?
Cu1 O7 2.363(9) 14_556 ?
P1 O10 1.499(9) 14 ?
P1 O11 1.534(10) . ?
P1 O9 1.579(8) . ?
P1 C1 1.772(13) . ?
O1 W2 1.900(3) 14 ?
O7 Cu1 2.363(9) 14_554 ?
O10 P1 1.499(9) 14 ?
O11 W3 2.395(8) 14 ?
N1 C7 1.346(17) . ?
N1 C11 1.361(16) . ?
N2 C16 1.330(17) . ?
N2 C12 1.369(18) . ?
N2 Cu1 2.035(10) 12_554 ?
C1 C6 1.36(2) . ?
C1 C2 1.39(2) . ?
C2 C3 1.39(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.34(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.35(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.39(3) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.371(19) . ?
C7 H7A 0.9300 . ?
C8 C9 1.396(18) . ?
C8 H8A 0.9300 . ?
C9 C10 1.38(2) . ?
C9 C14 1.502(18) . ?
C10 C11 1.394(19) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 C13 1.357(19) . ?
C12 H12A 0.9300 . ?
C13 C14 1.41(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.400(18) . ?
C15 C16 1.356(19) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
O1W H1WA 0.849(14) . ?
O1W H1WB 0.849(14) . ?

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
O7 W1 O7 102.2(6) 14 . ?
O7 W1 O3 100.4(4) 14 . ?
O7 W1 O3 101.4(4) . . ?
O7 W1 O3 101.4(4) 14 14 ?
O7 W1 O3 100.4(4) . 14 ?
O3 W1 O3 145.0(6) . 14 ?
O7 W1 O11 168.0(4) 14 . ?
O7 W1 O11 89.3(4) . . ?
O3 W1 O11 80.4(3) . . ?
O3 W1 O11 72.9(4) 14 . ?
O7 W1 O11 89.3(4) 14 14 ?
O7 W1 O11 168.0(4) . 14 ?
O3 W1 O11 72.9(4) . 14 ?
O3 W1 O11 80.4(3) 14 14 ?
O11 W1 O11 79.4(4) . 14 ?
O6 W2 O2 102.5(4) . . ?
O6 W2 O1 96.9(3) . . ?
O2 W2 O1 100.4(4) . . ?
O6 W2 O8 100.2(4) . . ?
O2 W2 O8 101.9(4) . . ?
O1 W2 O8 148.0(4) . . ?
O6 W2 O10 170.2(4) . . ?
O2 W2 O10 87.1(4) . . ?
O1 W2 O10 79.2(3) . . ?
O8 W2 O10 79.5(3) . . ?
O6 W2 O9 86.5(4) . . ?
O2 W2 O9 168.5(4) . . ?
O1 W2 O9 85.3(4) . . ?
O8 W2 O9 69.1(3) . . ?
O10 W2 O9 84.3(3) . . ?
O4 W3 O5 103.7(5) . . ?
O4 W3 O3 95.3(4) . . ?
O5 W3 O3 104.1(4) . . ?
O4 W3 O8 98.8(4) . . ?
O5 W3 O8 95.7(4) . . ?
O3 W3 O8 152.2(3) . . ?
O4 W3 O9 102.0(4) . . ?
O5 W3 O9 152.4(4) . . ?
O3 W3 O9 83.1(3) . . ?
O8 W3 O9 70.6(3) . . ?
O4 W3 O11 164.7(4) . 14 ?
O5 W3 O11 85.3(4) . 14 ?
O3 W3 O11 70.2(3) . 14 ?
O8 W3 O11 92.4(3) . 14 ?
O9 W3 O11 72.0(3) . 14 ?
O2 Cu1 O1W 160.8(4) . . ?
O2 Cu1 N1 90.3(4) . . ?
O1W Cu1 N1 91.7(4) . . ?
O2 Cu1 N2 87.6(4) . 16_545 ?
O1W Cu1 N2 92.8(4) . 16_545 ?
N1 Cu1 N2 171.9(4) . 16_545 ?
O2 Cu1 O7 112.8(3) . 14_556 ?
O1W Cu1 O7 86.4(4) . 14_556 ?
N1 Cu1 O7 82.9(4) . 14_556 ?
N2 Cu1 O7 90.6(4) 16_545 14_556 ?
O10 P1 O11 111.2(5) 14 . ?
O10 P1 O9 108.5(5) 14 . ?
O11 P1 O9 110.3(5) . . ?
O10 P1 C1 110.1(6) 14 . ?
O11 P1 C1 108.6(6) . . ?
O9 P1 C1 108.1(5) . . ?
W2 O1 W2 149.4(7) . 14 ?
W2 O2 Cu1 152.0(5) . . ?
W1 O3 W3 124.0(4) . . ?
W1 O7 Cu1 148.8(5) . 14_554 ?
W2 O8 W3 121.6(4) . . ?
P1 O9 W3 129.3(5) . . ?
P1 O9 W2 132.1(5) . . ?
W3 O9 W2 97.5(3) . . ?
P1 O10 W2 124.8(5) 14 . ?
P1 O11 W1 129.3(5) . . ?
P1 O11 W3 125.0(5) . 14 ?
W1 O11 W3 92.7(3) . 14 ?
C7 N1 C11 117.1(11) . . ?
C7 N1 Cu1 118.2(8) . . ?
C11 N1 Cu1 124.5(9) . . ?
C16 N2 C12 117.2(11) . . ?
C16 N2 Cu1 114.9(8) . 12_554 ?
C12 N2 Cu1 127.9(9) . 12_554 ?
C6 C1 C2 119.3(14) . . ?
C6 C1 P1 122.1(12) . . ?
C2 C1 P1 118.7(12) . . ?
C1 C2 C3 119.3(18) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 H2A 120.3 . . ?
C4 C3 C2 121(2) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C3 C4 C5 120.1(17) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C4 C5 C6 120.6(18) . . ?
C4 C5 H5A 119.7 . . ?
C6 C5 H5A 119.7 . . ?
C1 C6 C5 120.0(17) . . ?
C1 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
N1 C7 C8 123.7(12) . . ?
N1 C7 H7A 118.2 . . ?
C8 C7 H7A 118.2 . . ?
C7 C8 C9 119.9(12) . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C10 C9 C8 116.6(12) . . ?
C10 C9 C14 121.8(11) . . ?
C8 C9 C14 121.6(12) . . ?
C9 C10 C11 121.1(12) . . ?
C9 C10 H10A 119.4 . . ?
C11 C10 H10A 119.4 . . ?
N1 C11 C10 121.4(12) . . ?
N1 C11 H11A 119.3 . . ?
C10 C11 H11A 119.3 . . ?
C13 C12 N2 123.1(13) . . ?
C13 C12 H12A 118.4 . . ?
N2 C12 H12A 118.4 . . ?
C12 C13 C14 119.0(12) . . ?
C12 C13 H13A 120.5 . . ?
C14 C13 H13A 120.5 . . ?
C15 C14 C13 117.3(12) . . ?
C15 C14 C9 118.6(12) . . ?
C13 C14 C9 124.1(12) . . ?
C16 C15 C14 119.7(13) . . ?
C16 C15 H15A 120.1 . . ?
C14 C15 H15A 120.1 . . ?
N2 C16 C15 123.7(12) . . ?
N2 C16 H16A 118.2 . . ?
C15 C16 H16A 118.2 . . ?
Cu1 O1W H1WA 121(10) . . ?
Cu1 O1W H1WB 103(10) . . ?
H1WA O1W H1WB 119(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 W2 O2 Cu1 -57.3(12) . . . . ?
O1 W2 O2 Cu1 42.3(12) . . . . ?
O8 W2 O2 Cu1 -160.7(11) . . . . ?
O10 W2 O2 Cu1 120.7(11) . . . . ?
O9 W2 O2 Cu1 161.7(12) . . . . ?
O7 W1 O7 Cu1 -87.3(10) 14 . . 14_554 ?
