# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 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_80319bm
_database_code_depnum_ccdc_archive 'CCDC 917301'
#TrackingRef '1.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H76 Cl3 Cu7 N24 O8 S8 W2'
_chemical_formula_sum            'C72 H76 Cl3 Cu7 N24 O8 S8 W2'
_chemical_formula_weight         2580.88
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m '
_symmetry_space_group_name_hall  '-P 6c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
_cell_length_a                   16.9317(8)
_cell_length_b                   16.9317(8)
_cell_length_c                   22.0782(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5481.4(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    6388
_cell_measurement_theta_min      2.308
_cell_measurement_theta_max      27.609
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2540
_exptl_absorpt_coefficient_mu    3.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_T_max  0.443
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      291(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29504
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3692
_reflns_number_gt                2798
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constra
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3692
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.0953
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
C1 C 0.2531(4) 0.3525(4) 0.5444(3) 0.0534(16) Uani 1 1 d . . .
H1 H 0.2304 0.3366 0.5052 0.064 Uiso 1 1 calc R . .
C2 C 0.2795(4) 0.3018(4) 0.5847(3) 0.0550(16) Uani 1 1 d . . .
H2 H 0.2788 0.2478 0.5755 0.066 Uiso 1 1 calc R . .
C3 C 0.2968(4) 0.4235(5) 0.6328(4) 0.0609(18) Uani 1 1 d . . .
H3 H 0.3087 0.4652 0.6637 0.073 Uiso 1 1 calc R . .
C4 C 0.3247(4) 0.3164(4) 0.6938(3) 0.0533(15) Uani 1 1 d . . .
C5 C 0.3759(4) 0.2711(4) 0.6953(4) 0.0630(19) Uani 1 1 d . . .
H5 H 0.3931 0.2548 0.6595 0.076 Uiso 1 1 calc R . .
C6 C 0.3996(6) 0.2517(5) 0.7500 0.054(2) Uani 1 2 d S . .
H6 H 0.4344 0.2232 0.7500 0.064 Uiso 1 2 calc SR . .
C7 C 0.3029(6) 0.3405(6) 0.7500 0.057(2) Uani 1 2 d S . .
H7 H 0.2727 0.3738 0.7500 0.069 Uiso 1 2 calc SR . .
C8 C 0.0287(4) 0.4154(4) 0.5465(3) 0.0595(18) Uani 1 1 d . . .
H8 H 0.0204 0.3954 0.5066 0.071 Uiso 1 1 calc R . .
C9 C -0.0418(4) 0.3959(4) 0.5879(3) 0.0523(15) Uani 1 1 d . . .
H9 H -0.1043 0.3620 0.5811 0.063 Uiso 1 1 calc R . .
C10 C 0.0945(4) 0.4832(4) 0.6337(3) 0.0606(18) Uani 1 1 d . . .
H10 H 0.1386 0.5175 0.6625 0.073 Uiso 1 1 calc R . .
C11 C -0.0423(4) 0.4336(5) 0.6965(3) 0.0642(19) Uani 1 1 d . . .
C12 C -0.1359(4) 0.4025(4) 0.6964(3) 0.0492(14) Uani 1 1 d . . .
H12 H -0.1670 0.3907 0.6598 0.059 Uiso 1 1 calc R . .
C13 C -0.1824(6) 0.3893(6) 0.7500 0.060(2) Uani 1 2 d S . .
H13 H -0.2440 0.3719 0.7500 0.072 Uiso 1 2 calc SR . .
C14 C 0.0043(6) 0.4480(6) 0.7500 0.052(2) Uani 1 2 d S . .
H14 H 0.0662 0.4673 0.7500 0.063 Uiso 1 2 calc SR . .
Cl1 Cl 0.48525(13) 0.72940(13) 0.7500 0.0476(5) Uani 1 2 d S . .
Cu1 Cu 0.24296(4) 0.52049(4) 0.54243(3) 0.03628(16) Uani 1 1 d . . .
Cu2 Cu 0.3333 0.6667 0.7500 0.0393(4) Uani 1 6 d S . .
N1 N 0.2690(4) 0.4295(3) 0.5766(2) 0.0533(13) Uani 1 1 d . . .
N2 N 0.3051(3) 0.3469(3) 0.6379(3) 0.0505(12) Uani 1 1 d . . .
N3 N 0.1103(3) 0.4676(4) 0.5737(3) 0.0633(16) Uani 1 1 d . . .
N4 N 0.0032(3) 0.4389(4) 0.6417(3) 0.0603(14) Uani 1 1 d . . .
O1 O 1.0018(5) 0.2060(6) 0.7257(4) 0.070(3) Uani 0.50 1 d P . .
H1A H 0.9739 0.1482 0.7231 0.084 Uiso 0.50 1 d PR . .
H1C H 0.9637 0.2246 0.7224 0.084 Uiso 0.50 1 d PR . .
O2 O 0.9622(6) 0.0871(6) 0.5457(4) 0.059(2) Uani 0.50 1 d P . .
H2B H 0.9558 0.0650 0.5103 0.071 Uiso 0.50 1 d PR . .
H2C H 1.0105 0.1390 0.5471 0.071 Uiso 0.50 1 d PR . .
O3 O 1.0000 0.0000 0.8696(3) 0.0509(17) Uani 1 3 d S . .
H3B H 1.0115 0.0523 0.8818 0.061 Uiso 0.33 1 d PR . .
H3C H 0.9574 -0.0198 0.8435 0.061 Uiso 0.33 1 d PR . .
S1 S 0.3333 0.6667 0.57365(11) 0.0381(5) Uani 1 3 d S . .
S2 S 0.27808(9) 0.75017(9) 0.43984(6) 0.0359(3) Uani 1 1 d . . .
