# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2
_publcif_datablock.id            {727f6899-d290-4359-9c2d-1d8058eca140}

_audit_update_record             
;
2013-12-19 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H34 B Cu4 N11 O S3 W'
_chemical_formula_sum            'C26 H34 B Cu4 N11 O S3 W'
_chemical_formula_weight         1061.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_HALL  '-P 2ac 2n'

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                   22.3102(12)
_cell_length_b                   10.5390(9)
_cell_length_c                   19.3846(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4557.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    5407
_cell_measurement_theta_min      3.3370
_cell_measurement_theta_max      28.3750

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2072
_exptl_absorpt_coefficient_mu    4.519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3442
_exptl_absorpt_correction_T_max  0.6607
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?

_diffrn_ambient_temperature      223(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'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_reflns_number            24256
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         27.10
_reflns_number_total             5302
_reflns_number_gt                3978
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_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)+(0.0844P)²+42.5871P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5302
_refine_ls_number_parameters     225
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.1878
_refine_ls_wR_factor_gt          0.1755
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.047
_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 -0.17229(2) 0.2500 1.20380(3) 0.02610(18) Uani 1 2 d S . .
Cu1 Cu -0.07381(5) 0.11119(13) 1.18729(7) 0.0424(3) Uani 1 1 d . . .
Cu2 Cu -0.13418(7) 0.2500 1.07463(8) 0.0363(4) Uani 1 2 d S . .
Cu3 Cu 0.06920(7) -0.2500 1.17104(9) 0.0373(4) Uani 1 2 d S . .
S1 S -0.08781(14) 0.2500 1.27186(18) 0.0349(8) Uani 1 2 d S . .
S2 S -0.15972(10) 0.0774(2) 1.13228(13) 0.0355(5) Uani 1 1 d . . .
N1 N 0.0211(4) -0.0934(11) 1.1866(5) 0.051(2) Uani 1 1 d . . .
N2 N -0.1009(5) 0.2500 0.9239(6) 0.042(3) Uani 1 2 d S . .
N3 N 0.1381(7) -0.2500 1.2443(9) 0.077(3) Uani 1 2 d S . .
N5 N -0.2646(3) 0.1325(8) 1.3137(4) 0.0336(18) Uani 1 1 d . . .
N6 N -0.2107(3) 0.1096(8) 1.2819(4) 0.0330(18) Uani 1 1 d . . .
N7 N -0.3149(4) 0.2500 1.2189(6) 0.040(3) Uani 1 2 d S . .
N8 N -0.2694(4) 0.2500 1.1694(6) 0.031(2) Uani 1 2 d S . .
B1 B -0.3013(7) 0.2500 1.2968(8) 0.036(4) Uani 1 2 d SD . .
H1 H -0.344(4) 0.2500 1.329(6) 0.043 Uiso 1 2 d SD . .
C1 C -0.0124(4) -0.0096(10) 1.1881(5) 0.033(2) Uani 1 1 d . . .
C2 C -0.1149(5) 0.2500 0.9800(6) 0.034(3) Uani 1 2 d S . .
C3 C 0.1604(6) -0.1416(18) 1.2678(7) 0.077(3) Uani 1 1 d . . .
H3 H 0.1431 -0.0652 1.2527 0.092 Uiso 1 1 calc R . .
C4 C 0.2079(6) -0.1359(18) 1.3136(7) 0.077(3) Uani 1 1 d . . .
H4 H 0.2226 -0.0583 1.3304 0.092 Uiso 1 1 calc R . .
C5 C 0.2322(9) -0.2500 1.3332(10) 0.077(3) Uani 1 2 d S . .
H5 H 0.2667 -0.2500 1.3610 0.092 Uiso 1 2 calc SR . .
C9 C -0.3319(6) 0.0458(14) 1.4058(7) 0.069(4) Uani 1 1 d . . .
H9A H -0.3363 0.1295 1.4260 0.103 Uiso 1 1 calc R . .
H9B H -0.3278 -0.0167 1.4422 0.103 Uiso 1 1 calc R . .
H9C H -0.3670 0.0262 1.3782 0.103 Uiso 1 1 calc R . .
C10 C -0.2767(5) 0.0432(10) 1.3606(5) 0.043(3) Uani 1 1 d . . .
C11 C -0.2304(6) -0.0408(11) 1.3594(6) 0.054(3) Uani 1 1 d . . .
H11 H -0.2263 -0.1136 1.3870 0.065 Uiso 1 1 calc R . .
C12 C -0.1904(5) 0.0018(11) 1.3095(6) 0.046(3) Uani 1 1 d . . .
C13 C -0.1342(6) -0.0610(13) 1.2921(8) 0.073(4) Uani 1 1 d . . .
H13A H -0.1386 -0.1052 1.2485 0.110 Uiso 1 1 calc R . .
H13B H -0.1241 -0.1214 1.3280 0.110 Uiso 1 1 calc R . .
H13C H -0.1026 0.0018 1.2883 0.110 Uiso 1 1 calc R . .
C14 C -0.4263(7) 0.2500 1.2276(10) 0.075(6) Uani 1 2 d S . .
H14A H -0.4174 0.2500 1.2765 0.112 Uiso 0.50 2 calc SPR . .
H14B H -0.4494 0.1749 1.2161 0.112 Uiso 0.25 1 calc PR . .
H14C H -0.4494 0.3251 1.2161 0.112 Uiso 0.25 1 calc PR . .
H14D H -0.4600 0.2500 1.1959 0.112 Uiso 0.50 2 calc SPR . .
H14E H -0.4281 0.3251 1.2564 0.112 Uiso 0.25 1 calc PR . .
H14F H -0.4281 0.1749 1.2564 0.112 Uiso 0.25 1 calc PR . .
C15 C -0.3682(6) 0.2500 1.1870(9) 0.056(5) Uani 1 2 d S . .
C16 C -0.3584(6) 0.2500 1.1179(8) 0.048(4) Uani 1 2 d S . .
H16 H -0.3879 0.2500 1.0832 0.058 Uiso 1 2 calc SR . .
C17 C -0.2973(6) 0.2500 1.1080(7) 0.036(3) Uani 1 2 d S . .
C18 C -0.2688(7) 0.2500 1.0395(7) 0.053(4) Uani 1 2 d S . .
H18A H -0.2256 0.2500 1.0447 0.079 Uiso 0.50 2 calc SPR . .
H18B H -0.2811 0.3251 1.0142 0.079 Uiso 0.25 1 calc PR . .
H18C H -0.2811 0.1749 1.0142 0.079 Uiso 0.25 1 calc PR . .
H18D H -0.2996 0.2500 1.0041 0.079 Uiso 0.50 2 calc SPR . .
H18E H -0.2441 0.1749 1.0346 0.079 Uiso 0.25 1 calc PR . .
H18F H -0.2441 0.3251 1.0346 0.079 Uiso 0.25 1 calc PR . .
O1 O -0.0175(4) 0.251(7) 1.1070(5) 0.048(2) Uani 0.50 1 d PD A -1
N4 N 0.0406(6) 0.2212(14) 1.0131(7) 0.048(2) Uani 0.50 1 d PD A -1
C6 C 0.0242(9) 0.0906(16) 1.0020(11) 0.048(2) Uani 0.50 1 d PD A -1
H6A H 0.0019 0.0596 1.0415 0.072 Uiso 0.50 1 calc PR A -1
H6B H 0.0602 0.0400 0.9961 0.072 Uiso 0.50 1 calc PR A -1
H6C H -0.0004 0.0841 0.9609 0.072 Uiso 0.50 1 calc PR A -1
C7 C 0.0767(8) 0.2779(19) 0.9586(8) 0.048(2) Uani 0.50 1 d PD A -1
H7A H 0.0545 0.2762 0.9156 0.072 Uiso 0.50 1 calc PR A -1
H7B H 0.1136 0.2302 0.9533 0.072 Uiso 0.50 1 calc PR A -1
H7C H 0.0861 0.3650 0.9706 0.072 Uiso 0.50 1 calc PR A -1
C8 C 0.0183(8) 0.2891(18) 1.0628(9) 0.048(2) Uani 0.50 1 d PD A -1
H8 H 0.0304 0.3744 1.0655 0.057 Uiso 0.50 1 calc PR A -1


_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 N8 2.268(10) . ?
W1 N6 2.284(7) 7_565 ?
W1 N6 2.284(7) . ?
W1 S1 2.301(3) . ?
W1 S2 2.304(3) . ?
W1 S2 2.304(3) 7_565 ?
W1 Cu2 2.6444(17) . ?
W1 Cu1 2.6589(12) . ?
W1 Cu1 2.6590(12) 7_565 ?
Cu1 C1 1.870(10) . ?
Cu1 S1 2.219(3) . ?
Cu1 S2 2.222(3) . ?
Cu1 Cu1 2.926(3) 7_565 ?
Cu1 Cu2 2.954(2) . ?
Cu2 C2 1.885(13) . ?
Cu2 S2 2.209(3) 7_565 ?
Cu2 S2 2.209(3) . ?
Cu2 Cu1 2.954(2) 7_565 ?
Cu3 N2 1.971(13) 5_557 ?
Cu3 N1 1.992(11) . ?
Cu3 N1 1.992(11) 7 ?
Cu3 N3 2.093(16) . ?
S1 Cu1 2.219(3) 7_565 ?
N1 C1 1.158(13) . ?
N2 C2 1.132(17) . ?
N2 Cu3 1.971(13) 5_557 ?
N3 C3 1.326(18) . ?
N3 C3 1.326(18) 7 ?
N5 C10 1.335(13) . ?
N5 N6 1.373(10) . ?
N5 B1 1.521(12) . ?
N6 C12 1.335(14) . ?
N7 C15 1.340(18) . ?
N7 N8 1.397(14) . ?
N7 B1 1.54(2) . ?
N8 C17 1.342(17) . ?
B1 N5 1.521(12) 7_565 ?
B1 H1 1.15(2) . ?
C3 C4 1.384(19) . ?
C3 H3 0.9400 . ?
C4 C5 1.373(19) . ?
C4 H4 0.9400 . ?
C5 C4 1.373(19) 7 ?
C5 H5 0.9400 . ?
C9 C10 1.511(15) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.361(16) . ?
C11 C12 1.391(16) . ?
C11 H11 0.9400 . ?
C12 C13 1.457(17) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 C15 1.52(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C14 H14D 0.9700 . ?
C14 H14E 0.9700 . ?
C14 H14F 0.9700 . ?
C15 C16 1.36(2) . ?
C16 C17 1.377(17) . ?
C16 H16 0.9400 . ?
C17 C18 1.472(19) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 H18E 0.9700 . ?
C18 H18F 0.9700 . ?
O1 C8 1.23(2) . ?
N4 C8 1.299(15) . ?
N4 C6 1.441(16) . ?
N4 C7 1.458(15) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8 0.9400 . ?

