# Electronic Supplementary Material (ESI) for Chemical Science.
# 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
#  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_st376

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H26 O5 S2'
_chemical_formula_weight         398.52

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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5289(5)
_cell_length_b                   10.9789(7)
_cell_length_c                   11.4493(7)
_cell_angle_alpha                87.759(5)
_cell_angle_beta                 72.017(5)
_cell_angle_gamma                78.159(5)
_cell_volume                     997.68(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2777
_cell_measurement_theta_min      3.4792
_cell_measurement_theta_max      32.3829

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9283
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9120
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         30.51
_reflns_number_total             6009
_reflns_number_gt                3438
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    4.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -94.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
  3 omega  -92.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000    0.0000 89

#__ type_ start__ end____ width___ exp.time_
  4 omega  -57.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  120.0000 97

;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0265P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6009
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0720
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_restrained_S_all      0.802
_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
S1 S 0.14396(6) 0.22220(4) 0.34388(4) 0.02143(11) Uani 1 1 d . . .
O1 O -0.26458(16) 0.54521(11) 0.32182(12) 0.0255(3) Uani 1 1 d . . .
H1O H -0.260(3) 0.575(2) 0.255(2) 0.062(8) Uiso 1 1 d . . .
O2 O 0.40571(18) 0.27028(12) 0.49692(12) 0.0307(3) Uani 1 1 d . . .
H2O H 0.367(3) 0.3281(18) 0.5411(18) 0.043(7) Uiso 1 1 d . . .
C1 C 0.1586(2) 0.38172(14) 0.34120(13) 0.0176(3) Uani 1 1 d . . .
C2 C 0.0249(2) 0.47536(14) 0.32924(13) 0.0187(4) Uani 1 1 d . . .
C3 C 0.0395(2) 0.59862(15) 0.33365(14) 0.0196(4) Uani 1 1 d . . .
H3 H -0.054(2) 0.6615(14) 0.3295(14) 0.019(4) Uiso 1 1 d . . .
C4 C 0.1813(2) 0.63171(14) 0.34769(14) 0.0214(4) Uani 1 1 d . . .
C5 C 0.3124(2) 0.53759(16) 0.35766(15) 0.0226(4) Uani 1 1 d . . .
H5 H 0.412(2) 0.5587(15) 0.3689(15) 0.029(5) Uiso 1 1 d . . .
C6 C 0.3031(2) 0.41254(15) 0.35534(14) 0.0198(4) Uani 1 1 d . . .
C7 C -0.1302(2) 0.44155(15) 0.31289(17) 0.0222(4) Uani 1 1 d . . .
H7A H -0.172(2) 0.3881(14) 0.3781(14) 0.016(4) Uiso 1 1 d . . .
H7B H -0.099(2) 0.3960(14) 0.2343(15) 0.019(4) Uiso 1 1 d . . .
C8 C 0.1945(3) 0.76595(18) 0.3530(2) 0.0318(5) Uani 1 1 d . . .
H8A H 0.307(4) 0.771(3) 0.339(3) 0.114(12) Uiso 1 1 d . . .
H8B H 0.139(4) 0.800(2) 0.426(3) 0.102(11) Uiso 1 1 d . . .
H8C H 0.159(3) 0.811(2) 0.300(2) 0.077(9) Uiso 1 1 d . . .
C9 C 0.4463(2) 0.31602(18) 0.37441(16) 0.0263(4) Uani 1 1 d . . .