W1 W 0.3333 0.6667 0.471144(17) 0.03265(12) Uani 1 3 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.057(4) 0.049(3) 0.051(4) 0.004(3) -0.006(3) 0.023(3)
C2 0.053(4) 0.044(3) 0.061(5) 0.013(3) -0.006(3) 0.019(3)
C3 0.049(4) 0.060(4) 0.064(5) 0.002(3) -0.003(3) 0.021(3)
C4 0.048(3) 0.053(4) 0.045(4) 0.008(3) 0.003(3) 0.015(3)
C5 0.050(4) 0.056(4) 0.073(5) 0.022(3) 0.024(3) 0.018(3)
C6 0.048(5) 0.037(4) 0.060(6) 0.000 0.000 0.010(4)
C7 0.048(5) 0.046(5) 0.065(7) 0.000 0.000 0.015(4)
C8 0.056(4) 0.051(3) 0.049(4) -0.010(3) 0.005(3) 0.010(3)
C9 0.056(4) 0.043(3) 0.048(4) -0.010(3) -0.013(3) 0.017(3)
C10 0.052(4) 0.049(4) 0.053(4) 0.000(3) -0.003(3) 0.005(3)
C11 0.037(3) 0.064(4) 0.068(5) 0.003(3) 0.002(3) 0.007(3)
C12 0.056(4) 0.050(3) 0.037(3) 0.006(3) -0.012(3) 0.023(3)
C13 0.040(4) 0.052(5) 0.047(6) 0.000 0.000 -0.008(4)
C14 0.037(4) 0.060(5) 0.037(5) 0.000 0.000 0.007(4)
Cl1 0.0377(10) 0.0419(10) 0.0535(13) 0.000 0.000 0.0126(8)
Cu1 0.0394(3) 0.0378(3) 0.0304(3) 0.0022(3) 0.0025(3) 0.0183(3)
Cu2 0.0372(5) 0.0372(5) 0.0437(10) 0.000 0.000 0.0186(2)
N1 0.070(3) 0.047(3) 0.042(3) 0.020(2) 0.016(3) 0.028(3)
N2 0.050(3) 0.035(3) 0.052(3) 0.016(2) 0.016(2) 0.011(2)
N3 0.048(3) 0.068(4) 0.042(4) -0.014(3) 0.007(2) 0.005(3)
N4 0.043(3) 0.063(3) 0.055(4) -0.004(3) 0.004(2) 0.011(3)
O1 0.035(4) 0.068(6) 0.063(7) -0.010(4) -0.016(4) -0.008(4)
O2 0.059(5) 0.057(5) 0.049(6) -0.025(4) -0.005(4) 0.020(4)
O3 0.047(2) 0.047(2) 0.058(5) 0.000 0.000 0.0236(12)
S1 0.0429(7) 0.0429(7) 0.0286(12) 0.000 0.000 0.0214(4)
S2 0.0393(7) 0.0374(6) 0.0338(7) -0.0009(5) 0.0009(5) 0.0213(5)
W1 0.03539(14) 0.03539(14) 0.0272(2) 0.000 0.000 0.01770(7)
_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
C1 N1 1.390(8) . ?
C1 C2 1.453(9) . ?
C1 H1 0.9300 . ?
C2 N2 1.349(9) . ?
C2 H2 0.9300 . ?
C3 N1 1.349(9) . ?
C3 N2 1.377(8) . ?
C3 H3 0.9300 . ?
C4 C7 1.412(8) . ?
C4 C5 1.417(10) . ?
C4 N2 1.440(8) . ?
C5 C6 1.364(8) . ?
C5 H5 0.9300 . ?
C6 C5 1.364(8) 10_557 ?
C6 H6 0.9300 . ?
C7 C4 1.412(8) 10_557 ?
C7 H7 0.9300 . ?
C8 N3 1.353(8) . ?
C8 C9 1.404(9) . ?
C8 H8 0.9300 . ?
C9 N4 1.402(8) . ?
C9 H9 0.9300 . ?
C10 N4 1.352(8) . ?
C10 N3 1.401(9) . ?
C10 H10 0.9300 . ?
C11 C14 1.373(8) . ?
C11 C12 1.399(9) . ?
C11 N4 1.413(9) . ?
C12 C13 1.377(8) . ?
C12 H12 0.9300 . ?
C13 C12 1.377(8) 10_557 ?
C13 H13 0.9300 . ?
C14 C11 1.373(8) 10_557 ?
C14 H14 0.9300 . ?
Cl1 Cu2 2.2388(19) . ?
Cu1 N1 1.952(5) . ?
Cu1 N3 2.076(5) . ?
Cu1 S2 2.2683(14) 2_665 ?
Cu1 S1 2.2705(10) . ?
Cu1 W1 2.6753(7) . ?
Cu2 Cl1 2.2388(19) 2_665 ?
Cu2 Cl1 2.239(2) 3_565 ?
O1 O1 1.075(18) 10_557 ?
O1 H1A 0.8499 . ?
O1 H1C 0.8500 . ?
O2 H2B 0.8500 . ?
O2 H2C 0.8501 . ?
O3 H3B 0.8500 . ?
O3 H3C 0.8500 . ?
S1 W1 2.263(2) . ?
S1 Cu1 2.2705(10) 3_565 ?
S1 Cu1 2.2705(10) 2_665 ?
S2 W1 2.1622(13) . ?
S2 Cu1 2.2684(14) 3_565 ?
W1 S2 2.1622(13) 2_665 ?
W1 S2 2.1622(13) 3_565 ?
W1 Cu1 2.6753(7) 3_565 ?
W1 Cu1 2.6753(7) 2_665 ?
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 C1 C2 105.6(6) . . ?
N1 C1 H1 127.2 . . ?
C2 C1 H1 127.2 . . ?
N2 C2 C1 107.8(6) . . ?
N2 C2 H2 126.1 . . ?
C1 C2 H2 126.1 . . ?
N1 C3 N2 110.6(6) . . ?
N1 C3 H3 124.7 . . ?
N2 C3 H3 124.7 . . ?
C7 C4 C5 117.2(7) . . ?
C7 C4 N2 120.6(7) . . ?
C5 C4 N2 121.8(6) . . ?
C6 C5 C4 118.9(7) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C5 124.7(10) . 10_557 ?
C5 C6 H6 117.7 . . ?
C5 C6 H6 117.7 10_557 . ?
C4 C7 C4 122.9(9) . 10_557 ?
C4 C7 H7 118.6 . . ?
C4 C7 H7 118.6 10_557 . ?
N3 C8 C9 109.6(6) . . ?
N3 C8 H8 125.2 . . ?
C9 C8 H8 125.2 . . ?
N4 C9 C8 104.6(5) . . ?
N4 C9 H9 127.7 . . ?
C8 C9 H9 127.7 . . ?
N4 C10 N3 107.0(6) . . ?
N4 C10 H10 126.5 . . ?
N3 C10 H10 126.5 . . ?
C14 C11 C12 120.7(7) . . ?
C14 C11 N4 118.7(6) . . ?
C12 C11 N4 120.1(6) . . ?
C13 C12 C11 120.6(6) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C12 118.6(8) . 10_557 ?
C12 C13 H13 120.7 . . ?
C12 C13 H13 120.7 10_557 . ?
C11 C14 C11 118.8(9) . 10_557 ?
C11 C14 H14 120.6 . . ?