O3 W1 O7 Cu1 169.3(9) . . . 14_554 ?
O3 W1 O7 Cu1 16.8(10) 14 . . 14_554 ?
O11 W1 O7 Cu1 89.2(10) . . . 14_554 ?
O11 W1 O7 Cu1 109.4(18) 14 . . 14_554 ?
O10 P1 O9 W3 -169.2(5) 14 . . . ?
O11 P1 O9 W3 -47.1(7) . . . . ?
C1 P1 O9 W3 71.4(8) . . . . ?
O10 P1 O9 W2 -4.1(8) 14 . . . ?
O11 P1 O9 W2 117.9(7) . . . . ?
C1 P1 O9 W2 -123.6(7) . . . . ?
O10 P1 O11 W1 151.2(5) 14 . . . ?
O9 P1 O11 W1 30.7(7) . . . . ?
C1 P1 O11 W1 -87.5(7) . . . . ?
O10 P1 O11 W3 20.8(7) 14 . . 14 ?
O9 P1 O11 W3 -99.7(6) . . . 14 ?
C1 P1 O11 W3 142.1(6) . . . 14 ?
O10 P1 C1 C6 113.2(14) 14 . . . ?
O11 P1 C1 C6 -8.8(15) . . . . ?
O9 P1 C1 C6 -128.4(13) . . . . ?
O10 P1 C1 C2 -66.7(14) 14 . . . ?
O11 P1 C1 C2 171.3(13) . . . . ?
O9 P1 C1 C2 51.7(14) . . . . ?
C6 C1 C2 C3 -3(3) . . . . ?
P1 C1 C2 C3 176.9(15) . . . . ?
C1 C2 C3 C4 4(3) . . . . ?
C2 C3 C4 C5 -2(3) . . . . ?
C3 C4 C5 C6 0(4) . . . . ?
C2 C1 C6 C5 1(3) . . . . ?
P1 C1 C6 C5 -179.1(18) . . . . ?
C4 C5 C6 C1 1(4) . . . . ?
C11 N1 C7 C8 1(2) . . . . ?
Cu1 N1 C7 C8 176.5(12) . . . . ?
N1 C7 C8 C9 2(2) . . . . ?
C7 C8 C9 C10 -5(2) . . . . ?
C7 C8 C9 C14 175.9(14) . . . . ?
C8 C9 C10 C11 4(2) . . . . ?
C14 C9 C10 C11 -176.3(14) . . . . ?
C7 N1 C11 C10 -1(2) . . . . ?
Cu1 N1 C11 C10 -176.6(11) . . . . ?
C9 C10 C11 N1 -1(2) . . . . ?
C16 N2 C12 C13 1(2) . . . . ?
Cu1 N2 C12 C13 -175.8(11) 12_554 . . . ?
N2 C12 C13 C14 0(2) . . . . ?
C12 C13 C14 C15 -1(2) . . . . ?
C12 C13 C14 C9 178.9(14) . . . . ?
C10 C9 C14 C15 37(2) . . . . ?
C8 C9 C14 C15 -143.7(14) . . . . ?
C10 C9 C14 C13 -143.0(15) . . . . ?
C8 C9 C14 C13 36(2) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C9 C14 C15 C16 -179.6(13) . . . . ?
C12 N2 C16 C15 -2(2) . . . . ?
Cu1 N2 C16 C15 175.4(11) 12_554 . . . ?
C14 C15 C16 N2 1(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O5 0.849(14) 1.89(5) 2.707(13) 161(15) 1_556
O1W H1WB O8 0.849(14) 1.83(3) 2.671(12) 170(15) 6_655

_refine_diff_density_max         2.100
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.203



####################################################################### 
# 
# 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 1417286'
_audit_update_record             
;
2015-11-27 deposited with the CCDC.
2015-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H50 Cu3 N12 O40 W12,12H2O'
_chemical_formula_sum            'C60 H74 Cu3 N12 O52 W12'
_chemical_formula_weight         4192.04

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.796(4)
_cell_length_b                   25.625(7)
_cell_length_c                   16.112(3)
_cell_angle_alpha                90
_cell_angle_beta                 119.955(16)
_cell_angle_gamma                90
_cell_volume                     4577(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8492
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      26.82

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.042
_exptl_crystal_F_000             3816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.051
_exptl_absorpt_coefficient_mu    15.791
_shelx_estimated_absorpt_T_min   0.361
_shelx_estimated_absorpt_T_max   0.500
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3611
_exptl_absorpt_correction_T_max  0.4998
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22894
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.661
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8059
_reflns_number_gt                7288
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
 During the refinement, the command 'omit-3 50' was used to omit the weak
 reflections above 50 degree. The restraint command 'ISOR' and was used 
 to restrain some non-H atoms with ADP and NPD problems. These atoms are 
 as follows:
 isor 0.005 o17 o18
 isor 0.01 o1 o2 o6 o7 o9 o11 o12 o14 o15 o16 
 isor 0.01 o20 o22
 isor 0.01 c1 c3 c6 c7 c8 c9 c10 c11 c12
 isor 0.01 c14 c15 c17 c18 c23 c28 c29 c30
 The restraint command 'SIMU' was also used to restrain the atoms on organic 
 ligands possess the similar thermal parameters. The refinement commands are 
 as follows:
 simu 0.01 0.02 3.8 w5 o18
 simu 0.01 0.02 3.8 w3 o16 o20
 All above restrained refinements led to a relative high restraint value of 211.
 Based on the elemental analysis and the TG analysis, another 1 lattice water
 molecules are directly included in the final molecular formula.
 Some of guest molecules such as water 
were not observed in the electron density map. 
 Water-H-atoms could not be localized and were not included in the refinement.
 The highest residual peak 2.421 eA^-3 and the deepest residual hole -3.328 eA^-3 
 are both very close to the heavy W5/W6 center with the distance of 0.84/1.00 A 
 and featureless, resulting from the series termination errors.
;

_computing_data_collection       'SMART (Bruker, 2005)'
_computing_cell_refinement       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997a)'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0091P)²+945.0200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8059
_refine_ls_number_parameters     672
_refine_ls_number_restraints     211
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0854
_refine_ls_wR_factor_ref         0.1888
_refine_ls_wR_factor_gt          0.1845
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W -0.21101(9) -0.02668(4) 1.02956(8) 0.0233(3) Uani 1 1 d . . . . .
W2 W -0.27824(10) 0.09868(5) 1.08325(8) 0.0288(3) Uani 1 1 d . . . . .
W3 W -0.25446(10) -0.00999(4) 1.22575(8) 0.0297(3) Uani 1 1 d . U . . .
W4 W -0.54002(11) 0.00351(4) 1.20116(8) 0.0279(3) Uani 1 1 d . . . . .
W5 W -0.44438(11) -0.11825(4) 0.92667(8) 0.0296(3) Uani 1 1 d . U . . .
W6 W -0.45532(11) -0.11265(5) 1.13651(11) 0.0408(4) Uani 1 1 d . . . . .
Cu1 Cu 0.0000 0.0000 1.5000 0.0172(8) Uani 1 2 d S . P . .
Cu2 Cu 0.4399(2) 0.25592(12) 1.2059(2) 0.0184(6) Uani 1 1 d . . . . .
O1 O -0.1379(16) -0.0131(7) 1.3401(12) 0.027(4) Uani 1 1 d . U . . .
O2 O -0.193(3) 0.0492(11) 1.054(2) 0.067(7) Uani 1 1 d . U . . .
O3 O -0.4428(15) -0.1672(6) 1.2031(12) 0.018(4) Uani 1 1 d . . . . .
O4 O -0.4263(16) -0.1772(7) 0.8883(13) 0.026(4) Uani 1 1 d . . . . .
O5 O -0.232(3) 0.0577(9) 1.1990(18) 0.071(9) Uani 1 1 d . . . . .