H9A H 0.550(2) 0.3521(15) 0.3572(15) 0.029(5) Uiso 1 1 d . . .
H9B H 0.478(2) 0.2424(16) 0.3175(16) 0.035(5) Uiso 1 1 d . . .
S2 S 0.18377(6) 0.17859(4) 0.16120(4) 0.02398(11) Uani 1 1 d . . .
O11 O 0.2588(2) 0.34741(13) -0.10574(12) 0.0375(4) Uani 1 1 d . . .
H11O H 0.300(3) 0.2798(19) -0.126(2) 0.054(8) Uiso 1 1 d . . .
O12 O 0.62551(19) -0.11299(11) 0.18949(13) 0.0370(4) Uani 1 1 d . . .
H12O H 0.656(3) -0.1013(18) 0.2445(19) 0.041(7) Uiso 1 1 d . . .
C11 C 0.3994(2) 0.18479(14) 0.09447(14) 0.0189(4) Uani 1 1 d . . .
C12 C 0.4427(2) 0.28570(14) 0.02101(14) 0.0222(4) Uani 1 1 d . . .
C13 C 0.6113(3) 0.29044(16) -0.02791(16) 0.0273(4) Uani 1 1 d . . .
H13 H 0.640(2) 0.3583(15) -0.0783(15) 0.024(5) Uiso 1 1 d . . .
C14 C 0.7387(3) 0.20079(18) -0.00561(15) 0.0294(4) Uani 1 1 d . . .
C15 C 0.6917(3) 0.10121(17) 0.06561(15) 0.0265(4) Uani 1 1 d . . .
H15 H 0.778(2) 0.0413(14) 0.0788(14) 0.022(5) Uiso 1 1 d . . .
C16 C 0.5259(2) 0.09041(14) 0.11519(14) 0.0199(4) Uani 1 1 d . . .
C17 C 0.3140(3) 0.38547(16) -0.01088(17) 0.0282(4) Uani 1 1 d . . .
H17A H 0.214(2) 0.4130(15) 0.0616(16) 0.027(5) Uiso 1 1 d . . .
H17B H 0.362(3) 0.4563(17) -0.0410(17) 0.041(6) Uiso 1 1 d . . .
C18 C 0.9202(3) 0.2101(3) -0.0580(3) 0.0530(7) Uani 1 1 d . . .
H18A H 0.983(3) 0.180(2) -0.008(2) 0.068(8) Uiso 1 1 d . . .
H18B H 0.937(4) 0.295(3) -0.073(3) 0.112(12) Uiso 1 1 d . . .
H18C H 0.968(4) 0.162(3) -0.131(3) 0.128(13) Uiso 1 1 d . . .
C19 C 0.4810(3) -0.02074(16) 0.19059(17) 0.0262(4) Uani 1 1 d . . .
H19A H 0.409(2) -0.0603(15) 0.1576(15) 0.024(5) Uiso 1 1 d . . .
H19B H 0.417(2) 0.0065(16) 0.2767(17) 0.035(5) Uiso 1 1 d . . .
O21 O 0.2561(2) 0.09049(13) 0.62545(14) 0.0461(4) Uani 1 1 d . . .
H21O H 0.316(3) 0.135(2) 0.567(2) 0.081(9) Uiso 1 1 d . . .
C21 C 0.2323(4) -0.0186(2) 0.5790(3) 0.0488(7) Uani 1 1 d . . .
H21A H 0.198(3) -0.067(2) 0.643(2) 0.066(8) Uiso 1 1 d . . .
H21B H 0.338(4) -0.070(2) 0.533(2) 0.090(10) Uiso 1 1 d . . .
H21C H 0.164(3) 0.001(2) 0.528(2) 0.082(9) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.7796(16) . ?
S1 S2 2.0717(6) . ?
O1 C7 1.4217(19) . ?
O1 H1O 0.81(2) . ?
O2 C9 1.434(2) . ?
O2 H2O 0.78(2) . ?
C1 C6 1.399(2) . ?
C1 C2 1.407(2) . ?
C2 C3 1.388(2) . ?
C2 C7 1.510(2) . ?
C3 C4 1.388(2) . ?
C3 H3 0.951(15) . ?
C4 C5 1.388(2) . ?
C4 C8 1.506(3) . ?
C5 C6 1.393(2) . ?
C5 H5 0.970(18) . ?
C6 C9 1.509(2) . ?
C7 H7A 0.958(16) . ?
C7 H7B 0.982(16) . ?
C8 H8A 0.93(3) . ?
C8 H8B 0.87(3) . ?
C8 H8C 0.86(2) . ?
C9 H9A 1.00(2) . ?
C9 H9B 0.998(18) . ?
S2 C11 1.7751(18) . ?
O11 C17 1.417(2) . ?
O11 H11O 0.77(2) . ?
O12 C19 1.422(2) . ?
O12 H12O 0.777(19) . ?
C11 C16 1.405(2) . ?
C11 C12 1.405(2) . ?
C12 C13 1.384(3) . ?
C12 C17 1.504(2) . ?
C13 C14 1.389(2) . ?
C13 H13 0.950(16) . ?
C14 C15 1.389(3) . ?
C14 C18 1.501(3) . ?
C15 C16 1.380(3) . ?
C15 H15 0.926(15) . ?
C16 C19 1.512(2) . ?
C17 H17A 0.992(18) . ?
C17 H17B 0.96(2) . ?
C18 H18A 0.91(2) . ?
C18 H18B 0.97(3) . ?
C18 H18C 0.94(3) . ?
C19 H19A 0.984(18) . ?
C19 H19B 0.991(19) . ?
O21 C21 1.405(3) . ?
O21 H21O 0.90(3) . ?
C21 H21A 0.89(2) . ?
C21 H21B 0.96(3) . ?
C21 H21C 0.94(2) . ?