C11 C14 H14 120.6 10_557 . ?
N1 Cu1 N3 98.8(2) . . ?
N1 Cu1 S2 113.81(17) . 2_665 ?
N3 Cu1 S2 111.74(17) . 2_665 ?
N1 Cu1 S1 116.59(18) . . ?
N3 Cu1 S1 111.31(15) . . ?
S2 Cu1 S1 104.77(7) 2_665 . ?
N1 Cu1 W1 134.96(16) . . ?
N3 Cu1 W1 126.14(18) . . ?
S2 Cu1 W1 51.06(4) 2_665 . ?
S1 Cu1 W1 53.71(6) . . ?
Cl1 Cu2 Cl1 120.0 2_665 3_565 ?
Cl1 Cu2 Cl1 120.000(1) 2_665 . ?
Cl1 Cu2 Cl1 120.0 3_565 . ?
C3 N1 C1 108.1(5) . . ?
C3 N1 Cu1 129.8(5) . . ?
C1 N1 Cu1 121.9(4) . . ?
C2 N2 C3 107.8(6) . . ?
C2 N2 C4 127.6(5) . . ?
C3 N2 C4 123.9(6) . . ?
C8 N3 C10 108.3(5) . . ?
C8 N3 Cu1 131.7(5) . . ?
C10 N3 Cu1 120.0(4) . . ?
C10 N4 C9 110.5(6) . . ?
C10 N4 C11 125.7(6) . . ?
C9 N4 C11 123.8(5) . . ?
O1 O1 H1A 93.8 10_557 . ?
O1 O1 H1C 94.9 10_557 . ?
H1A O1 H1C 109.5 . . ?
H2B O2 H2C 109.5 . . ?
H3B O3 H3C 109.5 . . ?
W1 S1 Cu1 72.33(6) . 3_565 ?
W1 S1 Cu1 72.33(6) . . ?
Cu1 S1 Cu1 111.21(6) 3_565 . ?
W1 S1 Cu1 72.33(6) . 2_665 ?
Cu1 S1 Cu1 111.21(6) 3_565 2_665 ?
Cu1 S1 Cu1 111.21(6) . 2_665 ?
W1 S2 Cu1 74.25(4) . 3_565 ?
S2 W1 S2 110.29(3) . 2_665 ?
S2 W1 S2 110.29(3) . 3_565 ?
S2 W1 S2 110.29(3) 2_665 3_565 ?
S2 W1 S1 108.64(4) . . ?
S2 W1 S1 108.64(4) 2_665 . ?
S2 W1 S1 108.64(4) 3_565 . ?
S2 W1 Cu1 54.69(4) . 3_565 ?
S2 W1 Cu1 125.70(4) 2_665 3_565 ?
S2 W1 Cu1 123.97(4) 3_565 3_565 ?
S1 W1 Cu1 53.964(16) . 3_565 ?
S2 W1 Cu1 123.97(4) . . ?
S2 W1 Cu1 54.69(4) 2_665 . ?
S2 W1 Cu1 125.70(4) 3_565 . ?
S1 W1 Cu1 53.964(16) . . ?
Cu1 W1 Cu1 88.90(2) 3_565 . ?
S2 W1 Cu1 125.70(4) . 2_665 ?
S2 W1 Cu1 123.97(4) 2_665 2_665 ?
S2 W1 Cu1 54.69(4) 3_565 2_665 ?
S1 W1 Cu1 53.964(16) . 2_665 ?
Cu1 W1 Cu1 88.90(2) 3_565 2_665 ?
Cu1 W1 Cu1 88.90(2) . 2_665 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2B O2 0.85 2.01 2.756(14) 145.9 9_546
O2 H2B O2 0.85 2.29 2.756(14) 114.8 8_666
O3 H3B O2 0.85 2.02 2.651(11) 129.9 10_557
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.113


data_90307dm
_database_code_depnum_ccdc_archive 'CCDC 917302'
#TrackingRef '2.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H60 Cu6 Mo2 N24 S8, 8(H2 O), Cl3 Cu'
_chemical_formula_sum            'C72 H76 Cl3 Cu7 Mo2 N24 O8 S8'
_chemical_formula_weight         2405.06
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P6(3)/m '
_symmetry_space_group_name_Hall  '-P 6c '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
_cell_length_a                   16.817(2)
_cell_length_b                   16.817(2)
_cell_length_c                   22.226(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5444.0(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    1609
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      16.772
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2412
_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            28792
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3675
_reflns_number_gt                3184
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.08P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3675
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1320
_refine_ls_wR_factor_gt          0.1257
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
C1 C 0.2532(3) 0.3524(3) 0.5447(2) 0.0420(10) Uani 1 1 d . . .
H1 H 0.2305 0.3367 0.5058 0.050 Uiso 1 1 calc R . .
C2 C 0.2791(3) 0.3012(3) 0.58432(18) 0.0387(9) Uani 1 1 d . . .
H2 H 0.2786 0.2471 0.5750 0.046 Uiso 1 1 calc R . .
C3 C 0.2961(3) 0.4230(3) 0.6324(2) 0.0407(10) Uani 1 1 d . . .
H3 H 0.3077 0.4650 0.6631 0.049 Uiso 1 1 calc R . .
C4 C 0.3245(3) 0.3163(3) 0.6943(2) 0.0426(10) Uani 1 1 d . . .
C5 C 0.3758(3) 0.2706(3) 0.69531(19) 0.0432(11) Uani 1 1 d . . .
H5 H 0.3928 0.2539 0.6598 0.052 Uiso 1 1 calc R . .
C6 C 0.3996(5) 0.2518(4) 0.7500 0.0421(14) Uani 1 2 d S . .
H6 H 0.4352 0.2236 0.7500 0.051 Uiso 1 2 calc SR . .
C7 C 0.3029(5) 0.3407(4) 0.7500 0.0457(15) Uani 1 2 d S . .
H7 H 0.2729 0.3745 0.7500 0.055 Uiso 1 2 calc SR . .
C8 C 0.0285(3) 0.4157(3) 0.5469(2) 0.0470(11) Uani 1 1 d . . .
H8 H 0.0201 0.3958 0.5072 0.056 Uiso 1 1 calc R . .
C9 C -0.0409(3) 0.3964(3) 0.5877(2) 0.0476(11) Uani 1 1 d . . .
H9 H -0.1038 0.3621 0.5809 0.057 Uiso 1 1 calc R . .
C10 C 0.0938(3) 0.4829(3) 0.6334(2) 0.0448(11) Uani 1 1 d . . .
H10 H 0.1382 0.5171 0.6621 0.054 Uiso 1 1 calc R . .