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
N8 W1 N6 80.6(3) . 7_565 ?
N8 W1 N6 80.6(3) . . ?
N6 W1 N6 80.8(4) 7_565 . ?
N8 W1 S1 162.1(3) . . ?
N6 W1 S1 85.8(2) 7_565 . ?
N6 W1 S1 85.8(2) . . ?
N8 W1 S2 86.51(18) . . ?
N6 W1 S2 162.9(2) 7_565 . ?
N6 W1 S2 86.2(2) . . ?
S1 W1 S2 104.20(8) . . ?
N8 W1 S2 86.51(18) . 7_565 ?
N6 W1 S2 86.2(2) 7_565 7_565 ?
N6 W1 S2 162.9(2) . 7_565 ?
S1 W1 S2 104.20(8) . 7_565 ?
S2 W1 S2 104.25(13) . 7_565 ?
N8 W1 Cu2 91.6(3) . . ?
N6 W1 Cu2 138.4(2) 7_565 . ?
N6 W1 Cu2 138.4(2) . . ?
S1 W1 Cu2 106.24(10) . . ?
S2 W1 Cu2 52.49(7) . . ?
S2 W1 Cu2 52.49(6) 7_565 . ?
N8 W1 Cu1 138.96(15) . . ?
N6 W1 Cu1 138.3(2) 7_565 . ?
N6 W1 Cu1 91.9(2) . . ?
S1 W1 Cu1 52.56(7) . . ?
S2 W1 Cu1 52.61(6) . . ?
S2 W1 Cu1 105.15(7) 7_565 . ?
Cu2 W1 Cu1 67.69(4) . . ?
N8 W1 Cu1 138.96(15) . 7_565 ?
N6 W1 Cu1 91.9(2) 7_565 7_565 ?
N6 W1 Cu1 138.3(2) . 7_565 ?
S1 W1 Cu1 52.56(7) . 7_565 ?
S2 W1 Cu1 105.15(7) . 7_565 ?
S2 W1 Cu1 52.61(6) 7_565 7_565 ?
Cu2 W1 Cu1 67.69(4) . 7_565 ?
Cu1 W1 Cu1 66.76(6) . 7_565 ?
C1 Cu1 S1 123.1(3) . . ?
C1 Cu1 S2 121.8(3) . . ?
S1 Cu1 S2 109.80(11) . . ?
C1 Cu1 W1 168.2(3) . . ?
S1 Cu1 W1 55.39(8) . . ?
S2 Cu1 W1 55.47(7) . . ?
C1 Cu1 Cu1 132.9(3) . 7_565 ?
S1 Cu1 Cu1 48.76(7) . 7_565 ?
S2 Cu1 Cu1 99.22(8) . 7_565 ?
W1 Cu1 Cu1 56.62(3) . 7_565 ?
C1 Cu1 Cu2 132.6(3) . . ?
S1 Cu1 Cu2 98.95(8) . . ?
S2 Cu1 Cu2 48.02(8) . . ?
W1 Cu1 Cu2 55.92(4) . . ?
Cu1 Cu1 Cu2 60.31(3) 7_565 . ?
C2 Cu2 S2 123.45(10) . 7_565 ?
C2 Cu2 S2 123.45(10) . . ?
S2 Cu2 S2 110.82(14) 7_565 . ?
C2 Cu2 W1 174.4(4) . . ?
S2 Cu2 W1 55.82(7) 7_565 . ?
S2 Cu2 W1 55.82(7) . . ?
C2 Cu2 Cu1 128.0(3) . . ?
S2 Cu2 Cu1 98.71(9) 7_565 . ?
S2 Cu2 Cu1 48.39(7) . . ?
W1 Cu2 Cu1 56.39(4) . . ?
C2 Cu2 Cu1 128.0(3) . 7_565 ?
S2 Cu2 Cu1 48.39(7) 7_565 7_565 ?
S2 Cu2 Cu1 98.71(9) . 7_565 ?
W1 Cu2 Cu1 56.39(4) . 7_565 ?
Cu1 Cu2 Cu1 59.38(6) . 7_565 ?
N2 Cu3 N1 109.6(3) 5_557 . ?
N2 Cu3 N1 109.6(3) 5_557 7 ?
N1 Cu3 N1 111.9(6) . 7 ?
N2 Cu3 N3 111.7(6) 5_557 . ?
N1 Cu3 N3 107.1(4) . . ?
N1 Cu3 N3 107.1(4) 7 . ?
Cu1 S1 Cu1 82.48(14) . 7_565 ?
Cu1 S1 W1 72.05(10) . . ?
Cu1 S1 W1 72.05(10) 7_565 . ?
Cu2 S2 Cu1 83.59(10) . . ?
Cu2 S2 W1 71.69(9) . . ?
Cu1 S2 W1 71.92(8) . . ?
C1 N1 Cu3 169.8(9) . . ?
C2 N2 Cu3 175.1(12) . 5_557 ?
C3 N3 C3 118.9(18) . 7 ?
C3 N3 Cu3 120.6(9) . . ?
C3 N3 Cu3 120.6(9) 7 . ?
C10 N5 N6 111.1(8) . . ?
C10 N5 B1 127.7(9) . . ?
N6 N5 B1 121.1(8) . . ?
C12 N6 N5 105.4(8) . . ?
C12 N6 W1 133.6(7) . . ?
N5 N6 W1 120.9(6) . . ?
C15 N7 N8 109.1(12) . . ?
C15 N7 B1 128.9(12) . . ?
N8 N7 B1 122.0(10) . . ?
C17 N8 N7 105.8(10) . . ?
C17 N8 W1 134.7(8) . . ?
N7 N8 W1 119.5(8) . . ?
N5 B1 N5 109.0(12) 7_565 . ?
N5 B1 N7 108.6(7) 7_565 . ?
N5 B1 N7 108.6(7) . . ?
N5 B1 H1 109(4) 7_565 . ?
N5 B1 H1 109(4) . . ?
N7 B1 H1 112(8) . . ?
N1 C1 Cu1 172.9(9) . . ?
N2 C2 Cu2 177.1(12) . . ?
N3 C3 C4 123.0(17) . . ?
N3 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C5 C4 C3 116.2(17) . . ?
C5 C4 H4 121.9 . . ?
C3 C4 H4 121.9 . . ?
C4 C5 C4 122(2) . 7 ?
C4 C5 H5 118.8 . . ?
C4 C5 H5 118.8 7 . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C10 C11 107.0(9) . . ?
N5 C10 C9 123.2(11) . . ?
C11 C10 C9 129.8(11) . . ?
C10 C11 C12 106.8(10) . . ?
C10 C11 H11 126.6 . . ?
C12 C11 H11 126.6 . . ?
N6 C12 C11 109.7(10) . . ?
N6 C12 C13 125.9(10) . . ?
C11 C12 C13 124.5(11) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C14 H14D 109.5 . . ?
H14A C14 H14D 141.1 . . ?
H14B C14 H14D 56.3 . . ?
H14C C14 H14D 56.3 . . ?
C15 C14 H14E 109.5 . . ?
H14A C14 H14E 56.3 . . ?
H14B C14 H14E 141.1 . . ?
H14C C14 H14E 56.3 . . ?
H14D C14 H14E 109.5 . . ?
C15 C14 H14F 109.5 . . ?
H14A C14 H14F 56.3 . . ?
H14B C14 H14F 56.3 . . ?
H14C C14 H14F 141.1 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
N7 C15 C16 108.2(13) . . ?
N7 C15 C14 121.2(15) . . ?
C16 C15 C14 130.6(14) . . ?
C15 C16 C17 107.3(13) . . ?
C15 C16 H16 126.4 . . ?
C17 C16 H16 126.4 . . ?
N8 C17 C16 109.6(12) . . ?
N8 C17 C18 126.9(11) . . ?
C16 C17 C18 123.5(13) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C18 H18D 109.5 . . ?
H18A C18 H18D 141.1 . . ?
H18B C18 H18D 56.3 . . ?
H18C C18 H18D 56.3 . . ?
C17 C18 H18E 109.5 . . ?
H18A C18 H18E 56.3 . . ?
H18B C18 H18E 141.1 . . ?
H18C C18 H18E 56.3 . . ?
H18D C18 H18E 109.5 . . ?
C17 C18 H18F 109.5 . . ?
H18A C18 H18F 56.3 . . ?
H18B C18 H18F 56.3 . . ?
H18C C18 H18F 141.1 . . ?
H18D C18 H18F 109.5 . . ?
H18E C18 H18F 109.5 . . ?
C8 N4 C6 122.7(15) . . ?
C8 N4 C7 121.6(15) . . ?
C6 N4 C7 115.0(14) . . ?
O1 C8 N4 126(3) . . ?
O1 C8 H8 117.2 . . ?
N4 C8 H8 117.2 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         6.672
_refine_diff_density_min         -1.779
_refine_diff_density_rms         0.220


# 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 0.500 0.012 0.000 622 123 ' '
2 0.000 -0.048 0.500 622 123 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 992891'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3
_publcif_datablock.id            {52f35d5f-e6d8-41c1-bc9d-45c6b10389d3}

_audit_update_record             
;
2013-12-01 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H29 B Cu4 N10 O S3 W'
_chemical_formula_sum            'C21 H29 B Cu4 N10 O S3 W'
_chemical_formula_weight         982.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_HALL  '-P 2ac 2n'

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                   29.866(6)
_cell_length_b                   10.387(2)
_cell_length_c                   13.906(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4313.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    12192
_cell_measurement_theta_min      3.0082
_cell_measurement_theta_max      27.4778

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    4.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2515
_exptl_absorpt_correction_T_max  0.6471
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      223(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  'Rigaku Mercury'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            15572
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.35
_reflns_number_total             4152
_reflns_number_gt                3508
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_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)+(0.0606P)²+10.1152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4152
_refine_ls_number_parameters     213
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1420
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.404706(16) 0.7500 0.84215(3) 0.04256(18) Uani 1 2 d S . .
Cu1 Cu 0.31584(6) 0.7500 0.84959(11) 0.0611(4) Uani 1 2 d S . .
C11 C 0.3743(4) 0.7500 0.6105(8) 0.052(3) Uani 1 2 d S . .
C10 C 0.3945(5) 0.7500 0.5199(8) 0.063(4) Uani 1 2 d S . .
H10 H 0.3798 0.7500 0.4601 0.076 Uiso 1 2 calc SR . .
C9 C 0.4394(5) 0.7500 0.5351(8) 0.061(3) Uani 1 2 d S . .
C12 C 0.3252(5) 0.7500 0.6291(10) 0.080(4) Uani 1 2 d S . .
H12A H 0.3159 0.6650 0.6500 0.119 Uiso 0.50 1 calc PR . .
H12B H 0.3094 0.7726 0.5705 0.119 Uiso 0.50 1 calc PR . .
H12C H 0.3183 0.8124 0.6788 0.119 Uiso 0.50 1 calc PR . .
C8 C 0.4780(5) 0.7500 0.4617(8) 0.080(5) Uani 1 2 d S . .
H8A H 0.4902 0.8363 0.4561 0.120 Uiso 0.50 1 calc PR . .
H8B H 0.4669 0.7220 0.3996 0.120 Uiso 0.50 1 calc PR . .
H8C H 0.5013 0.6917 0.4832 0.120 Uiso 0.50 1 calc PR . .
C6 C 0.4742(3) 1.0044(7) 0.8579(5) 0.054(2) Uani 1 1 d . . .
C5 C 0.5129(3) 1.0492(8) 0.8132(6) 0.062(2) Uani 1 1 d . . .
H5 H 0.5282 1.1256 0.8283 0.074 Uiso 1 1 calc R . .
C4 C 0.5246(3) 0.9649(8) 0.7453(6) 0.058(2) Uani 1 1 d . . .
C7 C 0.4504(4) 1.0695(8) 0.9384(6) 0.063(2) Uani 1 1 d . . .
H7A H 0.4201 1.0901 0.9186 0.095 Uiso 1 1 calc R . .
H7B H 0.4661 1.1481 0.9552 0.095 Uiso 1 1 calc R . .
H7C H 0.4495 1.0127 0.9937 0.095 Uiso 1 1 calc R . .
C3 C 0.5634(4) 0.9675(11) 0.6789(7) 0.082(3) Uani 1 1 d . . .
H3A H 0.5805 1.0455 0.6895 0.123 Uiso 1 1 calc R . .
H3B H 0.5528 0.9655 0.6130 0.123 Uiso 1 1 calc R . .
H3C H 0.5822 0.8931 0.6908 0.123 Uiso 1 1 calc R . .
C2 C 0.3486(3) 1.0958(8) 1.1361(6) 0.053(2) Uani 1 1 d . . .
C1 C 0.2566(5) 0.7500 0.8212(9) 0.063(3) Uani 1 2 d S . .
N6 N 0.4070(3) 0.7500 0.6771(6) 0.051(2) Uani 1 2 d S . .
N5 N 0.4462(3) 0.7500 0.6299(6) 0.048(2) Uani 1 2 d S . .
N4 N 0.4622(2) 0.8919(6) 0.8153(4) 0.0489(16) Uani 1 1 d . . .
N3 N 0.4936(2) 0.8695(6) 0.7460(4) 0.0477(15) Uani 1 1 d . . .
N1 N 0.2206(5) 0.7500 0.7885(8) 0.080(4) Uani 1 2 d S . .
N2 N 0.3578(3) 1.0140(8) 1.0826(6) 0.076(2) Uani 1 1 d . . .
S1 S 0.35756(8) 0.9254(2) 0.83094(14) 0.0546(5) Uani 1 1 d . . .
S2 S 0.42767(11) 0.7500 1.00045(19) 0.0501(7) Uani 1 2 d S . .
B1 B 0.4913(6) 0.7500 0.6821(10) 0.059(4) Uani 1 2 d SD . .
H1 H 0.523(3) 0.7500 0.634(8) 0.088 Uiso 1 2 d SD . .
Cu2 Cu 0.37250(4) 0.89166(10) 0.98584(7) 0.0597(3) Uani 1 1 d . . .
Cu3 Cu 0.32877(5) 1.2500 1.19552(10) 0.0528(4) Uani 1 2 d S . .
O1 O 0.3061(4) 0.746(5) 1.0281(7) 0.082(2) Uani 0.50 1 d PD A -1
N7 N 0.2431(4) 0.762(2) 1.1174(8) 0.082(2) Uani 0.50 1 d PD A -1
C13 C 0.2113(6) 0.6996(17) 1.1779(12) 0.082(2) Uani 0.50 1 d PD A -1
H13A H 0.2218 0.6139 1.1939 0.123 Uiso 0.50 1 calc PR A -1
H13B H 0.1828 0.6933 1.1446 0.123 Uiso 0.50 1 calc PR A -1
H13C H 0.2074 0.7491 1.2365 0.123 Uiso 0.50 1 calc PR A -1
C14 C 0.2395(7) 0.8976(15) 1.1075(13) 0.082(2) Uani 0.50 1 d PD A -1
H14A H 0.2664 0.9310 1.0776 0.123 Uiso 0.50 1 calc PR A -1
H14B H 0.2358 0.9364 1.1704 0.123 Uiso 0.50 1 calc PR A -1
H14C H 0.2138 0.9181 1.0677 0.123 Uiso 0.50 1 calc PR A -1
C15 C 0.2771(6) 0.6979(16) 1.0785(12) 0.082(2) Uani 0.50 1 d PD A -1
H15 H 0.2790 0.6090 1.0906 0.099 Uiso 0.50 1 calc PR A -1