O6 O -0.520(3) -0.0731(13) 1.223(2) 0.020(7) Uani 0.5 1 d . U P A 1
O6A O -0.536(3) -0.0635(12) 1.167(2) 0.011(6) Uiso 0.5 1 d . . P A 2
O7 O -0.415(3) -0.0307(14) 0.959(2) 0.024(8) Uani 0.5 1 d . U P B 1
O8 O -0.346(3) 0.0102(13) 1.064(3) 0.028(8) Uani 0.5 1 d . . P B 2
O9 O -0.280(2) -0.0943(9) 0.9954(17) 0.058(6) Uani 1 1 d . U . . .
O10 O -0.557(2) 0.0084(9) 1.2979(16) 0.052(6) Uani 1 1 d . . . . .
O11 O -0.325(3) -0.0018(13) 0.904(2) 0.018(7) Uani 0.5 1 d . U P B 1
O11A O -0.281(3) -0.0107(13) 0.887(2) 0.018(7) Uiso 0.5 1 d . . P B 2
O12 O -0.173(2) 0.1450(9) 1.1307(15) 0.049(6) Uani 1 1 d . U . . .
O13 O -0.072(2) -0.0362(10) 1.043(2) 0.059(8) Uani 1 1 d . . . . .
O14 O -0.529(2) 0.0783(9) 1.1772(17) 0.055(6) Uani 1 1 d . U . . .
O15 O -0.207(3) -0.0361(13) 1.143(2) 0.018(7) Uani 0.5 1 d . U P B 1
O15A O -0.143(3) -0.0342(13) 1.172(2) 0.016(7) Uiso 0.5 1 d . . P B 2
O16 O -0.379(3) 0.0123(12) 1.234(2) 0.022(4) Uani 0.5 1 d D U P A 1
O16A O -0.355(3) 0.0075(15) 1.295(3) 0.031(9) Uiso 0.5 1 d . . P A 2
O17 O -0.382(3) 0.1071(13) 0.962(2) 0.012(6) Uani 0.5 1 d . U P B 1
O17A O -0.357(3) 0.1375(15) 0.968(2) 0.022(8) Uiso 0.5 1 d . . P B 2
O18 O -0.402(3) -0.1251(15) 1.059(2) 0.024(5) Uani 0.5 1 d . U P A 1
O18A O -0.414(4) -0.1562(17) 1.052(3) 0.032(9) Uiso 0.5 1 d . . P A 2
O19 O -0.406(3) 0.1117(14) 1.108(2) 0.021(7) Uani 0.5 1 d . . P B 1
O19A O -0.381(4) 0.1419(18) 1.121(3) 0.031(9) Uiso 0.5 1 d . . P B 2
O20 O -0.321(3) -0.0774(13) 1.184(3) 0.023(4) Uani 0.5 1 d . U P A 1
O20A O -0.290(3) -0.0887(14) 1.243(3) 0.025(8) Uiso 0.5 1 d . . P A 2
O21 O -0.439(3) -0.0276(13) 1.123(2) 0.025(8) Uani 0.5 1 d D . P A 1
O22 O -0.476(3) 0.0715(13) 1.005(2) 0.017(7) Uani 0.5 1 d . U P B 2
N1 N 0.0849(19) 0.0541(8) 1.4636(15) 0.022(5) Uani 1 1 d . . . . .
N2 N 0.383(2) 0.2143(8) 1.2849(16) 0.025(5) Uani 1 1 d . . . . .
N3 N -0.4973(18) 0.2012(8) 1.6335(16) 0.024(5) Uani 1 1 d . . . . .
N4 N -0.1100(18) 0.0565(9) 1.5190(16) 0.025(5) Uani 1 1 d . . . . .
N5 N -0.3802(18) 0.2580(9) 0.8051(17) 0.028(5) Uani 1 1 d . . . . .
N6 N 0.257(2) 0.2659(9) 1.1055(17) 0.030(5) Uani 1 1 d . . . . .
C1 C 0.210(2) 0.0560(10) 1.5096(17) 0.020(5) Uani 1 1 d . U . . .
H1A H 0.2540 0.0357 1.5639 0.024 Uiso 1 1 calc R U . . .
C2 C 0.269(2) 0.0864(11) 1.478(2) 0.030(7) Uani 1 1 d . . . . .
H2A H 0.3532 0.0863 1.5106 0.037 Uiso 1 1 calc R U . . .
C3 C 0.206(2) 0.1176(10) 1.3987(19) 0.025(6) Uani 1 1 d . U . . .
C4 C 0.083(3) 0.1178(11) 1.350(2) 0.041(8) Uani 1 1 d . . . . .
H4A H 0.0379 0.1388 1.2969 0.049 Uiso 1 1 calc R U . . .
C5 C 0.027(3) 0.0840(12) 1.386(2) 0.033(7) Uani 1 1 d . . . . .
H5A H -0.0567 0.0827 1.3535 0.040 Uiso 1 1 calc R U . . .
C6 C 0.401(2) 0.1627(10) 1.2951(19) 0.026(6) Uani 1 1 d . U . . .
H6A H 0.4497 0.1475 1.2736 0.031 Uiso 1 1 calc R U . . .
C7 C 0.352(2) 0.1306(11) 1.3358(19) 0.028(6) Uani 1 1 d . U . . .
H7A H 0.3719 0.0954 1.3461 0.034 Uiso 1 1 calc R U . . .
C8 C 0.272(2) 0.1524(10) 1.3609(18) 0.024(6) Uani 1 1 d . U . . .
C9 C 0.248(3) 0.2042(11) 1.348(2) 0.032(6) Uani 1 1 d . U . . .
H9A H 0.1961 0.2197 1.3656 0.038 Uiso 1 1 calc R U . . .
C10 C 0.305(2) 0.2336(11) 1.3087(19) 0.027(6) Uani 1 1 d . U . . .
H10A H 0.2865 0.2689 1.2982 0.032 Uiso 1 1 calc R U . . .
C11 C -0.458(3) 0.1530(13) 1.666(2) 0.041(7) Uani 1 1 d . U . . .
H11A H -0.4811 0.1385 1.7068 0.049 Uiso 1 1 calc R U . . .
C12 C -0.386(3) 0.1228(14) 1.643(2) 0.047(8) Uani 1 1 d . U . . .
H12A H -0.3612 0.0897 1.6691 0.056 Uiso 1 1 calc R U . . .
C13 C -0.354(3) 0.1435(12) 1.580(2) 0.034(7) Uani 1 1 d . . . . .
C14 C -0.401(3) 0.1911(13) 1.541(2) 0.042(8) Uani 1 1 d . U . . .
H14A H -0.3858 0.2048 1.4944 0.051 Uiso 1 1 calc R U . . .
C15 C -0.469(3) 0.2185(12) 1.568(2) 0.038(7) Uani 1 1 d . U . . .
H15A H -0.4983 0.2510 1.5403 0.046 Uiso 1 1 calc R U . . .
C16 C -0.097(4) 0.0586(19) 1.604(3) 0.078(15) Uani 1 1 d . . . . .
H16A H -0.0334 0.0400 1.6525 0.094 Uiso 1 1 calc R U . . .
C17 C -0.171(4) 0.0865(17) 1.629(3) 0.066(11) Uani 1 1 d . U . . .
H17A H -0.1566 0.0867 1.6917 0.080 Uiso 1 1 calc R U . . .
C18 C -0.269(2) 0.1144(10) 1.5551(17) 0.021(5) Uani 1 1 d . U . . .
C19 C -0.281(3) 0.1113(14) 1.467(3) 0.048(9) Uani 1 1 d . . . . .
H19A H -0.3439 0.1290 1.4160 0.058 Uiso 1 1 calc R U . . .
C20 C -0.200(3) 0.0814(13) 1.451(2) 0.040(8) Uani 1 1 d . . . . .
H20A H -0.2116 0.0796 1.3896 0.048 Uiso 1 1 calc R U . . .
C21 C -0.319(2) 0.2361(12) 0.891(2) 0.036(7) Uani 1 1 d . . . . .
H21A H -0.3657 0.2188 0.9119 0.043 Uiso 1 1 calc R U . . .