C11 C -0.0422(3) 0.4342(3) 0.6960(2) 0.0430(10) Uani 1 1 d . . .
C12 C -0.1365(3) 0.4031(3) 0.6961(2) 0.0400(10) Uani 1 1 d . . .
H12 H -0.1682 0.3923 0.6600 0.048 Uiso 1 1 calc R . .
C13 C -0.1818(4) 0.3886(4) 0.7500 0.0450(15) Uani 1 2 d S . .
H13 H -0.2443 0.3686 0.7500 0.054 Uiso 1 2 calc SR . .
C14 C 0.0033(4) 0.4480(4) 0.7500 0.0427(15) Uani 1 2 d S . .
H14 H 0.0656 0.4669 0.7500 0.051 Uiso 1 2 calc SR . .
Cl1 Cl 0.48518(9) 0.72900(10) 0.7500 0.0381(3) Uani 1 2 d S . .
Cu1 Cu 0.24399(3) 0.52208(3) 0.54174(2) 0.03395(17) Uani 1 1 d . . .
Cu2 Cu 0.3333 0.6667 0.7500 0.0362(3) Uani 1 6 d S . .
Mo1 Mo 0.3333 0.6667 0.47126(3) 0.03311(18) Uani 1 3 d S . .
N1 N 0.2690(2) 0.4295(2) 0.57657(16) 0.0391(8) Uani 1 1 d . . .
N2 N 0.3043(2) 0.3466(2) 0.63793(16) 0.0404(8) Uani 1 1 d . . .
N3 N 0.1104(2) 0.4680(2) 0.57396(18) 0.0450(9) Uani 1 1 d . . .
N4 N 0.0035(2) 0.4397(3) 0.64183(16) 0.0431(9) Uani 1 1 d . . .
O1 O 1.0016(4) 0.2057(4) 0.7250(3) 0.0519(16) Uani 0.50 1 d P . .
H1A H 0.9604 0.2203 0.7201 0.062 Uiso 0.50 1 d PR . .
H1B H 0.9770 0.1476 0.7247 0.062 Uiso 0.50 1 d PR . .
O2 O 0.9638(4) 0.0872(4) 0.5446(3) 0.0455(15) Uani 0.50 1 d P . .
H2A H 1.0001 0.1126 0.5152 0.055 Uiso 0.50 1 d PR . .
H2B H 0.9938 0.1044 0.5773 0.055 Uiso 0.50 1 d PR . .
O3 O 1.0000 1.0000 0.8702(3) 0.0461(13) Uani 1 3 d S . .
H3A H 0.9846 0.9643 0.9004 0.055 Uiso 0.3333 1 d PR . .
H3B H 1.0110 1.0528 0.8816 0.055 Uiso 0.3333 1 d PR . .
S1 S 0.3333 0.6667 0.57229(8) 0.0352(4) Uani 1 3 d S . .
S2 S 0.27852(7) 0.74926(7) 0.44013(5) 0.0336(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.047(3) 0.046(2) 0.032(2) 0.0031(18) -0.0093(18) 0.022(2)
C2 0.040(2) 0.044(2) 0.028(2) 0.0081(18) 0.0018(17) 0.0178(19)
C3 0.043(2) 0.035(2) 0.042(2) 0.0015(18) -0.0027(19) 0.0183(19)
C4 0.041(2) 0.041(2) 0.033(2) 0.0049(18) -0.0007(17) 0.0105(19)
C5 0.049(3) 0.045(2) 0.028(2) 0.0232(18) 0.0244(18) 0.018(2)
C6 0.056(4) 0.032(3) 0.029(3) 0.000 0.000 0.015(3)
C7 0.053(4) 0.047(4) 0.024(3) 0.000 0.000 0.015(3)
C8 0.045(2) 0.041(2) 0.039(2) -0.0102(19) 0.007(2) 0.009(2)
C9 0.047(3) 0.037(2) 0.042(3) 0.0012(19) 0.013(2) 0.008(2)
C10 0.039(2) 0.041(2) 0.027(2) -0.0002(18) -0.0033(17) -0.0006(19)
C11 0.035(2) 0.039(2) 0.039(3) 0.0045(18) 0.0019(18) 0.0064(19)
C12 0.039(2) 0.039(2) 0.046(3) 0.0049(19) 0.0133(19) 0.0223(19)
C13 0.044(3) 0.046(3) 0.033(3) 0.000 0.000 0.013(3)
C14 0.034(3) 0.036(3) 0.033(3) 0.000 0.000 -0.001(2)
Cl1 0.0353(7) 0.0389(7) 0.0315(7) 0.000 0.000 0.0120(6)
Cu1 0.0372(3) 0.0354(3) 0.0275(3) 0.00246(19) 0.00298(19) 0.0169(2)
Cu2 0.0334(4) 0.0334(4) 0.0418(7) 0.000 0.000 0.0167(2)
Mo1 0.0367(2) 0.0367(2) 0.0259(3) 0.000 0.000 0.01837(12)
N1 0.0364(18) 0.0329(18) 0.039(2) 0.0171(15) 0.0155(16) 0.0105(15)
N2 0.0421(19) 0.043(2) 0.030(2) 0.0154(15) 0.0099(15) 0.0174(17)
N3 0.038(2) 0.039(2) 0.043(2) -0.0071(16) 0.0028(16) 0.0077(16)
N4 0.044(2) 0.046(2) 0.029(2) 0.0116(16) 0.0101(15) 0.0152(17)
O1 0.052(4) 0.045(3) 0.056(4) -0.025(3) -0.005(3) 0.022(3)
O2 0.046(3) 0.047(4) 0.040(4) -0.006(3) 0.003(3) 0.020(3)
O3 0.0434(18) 0.0434(18) 0.052(3) 0.000 0.000 0.0217(9)
S1 0.0383(6) 0.0383(6) 0.0289(9) 0.000 0.000 0.0192(3)
S2 0.0365(5) 0.0350(5) 0.0280(5) 0.0026(4) 0.0024(4) 0.0169(4)
_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
C1 N1 1.382(6) . ?
C1 C2 1.442(6) . ?
C1 H1 0.9300 . ?
C2 N2 1.363(6) . ?
C2 H2 0.9300 . ?
C3 N1 1.345(6) . ?
C3 N2 1.365(5) . ?
C3 H3 0.9300 . ?
C4 C7 1.407(6) . ?
C4 C5 1.414(7) . ?
C4 N2 1.455(6) . ?
C5 C6 1.366(5) . ?
C5 H5 0.9300 . ?
