# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_xc
_database_code_depnum_ccdc_archive 'CCDC 938554'
_audit_update_record             
;
2013-05-10 deposited with the CCDC.
2015-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H158 Cu3 N24 O170 P4 W36'
_chemical_formula_weight         11157.44

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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'I 4 3 2'

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

_cell_length_a                   28.9058(4)
_cell_length_b                   28.9058(4)
_cell_length_c                   28.9058(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     24152.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.73
_cell_measurement_theta_max      26.03

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             20004
_exptl_absorpt_coefficient_mu    17.453
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1794
_exptl_absorpt_correction_T_max  0.2100
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4006
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       -2
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.03
_reflns_number_total             4006
_reflns_number_gt                3909
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0354P)²+306.5963P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.076(14)
_refine_ls_number_reflns         4006
_refine_ls_number_parameters     225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0594
_refine_ls_wR_factor_gt          0.0591
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.80544(9) 0.5000 0.0344(5) Uani 1 4 d S . .
O1W O 0.5000 0.7220(5) 0.5000 0.043(3) Uani 1 4 d S . .
O12 O 0.3585(3) 0.9201(3) 0.5472(3) 0.058(2) Uani 1 1 d . . .
N1 N 0.4294(2) 0.8070(2) 0.4960(3) 0.0281(14) Uani 1 1 d . . .
N2 N 0.2939(3) 0.8766(3) 0.5584(3) 0.043(2) Uani 1 1 d . . .
H2B H 0.2781 0.8527 0.5504 0.051 Uiso 1 1 d R . .
C1 C 0.4056(3) 0.7754(3) 0.4723(3) 0.0318(19) Uani 1 1 d . . .
H1A H 0.4215 0.7525 0.4562 0.038 Uiso 1 1 calc R . .
C2 C 0.3576(3) 0.7759(3) 0.4710(3) 0.0279(18) Uani 1 1 d . . .
H2A H 0.3418 0.7529 0.4550 0.033 Uiso 1 1 calc R . .
C3 C 0.3340(3) 0.8092(3) 0.4927(3) 0.0309(18) Uani 1 1 d . . .
H3A H 0.3019 0.8098 0.4917 0.037 Uiso 1 1 calc R . .
C4 C 0.3585(3) 0.8429(3) 0.5168(3) 0.0283(17) Uani 1 1 d . . .
C5 C 0.4055(3) 0.8405(3) 0.5178(3) 0.0304(19) Uani 1 1 d . . .
H5A H 0.4217 0.8630 0.5342 0.037 Uiso 1 1 calc R . .
C6 C 0.3369(3) 0.8831(4) 0.5411(3) 0.036(2) Uani 1 1 d . . .
C7 C 0.2746(4) 0.9106(5) 0.5902(4) 0.056(3) Uani 1 1 d . . .
H7A H 0.2853 0.9040 0.6213 0.067 Uiso 1 1 calc R . .
H7B H 0.2854 0.9412 0.5818 0.067 Uiso 1 1 calc R . .
W1 W 0.333674(10) 0.657362(10) 0.810795(10) 0.01966(8) Uani 1 1 d . . .
W2 W 0.236874(11) 0.613932(9) 0.763451(11) 0.01929(8) Uani 1 1 d . . .
W3 W 0.396535(10) 0.652972(11) 0.699304(11) 0.02078(8) Uani 1 1 d . . .
P1 P 0.28963(6) 0.71037(6) 0.71037(6) 0.0147(5) Uani 1 3 d S . .
O1 O 0.32079(15) 0.67921(15) 0.67921(15) 0.0163(16) Uani 1 3 d S . .
O2 O 0.27991(17) 0.68309(17) 0.75457(17) 0.0182(11) Uani 1 1 d . . .
O3 O 0.28997(18) 0.60976(17) 0.80342(18) 0.0201(11) Uani 1 1 d . . .
O4 O 0.36153(17) 0.71731(17) 0.80121(18) 0.0199(11) Uani 1 1 d . . .
O5 O 0.36737(18) 0.63938(17) 0.75720(16) 0.0199(10) Uani 1 1 d . . .
O6 O 0.40042(18) 0.67479(18) 0.63743(19) 0.0225(11) Uani 1 1 d . . .
O7 O 0.27842(19) 0.59518(17) 0.71293(18) 0.0220(11) Uani 1 1 d . . .
O8 O 0.44971(18) 0.6281(2) 0.7054(2) 0.0292(13) Uani 1 1 d . . .
O9 O 0.2115(2) 0.56066(18) 0.7731(2) 0.0293(13) Uani 1 1 d . . .
O10 O 0.36929(19) 0.6330(2) 0.85139(18) 0.0282(11) Uani 1 1 d . . .
O11 O 0.29329(17) 0.69015(17) 0.85196(17) 0.0201(11) Uani 1 1 d . . .
O2W O 0.5000 0.8928(6) 0.5000 0.036(4) Uani 0.72(2) 4 d SP A 1
O2W' O 0.5000 0.9380(15) 0.5000 0.036(4) Uani 0.28(2) 4 d SP A 2