_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 N4 2.293(7) . ?
W1 N4 2.293(7) 7_575 ?
W1 N6 2.296(9) . ?
W1 S2 2.306(3) . ?
W1 S1 2.308(2) 7_575 ?
W1 S1 2.308(2) . ?
W1 Cu1 2.6560(18) . ?
W1 Cu2 2.6614(11) 7_575 ?
W1 Cu2 2.6614(11) . ?
Cu1 C1 1.814(14) . ?
Cu1 S1 2.223(3) 7_575 ?
Cu1 S1 2.223(3) . ?
Cu1 Cu2 2.9355(17) 7_575 ?
Cu1 Cu2 2.9356(17) . ?
C11 N6 1.345(14) . ?
C11 C10 1.395(17) . ?
C11 C12 1.489(19) . ?
C10 C9 1.358(19) . ?
C10 H10 0.9400 . ?
C9 N5 1.334(14) . ?
C9 C8 1.541(19) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C6 N4 1.359(10) . ?
C6 C5 1.392(13) . ?
C6 C7 1.488(12) . ?
C5 C4 1.335(12) . ?
C5 H5 0.9400 . ?
C4 N3 1.357(10) . ?
C4 C3 1.481(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C2 N2 1.162(10) . ?
C2 Cu3 1.898(8) . ?
C1 N1 1.166(18) . ?
N6 N5 1.343(14) . ?
N5 B1 1.531(19) . ?
N4 N3 1.365(9) . ?
N3 B1 1.528(10) . ?
N1 Cu3 1.961(15) 2_574 ?
N2 Cu2 1.902(9) . ?
S1 Cu2 2.227(2) . ?
S2 Cu2 2.218(3) . ?
S2 Cu2 2.218(3) 7_575 ?
B1 N3 1.528(10) 7_575 ?
B1 H1 1.15(2) . ?
Cu2 Cu2 2.943(2) 7_575 ?
Cu3 C2 1.897(8) 7_585 ?
Cu3 N1 1.961(15) 2_575 ?
O1 C15 1.221(17) . ?
N7 C15 1.328(14) . ?
N7 C14 1.422(17) . ?
N7 C13 1.425(14) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15 0.9400 . ?

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
N4 W1 N4 80.0(3) . 7_575 ?
N4 W1 N6 79.4(2) . . ?
N4 W1 N6 79.4(2) 7_575 . ?
N4 W1 S2 86.14(16) . . ?
N4 W1 S2 86.14(16) 7_575 . ?
N6 W1 S2 161.0(3) . . ?
N4 W1 S1 162.40(17) . 7_575 ?
N4 W1 S1 86.45(18) 7_575 7_575 ?
N6 W1 S1 87.16(17) . 7_575 ?
S2 W1 S1 104.24(7) . 7_575 ?
N4 W1 S1 86.45(18) . . ?
N4 W1 S1 162.40(17) 7_575 . ?
N6 W1 S1 87.16(17) . . ?
S2 W1 S1 104.23(7) . . ?
S1 W1 S1 104.28(12) 7_575 . ?
N4 W1 Cu1 138.96(16) . . ?
N4 W1 Cu1 138.96(16) 7_575 . ?
N6 W1 Cu1 93.9(3) . . ?
S2 W1 Cu1 105.07(9) . . ?
S1 W1 Cu1 52.63(6) 7_575 . ?
S1 W1 Cu1 52.63(6) . . ?
N4 W1 Cu2 138.43(15) . 7_575 ?
N4 W1 Cu2 92.13(16) 7_575 7_575 ?
N6 W1 Cu2 139.56(14) . 7_575 ?
S2 W1 Cu2 52.46(7) . 7_575 ?
S1 W1 Cu2 52.68(6) 7_575 7_575 ?
S1 W1 Cu2 105.47(6) . 7_575 ?
Cu1 W1 Cu2 67.02(4) . 7_575 ?
N4 W1 Cu2 92.13(16) . . ?
N4 W1 Cu2 138.42(15) 7_575 . ?
N6 W1 Cu2 139.56(14) . . ?
S2 W1 Cu2 52.46(7) . . ?
S1 W1 Cu2 105.47(6) 7_575 . ?
S1 W1 Cu2 52.68(6) . . ?
Cu1 W1 Cu2 67.02(4) . . ?
Cu2 W1 Cu2 67.13(5) 7_575 . ?
C1 Cu1 S1 121.45(13) . 7_575 ?
C1 Cu1 S1 121.45(13) . . ?
S1 Cu1 S1 110.14(14) 7_575 . ?
C1 Cu1 W1 165.2(4) . . ?
S1 Cu1 W1 55.62(7) 7_575 . ?
S1 Cu1 W1 55.62(7) . . ?
C1 Cu1 Cu2 134.7(3) . 7_575 ?
S1 Cu1 Cu2 48.80(6) 7_575 7_575 ?
S1 Cu1 Cu2 99.39(8) . 7_575 ?
W1 Cu1 Cu2 56.58(4) . 7_575 ?
C1 Cu1 Cu2 134.7(3) . . ?
S1 Cu1 Cu2 99.39(8) 7_575 . ?
S1 Cu1 Cu2 48.80(6) . . ?
W1 Cu1 Cu2 56.58(4) . . ?
Cu2 Cu1 Cu2 60.16(5) 7_575 . ?
N6 C11 C10 108.0(12) . . ?
N6 C11 C12 126.4(11) . . ?
C10 C11 C12 125.5(11) . . ?
C9 C10 C11 106.6(10) . . ?
C9 C10 H10 126.7 . . ?
C11 C10 H10 126.7 . . ?
N5 C9 C10 107.7(12) . . ?
N5 C9 C8 122.7(12) . . ?
C10 C9 C8 129.6(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C6 C5 108.2(8) . . ?
N4 C6 C7 126.3(8) . . ?
C5 C6 C7 125.5(8) . . ?
C4 C5 C6 108.3(8) . . ?
C4 C5 H5 125.9 . . ?
C6 C5 H5 125.9 . . ?
C5 C4 N3 107.2(8) . . ?
C5 C4 C3 129.3(9) . . ?
N3 C4 C3 123.5(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C2 Cu3 165.8(7) . . ?
N1 C1 Cu1 169.6(13) . . ?
N5 N6 C11 107.2(9) . . ?
N5 N6 W1 120.9(7) . . ?
C11 N6 W1 131.9(9) . . ?
C9 N5 N6 110.5(10) . . ?
C9 N5 B1 127.1(11) . . ?
N6 N5 B1 122.5(9) . . ?
C6 N4 N3 105.8(7) . . ?
C6 N4 W1 132.9(6) . . ?
N3 N4 W1 121.3(4) . . ?
C4 N3 N4 110.5(7) . . ?
C4 N3 B1 128.2(9) . . ?
N4 N3 B1 121.3(8) . . ?
C1 N1 Cu3 161.7(12) . 2_574 ?
C2 N2 Cu2 174.7(7) . . ?
Cu1 S1 Cu2 82.55(9) . . ?
Cu1 S1 W1 71.75(8) . . ?
Cu2 S1 W1 71.83(7) . . ?
Cu2 S2 Cu2 83.09(13) . 7_575 ?
Cu2 S2 W1 72.04(8) . . ?
Cu2 S2 W1 72.04(8) 7_575 . ?
N3 B1 N3 108.6(10) 7_575 . ?
N3 B1 N5 108.3(8) 7_575 . ?
N3 B1 N5 108.3(8) . . ?
N3 B1 H1 108(4) 7_575 . ?
N3 B1 H1 108(4) . . ?
N5 B1 H1 116(7) . . ?
N2 Cu2 S2 123.3(3) . . ?
N2 Cu2 S1 122.2(2) . . ?
S2 Cu2 S1 109.98(10) . . ?
N2 Cu2 W1 169.7(3) . . ?
S2 Cu2 W1 55.50(7) . . ?
S1 Cu2 W1 55.49(6) . . ?
N2 Cu2 Cu1 131.2(3) . . ?
S2 Cu2 Cu1 98.91(7) . . ?
S1 Cu2 Cu1 48.66(7) . . ?
W1 Cu2 Cu1 56.40(4) . . ?
N2 Cu2 Cu2 131.9(2) . 7_575 ?
S2 Cu2 Cu2 48.45(6) . 7_575 ?
S1 Cu2 Cu2 99.06(6) . 7_575 ?
W1 Cu2 Cu2 56.44(2) . 7_575 ?
Cu1 Cu2 Cu2 59.92(3) . 7_575 ?
C2 Cu3 C2 115.2(5) 7_585 . ?
C2 Cu3 N1 121.5(3) 7_585 2_575 ?
C2 Cu3 N1 121.5(3) . 2_575 ?
C15 N7 C14 121.0(13) . . ?
C15 N7 C13 121.6(15) . . ?
C14 N7 C13 117.2(13) . . ?
O1 C15 N7 125(2) . . ?
O1 C15 H15 117.6 . . ?
N7 C15 H15 117.6 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.918
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.166