C22 C -0.196(3) 0.2357(14) 0.953(2) 0.051(10) Uani 1 1 d . . . . .
H22A H -0.1600 0.2147 1.0074 0.061 Uiso 1 1 calc R U . . .
C23 C -0.130(2) 0.2680(11) 0.930(2) 0.032(6) Uani 1 1 d . U . . .
C24 C -0.188(3) 0.2950(12) 0.843(3) 0.044(9) Uani 1 1 d . . . . .
H24A H -0.1440 0.3161 0.8246 0.053 Uiso 1 1 calc R U . . .
C25 C -0.313(3) 0.2904(16) 0.783(3) 0.059(12) Uani 1 1 d . . . . .
H25A H -0.3513 0.3099 0.7271 0.070 Uiso 1 1 calc R U . . .
C26 C 0.195(3) 0.3090(11) 1.099(2) 0.041(8) Uani 1 1 d . . . . .
H26A H 0.2370 0.3385 1.1330 0.049 Uiso 1 1 calc R U . . .
C27 C 0.070(3) 0.3115(13) 1.044(3) 0.054(10) Uani 1 1 d . . . . .
H27A H 0.0300 0.3419 1.0428 0.065 Uiso 1 1 calc R U . . .
C28 C 0.008(2) 0.2690(12) 0.992(2) 0.032(6) Uani 1 1 d . U . . .
C29 C 0.067(4) 0.2251(18) 0.993(3) 0.077(13) Uani 1 1 d . U . . .
H29A H 0.0300 0.1974 0.9515 0.092 Uiso 1 1 calc R U . . .
C30 C 0.192(4) 0.2249(19) 1.063(3) 0.077(13) Uani 1 1 d . U . . .
H30A H 0.2304 0.1926 1.0805 0.092 Uiso 1 1 calc R U . . .
O1W O -0.125(4) -0.1617(17) 1.191(3) 0.122(14) Uiso 1 1 d . . . . .
O2W O 0.145(8) -0.112(3) 1.099(6) 0.11(3) Uiso 0.5 1 d . . P C 1
O3W O 0.167(7) -0.090(3) 1.145(6) 0.10(2) Uiso 0.5 1 d . . P D 2
O4W O -0.122(11) -0.050(5) 0.802(9) 0.15(4) Uiso 0.45 1 d . . P E 1
O5W O 0.163(9) 0.004(4) 1.235(7) 0.14(3) Uiso 0.5 1 d . . P F 2
O6W O -0.079(8) -0.111(3) 0.874(6) 0.13(3) Uiso 0.55 1 d . . P E 1
O6WA O 0.027(17) -0.143(7) 0.976(13) 0.13(6) Uiso 0.25 1 d . . P G 2
O7W O -0.065(16) 0.259(7) 1.245(14) 0.15(6) Uiso 0.3 1 d . . P H 1
O7WA O -0.070(14) 0.252(6) 1.178(12) 0.16(6) Uiso 0.35 1 d . . P I 2
O8W O 0.521(16) 0.016(6) 1.508(13) 0.15(5) Uiso 0.35 1 d . . P J 1
O9W O -0.090(15) 0.166(7) 1.798(12) 0.15(6) Uiso 0.3 1 d . . P . .
O10W O -0.349(10) 0.115(4) 1.225(8) 0.14(4) Uiso 0.45 1 d . . P K 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O13 1.71(2) . ?
W1 O15 1.82(3) . ?
W1 O9 1.90(2) . ?
W1 O11 1.92(3) . ?
W1 O2 1.97(3) . ?
W1 O15A 2.02(3) . ?
W1 O11A 2.05(3) . ?
W1 O8 2.27(4) . ?
W1 O7 2.27(3) . ?
W2 O12 1.66(2) . ?
W2 O17 1.74(3) . ?
W2 O2 1.88(3) . ?
W2 O17A 1.90(3) . ?
W2 O19 1.90(3) . ?
W2 O5 1.96(2) . ?
W2 O19A 2.04(4) . ?
W2 O22 2.30(3) . ?
W2 O8 2.39(3) . ?
W3 O1 1.697(17) . ?
W3 O16 1.76(3) . ?
W3 O15 1.84(3) . ?
W3 O5 1.84(2) . ?
W3 O20 1.89(3) . ?
W3 O15A 2.09(3) . ?
W3 O20A 2.12(4) . ?
W3 O16A 2.13(4) . ?
W3 O21 2.14(3) . ?
W3 O8 2.32(4) . ?
W4 O10 1.69(2) . ?
W4 O11 1.71(3) 3_457 ?
W4 O6A 1.81(3) . ?
W4 O16 1.86(3) . ?
W4 O14 1.97(2) . ?
W4 O6 1.99(3) . ?
W4 O11A 2.01(3) 3_457 ?
W4 O16A 2.08(4) . ?
W4 O21 2.35(3) . ?
W4 O7 2.45(3) 3_457 ?
W5 O4 1.691(17) . ?
W5 O19 1.72(3) 3_457 ?
W5 O14 1.84(2) 3_457 ?
W5 O18 1.93(3) . ?
W5 O9 1.93(2) . ?
W5 O19A 2.05(4) 3_457 ?
W5 O18A 2.10(4) . ?
W5 O22 2.19(3) 3_457 ?
W5 O7 2.29(3) . ?
W5 O10W 2.55(11) 3_457 ?
W6 O3 1.719(15) . ?
W6 O18 1.73(3) . ?
W6 O20 1.75(3) . ?
W6 O6A 1.84(3) . ?
W6 O17 1.89(3) 3_457 ?
W6 O18A 2.02(4) . ?
W6 O20A 2.04(4) . ?
W6 O6 2.20(3) . ?
W6 O21 2.21(3) . ?
W6 O17A 2.23(4) 3_457 ?
W6 O22 2.26(3) 3_457 ?
Cu1 N1 2.02(2) 3_558 ?
Cu1 N1 2.02(2) . ?
Cu1 N4 2.15(2) 3_558 ?
Cu1 N4 2.15(2) . ?
Cu1 O1 2.308(17) . ?
Cu1 O1 2.308(17) 3_558 ?
Cu2 N3 2.04(2) 4_665 ?
Cu2 N2 2.05(2) . ?
Cu2 N5 2.08(2) 4_666 ?
Cu2 N6 2.09(2) . ?
Cu2 O3 2.446(16) 2_557 ?
Cu2 O4 2.478(17) 3_557 ?
O3 Cu2 2.446(16) 2_547 ?
O4 Cu2 2.478(17) 3_557 ?
O7 W4 2.45(3) 3_457 ?
O11 W4 1.71(3) 3_457 ?
O11A W4 2.01(3) 3_457 ?
O14 W5 1.84(2) 3_457 ?
O16 O21 1.855(10) . ?
O17 W6 1.89(3) 3_457 ?
O17A W6 2.23(4) 3_457 ?
O19 W5 1.72(3) 3_457 ?
O19A W5 2.05(4) 3_457 ?
O20 O21 1.84(5) . ?
O22 W5 2.19(3) 3_457 ?
O22 W6 2.26(3) 3_457 ?
N1 C5 1.33(4) . ?
N1 C1 1.38(3) . ?
N2 C10 1.34(3) . ?
N2 C6 1.34(3) . ?
N3 C11 1.34(4) . ?
N3 C15 1.34(4) . ?
N3 Cu2 2.04(2) 4_466 ?
N4 C20 1.29(4) . ?
N4 C16 1.30(4) . ?
N5 C21 1.32(4) . ?
N5 C25 1.36(4) . ?
N5 Cu2 2.08(2) 4_465 ?
N6 C30 1.30(5) . ?
N6 C26 1.34(4) . ?
C1 C2 1.35(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.38(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.37(4) . ?
C3 C8 1.55(4) . ?
C4 C5 1.42(4) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.38(4) . ?
C6 H6A 0.9300 . ?
C7 C8 1.39(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.36(4) . ?
C9 C10 1.40(4) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.38(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.38(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.37(4) . ?