C6 C5 1.366(5) 10_557 ?
C6 H6 0.9300 . ?
C7 C4 1.407(6) 10_557 ?
C7 H7 0.9300 . ?
C8 N3 1.350(6) . ?
C8 C9 1.383(6) . ?
C8 H8 0.9300 . ?
C9 N4 1.411(6) . ?
C9 H9 0.9300 . ?
C10 N4 1.328(6) . ?
C10 N3 1.399(6) . ?
C10 H10 0.9300 . ?
C11 C14 1.380(5) . ?
C11 C12 1.400(6) . ?
C11 N4 1.405(6) . ?
C12 C13 1.374(5) . ?
C12 H12 0.9300 . ?
C13 C12 1.374(5) 10_557 ?
C13 H13 0.9300 . ?
C14 C11 1.380(5) 10_557 ?
C14 H14 0.9300 . ?
Cl1 Cu2 2.2233(14) . ?
Cu1 N1 1.963(3) . ?
Cu1 N3 2.083(4) . ?
Cu1 S1 2.2310(8) . ?
Cu1 S2 2.2616(13) 2_665 ?
Cu1 Mo1 2.6403(7) . ?
Cu2 Cl1 2.2233(14) 2_665 ?
Cu2 Cl1 2.2233(14) 3_565 ?
Mo1 S2 2.1304(10) . ?
Mo1 S2 2.1304(11) 2_665 ?
Mo1 S2 2.1304(10) 3_565 ?
Mo1 S1 2.2455(19) . ?
Mo1 Cu1 2.6403(7) 3_565 ?
Mo1 Cu1 2.6403(7) 2_665 ?
O1 O1 1.110(13) 10_557 ?
O1 H1A 0.8501 . ?
O1 H1B 0.8499 . ?
O2 H2A 0.8501 . ?
O2 H2B 0.8499 . ?
O3 H3A 0.8499 . ?
O3 H3B 0.8500 . ?
S1 Cu1 2.2310(8) 3_565 ?
S1 Cu1 2.2310(8) 2_665 ?
S2 Cu1 2.2616(13) 3_565 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 105.9(4) . . ?
N1 C1 H1 127.0 . . ?
C2 C1 H1 127.0 . . ?
N2 C2 C1 107.5(4) . . ?
N2 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
N1 C3 N2 111.0(4) . . ?
N1 C3 H3 124.5 . . ?
N2 C3 H3 124.5 . . ?
C7 C4 C5 117.4(4) . . ?
C7 C4 N2 121.1(5) . . ?
C5 C4 N2 121.1(4) . . ?
C6 C5 C4 118.0(4) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C5 C6 C5 125.7(7) . 10_557 ?
C5 C6 H6 117.1 . . ?
C5 C6 H6 117.1 10_557 . ?
C4 C7 C4 123.2(7) . 10_557 ?
C4 C7 H7 118.4 . . ?
C4 C7 H7 118.4 10_557 . ?
N3 C8 C9 109.1(4) . . ?
N3 C8 H8 125.4 . . ?
C9 C8 H8 125.4 . . ?
C8 C9 N4 105.7(4) . . ?
C8 C9 H9 127.2 . . ?
N4 C9 H9 127.2 . . ?
N4 C10 N3 108.1(4) . . ?
N4 C10 H10 125.9 . . ?
N3 C10 H10 125.9 . . ?
C14 C11 C12 119.3(4) . . ?
C14 C11 N4 119.7(4) . . ?
C12 C11 N4 120.5(4) . . ?
C13 C12 C11 119.6(5) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C12 121.2(6) . 10_557 ?
C12 C13 H13 119.4 . . ?
C12 C13 H13 119.4 10_557 . ?
C11 C14 C11 121.1(6) . 10_557 ?
C11 C14 H14 119.5 . . ?
C11 C14 H14 119.5 10_557 . ?
N1 Cu1 N3 97.45(15) . . ?
N1 Cu1 S1 116.73(11) . . ?
N3 Cu1 S1 111.27(10) . . ?
N1 Cu1 S2 114.27(11) . 2_665 ?
N3 Cu1 S2 112.39(11) . 2_665 ?
S1 Cu1 S2 104.91(5) . 2_665 ?
N1 Cu1 Mo1 135.68(9) . . ?
N3 Cu1 Mo1 126.79(11) . . ?
S1 Cu1 Mo1 54.11(5) . . ?
S2 Cu1 Mo1 50.80(3) 2_665 . ?
Cl1 Cu2 Cl1 120.0 2_665 3_565 ?
Cl1 Cu2 Cl1 120.000(1) 2_665 . ?
Cl1 Cu2 Cl1 120.0 3_565 . ?
S2 Mo1 S2 109.99(3) . 2_665 ?
S2 Mo1 S2 109.99(3) . 3_565 ?
S2 Mo1 S2 109.99(3) 2_665 3_565 ?
S2 Mo1 S1 108.95(3) . . ?
S2 Mo1 S1 108.95(3) 2_665 . ?
S2 Mo1 S1 108.95(3) 3_565 . ?
S2 Mo1 Cu1 55.36(3) . 3_565 ?
S2 Mo1 Cu1 125.87(3) 2_665 3_565 ?
S2 Mo1 Cu1 124.10(3) 3_565 3_565 ?
S1 Mo1 Cu1 53.604(17) . 3_565 ?
S2 Mo1 Cu1 124.10(3) . . ?
S2 Mo1 Cu1 55.36(3) 2_665 . ?
S2 Mo1 Cu1 125.87(3) 3_565 . ?
S1 Mo1 Cu1 53.604(17) . . ?
Cu1 Mo1 Cu1 88.39(2) 3_565 . ?
S2 Mo1 Cu1 125.87(3) . 2_665 ?
S2 Mo1 Cu1 124.10(3) 2_665 2_665 ?
S2 Mo1 Cu1 55.36(3) 3_565 2_665 ?
S1 Mo1 Cu1 53.604(17) . 2_665 ?
Cu1 Mo1 Cu1 88.39(2) 3_565 2_665 ?
Cu1 Mo1 Cu1 88.39(2) . 2_665 ?
C3 N1 C1 108.0(3) . . ?
C3 N1 Cu1 130.1(3) . . ?
C1 N1 Cu1 121.7(3) . . ?
C2 N2 C3 107.4(4) . . ?
C2 N2 C4 128.2(4) . . ?
C3 N2 C4 124.0(4) . . ?
C8 N3 C10 107.9(4) . . ?
C8 N3 Cu1 131.1(3) . . ?
C10 N3 Cu1 121.0(3) . . ?