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
C1 S1 S2 103.31(5) . . ?
C7 O1 H1O 111.4(16) . . ?
C9 O2 H2O 106.8(15) . . ?
C6 C1 C2 120.63(14) . . ?
C6 C1 S1 118.76(11) . . ?
C2 C1 S1 120.57(13) . . ?
C3 C2 C1 118.22(16) . . ?
C3 C2 C7 121.36(14) . . ?
C1 C2 C7 120.42(14) . . ?
C4 C3 C2 122.29(15) . . ?
C4 C3 H3 119.9(10) . . ?
C2 C3 H3 117.8(10) . . ?
C5 C4 C3 118.39(15) . . ?
C5 C4 C8 120.08(18) . . ?
C3 C4 C8 121.53(17) . . ?
C4 C5 C6 121.53(17) . . ?
C4 C5 H5 119.7(10) . . ?
C6 C5 H5 118.7(10) . . ?
C5 C6 C1 118.93(15) . . ?
C5 C6 C9 118.35(16) . . ?
C1 C6 C9 122.65(15) . . ?
O1 C7 C2 113.83(14) . . ?
O1 C7 H7A 105.8(10) . . ?
C2 C7 H7A 108.1(10) . . ?
O1 C7 H7B 111.0(9) . . ?
C2 C7 H7B 109.3(10) . . ?
H7A C7 H7B 108.7(13) . . ?
C4 C8 H8A 109.8(18) . . ?
C4 C8 H8B 111.4(19) . . ?
H8A C8 H8B 106(2) . . ?
C4 C8 H8C 113.5(17) . . ?
H8A C8 H8C 107(2) . . ?
H8B C8 H8C 108(2) . . ?
O2 C9 C6 111.92(15) . . ?
O2 C9 H9A 109.2(9) . . ?
C6 C9 H9A 110.1(9) . . ?
O2 C9 H9B 107.0(10) . . ?
C6 C9 H9B 112.4(10) . . ?
H9A C9 H9B 106.1(15) . . ?
C11 S2 S1 101.84(5) . . ?
C17 O11 H11O 111.5(16) . . ?
C19 O12 H12O 109.9(15) . . ?
C16 C11 C12 120.13(17) . . ?
C16 C11 S2 120.57(12) . . ?
C12 C11 S2 119.29(12) . . ?
C13 C12 C11 118.48(15) . . ?
C13 C12 C17 118.81(16) . . ?
C11 C12 C17 122.66(18) . . ?
C12 C13 C14 122.68(17) . . ?
C12 C13 H13 118.3(11) . . ?
C14 C13 H13 119.0(11) . . ?
C13 C14 C15 117.31(19) . . ?
C13 C14 C18 121.32(19) . . ?
C15 C14 C18 121.36(19) . . ?
C16 C15 C14 122.60(17) . . ?
C16 C15 H15 120.8(11) . . ?
C14 C15 H15 116.6(11) . . ?
C15 C16 C11 118.74(15) . . ?
C15 C16 C19 120.68(15) . . ?
C11 C16 C19 120.57(17) . . ?
O11 C17 C12 112.77(14) . . ?
O11 C17 H17A 108.4(10) . . ?
C12 C17 H17A 111.6(9) . . ?
O11 C17 H17B 105.9(11) . . ?
C12 C17 H17B 109.7(12) . . ?
H17A C17 H17B 108.2(15) . . ?
C14 C18 H18A 113.2(15) . . ?
C14 C18 H18B 113.7(19) . . ?
H18A C18 H18B 105(2) . . ?
C14 C18 H18C 109(2) . . ?
H18A C18 H18C 106(2) . . ?
H18B C18 H18C 110(3) . . ?
O12 C19 C16 112.42(17) . . ?
O12 C19 H19A 107.3(9) . . ?
C16 C19 H19A 110.0(9) . . ?
O12 C19 H19B 109.0(10) . . ?
C16 C19 H19B 109.8(10) . . ?
H19A C19 H19B 108.1(15) . . ?
C21 O21 H21O 113.0(17) . . ?
O21 C21 H21A 107.7(16) . . ?
O21 C21 H21B 111.2(17) . . ?
H21A C21 H21B 101(2) . . ?
O21 C21 H21C 110.5(15) . . ?
H21A C21 H21C 117(2) . . ?
H21B C21 H21C 109(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O21 H21O O2 0.90(3) 1.85(3) 2.709(2) 158(2) .
O11 H11O O12 0.77(2) 1.90(2) 2.6615(18) 171(2) 2_655
O12 H12O O21 0.777(19) 1.878(19) 2.6520(19) 174(2) 2_656
O2 H2O O1 0.78(2) 2.00(2) 2.7649(18) 170(2) 2_566
O1 H1O O11 0.81(2) 1.88(2) 2.6895(18) 176(2) 2_565