C13 C18 1.53(4) . ?
C14 C15 1.36(4) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 C17 1.39(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.42(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.35(4) . ?
C19 C20 1.41(4) . ?
C19 H19A 0.9300 . ?
C20 H20A 0.9300 . ?
C21 C22 1.39(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.36(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.39(4) . ?
C23 C28 1.53(4) . ?
C24 C25 1.40(4) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.39(4) . ?
C26 H26A 0.9300 . ?
C27 C28 1.36(4) . ?
C27 H27A 0.9300 . ?
C28 C29 1.36(5) . ?
C29 C30 1.42(6) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
O4W O6W 1.85(14) . ?
O8W O8W 0.9(3) 3_658 ?
O10W W5 2.55(11) 3_457 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 W1 O15 110.8(14) . . ?
O13 W1 O9 102.1(13) . . ?
O15 W1 O9 87.0(13) . . ?
O13 W1 O11 111.8(14) . . ?
O15 W1 O11 137.0(15) . . ?
O9 W1 O11 90.1(12) . . ?
O13 W1 O2 96.2(13) . . ?
O15 W1 O2 89.3(13) . . ?
O9 W1 O2 161.5(12) . . ?
O11 W1 O2 80.4(13) . . ?
O13 W1 O15A 91.0(14) . . ?
O9 W1 O15A 96.7(12) . . ?
O2 W1 O15A 85.7(12) . . ?
O13 W1 O11A 90.8(14) . . ?
O9 W1 O11A 88.7(12) . . ?
O2 W1 O11A 88.2(12) . . ?
O15A W1 O11A 173.8(14) . . ?
O13 W1 O8 155.1(14) . . ?
O9 W1 O8 98.8(12) . . ?
O2 W1 O8 64.3(12) . . ?
O15A W1 O8 73.1(14) . . ?
O11A W1 O8 103.2(14) . . ?
O13 W1 O7 157.7(13) . . ?
O15 W1 O7 86.9(14) . . ?
O9 W1 O7 64.1(12) . . ?
O11 W1 O7 54.0(14) . . ?
O2 W1 O7 97.6(12) . . ?
O12 W2 O17 114.6(13) . . ?
O12 W2 O2 99.3(12) . . ?
O17 W2 O2 90.9(13) . . ?
O12 W2 O17A 89.2(14) . . ?
O2 W2 O17A 101.4(14) . . ?
O12 W2 O19 111.1(14) . . ?
O17 W2 O19 87.7(14) . . ?
O2 W2 O19 147.1(14) . . ?
O12 W2 O5 98.9(13) . . ?
O17 W2 O5 146.3(14) . . ?
O2 W2 O5 86.6(11) . . ?
O17A W2 O5 167.6(14) . . ?
O19 W2 O5 76.8(14) . . ?
O12 W2 O19A 88.3(15) . . ?
O2 W2 O19A 170.4(16) . . ?
O17A W2 O19A 84.6(15) . . ?
O5 W2 O19A 86.3(13) . . ?
O12 W2 O22 151.9(12) . . ?
O2 W2 O22 105.9(12) . . ?
O17A W2 O22 74.0(14) . . ?
O5 W2 O22 94.8(13) . . ?
O19A W2 O22 68.2(15) . . ?
O12 W2 O8 153.2(12) . . ?
O2 W2 O8 62.9(13) . . ?
O17A W2 O8 112.9(15) . . ?
O5 W2 O8 62.2(12) . . ?
O19A W2 O8 107.9(16) . . ?
O22 W2 O8 54.0(12) . . ?
O1 W3 O16 105.8(11) . . ?
O1 W3 O15 109.8(13) . . ?
O16 W3 O15 144.1(14) . . ?
O1 W3 O5 98.3(12) . . ?
O16 W3 O5 87.9(14) . . ?
O15 W3 O5 91.6(12) . . ?
O1 W3 O20 109.6(13) . . ?
O16 W3 O20 93.3(15) . . ?
O15 W3 O20 70.5(16) . . ?
O5 W3 O20 150.5(14) . . ?
O1 W3 O15A 91.4(12) . . ?
O5 W3 O15A 88.0(12) . . ?
O1 W3 O20A 86.6(12) . . ?
O5 W3 O20A 174.9(13) . . ?
O15A W3 O20A 90.5(13) . . ?
O1 W3 O16A 82.9(12) . . ?
O5 W3 O16A 97.4(13) . . ?
O15A W3 O16A 172.6(14) . . ?
O20A W3 O16A 84.5(14) . . ?
O1 W3 O21 149.0(11) . . ?
O16 W3 O21 55.7(8) . . ?
O15 W3 O21 90.0(14) . . ?
O5 W3 O21 104.9(14) . . ?
O20 W3 O21 53.8(14) . . ?
O1 W3 O8 155.1(11) . . ?
O5 W3 O8 65.1(12) . . ?
O15A W3 O8 70.6(13) . . ?
O20A W3 O8 109.9(14) . . ?
O16A W3 O8 116.2(14) . . ?
O10 W4 O11 112.3(15) . 3_457 ?
O10 W4 O6A 112.9(13) . . ?
O10 W4 O16 111.4(12) . . ?
O11 W4 O16 135.3(15) 3_457 . ?
O10 W4 O14 99.4(11) . . ?
O11 W4 O14 88.1(13) 3_457 . ?
O6A W4 O14 147.7(12) . . ?
O16 W4 O14 76.3(13) . . ?
O10 W4 O6 88.4(13) . . ?
O11 W4 O6 97.4(15) 3_457 . ?
O16 W4 O6 92.5(14) . . ?
O14 W4 O6 168.0(13) . . ?
O10 W4 O11A 91.1(14) . 3_457 ?
O6A W4 O11A 93.9(14) . 3_457 ?
O14 W4 O11A 86.5(12) . 3_457 ?
O10 W4 O16A 87.2(14) . . ?
O6A W4 O16A 94.1(14) . . ?
O14 W4 O16A 85.9(13) . . ?
O11A W4 O16A 171.8(14) 3_457 . ?
O10 W4 O21 151.8(13) . . ?
O11 W4 O21 91.2(14) 3_457 . ?
O16 W4 O21 50.7(7) . . ?
O14 W4 O21 96.5(12) . . ?
O6 W4 O21 72.8(13) . . ?
O10 W4 O7 152.1(12) . 3_457 ?
O11 W4 O7 51.4(14) 3_457 3_457 ?
O16 W4 O7 84.9(13) . 3_457 ?
O14 W4 O7 61.3(11) . 3_457 ?
O6 W4 O7 114.3(13) . 3_457 ?
O21 W4 O7 55.7(12) . 3_457 ?
O4 W5 O19 107.6(13) . 3_457 ?
O4 W5 O14 99.2(10) . 3_457 ?
O19 W5 O14 88.8(14) 3_457 3_457 ?
O4 W5 O18 108.0(13) . . ?
O19 W5 O18 91.4(15) 3_457 . ?
O14 W5 O18 151.3(14) 3_457 . ?
O4 W5 O9 100.6(10) . . ?
O19 W5 O9 151.6(15) 3_457 . ?
O14 W5 O9 89.8(10) 3_457 . ?
O18 W5 O9 76.7(13) . . ?
O4 W5 O19A 85.4(14) . 3_457 ?
O14 W5 O19A 98.6(14) 3_457 3_457 ?
O9 W5 O19A 168.8(14) . 3_457 ?
O4 W5 O18A 86.9(13) . . ?
O14 W5 O18A 173.9(14) 3_457 . ?
O9 W5 O18A 88.3(13) . . ?
O19A W5 O18A 82.6(16) 3_457 . ?
O4 W5 O22 148.7(11) . 3_457 ?
O14 W5 O22 103.3(12) 3_457 3_457 ?
O9 W5 O22 100.8(12) . 3_457 ?
O19A W5 O22 70.1(14) 3_457 3_457 ?
O18A W5 O22 71.3(14) . 3_457 ?