C10 N4 C11 126.5(4) . . ?
C10 N4 C9 109.1(4) . . ?
C11 N4 C9 124.3(4) . . ?
O1 O1 H1A 97.4 10_557 . ?
O1 O1 H1B 90.5 10_557 . ?
H1A O1 H1B 109.5 . . ?
H2A O2 H2B 109.5 . . ?
H3A O3 H3B 109.5 . . ?
Cu1 S1 Cu1 111.17(4) 3_565 . ?
Cu1 S1 Cu1 111.17(4) 3_565 2_665 ?
Cu1 S1 Cu1 111.17(4) . 2_665 ?
Cu1 S1 Mo1 72.29(5) 3_565 . ?
Cu1 S1 Mo1 72.29(5) . . ?
Cu1 S1 Mo1 72.29(5) 2_665 . ?
Mo1 S2 Cu1 73.84(4) . 3_565 ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.063


data_80311am
_database_code_depnum_ccdc_archive 'CCDC 917303'
#TrackingRef '3.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C72 H60 Cu6 N24 S8 W2, H2 O, H4.80 O2.40, 3(H1.80 O1.20), Br3 Cu, 0.9(H2)'
_chemical_formula_sum            'C72 H74 Br3 Cu7 N24 O7 S8 W2'
_chemical_formula_weight         2696.24
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Br Br -0.2901 2.4595 '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           Hexagonal
_symmetry_space_group_name_H-M   'P6(3)/m '
_symmetry_space_group_name_Hall  '-P 6c '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
_cell_length_a                   17.0636(14)
_cell_length_b                   17.0636(14)
_cell_length_c                   22.372(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5641.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    5735
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      27.41
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2628
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            30597
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.99
_reflns_number_total             3801
_reflns_number_gt                3059
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.06P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/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         3801
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1186
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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
C1 C 0.3095(4) 0.4375(4) 0.6333(3) 0.0377(14) Uani 1 1 d . . .
H1 H 0.3285 0.4847 0.6606 0.045 Uiso 1 1 calc R . .
C2 C 0.2464(4) 0.3498(4) 0.5506(3) 0.0363(13) Uani 1 1 d . . .
H2 H 0.2168 0.3284 0.5142 0.044 Uiso 1 1 calc R . .
C3 C 0.2777(5) 0.3067(5) 0.5916(3) 0.0451(16) Uani 1 1 d . . .
H3 H 0.2733 0.2507 0.5856 0.054 Uiso 1 1 calc R . .
C4 C 0.3337(4) 0.3403(4) 0.6967(3) 0.0393(15) Uani 1 1 d . . .
C5 C 0.3691(5) 0.2805(5) 0.6953(3) 0.0450(16) Uani 1 1 d . . .
H5 H 0.3863 0.2661 0.6594 0.054 Uiso 1 1 calc R . .
C6 C 0.3774(6) 0.2437(6) 0.7500 0.037(2) Uani 1 2 d S . .
H6 H 0.3883 0.1955 0.7500 0.044 Uiso 1 2 calc SR . .
C7 C 0.3229(6) 0.3723(6) 0.7500 0.038(2) Uani 1 2 d S . .
H7 H 0.3076 0.4175 0.7500 0.046 Uiso 1 2 calc SR . .
C8 C 0.0901(4) 0.4558(4) 0.6370(3) 0.0363(14) Uani 1 1 d . . .
H8 H 0.1232 0.4487 0.6674 0.044 Uiso 1 1 calc R . .
C9 C 0.0541(4) 0.4802(5) 0.5542(3) 0.0466(16) Uani 1 1 d . . .
H9 H 0.0564 0.4925 0.5135 0.056 Uiso 1 1 calc R . .
C10 C -0.0239(5) 0.4649(5) 0.5901(3) 0.0457(16) Uani 1 1 d . . .
H10 H -0.0761 0.4665 0.5804 0.055 Uiso 1 1 calc R . .
C11 C -0.0434(4) 0.4349(4) 0.6976(3) 0.0410(15) Uani 1 1 d . . .
C12 C -0.1354(4) 0.4027(5) 0.6970(3) 0.0410(15) Uani 1 1 d . . .
H12 H -0.1658 0.3910 0.6607 0.049 Uiso 1 1 calc R . .
C13 C -0.1827(7) 0.3879(6) 0.7500 0.043(2) Uani 1 2 d S . .
H13 H -0.2442 0.3686 0.7500 0.051 Uiso 1 2 calc SR . .
C14 C 0.0022(6) 0.4480(6) 0.7500 0.035(2) Uani 1 2 d S . .
H14 H 0.0633 0.4656 0.7500 0.042 Uiso 1 2 calc SR . .
Cu2 Cu 1.0000 0.0000 0.5000 0.0480(5) Uani 1 6 d S . .
Br1 Br 0.94899(10) 0.09582(10) 0.53400(6) 0.0496(4) Uani 0.50 1 d P . .
N1 N 0.2707(3) 0.4298(3) 0.5781(2) 0.0326(11) Uani 1 1 d . . .
N2 N 0.3136(4) 0.3583(3) 0.6389(2) 0.0402(13) Uani 1 1 d . . .
N3 N 0.1155(4) 0.4766(3) 0.5782(2) 0.0316(11) Uani 1 1 d . . .
N4 N 0.0049(3) 0.4476(3) 0.6417(2) 0.0345(12) Uani 1 1 d . . .
O1 O 0.3333 0.6667 0.7500 0.038(2) Uani 1 6 d S . .
H1A H 0.36(4) 0.67(7) 0.78(2) 0.046 Uiso 0.1667 1 d P . .
H1B H 0.36(3) 0.72(3) 0.73(2) 0.046 Uiso 0.1667 1 d P . .
O2 O 1.00(6) 0.99(6) 0.7500 0.06(11) Uani 0.80 2 d SP . .
H2D H 0.946(18) 0.941(16) 0.7500 0.071 Uiso 0.80 2 d SP . .
H2B H 1.03(2) 0.99(3) 0.722(8) 0.071 Uiso 0.40 1 d P . .
O3 O 0.0333(9) 0.2327(10) 0.7110(5) 0.031(3) Uani 0.30 1 d P . .
H3B H 0.063(14) 0.286(15) 0.725(9) 0.037 Uiso 0.30 1 d P . .
H3C H 0.048(14) 0.232(15) 0.675(10) 0.037 Uiso 0.30 1 d P . .
O4 O 0.0507(9) 0.1548(9) 0.7500 0.048(3) Uani 0.60 2 d SP . .