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 948576'
#######################################################################
#
#                 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_ec88

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H9 Cl2 S'
_chemical_formula_weight         220.12

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   16.8843(16)
_cell_length_b                   7.6695(4)
_cell_length_c                   16.974(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.956(15)
_cell_angle_gamma                90.00
_cell_volume                     1976.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3027
_cell_measurement_theta_min      3.4747
_cell_measurement_theta_max      32.4257

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5099
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_process_details   
; 
'Wed Jul 04 08:47:01 2012' 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9370
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         28.28
_reflns_number_total             4674
_reflns_number_gt                3746
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -100.00   -5.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -37.0000 -180.0000 63

#__ type_ start__ end____ width___ exp.time_
  2 omega  -27.00   28.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364   57.0000    0.0000 37

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00  -18.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -74.0000   29.0000 20

#__ type_ start__ end____ width___ exp.time_
  4 omega  -53.00    7.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364   37.0000 -150.0000 40

;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0353P)²+1.5994P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4674
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.003

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
S1 S 0.75963(4) 0.35720(8) 0.86836(4) 0.02545(15) Uani 1 1 d . . .
S2 S 0.85010(4) 0.19375(9) 0.85460(5) 0.02931(16) Uani 1 1 d . . .
Cl1 Cl 0.61319(4) 0.15564(9) 0.94340(4) 0.03290(16) Uani 1 1 d . . .
Cl2 Cl 0.63640(5) 0.74410(8) 0.70874(6) 0.0415(2) Uani 1 1 d . . .
Cl11 Cl 0.81344(5) -0.11192(9) 0.64417(7) 0.0500(2) Uani 1 1 d . . .
Cl12 Cl 0.92053(5) 0.69969(9) 0.89314(5) 0.03742(17) Uani 1 1 d . . .
C1 C 0.66048(14) 0.2980(3) 0.77604(16) 0.0184(4) Uani 1 1 d . . .
C2 C 0.60990(15) 0.1561(3) 0.78084(16) 0.0196(5) Uani 1 1 d . . .
C3 C 0.53337(16) 0.1111(3) 0.70715(18) 0.0231(5) Uani 1 1 d . . .
H3 H 0.4986(15) 0.023(3) 0.7119(16) 0.016(6) Uiso 1 1 d . . .
C4 C 0.50610(15) 0.1997(3) 0.62787(17) 0.0243(5) Uani 1 1 d . . .
C5 C 0.55670(16) 0.3403(3) 0.62477(17) 0.0232(5) Uani 1 1 d . . .
H5 H 0.5371(18) 0.408(4) 0.571(2) 0.032(8) Uiso 1 1 d . . .
C6 C 0.63298(15) 0.3923(3) 0.69724(16) 0.0203(5) Uani 1 1 d . . .
C7 C 0.63767(18) 0.0475(3) 0.86167(18) 0.0259(5) Uani 1 1 d . . .
H7A H 0.6049(19) -0.061(4) 0.848(2) 0.039(8) Uiso 1 1 d . . .
H7B H 0.7005(18) 0.021(3) 0.8894(19) 0.026(7) Uiso 1 1 d . . .
C8 C 0.68226(18) 0.5477(3) 0.6885(2) 0.0247(5) Uani 1 1 d . . .
H8A H 0.7436(19) 0.549(3) 0.7268(19) 0.028(7) Uiso 1 1 d . . .
H8B H 0.6754(18) 0.555(4) 0.631(2) 0.028(7) Uiso 1 1 d . . .
C9 C 0.4241(2) 0.1466(5) 0.5483(2) 0.0405(7) Uani 1 1 d . . .
H9A H 0.436(3) 0.053(6) 0.522(3) 0.087(15) Uiso 1 1 d . . .
H9B H 0.381(3) 0.108(7) 0.557(3) 0.102(18) Uiso 1 1 d . . .
H9C H 0.400(3) 0.234(7) 0.509(4) 0.118(19) Uiso 1 1 d . . .
C11 C 0.86872(14) 0.2950(3) 0.76963(16) 0.0183(5) Uani 1 1 d . . .
C12 C 0.82514(14) 0.2330(3) 0.68338(17) 0.0196(5) Uani 1 1 d . . .
C13 C 0.83954(15) 0.3162(3) 0.61760(17) 0.0207(5) Uani 1 1 d . . .
H13 H 0.8098(16) 0.278(3) 0.5603(18) 0.018(6) Uiso 1 1 d . . .
C14 C 0.89601(14) 0.4579(3) 0.63532(16) 0.0198(5) Uani 1 1 d . . .
C15 C 0.93961(14) 0.5146(3) 0.72086(16) 0.0183(4) Uani 1 1 d . . .
H15 H 0.9779(18) 0.605(4) 0.7322(19) 0.029(7) Uiso 1 1 d . . .
C16 C 0.92729(14) 0.4367(3) 0.78911(15) 0.0177(4) Uani 1 1 d . . .
C17 C 0.76241(17) 0.0815(3) 0.6574(2) 0.0285(6) Uani 1 1 d . . .
H17A H 0.7436(19) 0.058(4) 0.700(2) 0.035(8) Uiso 1 1 d . . .
H17B H 0.715(2) 0.106(4) 0.605(3) 0.054(11) Uiso 1 1 d . . .
C18 C 0.97629(17) 0.5105(3) 0.87882(18) 0.0259(5) Uani 1 1 d . . .
H18A H 1.0317(18) 0.553(3) 0.8894(18) 0.022(7) Uiso 1 1 d . . .
H18B H 0.9815(17) 0.433(4) 0.921(2) 0.026(7) Uiso 1 1 d . . .
C19 C 0.9076(2) 0.5483(4) 0.5624(2) 0.0294(6) Uani 1 1 d . . .
H19A H 0.855(3) 0.564(6) 0.514(3) 0.084(14) Uiso 1 1 d . . .
H19B H 0.936(4) 0.639(7) 0.575(4) 0.12(2) Uiso 1 1 d . . .
H19C H 0.937(3) 0.490(6) 0.542(3) 0.074(13) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.780(2) . ?
S1 S2 2.0668(9) . ?
S2 C11 1.783(2) . ?
Cl1 C7 1.812(3) . ?
Cl2 C8 1.794(2) . ?
Cl11 C17 1.778(3) . ?
Cl12 C18 1.803(3) . ?
C1 C2 1.408(3) . ?
C1 C6 1.409(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.494(3) . ?
C3 C4 1.394(4) . ?
C3 H3 0.92(2) . ?
C4 C5 1.391(3) . ?
C4 C9 1.507(4) . ?
C5 C6 1.394(4) . ?
C5 H5 0.97(3) . ?
C6 C8 1.498(3) . ?
C7 H7A 0.97(3) . ?
C7 H7B 0.97(3) . ?
C8 H8A 0.95(3) . ?
C8 H8B 0.93(3) . ?
C9 H9A 0.91(5) . ?
C9 H9B 0.85(5) . ?
C9 H9C 0.91(6) . ?
C11 C12 1.403(3) . ?
C11 C16 1.408(3) . ?
C12 C13 1.396(3) . ?
C12 C17 1.503(3) . ?
C13 C14 1.389(3) . ?
C13 H13 0.93(3) . ?
C14 C15 1.380(3) . ?
C14 C19 1.504(4) . ?
C15 C16 1.398(3) . ?
C15 H15 0.91(3) . ?
C16 C18 1.490(3) . ?
C17 H17A 0.92(3) . ?
C17 H17B 0.92(4) . ?
C18 H18A 0.93(3) . ?
C18 H18B 0.91(3) . ?
C19 H19A 0.91(5) . ?
C19 H19B 0.82(6) . ?
C19 H19C 0.85(5) . ?