# 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 0.250 -0.025 1.006 731 146 ' '
2 0.750 -0.037 0.481 731 146 ' '
3 0.441 0.250 0.121 14 2 ' '
4 0.941 0.250 0.379 14 2 ' '
5 0.059 0.750 0.621 14 2 ' '
6 0.559 0.750 0.879 14 2 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 992892'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_update_record             
;
2014-09-28 # Formatted by publCIF

;
_publcif_datablock.id            {a3036823-3b3d-48f3-8867-2a8c825a0188}

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H29 B Cu4 N10 O S3 W, 4(C6 H7 N)'
_chemical_formula_sum            'C45 H57 B Cu4 N14 O S3 W'
_chemical_formula_weight         1355.04

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      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                   17.767(4)
_cell_length_b                   17.553(4)
_cell_length_c                   18.214(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.49(3)
_cell_angle_gamma                90
_cell_volume                     5387(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    21598
_cell_measurement_theta_min      3.0078
_cell_measurement_theta_max      27.5943

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      1.671
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_F_000             2704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.845
_shelx_estimated_absorpt_T_min   0.206
_shelx_estimated_absorpt_T_max   0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2062
_exptl_absorpt_correction_T_max  0.5692
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            26939
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.023
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10956
_reflns_number_gt                9169
_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0851P)²+48.7388P]
 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10956
_refine_ls_number_parameters     637
_refine_ls_number_restraints     363
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0795
_refine_ls_wR_factor_ref         0.2153
_refine_ls_wR_factor_gt          0.2062
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.176
_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 0.32316(2) 0.03598(2) 0.24688(2) 0.02856(15) Uani 1 1 d . . . . .
Cu1 Cu 0.18930(8) -0.04539(8) 0.20656(8) 0.0400(3) Uani 1 1 d . . . . .
Cu2 Cu 0.21916(8) 0.08689(8) 0.11609(8) 0.0413(3) Uani 1 1 d . . . . .
Cu3 Cu 0.20319(8) 0.11024(9) 0.27222(8) 0.0422(3) Uani 1 1 d . . . . .
Cu4 Cu -0.04868(9) -0.20700(11) 0.12944(10) 0.0594(5) Uani 1 1 d . . . . .
S1 S 0.25002(15) -0.00145(16) 0.32500(15) 0.0349(6) Uani 1 1 d . . . . .
S2 S 0.26783(16) -0.03099(16) 0.13312(16) 0.0368(6) Uani 1 1 d . . . . .
S3 S 0.28521(17) 0.16041(16) 0.21482(16) 0.0371(6) Uani 1 1 d . . . . .
O1 O 0.0977(5) 0.0566(5) 0.1584(5) 0.051(2) Uani 1 1 d . . . . .
N1 N 0.0518(7) -0.1559(7) 0.1707(6) 0.056(3) Uani 1 1 d . . . . .
N2 N 0.1169(7) 0.1552(8) -0.0350(7) 0.064(3) Uani 1 1 d . . . . .
N3 N -0.0978(7) -0.2859(7) 0.1711(6) 0.056(3) Uani 1 1 d . . . . .
N4 N -0.0130(6) 0.1102(6) 0.0771(6) 0.049(3) Uani 1 1 d . . . . .
N5 N 0.4811(5) -0.0631(5) 0.3112(6) 0.036(2) Uani 1 1 d . . . . .
N6 N 0.4004(5) -0.0688(5) 0.2882(5) 0.0326(19) Uani 1 1 d . . . . .
N7 N 0.4883(5) 0.0586(5) 0.3812(5) 0.036(2) Uani 1 1 d . . . . .
N8 N 0.4110(5) 0.0823(5) 0.3576(5) 0.0345(19) Uani 1 1 d . . . . .
N9 N 0.5045(6) 0.0584(5) 0.2505(5) 0.036(2) Uani 1 1 d . . . . .
N10 N 0.4274(5) 0.0654(5) 0.2029(5) 0.036(2) Uani 1 1 d . . . . .
C1 C 0.1063(6) -0.1187(6) 0.1873(6) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.1551(7) 0.1280(7) 0.0207(6) 0.043(3) Uani 1 1 d . . . . .
C3 C -0.1336(6) -0.3263(7) 0.1931(7) 0.040(3) Uani 1 1 d . . . . .
C4 C 0.0096(9) 0.1887(8) 0.1026(10) 0.066(4) Uani 1 1 d . . . . .
H4A H 0.0176 0.2177 0.0603 0.098 Uiso 1 1 calc R U . . .
H4B H 0.0585 0.1882 0.1459 0.098 Uiso 1 1 calc R U . . .
H4C H -0.0322 0.2121 0.1186 0.098 Uiso 1 1 calc R U . . .
C5 C -0.0888(8) 0.1023(10) 0.0152(8) 0.061(4) Uani 1 1 d . . . . .
H5A H -0.0983 0.0489 0.0016 0.092 Uiso 1 1 calc R U . . .
H5B H -0.0870 0.1309 -0.0298 0.092 Uiso 1 1 calc R U . . .
H5C H -0.1312 0.1217 0.0329 0.092 Uiso 1 1 calc R U . . .
C6 C 0.0317(7) 0.0530(7) 0.1078(8) 0.045(3) Uani 1 1 d . . . . .
H6 H 0.0125 0.0042 0.0902 0.054 Uiso 1 1 calc R U . . .
C7 C 0.6035(7) -0.1453(9) 0.3501(8) 0.058(4) Uani 1 1 d . . . . .
H7A H 0.6278 -0.1200 0.3993 0.086 Uiso 1 1 calc R U . . .
H7B H 0.6251 -0.1247 0.3116 0.086 Uiso 1 1 calc R U . . .
H7C H 0.6144 -0.1995 0.3559 0.086 Uiso 1 1 calc R U . . .
C8 C 0.5162(7) -0.1326(7) 0.3247(7) 0.043(3) Uani 1 1 d . . . . .
C9 C 0.4542(7) -0.1862(7) 0.3104(7) 0.048(3) Uani 1 1 d . . . . .
H9 H 0.4594 -0.2393 0.3160 0.058 Uiso 1 1 calc R U . . .
C10 C 0.3837(7) -0.1451(7) 0.2864(7) 0.041(3) Uani 1 1 d . . . . .
C11 C 0.3048(8) -0.1790(7) 0.2659(9) 0.057(3) Uani 1 1 d . . . . .
H11A H 0.2814 -0.1798 0.2100 0.086 Uiso 1 1 calc R U . . .
H11B H 0.2717 -0.1490 0.2882 0.086 Uiso 1 1 calc R U . . .
H11C H 0.3088 -0.2306 0.2857 0.086 Uiso 1 1 calc R U . . .
C12 C 0.6132(8) 0.0699(10) 0.4952(8) 0.061(4) Uani 1 1 d . . . . .
H12A H 0.6238 0.0770 0.5504 0.092 Uiso 1 1 calc R U . . .
H12B H 0.6471 0.1034 0.4773 0.092 Uiso 1 1 calc R U . . .
H12C H 0.6238 0.0174 0.4851 0.092 Uiso 1 1 calc R U . . .
C13 C 0.5282(7) 0.0882(7) 0.4534(7) 0.044(3) Uani 1 1 d . . . . .
C14 C 0.4754(7) 0.1284(7) 0.4757(7) 0.049(3) Uani 1 1 d . . . . .
H14 H 0.4859 0.1538 0.5233 0.058 Uiso 1 1 calc R U . . .
C15 C 0.4026(7) 0.1267(7) 0.4173(7) 0.043(3) Uani 1 1 d . . . . .
C16 C 0.3299(8) 0.1684(9) 0.4182(8) 0.056(3) Uani 1 1 d . . . . .
H16A H 0.2862 0.1327 0.4094 0.084 Uiso 1 1 calc R U . . .
H16B H 0.3166 0.2067 0.3777 0.084 Uiso 1 1 calc R U . . .
H16C H 0.3394 0.1928 0.4681 0.084 Uiso 1 1 calc R U . . .
C17 C 0.6420(8) 0.0879(10) 0.2550(9) 0.066(4) Uani 1 1 d . . . . .
H17A H 0.6601 0.0383 0.2772 0.098 Uiso 1 1 calc R U . . .
H17B H 0.6556 0.1261 0.2955 0.098 Uiso 1 1 calc R U . . .
H17C H 0.6674 0.1003 0.2165 0.098 Uiso 1 1 calc R U . . .
C18 C 0.5564(7) 0.0862(7) 0.2185(8) 0.048(3) Uani 1 1 d . . . . .
C19 C 0.5112(7) 0.1119(7) 0.1452(7) 0.044(3) Uani 1 1 d . . . . .
H19 H 0.5309 0.1345 0.1082 0.053 Uiso 1 1 calc R U . . .
C20 C 0.4322(7) 0.0983(6) 0.1369(6) 0.038(2) Uani 1 1 d . . . . .
C21 C 0.3647(8) 0.1184(8) 0.0658(7) 0.054(3) Uani 1 1 d . . . . .
H21A H 0.3325 0.1579 0.0783 0.081 Uiso 1 1 calc R U . . .
H21B H 0.3324 0.0736 0.0472 0.081 Uiso 1 1 calc R U . . .
H21C H 0.3856 0.1368 0.0259 0.081 Uiso 1 1 calc R U . . .
B1 B 0.5228(8) 0.0155(8) 0.3294(8) 0.043(3) Uani 1 1 d D . . . .
H1 H 0.5908(18) 0.017(8) 0.358(7) 0.064 Uiso 1 1 d D U . . .
N11 N 0.8133(11) 0.6524(9) 0.7679(9) 0.104(6) Uani 1 1 d . . . . .
H11D H 0.8098 0.6213 0.7298 0.124 Uiso 1 1 calc R U . . .
H11E H 0.8161 0.7013 0.7613 0.124 Uiso 1 1 calc R U . . .
C22 C 0.8145(8) 0.6237(8) 0.8403(8) 0.055(3) Uani 1 1 d . . . . .
C23 C 0.8101(9) 0.5465(8) 0.8516(11) 0.067(4) Uani 1 1 d . . . . .
H23 H 0.8073 0.5125 0.8110 0.080 Uiso 1 1 calc R U . . .
C24 C 0.8098(10) 0.5199(9) 0.9203(11) 0.071(4) Uani 1 1 d . . . . .
H24 H 0.8096 0.4669 0.9276 0.085 Uiso 1 1 calc R U . . .