H4A H 0.002(17) 0.113(19) 0.766(12) 0.057 Uiso 0.30 1 d P . .
H4B H 0.073(18) 0.131(18) 0.727(12) 0.057 Uiso 0.30 1 d P . .
S1 S 0.24443(10) 0.52848(10) 0.44025(7) 0.0350(3) Uani 1 1 d . . .
S2 S 0.3333 0.6667 0.57003(12) 0.0367(6) Uani 1 3 d S . .
Cu1 Cu 0.23842(5) 0.52149(5) 0.54333(3) 0.0354(2) Uani 1 1 d . . .
W1 W 0.3333 0.6667 0.472952(18) 0.03390(15) Uani 1 3 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.034(3) 0.031(3) 0.041(3) 0.012(3) 0.004(3) 0.011(3)
C2 0.040(3) 0.029(3) 0.038(3) -0.001(3) -0.012(3) 0.015(3)
C3 0.043(4) 0.045(4) 0.044(4) -0.005(3) -0.013(3) 0.019(3)
C4 0.036(4) 0.028(3) 0.044(4) 0.001(3) 0.006(3) 0.008(3)
C5 0.038(4) 0.043(4) 0.046(4) -0.012(3) -0.006(3) 0.014(3)
C6 0.036(5) 0.047(5) 0.023(4) 0.000 0.000 0.017(4)
C7 0.042(5) 0.036(5) 0.023(4) 0.000 0.000 0.009(4)
C8 0.033(3) 0.038(3) 0.029(3) 0.009(2) 0.002(2) 0.011(3)
C9 0.032(3) 0.045(4) 0.049(4) 0.010(3) 0.006(3) 0.008(3)
C10 0.043(4) 0.056(4) 0.032(3) 0.008(3) 0.010(3) 0.020(3)
C11 0.029(3) 0.037(4) 0.044(4) 0.016(3) -0.006(3) 0.008(3)
C12 0.033(3) 0.046(4) 0.039(3) 0.001(3) 0.013(3) 0.016(3)
C13 0.052(6) 0.030(5) 0.030(4) 0.000 0.000 0.009(4)
C14 0.024(4) 0.039(5) 0.031(4) 0.000 0.000 0.007(4)
Cu2 0.0430(7) 0.0430(7) 0.0580(13) 0.000 0.000 0.0215(4)
Br1 0.0468(8) 0.0475(8) 0.0485(8) 0.0008(6) 0.0001(6) 0.0191(6)
N1 0.029(3) 0.029(3) 0.032(2) -0.001(2) 0.010(2) 0.008(2)
N2 0.036(3) 0.034(3) 0.042(3) 0.009(2) -0.013(2) 0.012(2)
N3 0.041(3) 0.023(2) 0.030(2) -0.0025(19) 0.007(2) 0.016(2)
N4 0.028(3) 0.036(3) 0.037(3) 0.004(2) -0.001(2) 0.014(2)
O1 0.034(5) 0.034(5) 0.047(9) 0.000 0.000 0.017(2)
O2 0.05(6) 0.06(4) 0.045(4) 0.000 0.000 0.01(19)
O3 0.036(8) 0.043(8) 0.010(5) 0.007(5) 0.014(5) 0.017(7)
O4 0.031(6) 0.052(8) 0.053(7) 0.000 0.000 0.016(6)
S1 0.0310(7) 0.0368(8) 0.0334(8) -0.0019(6) -0.0041(6) 0.0141(7)
S2 0.0388(9) 0.0388(9) 0.0327(13) 0.000 0.000 0.0194(4)
Cu1 0.0373(4) 0.0352(4) 0.0310(4) -0.0014(3) 0.0012(3) 0.0160(3)
W1 0.03590(18) 0.03590(18) 0.0299(2) 0.000 0.000 0.01795(9)
_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
C1 N1 1.377(8) . ?
C1 N2 1.394(8) . ?
C1 H1 0.9300 . ?
C2 N1 1.359(7) . ?
C2 C3 1.436(9) . ?
C2 H2 0.9300 . ?
C3 N2 1.316(8) . ?
C3 H3 0.9300 . ?
C4 C7 1.361(8) . ?
C4 N2 1.411(8) . ?
C4 C5 1.422(10) . ?
C5 C6 1.415(9) . ?
C5 H5 0.9300 . ?
C6 C5 1.415(9) 10_557 ?
C6 H6 0.9300 . ?
C7 C4 1.361(8) 10_557 ?
C7 H7 0.9300 . ?
C8 N3 1.373(7) . ?
C8 N4 1.393(8) . ?
C8 H8 0.9300 . ?
C9 N3 1.205(8) . ?
C9 C10 1.462(9) . ?
C9 H9 0.9300 . ?
C10 N4 1.345(8) . ?
C10 H10 0.9300 . ?
C11 C14 1.361(7) . ?
C11 C12 1.380(9) . ?
C11 N4 1.453(8) . ?
C12 C13 1.384(8) . ?
C12 H12 0.9300 . ?
C13 C12 1.384(8) 10_557 ?
C13 H13 0.9300 . ?
C14 C11 1.361(7) 10_557 ?
C14 H14 0.9300 . ?
Cu2 Br1 2.3308(16) 3_765 ?
Cu2 Br1 2.3308(16) 9_546 ?
Cu2 Br1 2.3308(16) 2_645 ?
Cu2 Br1 2.3308(16) 7_756 ?
Cu2 Br1 2.3308(16) 8_666 ?
Cu2 Br1 2.3308(16) . ?
Br1 Br1 2.677(2) 9_546 ?
Br1 Br1 2.677(2) 8_666 ?
N1 Cu1 2.053(5) . ?
N3 Cu1 1.998(5) . ?
O1 H1A 0.9(6) . ?
O1 H1B 0.9(6) . ?
O2 H2D 0.8(3) . ?
O2 H2B 0.9(10) . ?
O3 O3 1.74(2) 10_557 ?
O3 H3B 0.8(2) . ?
O3 H3C 0.8(2) . ?
O4 O3 1.733(18) 10_557 ?
O4 H4A 0.9(3) . ?
O4 H4B 0.8(3) . ?
S1 W1 2.1953(15) . ?
S1 Cu1 2.3087(17) . ?
S2 W1 2.172(3) . ?
S2 Cu1 2.2594(10) 3_565 ?
S2 Cu1 2.2594(10) . ?
S2 Cu1 2.2594(10) 2_665 ?
Cu1 W1 2.6883(8) . ?
W1 S1 2.1953(15) 3_565 ?
W1 S1 2.1953(15) 2_665 ?
W1 Cu1 2.6883(8) 3_565 ?