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
C1 S1 S2 101.68(8) . . ?
C11 S2 S1 103.18(7) . . ?
C2 C1 C6 119.7(2) . . ?
C2 C1 S1 120.47(18) . . ?
C6 C1 S1 119.80(17) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 C7 118.8(2) . . ?
C1 C2 C7 122.0(2) . . ?
C2 C3 C4 122.1(2) . . ?
C2 C3 H3 118.6(15) . . ?
C4 C3 H3 119.2(16) . . ?
C5 C4 C3 117.8(2) . . ?
C5 C4 C9 120.9(3) . . ?
C3 C4 C9 121.3(3) . . ?
C4 C5 C6 122.3(2) . . ?
C4 C5 H5 119.2(17) . . ?
C6 C5 H5 118.5(17) . . ?
C5 C6 C1 119.0(2) . . ?
C5 C6 C8 118.6(2) . . ?
C1 C6 C8 122.4(2) . . ?
C2 C7 Cl1 111.29(17) . . ?
C2 C7 H7A 110.3(19) . . ?
Cl1 C7 H7A 105.9(19) . . ?
C2 C7 H7B 113.4(16) . . ?
Cl1 C7 H7B 106.7(17) . . ?
H7A C7 H7B 109(2) . . ?
C6 C8 Cl2 110.16(16) . . ?
C6 C8 H8A 115.2(17) . . ?
Cl2 C8 H8A 107.1(17) . . ?
C6 C8 H8B 109.3(18) . . ?
Cl2 C8 H8B 106.5(17) . . ?
H8A C8 H8B 108(2) . . ?
C4 C9 H9A 110(3) . . ?
C4 C9 H9B 117(4) . . ?
H9A C9 H9B 101(4) . . ?
C4 C9 H9C 114(3) . . ?
H9A C9 H9C 111(4) . . ?
H9B C9 H9C 104(4) . . ?
C12 C11 C16 120.0(2) . . ?
C12 C11 S2 119.94(17) . . ?
C16 C11 S2 120.04(18) . . ?
C13 C12 C11 119.0(2) . . ?
C13 C12 C17 117.8(2) . . ?
C11 C12 C17 123.3(2) . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 118.8(16) . . ?
C12 C13 H13 119.3(16) . . ?
C15 C14 C13 118.3(2) . . ?
C15 C14 C19 121.3(2) . . ?
C13 C14 C19 120.4(2) . . ?
C14 C15 C16 122.2(2) . . ?
C14 C15 H15 117.7(19) . . ?
C16 C15 H15 120.1(19) . . ?
C15 C16 C11 118.6(2) . . ?
C15 C16 C18 117.9(2) . . ?
C11 C16 C18 123.5(2) . . ?
C12 C17 Cl11 111.34(17) . . ?
C12 C17 H17A 111(2) . . ?
Cl11 C17 H17A 106.7(19) . . ?
C12 C17 H17B 109(2) . . ?
Cl11 C17 H17B 108(2) . . ?
H17A C17 H17B 110(3) . . ?
C16 C18 Cl12 110.75(18) . . ?
C16 C18 H18A 113.0(17) . . ?
Cl12 C18 H18A 103.6(16) . . ?
C16 C18 H18B 112.4(18) . . ?
Cl12 C18 H18B 107.0(17) . . ?
H18A C18 H18B 110(2) . . ?
C14 C19 H19A 112(3) . . ?
C14 C19 H19B 117(4) . . ?
H19A C19 H19B 111(4) . . ?
C14 C19 H19C 114(3) . . ?
H19A C19 H19C 102(4) . . ?
H19B C19 H19C 99(4) . . ?

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 948575'
#######################################################################
#
#                 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_st450

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H29 Cu2 F6 N4 O7 S3'
_chemical_formula_weight         834.78

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8541(6)
_cell_length_b                   11.4575(8)
_cell_length_c                   15.9521(13)
_cell_angle_alpha                93.504(6)
_cell_angle_beta                 98.701(6)
_cell_angle_gamma                114.179(7)
_cell_volume                     1608.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6890
_cell_measurement_theta_min      3.3434
_cell_measurement_theta_max      32.4763

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 0 0 0.0557 -1.0000 -0.0000 -0.0000 -0.0046 -0.0783 -0.0178
0 1 0 0.1039 -0.0000 1.0000 -0.0000 0.0537 0.0180 0.0385
0 -1 1 0.1159 0.0000 -1.0000 1.0000 -0.0269 -0.0029 -0.0719
0 -1 0 0.0928 0.0000 -1.0000 0.0000 -0.0537 -0.0180 -0.0385
0 -1 -1 0.1573 0.0000 -1.0000 -1.0000 -0.0805 -0.0330 -0.0052
1 0 1 0.0701 1.0000 0.0000 1.0000 0.0314 0.0934 -0.0156
1 0 -1 0.1207 1.0000 -0.0000 -1.0000 -0.0223 0.0633 0.0512
0 1 -1 0.1029 -0.0000 1.0000 -1.0000 0.0269 0.0029 0.0719
1 0 0 0.0881 1.0000 0.0000 0.0000 0.0046 0.0783 0.0178
-1 1 1 0.2085 -1.0000 1.0000 1.0000 0.0760 -0.0453 -0.0126
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             846
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5194
_exptl_absorpt_correction_T_max  0.8023
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19709
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         30.51
_reflns_number_total             9796
_reflns_number_gt                7872
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -2.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   77.0000   60.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000  -60.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega  -21.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega  -24.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
  5 omega  -96.00  -20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -57.0000 -180.0000 76

#__ type_ start__ end____ width___ exp.time_
  6 omega   -6.00   42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   57.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
  7 omega  -96.00  -22.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -57.0000  -90.0000 74