C25 C 0.8097(10) 0.5675(10) 0.9817(10) 0.071(4) Uani 1 1 d . . . . .
H25 H 0.8062 0.5478 1.0285 0.085 Uiso 1 1 calc R U . . .
C26 C 0.8149(9) 0.6445(9) 0.9703(9) 0.066(4) Uani 1 1 d . . . . .
H26 H 0.8173 0.6784 1.0109 0.079 Uiso 1 1 calc R U . . .
C27 C 0.8165(8) 0.6723(8) 0.9010(8) 0.053(3) Uani 1 1 d . . . . .
H27 H 0.8190 0.7252 0.8942 0.064 Uiso 1 1 calc R U . . .
N12 N 0.6471(14) 0.6084(12) 0.6486(11) 0.149(6) Uani 1 1 d D U . . .
H12D H 0.6845 0.6388 0.6752 0.179 Uiso 1 1 calc R U . . .
H12E H 0.6592 0.5641 0.6340 0.179 Uiso 1 1 calc R U . . .
C28 C 0.5709(9) 0.6297(9) 0.6300(9) 0.149(6) Uani 1 1 d G U . . .
C29 C 0.5511(10) 0.7004(8) 0.6531(8) 0.119(6) Uani 1 1 d DG U . . .
H29 H 0.5911 0.7327 0.6834 0.143 Uiso 1 1 calc R U . . .
C30 C 0.4722(12) 0.7233(10) 0.6312(10) 0.144(7) Uani 1 1 d G U . . .
H30 H 0.4589 0.7711 0.6468 0.173 Uiso 1 1 calc R U . . .
C31 C 0.4130(9) 0.6756(14) 0.5863(11) 0.154(9) Uani 1 1 d G U . . .
H31 H 0.3597 0.6911 0.5716 0.184 Uiso 1 1 calc R U . . .
C32 C 0.4328(10) 0.6049(12) 0.5633(9) 0.163(9) Uani 1 1 d G U . . .
H32 H 0.3927 0.5726 0.5329 0.195 Uiso 1 1 calc R U . . .
C33 C 0.5117(12) 0.5820(9) 0.5851(9) 0.147(7) Uani 1 1 d DG U . . .
H33 H 0.5250 0.5342 0.5695 0.177 Uiso 1 1 calc R U . . .
N13 N 0.0167(14) 0.6600(15) 0.0739(14) 0.153(6) Uani 1 1 d . U . . .
H13A H 0.0295 0.6894 0.1144 0.184 Uiso 1 1 calc R U . . .
H13B H -0.0288 0.6365 0.0599 0.184 Uiso 1 1 calc R U . . .
C34 C 0.0663(10) 0.6508(11) 0.0337(12) 0.153(6) Uani 1 1 d G U . . .
C35 C 0.1348(12) 0.6933(9) 0.0663(9) 0.117(6) Uani 1 1 d G U . . .
H35 H 0.1445 0.7156 0.1154 0.141 Uiso 1 1 calc R U . . .
C36 C 0.1891(9) 0.7027(8) 0.0263(12) 0.137(7) Uani 1 1 d G U . . .
H36 H 0.2354 0.7315 0.0484 0.165 Uiso 1 1 calc R U . . .
C37 C 0.1748(12) 0.6698(10) -0.0462(12) 0.142(8) Uani 1 1 d G U . . .
H37 H 0.2115 0.6762 -0.0732 0.170 Uiso 1 1 calc R U . . .
C38 C 0.1062(14) 0.6273(9) -0.0788(9) 0.148(8) Uani 1 1 d G U . . .
H38 H 0.0966 0.6050 -0.1278 0.177 Uiso 1 1 calc R U . . .
C39 C 0.0520(10) 0.6179(9) -0.0388(12) 0.133(6) Uani 1 1 d G U . . .
H39 H 0.0056 0.5891 -0.0608 0.159 Uiso 1 1 calc R U . . .
N14 N 0.999(2) 0.022(2) 0.274(2) 0.128(12) Uani 0.47(2) 1 d D U P A 1
H14A H 1.0291 0.0512 0.3095 0.154 Uiso 0.47(2) 1 calc R U P A 1
H14B H 1.0140 -0.0243 0.2679 0.154 Uiso 0.47(2) 1 calc R U P A 1
C40 C 0.9208(17) 0.0511(16) 0.2213(18) 0.107(8) Uani 0.47(2) 1 d DG U P A 1
C41 C 0.8968(19) 0.1249(16) 0.230(2) 0.108(8) Uani 0.47(2) 1 d DG U P A 1
H41 H 0.9311 0.1577 0.2667 0.129 Uiso 0.47(2) 1 calc R U P A 1
C42 C 0.822(2) 0.1502(17) 0.186(2) 0.107(9) Uani 0.47(2) 1 d G U P A 1
H42 H 0.8060 0.2001 0.1919 0.129 Uiso 0.47(2) 1 calc R U P A 1
C43 C 0.7716(18) 0.102(2) 0.132(2) 0.114(8) Uani 0.47(2) 1 d G U P A 1
H43 H 0.7211 0.1188 0.1019 0.137 Uiso 0.47(2) 1 calc R U P A 1
C44 C 0.796(2) 0.028(2) 0.123(2) 0.114(9) Uani 0.47(2) 1 d G U P A 1
H44 H 0.7613 -0.0049 0.0867 0.137 Uiso 0.47(2) 1 calc R U P A 1
C45 C 0.870(2) 0.0026(16) 0.168(2) 0.106(8) Uani 0.47(2) 1 d DG U P A 1
H45 H 0.8864 -0.0473 0.1615 0.127 Uiso 0.47(2) 1 calc R U P A 1
N14A N 0.925(2) -0.0364(19) 0.199(2) 0.140(12) Uani 0.53(2) 1 d D U P A 2
H14C H 0.9712 -0.0289 0.2330 0.169 Uiso 0.53(2) 1 calc R U P A 2
H14D H 0.9122 -0.0809 0.1781 0.169 Uiso 0.53(2) 1 calc R U P A 2
C40A C 0.8655(17) 0.0276(14) 0.1784(18) 0.103(7) Uani 0.53(2) 1 d DG U P A 2
C41A C 0.8854(16) 0.0987(16) 0.2125(17) 0.100(7) Uani 0.53(2) 1 d DG U P A 2
H41A H 0.9336 0.1054 0.2526 0.120 Uiso 0.53(2) 1 calc R U P A 2
C42A C 0.834(2) 0.1599(14) 0.187(2) 0.110(8) Uani 0.53(2) 1 d G U P A 2
H42A H 0.8475 0.2080 0.2105 0.132 Uiso 0.53(2) 1 calc R U P A 2
C43A C 0.7628(18) 0.1500(16) 0.1281(19) 0.110(8) Uani 0.53(2) 1 d G U P A 2
H43A H 0.7280 0.1914 0.1111 0.132 Uiso 0.53(2) 1 calc R U P A 2
C44A C 0.7429(15) 0.0788(19) 0.0940(16) 0.111(8) Uani 0.53(2) 1 d G U P A 2
H44A H 0.6947 0.0721 0.0539 0.133 Uiso 0.53(2) 1 calc R U P A 2
C45A C 0.7942(18) 0.0176(15) 0.1191(19) 0.109(8) Uani 0.53(2) 1 d DG U P A 2
H45A H 0.7808 -0.0305 0.0960 0.131 Uiso 0.53(2) 1 calc R U P 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 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 N8 2.273(9) . ?
W1 N6 2.276(8) . ?
W1 N10 2.297(9) . ?
W1 S3 2.306(3) . ?
W1 S1 2.306(3) . ?
W1 S2 2.313(3) . ?
W1 Cu3 2.6607(15) . ?
W1 Cu2 2.6637(16) . ?
W1 Cu1 2.6698(15) . ?
Cu1 C1 1.904(11) . ?
Cu1 S1 2.222(3) . ?
Cu1 S2 2.232(3) . ?
Cu1 O1 2.391(9) . ?
Cu1 Cu3 2.961(2) . ?
Cu1 Cu2 2.990(2) . ?
Cu2 C2 1.892(11) . ?
Cu2 S3 2.222(3) . ?
Cu2 S2 2.226(3) . ?
Cu2 Cu3 2.974(2) . ?
Cu3 C3 1.914(10) 2 ?
Cu3 S1 2.225(3) . ?
Cu3 S3 2.227(3) . ?
Cu4 N3 1.917(12) . ?
Cu4 N1 1.925(12) . ?
Cu4 N2 1.983(13) 3 ?
O1 C6 1.242(15) . ?
N1 C1 1.127(14) . ?
N2 C2 1.132(15) . ?
N2 Cu4 1.983(13) 3 ?
N3 C3 1.109(14) . ?
N4 C6 1.293(16) . ?
N4 C5 1.462(16) . ?
N4 C4 1.468(18) . ?
N5 C8 1.356(14) . ?
N5 N6 1.363(12) . ?
N5 B1 1.552(17) . ?
N6 C10 1.370(14) . ?
N7 N8 1.367(12) . ?
N7 C13 1.381(14) . ?
N7 B1 1.484(17) . ?
N8 C15 1.385(15) . ?
N9 C18 1.330(14) . ?
N9 N10 1.374(13) . ?
N9 B1 1.563(17) . ?
N10 C20 1.362(14) . ?
C3 Cu3 1.914(10) 2_545 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6 0.9400 . ?
C7 C8 1.488(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 C9 1.408(17) . ?
C9 C10 1.389(17) . ?
C9 H9 0.9400 . ?
C10 C11 1.459(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 C13 1.495(17) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 C14 1.335(18) . ?
C14 C15 1.390(16) . ?
C14 H14 0.9400 . ?
C15 C16 1.490(18) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 C18 1.454(18) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 C19 1.398(18) . ?
C19 C20 1.383(16) . ?
C19 H19 0.9400 . ?
C20 C21 1.502(17) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
B1 H1 1.15(2) . ?
N11 C22 1.40(2) . ?
N11 H11D 0.8700 . ?
N11 H11E 0.8700 . ?
C22 C23 1.38(2) . ?
C22 C27 1.388(19) . ?
C23 C24 1.34(2) . ?
C23 H23 0.9400 . ?
C24 C25 1.39(2) . ?
C24 H24 0.9400 . ?
C25 C26 1.37(2) . ?
C25 H25 0.9400 . ?
C26 C27 1.36(2) . ?
C26 H26 0.9400 . ?
C27 H27 0.9400 . ?
N12 C28 1.34(3) . ?
N12 H12D 0.8700 . ?
N12 H12E 0.8700 . ?
C28 C29 1.3900 . ?
C28 C33 1.3900 . ?
C29 C30 1.3900 . ?
C29 H29 0.9400 . ?
C30 C31 1.3900 . ?
C30 H30 0.9400 . ?
C31 C32 1.3900 . ?
C31 H31 0.9400 . ?
C32 C33 1.3900 . ?
C32 H32 0.9400 . ?
C33 H33 0.9400 . ?
N13 C34 1.32(2) . ?
N13 H13A 0.8700 . ?
N13 H13B 0.8700 . ?
C34 C35 1.3900 . ?
C34 C39 1.3900 . ?
C35 C36 1.3900 . ?
C35 H35 0.9400 . ?
C36 C37 1.3900 . ?
C36 H36 0.9400 . ?
C37 C38 1.3900 . ?
C37 H37 0.9400 . ?
C38 C39 1.3900 . ?
C38 H38 0.9400 . ?
C39 H39 0.9400 . ?
N14 C40 1.50(3) . ?
N14 H14A 0.8700 . ?
N14 H14B 0.8700 . ?
C40 C41 1.3900 . ?
C40 C45 1.3900 . ?
C41 C42 1.3900 . ?
C41 H41 0.9400 . ?
C42 C43 1.3900 . ?
C42 H42 0.9400 . ?
C43 C44 1.3900 . ?
C43 H43 0.9400 . ?
C44 C45 1.3900 . ?
C44 H44 0.9400 . ?
C45 H45 0.9400 . ?
N14A C40A 1.50(3) . ?
N14A H14C 0.8700 . ?
N14A H14D 0.8700 . ?
C40A C41A 1.3900 . ?
C40A C45A 1.3900 . ?
C41A C42A 1.3900 . ?
C41A H41A 0.9400 . ?
C42A C43A 1.3900 . ?
C42A H42A 0.9400 . ?
C43A C44A 1.3900 . ?
C43A H43A 0.9400 . ?
C44A C45A 1.3900 . ?
C44A H44A 0.9400 . ?
C45A H45A 0.9400 . ?