O4 W5 O7 157.0(11) . . ?
O19 W5 O7 90.5(15) 3_457 . ?
O14 W5 O7 66.3(11) 3_457 . ?
O18 W5 O7 85.0(14) . . ?
O9 W5 O7 63.2(12) . . ?
O4 W5 O10W 87(3) . 3_457 ?
O14 W5 O10W 59(3) 3_457 3_457 ?
O9 W5 O10W 148(3) . 3_457 ?
O3 W6 O18 110.8(14) . . ?
O3 W6 O20 112.4(13) . . ?
O18 W6 O20 75.8(18) . . ?
O3 W6 O6A 106.2(11) . . ?
O3 W6 O17 107.8(11) . 3_457 ?
O18 W6 O17 94.2(15) . 3_457 ?
O20 W6 O17 139.5(15) . 3_457 ?
O3 W6 O18A 89.8(13) . . ?
O6A W6 O18A 157.7(15) . . ?
O3 W6 O20A 89.1(12) . . ?
O6A W6 O20A 93.0(14) . . ?
O18A W6 O20A 102.8(15) . . ?
O3 W6 O6 85.7(10) . . ?
O18 W6 O6 163.1(15) . . ?
O20 W6 O6 94.7(15) . . ?
O17 W6 O6 83.9(13) 3_457 . ?
O3 W6 O21 151.3(9) . . ?
O18 W6 O21 91.2(15) . . ?
O20 W6 O21 53.8(14) . . ?
O17 W6 O21 87.9(13) 3_457 . ?
O6 W6 O21 72.0(12) . . ?
O3 W6 O17A 88.1(11) . 3_457 ?
O6A W6 O17A 82.0(13) . 3_457 ?
O18A W6 O17A 83.2(14) . 3_457 ?
O20A W6 O17A 173.3(13) . 3_457 ?
O3 W6 O22 151.4(10) . 3_457 ?
O6A W6 O22 87.8(13) . 3_457 ?
O18A W6 O22 71.3(14) . 3_457 ?
O20A W6 O22 115.3(13) . 3_457 ?
O17A W6 O22 69.0(12) 3_457 3_457 ?
N1 Cu1 N1 180.0 3_558 . ?
N1 Cu1 N4 93.7(8) 3_558 3_558 ?
N1 Cu1 N4 86.3(8) . 3_558 ?
N1 Cu1 N4 86.3(8) 3_558 . ?
N1 Cu1 N4 93.7(8) . . ?
N4 Cu1 N4 180.0(8) 3_558 . ?
N1 Cu1 O1 90.1(8) 3_558 . ?
N1 Cu1 O1 89.9(8) . . ?
N4 Cu1 O1 86.2(7) 3_558 . ?
N4 Cu1 O1 93.8(7) . . ?
N1 Cu1 O1 89.9(8) 3_558 3_558 ?
N1 Cu1 O1 90.1(8) . 3_558 ?
N4 Cu1 O1 93.8(7) 3_558 3_558 ?
N4 Cu1 O1 86.2(7) . 3_558 ?
O1 Cu1 O1 180.0 . 3_558 ?
N3 Cu2 N2 177.2(9) 4_665 . ?
N3 Cu2 N5 86.0(9) 4_665 4_666 ?
N2 Cu2 N5 91.9(9) . 4_666 ?
N3 Cu2 N6 95.6(8) 4_665 . ?
N2 Cu2 N6 86.6(9) . . ?
N5 Cu2 N6 177.1(9) 4_666 . ?
N3 Cu2 O3 91.0(8) 4_665 2_557 ?
N2 Cu2 O3 87.2(7) . 2_557 ?
N5 Cu2 O3 89.9(7) 4_666 2_557 ?
N6 Cu2 O3 92.4(8) . 2_557 ?
N3 Cu2 O4 90.9(8) 4_665 3_557 ?
N2 Cu2 O4 91.0(7) . 3_557 ?
N5 Cu2 O4 92.4(8) 4_666 3_557 ?
N6 Cu2 O4 85.1(8) . 3_557 ?
O3 Cu2 O4 177.1(6) 2_557 3_557 ?
W3 O1 Cu1 166.5(10) . . ?
W2 O2 W1 133.8(16) . . ?
W6 O3 Cu2 176.0(9) . 2_547 ?
W5 O4 Cu2 166.0(10) . 3_557 ?
W3 O5 W2 136.0(16) . . ?
W4 O6 W6 113.4(16) . . ?
W4 O6A W6 146.6(18) . . ?
W1 O7 W5 100.2(13) . . ?
W1 O7 W4 97.0(13) . 3_457 ?
W5 O7 W4 96.4(12) . 3_457 ?
W1 O8 W3 99.3(13) . . ?
W1 O8 W2 98.9(13) . . ?
W3 O8 W2 96.7(14) . . ?
W1 O9 W5 132.3(15) . . ?
W4 O11 W1 153(2) 3_457 . ?
W4 O11A W1 121.4(18) 3_457 . ?
W5 O14 W4 135.9(14) 3_457 . ?
W1 O15 W3 145(2) . . ?
W1 O15A W3 116.5(17) . . ?
W3 O16 O21 72.6(15) . . ?
W3 O16 W4 148.5(16) . . ?
O21 O16 W4 78.3(15) . . ?
W4 O16A W3 112.1(18) . . ?
W2 O17 W6 148.8(18) . 3_457 ?
W2 O17A W6 115.7(18) . 3_457 ?
W6 O18 W5 142(2) . . ?
W6 O18A W5 114(2) . . ?
W5 O19 W2 152(2) 3_457 . ?
W2 O19A W5 118(2) . 3_457 ?
W6 O20 O21 76.1(17) . . ?
W6 O20 W3 143(2) . . ?
O21 O20 W3 70.1(15) . . ?
W6 O20A W3 112.0(17) . . ?
O20 O21 O16 92(2) . . ?
O20 O21 W3 56.2(14) . . ?
O16 O21 W3 51.7(13) . . ?
O20 O21 W6 50.0(14) . . ?
O16 O21 W6 117.7(19) . . ?
W3 O21 W6 104.8(15) . . ?
O20 O21 W4 118.3(19) . . ?
O16 O21 W4 51.0(13) . . ?
W3 O21 W4 101.9(10) . . ?
W6 O21 W4 100.3(13) . . ?
W5 O22 W6 101.9(13) 3_457 3_457 ?
W5 O22 W2 102.8(13) 3_457 . ?
W6 O22 W2 100.3(12) 3_457 . ?
C5 N1 C1 116(2) . . ?
C5 N1 Cu1 122.6(18) . . ?
C1 N1 Cu1 120.8(16) . . ?
C10 N2 C6 116(2) . . ?
C10 N2 Cu2 122.3(18) . . ?
C6 N2 Cu2 119.8(17) . . ?
C11 N3 C15 114(2) . . ?
C11 N3 Cu2 117.1(19) . 4_466 ?
C15 N3 Cu2 127.3(19) . 4_466 ?
C20 N4 C16 117(3) . . ?
C20 N4 Cu1 125.8(19) . . ?
C16 N4 Cu1 116(2) . . ?
C21 N5 C25 114(2) . . ?
C21 N5 Cu2 125.2(19) . 4_465 ?
C25 N5 Cu2 120(2) . 4_465 ?
C30 N6 C26 115(3) . . ?
C30 N6 Cu2 119(3) . . ?
C26 N6 Cu2 124(2) . . ?
C2 C1 N1 122(2) . . ?
C2 C1 H1A 118.8 . . ?
N1 C1 H1A 118.8 . . ?
C1 C2 C3 120(2) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C4 C3 C2 120(2) . . ?
C4 C3 C8 118(2) . . ?
C2 C3 C8 121(2) . . ?
C3 C4 C5 116(3) . . ?
C3 C4 H4A 122.1 . . ?
C5 C4 H4A 122.1 . . ?
N1 C5 C4 125(3) . . ?
N1 C5 H5A 117.3 . . ?
C4 C5 H5A 117.3 . . ?