;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0367P)²+0.4284P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9796
_refine_ls_number_parameters     540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0783
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.75417(3) 0.41415(2) 0.202602(14) 0.01696(6) Uani 1 1 d . . .
Cu2 Cu 0.60208(3) 0.45330(2) 0.309601(14) 0.01791(6) Uani 1 1 d . . .
S1 S 0.63490(5) 0.53793(5) 0.19217(3) 0.01792(9) Uani 1 1 d . . .
O1 O 0.99258(19) 0.53398(17) 0.25142(13) 0.0279(3) Uani 1 1 d . . .
H1O H 1.044(3) 0.592(3) 0.2289(17) 0.031(7) Uiso 1 1 d . . .
H2O H 1.003(3) 0.561(3) 0.2927(19) 0.033(9) Uiso 1 1 d . . .
N1 N 0.72232(18) 0.35185(15) 0.07407(10) 0.0178(3) Uani 1 1 d . . .
N2 N 0.38105(19) 0.42703(16) 0.30983(10) 0.0187(3) Uani 1 1 d . . .
N3 N 0.77869(19) 0.25356(16) 0.21725(10) 0.0194(3) Uani 1 1 d . . .
N4 N 0.56195(19) 0.32288(16) 0.38754(10) 0.0200(3) Uani 1 1 d . . .
C1 C 0.4642(2) 0.41962(19) 0.12429(12) 0.0181(4) Uani 1 1 d . . .
C2 C 0.4724(2) 0.36251(19) 0.04595(12) 0.0188(4) Uani 1 1 d . . .
C3 C 0.3392(2) 0.2760(2) -0.00854(13) 0.0228(4) Uani 1 1 d . . .
H3 H 0.345(3) 0.238(2) -0.0604(16) 0.026(6) Uiso 1 1 d . . .
C4 C 0.1978(2) 0.2422(2) 0.01367(13) 0.0248(4) Uani 1 1 d . . .
C5 C 0.1938(2) 0.2971(2) 0.09308(14) 0.0242(4) Uani 1 1 d . . .
H5 H 0.100(3) 0.274(2) 0.1087(16) 0.031(7) Uiso 1 1 d . . .
C6 C 0.3233(2) 0.3867(2) 0.14832(12) 0.0205(4) Uani 1 1 d . . .
C7 C 0.6216(2) 0.3954(2) 0.01822(12) 0.0193(4) Uani 1 1 d . . .
H7A H 0.677(3) 0.488(2) 0.0202(14) 0.016(5) Uiso 1 1 d . . .
H7B H 0.603(2) 0.356(2) -0.0373(15) 0.016(5) Uiso 1 1 d . . .
C8 C 0.3071(2) 0.4521(2) 0.22922(13) 0.0230(4) Uani 1 1 d . . .
H8A H 0.204(3) 0.424(2) 0.2279(15) 0.025(6) Uiso 1 1 d . . .
H8B H 0.352(2) 0.546(2) 0.2289(13) 0.015(5) Uiso 1 1 d . . .
C9 C 0.0542(3) 0.1538(3) -0.04754(18) 0.0357(5) Uani 1 1 d . . .
H9A H 0.060(3) 0.079(3) -0.0682(19) 0.046(8) Uiso 1 1 d . . .
H9B H 0.034(4) 0.189(3) -0.096(2) 0.068(11) Uiso 1 1 d . . .
H9C H -0.035(4) 0.129(4) -0.024(2) 0.076(12) Uiso 1 1 d . . .
C10 C 0.6561(2) 0.2091(2) 0.06828(13) 0.0214(4) Uani 1 1 d . . .
H10A H 0.549(3) 0.175(2) 0.0698(14) 0.022(6) Uiso 1 1 d . . .
H10B H 0.665(3) 0.168(2) 0.0153(16) 0.027(6) Uiso 1 1 d . . .
C11 C 0.7303(2) 0.17005(19) 0.14398(13) 0.0204(4) Uani 1 1 d . . .
C12 C 0.7432(3) 0.0545(2) 0.14045(15) 0.0280(5) Uani 1 1 d . . .
H12 H 0.703(3) -0.002(2) 0.0895(16) 0.028(6) Uiso 1 1 d . . .
C13 C 0.8061(3) 0.0228(2) 0.21431(16) 0.0343(5) Uani 1 1 d . . .
H13 H 0.814(3) -0.054(3) 0.2118(18) 0.041(8) Uiso 1 1 d . . .
C14 C 0.8588(3) 0.1091(2) 0.28842(15) 0.0307(5) Uani 1 1 d . . .
H14 H 0.902(3) 0.096(3) 0.3377(17) 0.038(7) Uiso 1 1 d . . .
C15 C 0.8442(2) 0.2238(2) 0.28758(14) 0.0240(4) Uani 1 1 d . . .
H15 H 0.886(3) 0.288(2) 0.3357(15) 0.020(6) Uiso 1 1 d . . .
C16 C 0.3083(2) 0.2896(2) 0.32258(14) 0.0231(4) Uani 1 1 d . . .
H16A H 0.292(3) 0.239(2) 0.2674(15) 0.022(6) Uiso 1 1 d . . .
H16B H 0.210(3) 0.269(3) 0.3404(17) 0.039(7) Uiso 1 1 d . . .
C17 C 0.4132(2) 0.26094(19) 0.38882(12) 0.0206(4) Uani 1 1 d . . .
C18 C 0.3609(3) 0.1763(2) 0.44722(14) 0.0275(4) Uani 1 1 d . . .
H18 H 0.256(3) 0.139(2) 0.4466(15) 0.026(6) Uiso 1 1 d . . .
C19 C 0.4650(3) 0.1540(2) 0.50520(15) 0.0312(5) Uani 1 1 d . . .
H19 H 0.430(3) 0.097(2) 0.5465(16) 0.030(7) Uiso 1 1 d . . .
C20 C 0.6178(3) 0.2181(2) 0.50388(14) 0.0288(5) Uani 1 1 d . . .
H20 H 0.682(3) 0.209(3) 0.5424(18) 0.042(8) Uiso 1 1 d . . .