_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 take n 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.043(6) 7_656 ?
Cu1 N1 2.043(6) . ?
Cu1 N1 2.043(6) 19_655 ?
Cu1 N1 2.043(6) 20_556 ?
Cu1 O1W 2.411(14) . ?
O12 C6 1.252(12) . ?
N1 C1 1.335(11) . ?
N1 C5 1.347(11) . ?
N2 C6 1.353(12) . ?
N2 C7 1.457(12) . ?
N2 H2B 0.8599 . ?
C1 C2 1.386(12) . ?
C1 H1A 0.9300 . ?
C2 C3 1.336(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.391(12) . ?
C3 H3A 0.9300 . ?
C4 C5 1.360(12) . ?
C4 C6 1.495(12) . ?
C5 H5A 0.9300 . ?
C7 C7 1.42(2) 40_566 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
W1 O10 1.713(5) . ?
W1 O3 1.880(5) . ?
W1 O5 1.902(5) . ?
W1 O11 1.917(5) . ?
W1 O4 1.931(5) . ?
W1 O2 2.369(5) . ?
W2 O9 1.728(5) . ?
W2 O4 1.869(5) 11_665 ?
W2 O11 1.879(5) 40_566 ?
W2 O3 1.925(5) . ?
W2 O7 1.967(5) . ?
W2 O2 2.368(5) . ?
W3 O8 1.707(5) . ?
W3 O7 1.864(5) 24_656 ?
W3 O6 1.900(5) . ?
W3 O5 1.915(5) . ?
W3 O6 1.961(5) 11_665 ?
W3 O1 2.389(4) . ?
P1 O2 1.527(5) 24_656 ?
P1 O2 1.527(5) . ?
P1 O2 1.527(5) 11_665 ?
P1 O1 1.560(8) . ?
O1 W3 2.389(4) 24_656 ?
O1 W3 2.389(4) 11_665 ?
O4 W2 1.869(5) 24_656 ?
O6 W3 1.962(5) 24_656 ?
O7 W3 1.864(5) 11_665 ?
O11 W2 1.879(5) 40_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 177.4(4) 7_656 . ?
N1 Cu1 N1 89.974(11) 7_656 19_655 ?
N1 Cu1 N1 89.968(10) . 19_655 ?
N1 Cu1 N1 89.973(11) 7_656 20_556 ?
N1 Cu1 N1 89.969(11) . 20_556 ?
N1 Cu1 N1 177.4(4) 19_655 20_556 ?
N1 Cu1 O1W 91.3(2) 7_656 . ?
N1 Cu1 O1W 91.3(2) . . ?
N1 Cu1 O1W 91.3(2) 19_655 . ?
N1 Cu1 O1W 91.3(2) 20_556 . ?
C1 N1 C5 117.8(7) . . ?
C1 N1 Cu1 122.0(6) . . ?
C5 N1 Cu1 120.2(5) . . ?
C6 N2 C7 119.5(10) . . ?
C6 N2 H2B 120.1 . . ?
C7 N2 H2B 120.5 . . ?
N1 C1 C2 121.6(8) . . ?
N1 C1 H1A 119.2 . . ?
C2 C1 H1A 119.2 . . ?
C3 C2 C1 120.3(8) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 118.7(8) . . ?
C2 C3 H3A 120.7 . . ?
C4 C3 H3A 120.7 . . ?
C5 C4 C3 119.0(8) . . ?
C5 C4 C6 116.4(8) . . ?
C3 C4 C6 124.6(8) . . ?
N1 C5 C4 122.6(8) . . ?
N1 C5 H5A 118.7 . . ?
C4 C5 H5A 118.7 . . ?
O12 C6 N2 121.7(9) . . ?
O12 C6 C4 121.5(9) . . ?
N2 C6 C4 116.7(9) . . ?
C7 C7 N2 111.2(13) 40_566 . ?
C7 C7 H7A 109.4 40_566 . ?
N2 C7 H7A 109.4 . . ?
C7 C7 H7B 109.4 40_566 . ?
N2 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O10 W1 O3 100.4(3) . . ?
O10 W1 O5 97.9(2) . . ?
O3 W1 O5 93.0(2) . . ?
O10 W1 O11 98.3(2) . . ?
O3 W1 O11 91.3(2) . . ?
O5 W1 O11 162.2(2) . . ?
O10 W1 O4 102.5(3) . . ?
O3 W1 O4 157.0(2) . . ?
O5 W1 O4 85.1(2) . . ?
O11 W1 O4 84.2(2) . . ?
O10 W1 O2 173.6(3) . . ?
O3 W1 O2 73.2(2) . . ?
O5 W1 O2 82.13(19) . . ?
O11 W1 O2 82.59(19) . . ?
O4 W1 O2 83.9(2) . . ?
O9 W2 O4 101.7(2) . 11_665 ?
O9 W2 O11 99.0(3) . 40_566 ?
O4 W2 O11 92.1(2) 11_665 40_566 ?
O9 W2 O3 100.7(2) . . ?
O4 W2 O3 157.2(2) 11_665 . ?
O11 W2 O3 88.5(2) 40_566 . ?
O9 W2 O7 97.6(2) . . ?
O4 W2 O7 86.2(2) 11_665 . ?
O11 W2 O7 163.3(2) 40_566 . ?
O3 W2 O7 86.7(2) . . ?
O9 W2 O2 172.9(2) . . ?
O4 W2 O2 84.93(19) 11_665 . ?
O11 W2 O2 83.00(19) 40_566 . ?
O3 W2 O2 72.50(19) . . ?
O7 W2 O2 80.30(19) . . ?
O8 W3 O7 103.9(2) . 24_656 ?
O8 W3 O6 100.6(3) . . ?
O7 W3 O6 90.5(2) 24_656 . ?
O8 W3 O5 102.7(3) . . ?
O7 W3 O5 86.9(2) 24_656 . ?
O6 W3 O5 156.5(2) . . ?
O8 W3 O6 99.0(2) . 11_665 ?
O7 W3 O6 157.0(2) 24_656 11_665 ?
O6 W3 O6 87.2(3) . 11_665 ?
O5 W3 O6 86.2(2) . 11_665 ?
O8 W3 O1 170.0(2) . . ?
O7 W3 O1 84.64(19) 24_656 . ?
O6 W3 O1 73.73(19) . . ?
O5 W3 O1 82.77(18) . . ?
O6 W3 O1 72.73(19) 11_665 . ?
O2 P1 O2 111.90(18) 24_656 . ?
O2 P1 O2 111.90(18) 24_656 11_665 ?
O2 P1 O2 111.90(18) . 11_665 ?
O2 P1 O1 106.9(2) 24_656 . ?
O2 P1 O1 106.9(2) . . ?
O2 P1 O1 106.9(2) 11_665 . ?
P1 O1 W3 124.89(15) . . ?
P1 O1 W3 124.89(15) . 24_656 ?
W3 O1 W3 90.5(2) . 24_656 ?
P1 O1 W3 124.89(15) . 11_665 ?
W3 O1 W3 90.5(2) . 11_665 ?
W3 O1 W3 90.5(2) 24_656 11_665 ?
P1 O2 W2 128.5(3) . . ?
P1 O2 W1 128.0(3) . . ?
W2 O2 W1 90.30(17) . . ?
W1 O3 W2 123.9(3) . . ?
W2 O4 W1 152.0(3) 24_656 . ?
W1 O5 W3 151.8(3) . . ?
W3 O6 W3 123.0(3) . 24_656 ?
W3 O7 W2 150.0(3) 11_665 . ?
W2 O11 W1 163.9(3) 40_566 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.140








# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 871.6 223.7
2 0.499 -0.011 -0.003 5934.9 1350.3
3 0.226 0.000 0.226 8.5 0.4
4 0.774 0.000 0.226 8.5 0.4
5 0.226 0.000 0.774 8.5 0.3
6 0.774 0.000 0.774 8.5 0.3
7 0.226 0.226 0.000 8.5 0.3
8 0.774 0.226 0.000 8.5 0.3
9 0.000 0.226 0.226 8.5 0.5
10 0.000 0.226 0.774 8.5 0.3
11 0.500 0.274 0.274 8.5 0.2
12 0.274 0.274 0.500 8.5 0.4
13 0.726 0.274 0.500 8.5 0.4
14 0.500 0.274 0.726 8.5 0.4
15 0.500 0.500 0.500 871.6 223.7
16 0.274 0.500 0.274 8.5 0.3
17 0.726 0.500 0.274 8.5 0.3
18 0.274 0.500 0.726 8.5 0.4
19 0.726 0.500 0.726 8.5 0.4
20 0.500 0.726 0.274 8.5 0.3
21 0.274 0.726 0.500 8.5 0.3
22 0.726 0.726 0.500 8.5 0.3
23 0.500 0.726 0.726 8.5 0.5
24 0.226 0.774 0.000 8.5 0.4
25 0.774 0.774 0.000 8.5 0.4
26 0.000 0.774 0.226 8.5 0.4
27 0.000 0.774 0.774 8.5 0.2
_platon_squeeze_details          ?





#=End