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
N8 W1 N6 79.8(3) . . ?
N8 W1 N10 80.0(3) . . ?
N6 W1 N10 80.1(3) . . ?
N8 W1 S3 87.1(2) . . ?
N6 W1 S3 161.2(2) . . ?
N10 W1 S3 84.4(2) . . ?
N8 W1 S1 85.3(2) . . ?
N6 W1 S1 88.0(2) . . ?
N10 W1 S1 162.4(2) . . ?
S3 W1 S1 104.44(10) . . ?
N8 W1 S2 162.5(2) . . ?
N6 W1 S2 85.7(2) . . ?
N10 W1 S2 87.9(2) . . ?
S3 W1 S2 104.33(10) . . ?
S1 W1 S2 104.20(10) . . ?
N8 W1 Cu3 91.9(2) . . ?
N6 W1 Cu3 140.5(2) . . ?
N10 W1 Cu3 136.8(2) . . ?
S3 W1 Cu3 52.69(8) . . ?
S1 W1 Cu3 52.65(8) . . ?
S2 W1 Cu3 105.56(8) . . ?
N8 W1 Cu2 139.5(2) . . ?
N6 W1 Cu2 137.8(2) . . ?
N10 W1 Cu2 91.2(2) . . ?
S3 W1 Cu2 52.52(7) . . ?
S1 W1 Cu2 106.30(8) . . ?
S2 W1 Cu2 52.57(8) . . ?
Cu3 W1 Cu2 67.92(5) . . ?
N8 W1 Cu1 137.4(2) . . ?
N6 W1 Cu1 92.9(2) . . ?
N10 W1 Cu1 140.4(2) . . ?
S3 W1 Cu1 105.88(8) . . ?
S1 W1 Cu1 52.42(8) . . ?
S2 W1 Cu1 52.64(8) . . ?
Cu3 W1 Cu1 67.49(5) . . ?
Cu2 W1 Cu1 68.21(5) . . ?
C1 Cu1 S1 121.5(3) . . ?
C1 Cu1 S2 124.1(3) . . ?
S1 Cu1 S2 109.83(11) . . ?
C1 Cu1 O1 92.4(4) . . ?
S1 Cu1 O1 99.2(2) . . ?
S2 Cu1 O1 100.2(2) . . ?
C1 Cu1 W1 169.3(3) . . ?
S1 Cu1 W1 55.34(8) . . ?
S2 Cu1 W1 55.44(8) . . ?
O1 Cu1 W1 98.3(2) . . ?
C1 Cu1 Cu3 131.2(4) . . ?
S1 Cu1 Cu3 48.31(8) . . ?
S2 Cu1 Cu3 98.61(9) . . ?
O1 Cu1 Cu3 54.4(2) . . ?
W1 Cu1 Cu3 56.11(4) . . ?
C1 Cu1 Cu2 133.3(3) . . ?
S1 Cu1 Cu2 98.57(9) . . ?
S2 Cu1 Cu2 47.79(8) . . ?
O1 Cu1 Cu2 55.7(2) . . ?
W1 Cu1 Cu2 55.80(4) . . ?
Cu3 Cu1 Cu2 59.97(5) . . ?
C2 Cu2 S3 122.1(4) . . ?
C2 Cu2 S2 125.2(4) . . ?
S3 Cu2 S2 110.18(11) . . ?
C2 Cu2 W1 173.5(4) . . ?
S3 Cu2 W1 55.43(8) . . ?
S2 Cu2 W1 55.59(7) . . ?
C2 Cu2 Cu3 127.9(4) . . ?
S3 Cu2 Cu3 48.11(9) . . ?
S2 Cu2 Cu3 98.37(9) . . ?
W1 Cu2 Cu3 55.99(4) . . ?
C2 Cu2 Cu1 130.0(4) . . ?
S3 Cu2 Cu1 98.37(9) . . ?
S2 Cu2 Cu1 47.97(8) . . ?
W1 Cu2 Cu1 55.99(4) . . ?
Cu3 Cu2 Cu1 59.52(5) . . ?
C3 Cu3 S1 124.2(4) 2 . ?
C3 Cu3 S3 120.8(4) 2 . ?
S1 Cu3 S3 109.91(11) . . ?
C3 Cu3 W1 168.3(4) 2 . ?
S1 Cu3 W1 55.46(8) . . ?
S3 Cu3 W1 55.44(8) . . ?
C3 Cu3 Cu1 133.7(4) 2 . ?
S1 Cu3 Cu1 48.20(8) . . ?
S3 Cu3 Cu1 99.11(9) . . ?
W1 Cu3 Cu1 56.40(4) . . ?
C3 Cu3 Cu2 131.5(4) 2 . ?
S1 Cu3 Cu2 98.95(9) . . ?
S3 Cu3 Cu2 47.97(8) . . ?
W1 Cu3 Cu2 56.09(4) . . ?
Cu1 Cu3 Cu2 60.51(5) . . ?
N3 Cu4 N1 131.6(5) . . ?
N3 Cu4 N2 116.4(5) . 3 ?
N1 Cu4 N2 111.2(5) . 3 ?
Cu1 S1 Cu3 83.49(11) . . ?
Cu1 S1 W1 72.24(9) . . ?
Cu3 S1 W1 71.89(9) . . ?
Cu2 S2 Cu1 84.25(11) . . ?
Cu2 S2 W1 71.84(9) . . ?
Cu1 S2 W1 71.92(9) . . ?
Cu2 S3 Cu3 83.92(11) . . ?
Cu2 S3 W1 72.05(9) . . ?
Cu3 S3 W1 71.87(9) . . ?
C6 O1 Cu1 127.3(8) . . ?
C1 N1 Cu4 170.5(10) . . ?
C2 N2 Cu4 177.1(13) . 3 ?
C3 N3 Cu4 172.0(12) . . ?
C6 N4 C5 123.2(12) . . ?
C6 N4 C4 121.5(11) . . ?
C5 N4 C4 115.3(11) . . ?
C8 N5 N6 111.6(9) . . ?
C8 N5 B1 126.9(10) . . ?
N6 N5 B1 121.0(9) . . ?
N5 N6 C10 106.1(8) . . ?
N5 N6 W1 120.5(6) . . ?
C10 N6 W1 132.8(7) . . ?
N8 N7 C13 110.2(9) . . ?
N8 N7 B1 122.0(9) . . ?
C13 N7 B1 127.3(10) . . ?
N7 N8 C15 105.7(8) . . ?
N7 N8 W1 120.6(7) . . ?
C15 N8 W1 133.1(7) . . ?
C18 N9 N10 112.5(10) . . ?
C18 N9 B1 127.5(10) . . ?
N10 N9 B1 119.9(9) . . ?
C20 N10 N9 105.4(8) . . ?
C20 N10 W1 133.3(8) . . ?
N9 N10 W1 120.8(7) . . ?
N1 C1 Cu1 172.1(11) . . ?
N2 C2 Cu2 177.4(13) . . ?
N3 C3 Cu3 174.9(12) . 2_545 ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 C6 N4 125.9(12) . . ?
O1 C6 H6 117.0 . . ?
N4 C6 H6 117.0 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 C9 106.2(10) . . ?
N5 C8 C7 124.4(12) . . ?
C9 C8 C7 129.3(11) . . ?
C10 C9 C8 106.6(11) . . ?
C10 C9 H9 126.7 . . ?
C8 C9 H9 126.7 . . ?
N6 C10 C9 109.4(10) . . ?
N6 C10 C11 126.0(10) . . ?
C9 C10 C11 124.5(11) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N7 106.9(10) . . ?
C14 C13 C12 130.6(12) . . ?
N7 C13 C12 122.3(12) . . ?
C13 C14 C15 109.1(12) . . ?
C13 C14 H14 125.4 . . ?
C15 C14 H14 125.4 . . ?
N8 C15 C14 107.9(11) . . ?
N8 C15 C16 126.5(10) . . ?
C14 C15 C16 125.5(12) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N9 C18 C19 105.6(10) . . ?
N9 C18 C17 125.3(12) . . ?
C19 C18 C17 129.1(11) . . ?
C20 C19 C18 107.8(10) . . ?
C20 C19 H19 126.1 . . ?
C18 C19 H19 126.1 . . ?
N10 C20 C19 108.8(10) . . ?
N10 C20 C21 127.2(11) . . ?
C19 C20 C21 124.0(10) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N7 B1 N5 108.9(10) . . ?
N7 B1 N9 109.4(10) . . ?
N5 B1 N9 106.6(10) . . ?
N7 B1 H1 107(7) . . ?
N5 B1 H1 118(7) . . ?
N9 B1 H1 107(7) . . ?
C22 N11 H11D 120.0 . . ?
C22 N11 H11E 120.0 . . ?
H11D N11 H11E 120.0 . . ?
C23 C22 C27 118.3(14) . . ?
C23 C22 N11 120.5(15) . . ?
C27 C22 N11 121.1(14) . . ?
C24 C23 C22 120.0(16) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 122.8(15) . . ?
C23 C24 H24 118.6 . . ?
C25 C24 H24 118.6 . . ?
C26 C25 C24 116.8(16) . . ?
C26 C25 H25 121.6 . . ?
C24 C25 H25 121.6 . . ?
C27 C26 C25 120.9(15) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C22 121.1(14) . . ?
C26 C27 H27 119.5 . . ?
C22 C27 H27 119.5 . . ?
C28 N12 H12D 120.0 . . ?
C28 N12 H12E 120.0 . . ?
H12D N12 H12E 120.0 . . ?
N12 C28 C29 120.3(4) . . ?
N12 C28 C33 119.6(4) . . ?
C29 C28 C33 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C28 120.0 . . ?
C32 C33 H33 120.0 . . ?
C28 C33 H33 120.0 . . ?
C34 N13 H13A 120.0 . . ?
C34 N13 H13B 120.0 . . ?
H13A N13 H13B 120.0 . . ?
N13 C34 C35 110(2) . . ?
N13 C34 C39 129(2) . . ?
C35 C34 C39 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 120.0 . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C39 C38 C37 120.0 . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C34 120.0 . . ?
C38 C39 H39 120.0 . . ?
C34 C39 H39 120.0 . . ?
C40 N14 H14A 120.0 . . ?
C40 N14 H14B 120.0 . . ?
H14A N14 H14B 120.0 . . ?
C41 C40 C45 120.0 . . ?
C41 C40 N14 119.9(4) . . ?
C45 C40 N14 119.9(4) . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C45 120.0 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C40 120.0 . . ?
C44 C45 H45 120.0 . . ?
C40 C45 H45 120.0 . . ?
C40A N14A H14C 120.0 . . ?
C40A N14A H14D 120.0 . . ?
H14C N14A H14D 120.0 . . ?
C41A C40A C45A 120.0 . . ?
C41A C40A N14A 120.0(4) . . ?
C45A C40A N14A 119.7(4) . . ?
C40A C41A C42A 120.0 . . ?
C40A C41A H41A 120.0 . . ?
C42A C41A H41A 120.0 . . ?
C43A C42A C41A 120.0 . . ?
C43A C42A H42A 120.0 . . ?
C41A C42A H42A 120.0 . . ?
C42A C43A C44A 120.0 . . ?
C42A C43A H43A 120.0 . . ?
C44A C43A H43A 120.0 . . ?
C45A C44A C43A 120.0 . . ?
C45A C44A H44A 120.0 . . ?
C43A C44A H44A 120.0 . . ?
C44A C45A C40A 120.0 . . ?
C44A C45A H45A 120.0 . . ?
C40A C45A H45A 120.0 . . ?

_refine_diff_density_max         3.875
_refine_diff_density_min         -2.163
_refine_diff_density_rms         0.214

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 992893'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_update_record             
;
2014-09-28 # Formatted by publCIF

;
_publcif_datablock.id            {799b7e00-cb44-49ac-982b-6547c8957cde}

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H58 B2 Cu8 N20 O2 S6 W2, 2(C3 H7 N O)'
_chemical_formula_sum            'C48 H72 B2 Cu8 N22 O4 S6 W2'
_chemical_formula_weight         2111.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   13.350(3)
_cell_length_b                   13.418(3)
_cell_length_c                   13.621(3)
_cell_angle_alpha                60.97(3)
_cell_angle_beta                 83.08(3)
_cell_angle_gamma                80.95(3)
_cell_volume                     2104.0(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    223(2)
_cell_measurement_theta_min      3.0154
_cell_measurement_theta_max      27.4932

_exptl_crystal_description       Platelet
_exptl_crystal_colour            black
_exptl_crystal_density_meas      1.666
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.896
_shelx_estimated_absorpt_T_min   0.527
_shelx_estimated_absorpt_T_max   0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'

_exptl_special_details           ?