C21 C 0.6624(3) 0.3025(2) 0.44508(13) 0.0236(4) Uani 1 1 d . . .
H21 H 0.767(3) 0.354(2) 0.4458(14) 0.021(6) Uiso 1 1 d . . .
C22 C 0.8713(3) 0.4016(2) 0.04857(15) 0.0266(4) Uani 1 1 d . . .
H22A H 0.912(3) 0.496(2) 0.0540(14) 0.024(6) Uiso 1 1 d . . .
H22B H 0.933(3) 0.378(2) 0.0839(15) 0.023(6) Uiso 1 1 d . . .
H22C H 0.862(3) 0.372(2) -0.0088(16) 0.028(6) Uiso 1 1 d . . .
C23 C 0.3722(3) 0.5102(2) 0.38179(14) 0.0261(4) Uani 1 1 d . . .
H23A H 0.266(3) 0.494(2) 0.3790(14) 0.022(6) Uiso 1 1 d . . .
H23B H 0.431(3) 0.592(3) 0.3747(17) 0.036(7) Uiso 1 1 d . . .
H23C H 0.412(3) 0.491(2) 0.4328(16) 0.028(6) Uiso 1 1 d . . .
S2 S 0.89770(6) 0.67729(5) 0.44791(3) 0.02249(10) Uani 1 1 d . . .
F1S2 F 0.9258(2) 0.78963(16) 0.30946(10) 0.0512(4) Uani 1 1 d . . .
F2S2 F 1.1048(2) 0.89235(17) 0.41815(13) 0.0673(6) Uani 1 1 d . . .
F3S2 F 0.8875(2) 0.89325(17) 0.41362(13) 0.0641(5) Uani 1 1 d . . .
O1S2 O 0.73621(17) 0.61280(15) 0.41509(10) 0.0292(3) Uani 1 1 d . . .
O2S2 O 0.98286(19) 0.61061(17) 0.41969(10) 0.0335(4) Uani 1 1 d . . .
O3S2 O 0.9385(2) 0.72814(17) 0.53697(10) 0.0360(4) Uani 1 1 d . . .
C2S C 0.9569(3) 0.8208(2) 0.39444(17) 0.0368(5) Uani 1 1 d . . .
S3 S 0.32832(7) 0.80637(6) 0.20597(4) 0.03072(12) Uani 1 1 d . . .
F1S3 F 0.2209(2) 0.97400(17) 0.24344(15) 0.0662(6) Uani 1 1 d . . .
F2S3 F 0.3145(2) 0.99718(18) 0.12870(13) 0.0670(5) Uani 1 1 d . . .
F3S3 F 0.46217(19) 1.05622(15) 0.25360(12) 0.0581(5) Uani 1 1 d . . .
O1S3 O 0.1738(2) 0.72262(16) 0.16410(11) 0.0370(4) Uani 1 1 d . . .
O2S3 O 0.4398(2) 0.81308(19) 0.15681(14) 0.0525(5) Uani 1 1 d . . .
O3S3 O 0.3628(3) 0.7942(2) 0.29476(12) 0.0625(6) Uani 1 1 d . . .
C3S C 0.3311(3) 0.9662(2) 0.20858(19) 0.0412(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N3 1.9744(16) . ?
Cu1 N1 2.0627(16) . ?
Cu1 O1 2.1643(17) . ?
Cu1 S1 2.1806(5) . ?
Cu1 Cu2 2.5674(4) . ?
Cu2 N4 1.9562(17) . ?
Cu2 N2 2.0737(16) . ?
Cu2 S1 2.1686(5) . ?
Cu2 O1S2 2.2115(15) . ?
S1 C1 1.800(2) . ?
O1 H1O 0.80(3) . ?
O1 H2O 0.68(3) . ?
N1 C22 1.473(3) . ?
N1 C10 1.483(3) . ?
N1 C7 1.490(2) . ?
N2 C16 1.481(3) . ?
N2 C23 1.483(3) . ?
N2 C8 1.483(3) . ?
N3 C15 1.342(3) . ?
N3 C11 1.353(3) . ?
N4 C17 1.346(3) . ?
N4 C21 1.348(3) . ?
C1 C6 1.403(3) . ?
C1 C2 1.404(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.504(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.93(2) . ?
C4 C5 1.393(3) . ?
C4 C9 1.506(3) . ?
C5 C6 1.391(3) . ?
C5 H5 0.93(3) . ?
C6 C8 1.515(3) . ?
C7 H7A 0.97(2) . ?
C7 H7B 0.92(2) . ?
C8 H8A 0.93(3) . ?
C8 H8B 0.99(2) . ?
C9 H9A 0.93(3) . ?
C9 H9B 0.92(4) . ?
C9 H9C 0.95(4) . ?
C10 C11 1.503(3) . ?
C10 H10A 0.97(2) . ?
C10 H10B 0.97(2) . ?
C11 C12 1.380(3) . ?
C12 C13 1.386(3) . ?
C12 H12 0.93(3) . ?
C13 C14 1.377(3) . ?
C13 H13 0.91(3) . ?
C14 C15 1.380(3) . ?
C14 H14 0.89(3) . ?
C15 H15 0.94(2) . ?
C16 C17 1.511(3) . ?
C16 H16A 0.98(2) . ?
C16 H16B 0.99(3) . ?
C17 C18 1.386(3) . ?
C18 C19 1.389(3) . ?
C18 H18 0.94(3) . ?
C19 C20 1.383(4) . ?
C19 H19 0.96(3) . ?
C20 C21 1.377(3) . ?
C20 H20 0.86(3) . ?
C21 H21 0.96(2) . ?
C22 H22A 0.98(2) . ?
C22 H22B 0.90(3) . ?
C22 H22C 0.93(2) . ?
C23 H23A 0.98(2) . ?
C23 H23B 0.90(3) . ?
C23 H23C 0.93(3) . ?
S2 O3S2 1.4330(16) . ?
S2 O2S2 1.4451(17) . ?
S2 O1S2 1.4456(16) . ?
S2 C2S 1.819(3) . ?
F1S2 C2S 1.336(3) . ?
F2S2 C2S 1.326(3) . ?
F3S2 C2S 1.322(3) . ?
S3 O2S3 1.423(2) . ?
S3 O3S3 1.435(2) . ?
S3 O1S3 1.4499(18) . ?
S3 C3S 1.818(3) . ?
F1S3 C3S 1.324(3) . ?
F2S3 C3S 1.348(3) . ?
F3S3 C3S 1.336(3) . ?