N2 C6 C7 124(3) . . ?
N2 C6 H6A 118.2 . . ?
C7 C6 H6A 118.2 . . ?
C6 C7 C8 118(3) . . ?
C6 C7 H7A 120.8 . . ?
C8 C7 H7A 120.8 . . ?
C9 C8 C7 120(3) . . ?
C9 C8 C3 120(2) . . ?
C7 C8 C3 121(2) . . ?
C8 C9 C10 118(3) . . ?
C8 C9 H9A 121.2 . . ?
C10 C9 H9A 121.2 . . ?
N2 C10 C9 124(3) . . ?
N2 C10 H10A 117.8 . . ?
C9 C10 H10A 117.8 . . ?
N3 C11 C12 126(3) . . ?
N3 C11 H11A 117.0 . . ?
C12 C11 H11A 117.0 . . ?
C13 C12 C11 117(3) . . ?
C13 C12 H12A 121.3 . . ?
C11 C12 H12A 121.3 . . ?
C14 C13 C12 117(3) . . ?
C14 C13 C18 121(3) . . ?
C12 C13 C18 122(3) . . ?
C15 C14 C13 121(3) . . ?
C15 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
N3 C15 C14 123(3) . . ?
N3 C15 H15A 118.3 . . ?
C14 C15 H15A 118.3 . . ?
N4 C16 C17 125(4) . . ?
N4 C16 H16A 117.3 . . ?
C17 C16 H16A 117.3 . . ?
C16 C17 C18 117(4) . . ?
C16 C17 H17A 121.4 . . ?
C18 C17 H17A 121.4 . . ?
C19 C18 C17 116(3) . . ?
C19 C18 C13 126(3) . . ?
C17 C18 C13 118(3) . . ?
C18 C19 C20 121(3) . . ?
C18 C19 H19A 119.7 . . ?
C20 C19 H19A 119.7 . . ?
N4 C20 C19 123(3) . . ?
N4 C20 H20A 118.5 . . ?
C19 C20 H20A 118.5 . . ?
N5 C21 C22 128(3) . . ?
N5 C21 H21A 115.8 . . ?
C22 C21 H21A 115.8 . . ?
C23 C22 C21 116(3) . . ?
C23 C22 H22A 122.1 . . ?
C21 C22 H22A 122.1 . . ?
C22 C23 C24 119(3) . . ?
C22 C23 C28 120(3) . . ?
C24 C23 C28 121(2) . . ?
C23 C24 C25 120(3) . . ?
C23 C24 H24A 119.8 . . ?
C25 C24 H24A 119.8 . . ?
N5 C25 C24 122(3) . . ?
N5 C25 H25A 119.2 . . ?
C24 C25 H25A 119.2 . . ?
N6 C26 C27 123(3) . . ?
N6 C26 H26A 118.7 . . ?
C27 C26 H26A 118.7 . . ?
C28 C27 C26 119(3) . . ?
C28 C27 H27A 120.3 . . ?
C26 C27 H27A 120.3 . . ?
C29 C28 C27 120(3) . . ?
C29 C28 C23 117(3) . . ?
C27 C28 C23 123(3) . . ?
C28 C29 C30 115(4) . . ?
C28 C29 H29A 122.7 . . ?
C30 C29 H29A 122.7 . . ?
N6 C30 C29 126(4) . . ?
N6 C30 H30A 117.1 . . ?
C29 C30 H30A 117.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O16 W3 O1 Cu1 -37(5) . . . . ?
O15 W3 O1 Cu1 148(5) . . . . ?
O5 W3 O1 Cu1 53(5) . . . . ?
O20 W3 O1 Cu1 -136(5) . . . . ?
O15A W3 O1 Cu1 141(5) . . . . ?
O20A W3 O1 Cu1 -128(5) . . . . ?
O16A W3 O1 Cu1 -43(5) . . . . ?
O21 W3 O1 Cu1 -85(5) . . . . ?
O8 W3 O1 Cu1 99(5) . . . . ?
O12 W2 O2 W1 160(2) . . . . ?
O17 W2 O2 W1 -85(2) . . . . ?
O17A W2 O2 W1 -109(2) . . . . ?
O19 W2 O2 W1 2(4) . . . . ?
O5 W2 O2 W1 61(2) . . . . ?
O22 W2 O2 W1 -33(2) . . . . ?
O8 W2 O2 W1 0.8(18) . . . . ?
O19 W5 O4 Cu2 52(5) 3_457 . . 3_557 ?
O14 W5 O4 Cu2 -39(5) 3_457 . . 3_557 ?
O18 W5 O4 Cu2 150(4) . . . 3_557 ?
O9 W5 O4 Cu2 -131(4) . . . 3_557 ?
O19A W5 O4 Cu2 59(5) 3_457 . . 3_557 ?
O18A W5 O4 Cu2 142(5) . . . 3_557 ?
O22 W5 O4 Cu2 97(5) 3_457 . . 3_557 ?
O7 W5 O4 Cu2 -88(5) . . . 3_557 ?
O10W W5 O4 Cu2 18(5) 3_457 . . 3_557 ?
O1 W3 O5 W2 158(2) . . . . ?
O16 W3 O5 W2 -96(2) . . . . ?
O15 W3 O5 W2 48(2) . . . . ?
O20 W3 O5 W2 -3(4) . . . . ?
O15A W3 O5 W2 67(2) . . . . ?
O16A W3 O5 W2 -118(2) . . . . ?
O21 W3 O5 W2 -42(2) . . . . ?
O8 W3 O5 W2 -2(2) . . . . ?
O10 W4 O6A W6 -129(3) . . . . ?
O14 W4 O6A W6 48(5) . . . . ?
O11A W4 O6A W6 138(3) 3_457 . . . ?
O16A W4 O6A W6 -41(4) . . . . ?
O3 W6 O6A W4 132(3) . . . . ?
O18A W6 O6A W4 -93(5) . . . . ?
O20A W6 O6A W4 42(4) . . . . ?
O17A W6 O6A W4 -142(4) 3_457 . . . ?
O22 W6 O6A W4 -73(3) 3_457 . . . ?
O13 W1 O9 W5 -155.9(18) . . . . ?
O15 W1 O9 W5 94(2) . . . . ?
O11 W1 O9 W5 -44(2) . . . . ?
O2 W1 O9 W5 15(5) . . . . ?
O15A W1 O9 W5 112(2) . . . . ?
O11A W1 O9 W5 -65(2) . . . . ?
O8 W1 O9 W5 38(2) . . . . ?
O7 W1 O9 W5 5.5(17) . . . . ?
O13 W1 O15 W3 135(3) . . . . ?
O9 W1 O15 W3 -124(4) . . . . ?
O11 W1 O15 W3 -37(5) . . . . ?
O2 W1 O15 W3 38(4) . . . . ?
O7 W1 O15 W3 -59(4) . . . . ?
O1 W3 O15 W1 -137(3) . . . . ?
O16 W3 O15 W1 52(5) . . . . ?
O5 W3 O15 W1 -37(4) . . . . ?
O20 W3 O15 W1 119(4) . . . . ?
O21 W3 O15 W1 68(4) . . . . ?
O1 W3 O16 O21 -152.3(14) . . . . ?
O15 W3 O16 O21 20(3) . . . . ?
O5 W3 O16 O21 109.6(17) . . . . ?
O20 W3 O16 O21 -40.8(18) . . . . ?
O1 W3 O16 W4 -129(4) . . . . ?
O15 W3 O16 W4 43(6) . . . . ?
O5 W3 O16 W4 133(4) . . . . ?
O20 W3 O16 W4 -18(4) . . . . ?
O21 W3 O16 W4 23(3) . . . . ?
O10 W4 O16 W3 132(4) . . . . ?
O11 W4 O16 W3 -60(5) 3_457 . . . ?
O14 W4 O16 W3 -133(4) . . . . ?
O6 W4 O16 W3 43(4) . . . . ?
O21 W4 O16 W3 -23(3) . . . . ?