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17388
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.015
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7673
_reflns_number_gt                6191
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0938P)²+17.8045P]
 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7673
_refine_ls_number_parameters     423
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_ref         0.1862
_refine_ls_wR_factor_gt          0.1689
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.002
_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 0.76603(3) 0.65885(4) 0.72882(3) 0.02769(17) Uani 1 1 d . . . . .
Cu1 Cu 0.68123(12) 0.73390(13) 0.53471(12) 0.0407(4) Uani 1 1 d . . . . .
Cu2 Cu 0.67004(12) 0.50009(12) 0.72648(13) 0.0411(4) Uani 1 1 d . . . . .
Cu3 Cu 0.86893(12) 0.57298(13) 0.60164(12) 0.0424(4) Uani 1 1 d . . . . .
Cu4 Cu 0.49169(12) 0.16468(13) 0.80744(12) 0.0409(4) Uani 1 1 d . . . . .
S1 S 0.8387(2) 0.7579(3) 0.5506(2) 0.0351(7) Uani 1 1 d . . . . .
S2 S 0.5963(2) 0.6703(3) 0.7007(2) 0.0354(7) Uani 1 1 d . . . . .
S3 S 0.8262(2) 0.4696(2) 0.7833(2) 0.0364(7) Uani 1 1 d . . . . .
N1 N 0.5768(9) 0.8177(9) 0.3183(9) 0.049(3) Uani 1 1 d . . . . .
N2 N 0.5575(9) 0.3022(10) 0.7677(9) 0.051(3) Uani 1 1 d . . . . .
N4 N 0.4963(10) 0.0382(10) 0.9555(9) 0.048(3) Uani 0.5 1 d . . P A 1
C4 C 0.4963(10) 0.0382(10) 0.9555(9) 0.048(3) Uani 0.5 1 d . . P A 2
N5 N 0.7567(7) 0.8505(8) 0.8068(8) 0.032(2) Uani 1 1 d . . . . .
N6 N 0.7286(7) 0.8332(8) 0.7223(8) 0.032(2) Uani 1 1 d . . . . .
N7 N 0.9090(7) 0.7071(8) 0.8712(8) 0.032(2) Uani 1 1 d . . . . .
N8 N 0.9124(7) 0.6655(8) 0.7958(8) 0.035(2) Uani 1 1 d . . . . .
N9 N 0.7389(7) 0.6582(8) 0.9676(8) 0.034(2) Uani 1 1 d . . . . .
N10 N 0.7176(7) 0.6005(8) 0.9134(7) 0.036(2) Uani 1 1 d . . . . .
C1 C 0.6176(10) 0.7944(10) 0.3980(9) 0.038(3) Uani 1 1 d . . . . .
C2 C 0.5992(9) 0.3786(11) 0.7508(10) 0.038(3) Uani 1 1 d . . . . .
C3 C 0.9689(9) 0.5162(10) 0.5243(10) 0.046(3) Uani 0.5 1 d . . P B 1
N3 N 0.9689(9) 0.5162(10) 0.5243(10) 0.046(3) Uani 0.5 1 d . . P B 2
C5 C 0.7495(12) 1.0073(11) 0.8585(12) 0.055(4) Uani 1 1 d . . . . .
H5A H 0.7057 0.9765 0.9263 0.082 Uiso 1 1 calc R U . . .
H5B H 0.7352 1.0902 0.8188 0.082 Uiso 1 1 calc R U . . .
H5C H 0.8199 0.9863 0.8785 0.082 Uiso 1 1 calc R U . . .
C6 C 0.7306(9) 0.9593(10) 0.7849(10) 0.039(3) Uani 1 1 d . . . . .
C7 C 0.6826(9) 1.0166(10) 0.6839(10) 0.040(3) Uani 1 1 d . . . . .
H7 H 0.6554 1.0942 0.6477 0.049 Uiso 1 1 calc R U . . .
C8 C 0.6828(9) 0.9372(9) 0.6473(10) 0.035(3) Uani 1 1 d . . . . .
C9 C 0.6396(11) 0.9629(11) 0.5410(10) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.6926 0.9476 0.4931 0.074 Uiso 1 1 calc R U . . .
H9B H 0.6119 1.0430 0.5027 0.074 Uiso 1 1 calc R U . . .
H9C H 0.5861 0.9149 0.5578 0.074 Uiso 1 1 calc R U . . .
C10 C 1.0242(11) 0.7351(13) 0.9847(12) 0.058(4) Uani 1 1 d . . . . .
H10A H 0.9983 0.8154 0.9565 0.087 Uiso 1 1 calc R U . . .
H10B H 1.0970 0.7256 0.9913 0.087 Uiso 1 1 calc R U . . .
H10C H 0.9917 0.6900 1.0579 0.087 Uiso 1 1 calc R U . . .
C11 C 1.0017(10) 0.6955(11) 0.9054(11) 0.046(3) Uani 1 1 d . . . . .
C12 C 1.0685(10) 0.6490(12) 0.8491(12) 0.049(3) Uani 1 1 d . . . . .
H12 H 1.1393 0.6337 0.8547 0.059 Uiso 1 1 calc R U . . .
C13 C 1.0124(10) 0.6291(11) 0.7833(11) 0.047(3) Uani 1 1 d . . . . .
C14 C 1.0565(11) 0.5861(14) 0.7055(14) 0.063(4) Uani 1 1 d . . . . .
H14A H 1.0299 0.5150 0.7257 0.094 Uiso 1 1 calc R U . . .
H14B H 1.1298 0.5723 0.7098 0.094 Uiso 1 1 calc R U . . .
H14C H 1.0391 0.6424 0.6294 0.094 Uiso 1 1 calc R U . . .
C15 C 0.7153(12) 0.6539(14) 1.1537(11) 0.062(4) Uani 1 1 d . . . . .
H15A H 0.7849 0.6313 1.1767 0.093 Uiso 1 1 calc R U . . .
H15B H 0.6693 0.6218 1.2194 0.093 Uiso 1 1 calc R U . . .
H15C H 0.7019 0.7369 1.1160 0.093 Uiso 1 1 calc R U . . .
C16 C 0.7002(10) 0.6105(11) 1.0759(9) 0.042(3) Uani 1 1 d . . . . .
C17 C 0.6512(10) 0.5191(11) 1.0923(9) 0.045(3) Uani 1 1 d . . . . .
H17 H 0.6172 0.4692 1.1589 0.054 Uiso 1 1 calc R U . . .
C18 C 0.6624(9) 0.5163(10) 0.9911(9) 0.036(3) Uani 1 1 d . . . . .
C19 C 0.6216(11) 0.4287(12) 0.9735(11) 0.051(3) Uani 1 1 d . . . . .
H19A H 0.5733 0.4669 0.9147 0.077 Uiso 1 1 calc R U . . .
H19B H 0.5880 0.3762 1.0428 0.077 Uiso 1 1 calc R U . . .
H19C H 0.6771 0.3863 0.9515 0.077 Uiso 1 1 calc R U . . .
B1 B 0.8066(10) 0.7541(13) 0.9100(11) 0.036(3) Uani 1 1 d . . . . .
H1 H 0.832(8) 0.771(9) 0.968(9) 0.03(3) Uiso 1 1 d . . . . .
O2 O 0.7602(16) 0.1433(16) 0.0316(19) 0.065(3) Uani 0.5 1 d . . P . .
N12 N 0.642(2) 0.140(2) 0.154(2) 0.065(3) Uani 0.5 1 d . . P . .
C23 C 0.701(2) 0.167(2) 0.211(3) 0.065(3) Uani 0.5 1 d . . P . .
H23A H 0.6597 0.1743 0.2718 0.097 Uiso 0.5 1 calc R U P . .
H23B H 0.7278 0.2387 0.1607 0.097 Uiso 0.5 1 calc R U P . .
H23C H 0.7565 0.1065 0.2428 0.097 Uiso 0.5 1 calc R U P . .
C24 C 0.544(2) 0.141(2) 0.168(3) 0.065(3) Uani 0.5 1 d . . P . .
H24A H 0.5205 0.1513 0.2335 0.097 Uiso 0.5 1 calc R U P . .
H24B H 0.5246 0.0695 0.1794 0.097 Uiso 0.5 1 calc R U P . .
H24C H 0.5122 0.2043 0.1021 0.097 Uiso 0.5 1 calc R U P . .
C25 C 0.686(3) 0.128(2) 0.067(3) 0.065(3) Uani 0.5 1 d . . P . .
H25 H 0.6466 0.1020 0.0335 0.078 Uiso 0.5 1 calc R U P . .
O3 O 1.0471(14) 0.9719(16) 0.0332(16) 0.059(3) Uani 0.5 1 d D . P C -1
N13 N 0.9503(15) 0.8603(18) 0.1962(17) 0.059(3) Uani 0.5 1 d D . P C -1
C26 C 0.8563(18) 0.821(2) 0.238(3) 0.059(3) Uani 0.5 1 d D . P C -1
H26A H 0.8605 0.7642 0.3171 0.089 Uiso 0.5 1 calc R U P C -1
H26B H 0.8364 0.7865 0.1965 0.089 Uiso 0.5 1 calc R U P C -1
H26C H 0.8063 0.8847 0.2310 0.089 Uiso 0.5 1 calc R U P C -1
C27 C 1.0415(19) 0.790(2) 0.240(3) 0.059(3) Uani 0.5 1 d D . P C -1
H27A H 1.0286 0.7332 0.3175 0.089 Uiso 0.5 1 calc R U P C -1
H27B H 1.0915 0.8369 0.2369 0.089 Uiso 0.5 1 calc R U P C -1
H27C H 1.0671 0.7515 0.1959 0.089 Uiso 0.5 1 calc R U P C -1
C28 C 0.9675(19) 0.941(2) 0.0879(19) 0.059(3) Uani 0.5 1 d D . P C -1
H28 H 0.9085 0.9804 0.0484 0.071 Uiso 0.5 1 calc R U P C -1
O1 O 0.7233(7) 0.5488(8) 0.5195(8) 0.052(2) Uani 1 1 d . . . D -1
N11 N 0.6839(9) 0.4134(9) 0.4809(9) 0.045(3) Uani 1 1 d . . . D -1
C20 C 0.7671(13) 0.3286(12) 0.5493(14) 0.066(4) Uani 1 1 d . . . D -1
H20A H 0.8172 0.3687 0.5577 0.099 Uiso 1 1 calc R U . D -1
H20B H 0.7989 0.2851 0.5119 0.099 Uiso 1 1 calc R U . D -1
H20C H 0.7393 0.2769 0.6229 0.099 Uiso 1 1 calc R U . D -1
C21 C 0.6159(14) 0.3753(15) 0.4353(14) 0.072(5) Uani 1 1 d . . . D -1
H21A H 0.6414 0.2989 0.4468 0.108 Uiso 1 1 calc R U . D -1
H21B H 0.6111 0.4275 0.3554 0.108 Uiso 1 1 calc R U . D -1
H21C H 0.5491 0.3740 0.4728 0.108 Uiso 1 1 calc R U . D -1
C22 C 0.6696(11) 0.5120(12) 0.4771(10) 0.049(3) Uani 1 1 d . . . D -1
H22 H 0.6132 0.5618 0.4388 0.059 Uiso 1 1 calc R U . D -1