W1 Cu1 2.6883(8) 2_665 ?
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 C1 N2 104.0(5) . . ?
N1 C1 H1 128.0 . . ?
N2 C1 H1 128.0 . . ?
N1 C2 C3 102.7(5) . . ?
N1 C2 H2 128.6 . . ?
C3 C2 H2 128.6 . . ?
N2 C3 C2 109.8(6) . . ?
N2 C3 H3 125.1 . . ?
C2 C3 H3 125.1 . . ?
C7 C4 N2 128.3(7) . . ?
C7 C4 C5 119.9(7) . . ?
N2 C4 C5 111.8(6) . . ?
C6 C5 C4 118.1(7) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C5 C6 C5 119.8(9) 10_557 . ?
C5 C6 H6 120.1 10_557 . ?
C5 C6 H6 120.1 . . ?
C4 C7 C4 122.2(10) 10_557 . ?
C4 C7 H7 118.9 10_557 . ?
C4 C7 H7 118.9 . . ?
N3 C8 N4 106.1(5) . . ?
N3 C8 H8 127.0 . . ?
N4 C8 H8 127.0 . . ?
N3 C9 C10 118.8(6) . . ?
N3 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N4 C10 C9 96.3(6) . . ?
N4 C10 H10 131.8 . . ?
C9 C10 H10 131.8 . . ?
C14 C11 C12 121.1(6) . . ?
C14 C11 N4 118.8(6) . . ?
C12 C11 N4 119.9(5) . . ?
C11 C12 C13 120.5(7) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C12 117.8(10) 10_557 . ?
C12 C13 H13 121.1 10_557 . ?
C12 C13 H13 121.1 . . ?
C11 C14 C11 118.7(8) . 10_557 ?
C11 C14 H14 120.6 . . ?
C11 C14 H14 120.6 10_557 . ?
Br1 Cu2 Br1 180.0 3_765 9_546 ?
Br1 Cu2 Br1 109.89(3) 3_765 2_645 ?
Br1 Cu2 Br1 70.11(4) 9_546 2_645 ?
Br1 Cu2 Br1 70.11(4) 3_765 7_756 ?
Br1 Cu2 Br1 109.89(4) 9_546 7_756 ?
Br1 Cu2 Br1 70.11(4) 2_645 7_756 ?
Br1 Cu2 Br1 70.11(4) 3_765 8_666 ?
Br1 Cu2 Br1 109.89(4) 9_546 8_666 ?
Br1 Cu2 Br1 180.0 2_645 8_666 ?
Br1 Cu2 Br1 109.89(4) 7_756 8_666 ?
Br1 Cu2 Br1 109.89(4) 3_765 . ?
Br1 Cu2 Br1 70.11(4) 9_546 . ?
Br1 Cu2 Br1 109.89(4) 2_645 . ?
Br1 Cu2 Br1 180.00(7) 7_756 . ?
Br1 Cu2 Br1 70.11(4) 8_666 . ?
Cu2 Br1 Br1 54.946(18) . 9_546 ?
Cu2 Br1 Br1 54.946(17) . 8_666 ?
Br1 Br1 Br1 90.90(8) 9_546 8_666 ?
C2 N1 C1 113.2(5) . . ?
C2 N1 Cu1 122.0(4) . . ?
C1 N1 Cu1 124.5(4) . . ?
C3 N2 C1 110.1(5) . . ?
C3 N2 C4 132.4(6) . . ?
C1 N2 C4 115.4(5) . . ?
C9 N3 C8 105.7(6) . . ?
C9 N3 Cu1 125.3(5) . . ?
C8 N3 Cu1 127.4(4) . . ?
C10 N4 C8 112.9(5) . . ?
C10 N4 C11 122.0(5) . . ?
C8 N4 C11 124.5(5) . . ?
H1A O1 H1B 111.00 . . ?
H2D O2 H2B 111.00 . . ?
O3 O3 H3B 69(10) 10_557 . ?
O3 O3 H3C 162(10) 10_557 . ?
H3B O3 H3C 109(10) . . ?
O3 O4 H4A 88(10) 10_557 . ?
O3 O4 H4B 163(10) 10_557 . ?
H4A O4 H4B 109(10) . . ?
W1 S1 Cu1 73.24(5) . . ?
W1 S2 Cu1 74.67(7) . 3_565 ?
W1 S2 Cu1 74.67(7) . . ?
Cu1 S2 Cu1 113.28(6) 3_565 . ?
W1 S2 Cu1 74.67(7) . 2_665 ?
Cu1 S2 Cu1 113.28(6) 3_565 2_665 ?
Cu1 S2 Cu1 113.28(6) . 2_665 ?
N3 Cu1 N1 100.97(19) . . ?
N3 Cu1 S2 110.89(14) . . ?
N1 Cu1 S2 114.65(14) . . ?
N3 Cu1 S1 114.92(15) . . ?
N1 Cu1 S1 113.29(14) . . ?
S2 Cu1 S1 102.62(8) . . ?
N3 Cu1 W1 127.99(14) . . ?
N1 Cu1 W1 131.01(13) . . ?
S2 Cu1 W1 51.18(7) . . ?
S1 Cu1 W1 51.44(4) . . ?
S2 W1 S1 109.46(4) . 3_565 ?
S2 W1 S1 109.46(4) . . ?
S1 W1 S1 109.48(4) 3_565 . ?
S2 W1 S1 109.46(4) . 2_665 ?
S1 W1 S1 109.48(4) 3_565 2_665 ?
S1 W1 S1 109.48(4) . 2_665 ?
S2 W1 Cu1 54.150(17) . 3_565 ?
S1 W1 Cu1 55.32(4) 3_565 3_565 ?
S1 W1 Cu1 125.80(4) . 3_565 ?
S1 W1 Cu1 124.71(4) 2_665 3_565 ?
S2 W1 Cu1 54.150(18) . 2_665 ?
S1 W1 Cu1 125.80(4) 3_565 2_665 ?
S1 W1 Cu1 124.71(4) . 2_665 ?
S1 W1 Cu1 55.32(4) 2_665 2_665 ?
Cu1 W1 Cu1 89.17(3) 3_565 2_665 ?
S2 W1 Cu1 54.150(18) . . ?
S1 W1 Cu1 124.71(4) 3_565 . ?
S1 W1 Cu1 55.32(4) . . ?
S1 W1 Cu1 125.80(4) 2_665 . ?
Cu1 W1 Cu1 89.17(3) 3_565 . ?
Cu1 W1 Cu1 89.17(3) 2_665 . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.548
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.103