O7 W4 O16 W3 -72(4) 3_457 . . . ?
O10 W4 O16 O21 154.5(16) . . . . ?
O11 W4 O16 O21 -38(3) 3_457 . . . ?
O14 W4 O16 O21 -110.6(17) . . . . ?
O6 W4 O16 O21 65.3(18) . . . . ?
O7 W4 O16 O21 -48.9(16) 3_457 . . . ?
O12 W2 O17 W6 -125(3) . . . 3_457 ?
O2 W2 O17 W6 134(4) . . . 3_457 ?
O19 W2 O17 W6 -13(4) . . . 3_457 ?
O5 W2 O17 W6 49(5) . . . 3_457 ?
O12 W2 O17A W6 -165.8(17) . . . 3_457 ?
O2 W2 O17A W6 94.8(18) . . . 3_457 ?
O5 W2 O17A W6 -34(7) . . . 3_457 ?
O19A W2 O17A W6 -78(2) . . . 3_457 ?
O22 W2 O17A W6 -8.7(15) . . . 3_457 ?
O8 W2 O17A W6 30(2) . . . 3_457 ?
O3 W6 O18 W5 130(3) . . . . ?
O20 W6 O18 W5 -121(4) . . . . ?
O17 W6 O18 W5 19(4) 3_457 . . . ?
O6 W6 O18 W5 -64(7) . . . . ?
O21 W6 O18 W5 -69(4) . . . . ?
O12 W2 O19 W5 130(4) . . . 3_457 ?
O17 W2 O19 W5 14(5) . . . 3_457 ?
O2 W2 O19 W5 -74(6) . . . 3_457 ?
O5 W2 O19 W5 -136(5) . . . 3_457 ?
O3 W6 O20 O21 -150.9(12) . . . . ?
O18 W6 O20 O21 102.2(18) . . . . ?
O17 W6 O20 O21 22(3) 3_457 . . . ?
O6 W6 O20 O21 -63.7(15) . . . . ?
O3 W6 O20 W3 -126(3) . . . . ?
O18 W6 O20 W3 127(4) . . . . ?
O17 W6 O20 W3 47(5) 3_457 . . . ?
O6 W6 O20 W3 -39(4) . . . . ?
O21 W6 O20 W3 24(3) . . . . ?
O1 W3 O20 W6 125(3) . . . . ?
O16 W3 O20 W6 17(4) . . . . ?
O15 W3 O20 W6 -130(4) . . . . ?
O5 W3 O20 W6 -75(5) . . . . ?
O21 W3 O20 W6 -25(3) . . . . ?
O1 W3 O20 O21 150.1(13) . . . . ?
O16 W3 O20 O21 42.1(15) . . . . ?
O15 W3 O20 O21 -105.1(18) . . . . ?
O5 W3 O20 O21 -50(3) . . . . ?
W6 O20 O21 O16 125.1(19) . . . . ?
W3 O20 O21 O16 -39.5(16) . . . . ?
W6 O20 O21 W3 164.6(18) . . . . ?
W3 O20 O21 W6 -164.6(18) . . . . ?
W6 O20 O21 W4 79.1(18) . . . . ?
W3 O20 O21 W4 -85.4(16) . . . . ?
W3 O16 O21 O20 42.3(17) . . . . ?
W4 O16 O21 O20 -125.5(19) . . . . ?
W4 O16 O21 W3 -167.8(18) . . . . ?
W3 O16 O21 W6 87.4(19) . . . . ?
W4 O16 O21 W6 -80.5(19) . . . . ?
W3 O16 O21 W4 167.8(18) . . . . ?
C5 N1 C1 C2 0(4) . . . . ?
Cu1 N1 C1 C2 170(2) . . . . ?
N1 C1 C2 C3 1(4) . . . . ?
C1 C2 C3 C4 0(5) . . . . ?
C1 C2 C3 C8 -179(3) . . . . ?
C2 C3 C4 C5 -1(4) . . . . ?
C8 C3 C4 C5 178(3) . . . . ?
C1 N1 C5 C4 -2(4) . . . . ?
Cu1 N1 C5 C4 -172(2) . . . . ?
C3 C4 C5 N1 2(5) . . . . ?
C10 N2 C6 C7 -6(4) . . . . ?
Cu2 N2 C6 C7 -171(2) . . . . ?
N2 C6 C7 C8 5(4) . . . . ?
C6 C7 C8 C9 -2(4) . . . . ?
C6 C7 C8 C3 175(2) . . . . ?
C4 C3 C8 C9 55(4) . . . . ?
C2 C3 C8 C9 -126(3) . . . . ?
C4 C3 C8 C7 -122(3) . . . . ?
C2 C3 C8 C7 57(4) . . . . ?
C7 C8 C9 C10 1(4) . . . . ?
C3 C8 C9 C10 -176(2) . . . . ?
C6 N2 C10 C9 4(4) . . . . ?
Cu2 N2 C10 C9 169(2) . . . . ?
C8 C9 C10 N2 -2(4) . . . . ?
C15 N3 C11 C12 5(5) . . . . ?
Cu2 N3 C11 C12 -163(3) 4_466 . . . ?
N3 C11 C12 C13 -1(5) . . . . ?
C11 C12 C13 C14 -4(5) . . . . ?
C11 C12 C13 C18 177(3) . . . . ?
C12 C13 C14 C15 5(5) . . . . ?
C18 C13 C14 C15 -175(3) . . . . ?
C11 N3 C15 C14 -4(4) . . . . ?
Cu2 N3 C15 C14 163(3) 4_466 . . . ?
C13 C14 C15 N3 -1(5) . . . . ?
C20 N4 C16 C17 -1(7) . . . . ?
Cu1 N4 C16 C17 -170(4) . . . . ?
N4 C16 C17 C18 1(7) . . . . ?
C16 C17 C18 C19 0(6) . . . . ?
C16 C17 C18 C13 178(4) . . . . ?
C14 C13 C18 C19 -40(4) . . . . ?
C12 C13 C18 C19 139(4) . . . . ?
C14 C13 C18 C17 142(3) . . . . ?
C12 C13 C18 C17 -38(4) . . . . ?
C17 C18 C19 C20 0(5) . . . . ?
C13 C18 C19 C20 -177(3) . . . . ?
C16 N4 C20 C19 2(5) . . . . ?
Cu1 N4 C20 C19 169(3) . . . . ?
C18 C19 C20 N4 -1(6) . . . . ?
C25 N5 C21 C22 -11(5) . . . . ?
Cu2 N5 C21 C22 167(3) 4_465 . . . ?
N5 C21 C22 C23 10(6) . . . . ?
C21 C22 C23 C24 -5(5) . . . . ?
C21 C22 C23 C28 -178(3) . . . . ?
C22 C23 C24 C25 3(5) . . . . ?
C28 C23 C24 C25 175(3) . . . . ?
C21 N5 C25 C24 7(5) . . . . ?
Cu2 N5 C25 C24 -171(3) 4_465 . . . ?
C23 C24 C25 N5 -3(6) . . . . ?
C30 N6 C26 C27 -6(5) . . . . ?
Cu2 N6 C26 C27 -168(3) . . . . ?
N6 C26 C27 C28 -2(6) . . . . ?
C26 C27 C28 C29 -1(6) . . . . ?
C26 C27 C28 C23 -180(3) . . . . ?
C22 C23 C28 C29 67(5) . . . . ?
C24 C23 C28 C29 -106(4) . . . . ?
C22 C23 C28 C27 -114(4) . . . . ?
C24 C23 C28 C27 73(4) . . . . ?
C27 C28 C29 C30 10(6) . . . . ?
C23 C28 C29 C30 -171(4) . . . . ?
C26 N6 C30 C29 17(6) . . . . ?
Cu2 N6 C30 C29 -180(4) . . . . ?
C28 C29 C30 N6 -20(7) . . . . ?

_refine_diff_density_max         2.421
_refine_diff_density_min         -3.328
_refine_diff_density_rms         0.378