_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 N6 2.274(9) . ?
W1 N10 2.282(9) . ?
W1 N8 2.285(9) . ?
W1 S1 2.304(3) . ?
W1 S3 2.305(3) . ?
W1 S2 2.312(3) . ?
W1 Cu1 2.6579(17) . ?
W1 Cu3 2.6610(17) . ?
W1 Cu2 2.6676(16) . ?
Cu1 C1 1.883(12) . ?
Cu1 S2 2.223(3) . ?
Cu1 S1 2.228(3) . ?
Cu1 Cu3 2.951(2) . ?
Cu1 Cu2 2.964(2) . ?
Cu2 C2 1.884(13) . ?
Cu2 S2 2.215(3) . ?
Cu2 S3 2.219(3) . ?
Cu2 Cu3 3.002(2) . ?
Cu3 C3 1.896(11) . ?
Cu3 S1 2.210(3) . ?
Cu3 S3 2.225(3) . ?
Cu4 N4 1.904(11) . ?
Cu4 N1 1.934(12) 2_666 ?
Cu4 N2 1.974(12) . ?
N1 C1 1.154(15) . ?
N1 Cu4 1.934(12) 2_666 ?
N2 C2 1.155(16) . ?
N4 N4 1.15(2) 2_657 ?
N5 C6 1.336(15) . ?
N5 N6 1.381(13) . ?
N5 B1 1.511(16) . ?
N6 C8 1.365(14) . ?
N7 C11 1.335(15) . ?
N7 N8 1.379(13) . ?
N7 B1 1.558(17) . ?
N8 C13 1.368(16) . ?
N9 C16 1.363(14) . ?
N9 N10 1.378(13) . ?
N9 B1 1.517(17) . ?
N10 C18 1.361(15) . ?
C3 C3 1.16(2) 2_766 ?
C5 C6 1.491(17) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 C7 1.387(17) . ?
C7 C8 1.378(17) . ?
C7 H7 0.9400 . ?
C8 C9 1.484(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.491(18) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 C12 1.376(19) . ?
C12 C13 1.376(18) . ?
C12 H12 0.9400 . ?
C13 C14 1.463(19) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 C16 1.480(18) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.390(18) . ?
C17 C18 1.388(16) . ?
C17 H17 0.9400 . ?
C18 C19 1.497(18) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
B1 H1 1.02(11) . ?
O2 C25 1.05(3) . ?
N12 C24 1.31(4) . ?
N12 C25 1.33(4) . ?
N12 C23 1.36(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25 0.9400 . ?
O3 C28 1.225(17) . ?
N13 C28 1.361(17) . ?
N13 C26 1.387(18) . ?
N13 C27 1.413(18) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 H28 0.9400 . ?
O1 C22 1.256(16) . ?
N11 C22 1.283(17) . ?
N11 C21 1.436(18) . ?
N11 C20 1.490(18) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22 0.9400 . ?

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
N6 W1 N10 80.7(3) . . ?
N6 W1 N8 80.9(3) . . ?
N10 W1 N8 79.0(3) . . ?
N6 W1 S1 85.5(2) . . ?
N10 W1 S1 161.9(3) . . ?
N8 W1 S1 87.4(3) . . ?
N6 W1 S3 163.0(2) . . ?
N10 W1 S3 86.7(3) . . ?
N8 W1 S3 85.4(2) . . ?
S1 W1 S3 104.12(11) . . ?
N6 W1 S2 86.9(3) . . ?
N10 W1 S2 86.5(3) . . ?
N8 W1 S2 162.3(3) . . ?
S1 W1 S2 104.41(11) . . ?
S3 W1 S2 103.92(11) . . ?
N6 W1 Cu1 92.0(2) . . ?
N10 W1 Cu1 138.9(2) . . ?
N8 W1 Cu1 140.1(3) . . ?
S1 W1 Cu1 52.77(8) . . ?
S3 W1 Cu1 104.99(9) . . ?
S2 W1 Cu1 52.57(9) . . ?
N6 W1 Cu3 137.5(2) . . ?
N10 W1 Cu3 139.1(2) . . ?
N8 W1 Cu3 91.7(2) . . ?
S1 W1 Cu3 52.25(9) . . ?
S3 W1 Cu3 52.63(9) . . ?
S2 W1 Cu3 105.93(9) . . ?
Cu1 W1 Cu3 67.41(5) . . ?
N6 W1 Cu2 138.9(2) . . ?
N10 W1 Cu2 91.7(3) . . ?
N8 W1 Cu2 137.4(2) . . ?
S1 W1 Cu2 106.36(9) . . ?
S3 W1 Cu2 52.39(9) . . ?
S2 W1 Cu2 52.24(8) . . ?
Cu1 W1 Cu2 67.64(6) . . ?
Cu3 W1 Cu2 68.58(5) . . ?
C1 Cu1 S2 123.1(4) . . ?
C1 Cu1 S1 124.9(4) . . ?
S2 Cu1 S1 110.10(12) . . ?
C1 Cu1 W1 176.7(4) . . ?
S2 Cu1 W1 55.70(8) . . ?
S1 Cu1 W1 55.42(8) . . ?
C1 Cu1 Cu3 126.6(4) . . ?
S2 Cu1 Cu3 99.45(10) . . ?
S1 Cu1 Cu3 48.05(9) . . ?
W1 Cu1 Cu3 56.35(5) . . ?
C1 Cu1 Cu2 125.7(4) . . ?
S2 Cu1 Cu2 47.99(9) . . ?
S1 Cu1 Cu2 99.31(10) . . ?
W1 Cu1 Cu2 56.33(5) . . ?
Cu3 Cu1 Cu2 60.99(6) . . ?
C2 Cu2 S2 124.3(4) . . ?
C2 Cu2 S3 121.8(4) . . ?
S2 Cu2 S3 110.20(12) . . ?
C2 Cu2 W1 170.5(4) . . ?
S2 Cu2 W1 55.60(8) . . ?
S3 Cu2 W1 55.38(9) . . ?
C2 Cu2 Cu1 132.2(4) . . ?
S2 Cu2 Cu1 48.19(9) . . ?
S3 Cu2 Cu1 98.03(10) . . ?
W1 Cu2 Cu1 56.02(5) . . ?
C2 Cu2 Cu3 130.8(4) . . ?
S2 Cu2 Cu3 98.15(10) . . ?
S3 Cu2 Cu3 47.58(9) . . ?
W1 Cu2 Cu3 55.60(5) . . ?
Cu1 Cu2 Cu3 59.29(6) . . ?
C3 Cu3 S1 121.7(4) . . ?
C3 Cu3 S3 122.6(4) . . ?
S1 Cu3 S3 110.12(12) . . ?
C3 Cu3 W1 166.6(4) . . ?
S1 Cu3 W1 55.53(9) . . ?
S3 Cu3 W1 55.45(8) . . ?
C3 Cu3 Cu1 133.8(4) . . ?
S1 Cu3 Cu1 48.57(9) . . ?
S3 Cu3 Cu1 98.27(10) . . ?
W1 Cu3 Cu1 56.25(5) . . ?
C3 Cu3 Cu2 134.6(4) . . ?
S1 Cu3 Cu2 98.63(10) . . ?
S3 Cu3 Cu2 47.42(9) . . ?
W1 Cu3 Cu2 55.81(5) . . ?
Cu1 Cu3 Cu2 59.72(6) . . ?
N4 Cu4 N1 127.8(5) . 2_666 ?
N4 Cu4 N2 120.8(5) . . ?
N1 Cu4 N2 111.4(4) 2_666 . ?
Cu3 S1 Cu1 83.39(12) . . ?
Cu3 S1 W1 72.22(10) . . ?
Cu1 S1 W1 71.81(10) . . ?
Cu2 S2 Cu1 83.82(12) . . ?
Cu2 S2 W1 72.16(10) . . ?
Cu1 S2 W1 71.73(10) . . ?
Cu2 S3 Cu3 85.01(12) . . ?
Cu2 S3 W1 72.23(10) . . ?
Cu3 S3 W1 71.92(10) . . ?
C1 N1 Cu4 172.5(10) . 2_666 ?
C2 N2 Cu4 175.6(11) . . ?
N4 N4 Cu4 177.0(17) 2_657 . ?
C6 N5 N6 110.9(9) . . ?
C6 N5 B1 127.0(10) . . ?
N6 N5 B1 122.1(9) . . ?
C8 N6 N5 105.0(9) . . ?
C8 N6 W1 134.5(8) . . ?
N5 N6 W1 120.5(7) . . ?
C11 N7 N8 110.5(10) . . ?
C11 N7 B1 128.1(10) . . ?
N8 N7 B1 121.3(9) . . ?
C13 N8 N7 105.7(9) . . ?
C13 N8 W1 133.7(8) . . ?
N7 N8 W1 120.5(7) . . ?
C16 N9 N10 111.4(10) . . ?
C16 N9 B1 127.8(10) . . ?
N10 N9 B1 120.5(9) . . ?
C18 N10 N9 104.8(9) . . ?
C18 N10 W1 133.6(8) . . ?
N9 N10 W1 121.5(7) . . ?
N1 C1 Cu1 171.5(11) . . ?
N2 C2 Cu2 178.2(12) . . ?
C3 C3 Cu3 178.4(17) 2_766 . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 C6 C7 107.7(10) . . ?
N5 C6 C5 125.0(11) . . ?
C7 C6 C5 127.3(11) . . ?
C8 C7 C6 106.2(10) . . ?
C8 C7 H7 126.9 . . ?
C6 C7 H7 126.9 . . ?
N6 C8 C7 110.2(11) . . ?
N6 C8 C9 125.6(11) . . ?
C7 C8 C9 124.2(10) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N7 C11 C12 107.5(11) . . ?
N7 C11 C10 123.7(12) . . ?
C12 C11 C10 128.7(13) . . ?
C13 C12 C11 107.4(12) . . ?
C13 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
N8 C13 C12 108.9(12) . . ?
N8 C13 C14 126.8(12) . . ?
C12 C13 C14 124.1(12) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N9 C16 C17 106.6(11) . . ?
N9 C16 C15 122.3(12) . . ?
C17 C16 C15 131.1(11) . . ?
C18 C17 C16 106.4(10) . . ?
C18 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
N10 C18 C17 110.8(11) . . ?
N10 C18 C19 125.7(10) . . ?
C17 C18 C19 123.5(11) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N5 B1 N9 109.2(10) . . ?
N5 B1 N7 108.0(10) . . ?
N9 B1 N7 108.4(10) . . ?
N5 B1 H1 120(6) . . ?
N9 B1 H1 111(6) . . ?
N7 B1 H1 100(6) . . ?
C24 N12 C25 117(3) . . ?
C24 N12 C23 124(3) . . ?
C25 N12 C23 118(3) . . ?
N12 C23 H23A 109.5 . . ?
N12 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N12 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N12 C24 H24A 109.5 . . ?
N12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 N12 128(4) . . ?
O2 C25 H25 116.0 . . ?
N12 C25 H25 116.0 . . ?
C28 N13 C26 123(2) . . ?
C28 N13 C27 110(2) . . ?
C26 N13 C27 121(2) . . ?
N13 C26 H26A 109.5 . . ?
N13 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N13 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N13 C27 H27A 109.5 . . ?
N13 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N13 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 N13 131(3) . . ?
O3 C28 H28 114.6 . . ?
N13 C28 H28 114.6 . . ?
C22 N11 C21 123.3(13) . . ?
C22 N11 C20 118.2(11) . . ?
C21 N11 C20 118.0(12) . . ?
N11 C20 H20A 109.5 . . ?
N11 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N11 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N11 C21 H21A 109.5 . . ?
N11 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N11 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C22 N11 126.6(14) . . ?
O1 C22 H22 116.7 . . ?
N11 C22 H22 116.7 . . ?

_refine_diff_density_max         2.480
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.199

_shelxl_version_number           2013-2


_database_code_depnum_ccdc_archive 'CCDC 992894'