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
N3 Cu1 N1 83.54(6) . . ?
N3 Cu1 O1 92.49(7) . . ?
N1 Cu1 O1 109.35(7) . . ?
N3 Cu1 S1 156.55(5) . . ?
N1 Cu1 S1 98.51(5) . . ?
O1 Cu1 S1 108.57(5) . . ?
N3 Cu1 Cu2 110.63(5) . . ?
N1 Cu1 Cu2 138.77(5) . . ?
O1 Cu1 Cu2 108.46(5) . . ?
S1 Cu1 Cu2 53.604(15) . . ?
N4 Cu2 N2 84.81(7) . . ?
N4 Cu2 S1 159.31(5) . . ?
N2 Cu2 S1 99.61(5) . . ?
N4 Cu2 O1S2 92.51(7) . . ?
N2 Cu2 O1S2 103.17(6) . . ?
S1 Cu2 O1S2 105.95(5) . . ?
N4 Cu2 Cu1 109.85(5) . . ?
N2 Cu2 Cu1 137.82(5) . . ?
S1 Cu2 Cu1 54.038(15) . . ?
O1S2 Cu2 Cu1 114.93(4) . . ?
C1 S1 Cu2 97.40(6) . . ?
C1 S1 Cu1 95.90(6) . . ?
Cu2 S1 Cu1 72.358(17) . . ?
Cu1 O1 H1O 124(2) . . ?
Cu1 O1 H2O 110(2) . . ?
H1O O1 H2O 105(3) . . ?
C22 N1 C10 110.76(16) . . ?
C22 N1 C7 108.56(16) . . ?
C10 N1 C7 111.39(16) . . ?
C22 N1 Cu1 108.40(13) . . ?
C10 N1 Cu1 104.09(12) . . ?
C7 N1 Cu1 113.58(11) . . ?
C16 N2 C23 110.11(16) . . ?
C16 N2 C8 111.94(17) . . ?
C23 N2 C8 108.00(16) . . ?
C16 N2 Cu2 101.55(12) . . ?
C23 N2 Cu2 111.90(13) . . ?
C8 N2 Cu2 113.28(12) . . ?
C15 N3 C11 118.64(17) . . ?
C15 N3 Cu1 128.08(14) . . ?
C11 N3 Cu1 113.13(13) . . ?
C17 N4 C21 118.95(18) . . ?
C17 N4 Cu2 112.00(13) . . ?
C21 N4 Cu2 128.38(15) . . ?
C6 C1 C2 120.00(18) . . ?
C6 C1 S1 120.41(14) . . ?
C2 C1 S1 119.57(15) . . ?
C3 C2 C1 119.41(18) . . ?
C3 C2 C7 119.14(17) . . ?
C1 C2 C7 121.42(18) . . ?
C4 C3 C2 121.66(19) . . ?
C4 C3 H3 119.3(15) . . ?
C2 C3 H3 119.0(15) . . ?
C5 C4 C3 117.56(19) . . ?
C5 C4 C9 121.3(2) . . ?
C3 C4 C9 121.1(2) . . ?
C6 C5 C4 122.7(2) . . ?
C6 C5 H5 119.2(16) . . ?
C4 C5 H5 118.1(16) . . ?
C5 C6 C1 118.59(18) . . ?
C5 C6 C8 119.22(18) . . ?
C1 C6 C8 122.05(18) . . ?
N1 C7 C2 112.51(15) . . ?
N1 C7 H7A 106.5(14) . . ?
C2 C7 H7A 111.2(13) . . ?
N1 C7 H7B 109.1(14) . . ?
C2 C7 H7B 108.6(14) . . ?
H7A C7 H7B 108.9(18) . . ?
N2 C8 C6 114.67(16) . . ?
N2 C8 H8A 110.3(15) . . ?
C6 C8 H8A 107.0(15) . . ?
N2 C8 H8B 107.2(13) . . ?
C6 C8 H8B 109.3(12) . . ?
H8A C8 H8B 108(2) . . ?
C4 C9 H9A 111.0(19) . . ?
C4 C9 H9B 114(2) . . ?
H9A C9 H9B 105(3) . . ?
C4 C9 H9C 115(2) . . ?
H9A C9 H9C 107(3) . . ?
H9B C9 H9C 105(3) . . ?
N1 C10 C11 109.96(16) . . ?
N1 C10 H10A 110.4(14) . . ?
C11 C10 H10A 107.0(14) . . ?
N1 C10 H10B 112.6(14) . . ?
C11 C10 H10B 110.0(15) . . ?
H10A C10 H10B 107(2) . . ?
N3 C11 C12 121.81(19) . . ?
N3 C11 C10 115.57(17) . . ?
C12 C11 C10 122.58(19) . . ?
C11 C12 C13 119.0(2) . . ?
C11 C12 H12 118.5(16) . . ?
C13 C12 H12 122.3(16) . . ?
C14 C13 C12 119.2(2) . . ?
C14 C13 H13 122.1(18) . . ?
C12 C13 H13 118.6(18) . . ?
C13 C14 C15 119.0(2) . . ?
C13 C14 H14 124.2(17) . . ?
C15 C14 H14 116.8(18) . . ?
N3 C15 C14 122.3(2) . . ?
N3 C15 H15 116.5(14) . . ?
C14 C15 H15 121.1(14) . . ?
N2 C16 C17 109.57(17) . . ?
N2 C16 H16A 106.4(14) . . ?
C17 C16 H16A 109.8(14) . . ?
N2 C16 H16B 110.6(16) . . ?
C17 C16 H16B 110.5(16) . . ?
H16A C16 H16B 110(2) . . ?
N4 C17 C18 121.73(19) . . ?
N4 C17 C16 115.64(17) . . ?
C18 C17 C16 122.63(19) . . ?
C17 C18 C19 118.9(2) . . ?
C17 C18 H18 117.8(15) . . ?
C19 C18 H18 123.3(15) . . ?
C20 C19 C18 119.2(2) . . ?
C20 C19 H19 121.5(16) . . ?
C18 C19 H19 119.2(16) . . ?
C21 C20 C19 118.9(2) . . ?
C21 C20 H20 122(2) . . ?
C19 C20 H20 119(2) . . ?
N4 C21 C20 122.2(2) . . ?
N4 C21 H21 116.5(14) . . ?
C20 C21 H21 121.1(14) . . ?
N1 C22 H22A 108.4(13) . . ?
N1 C22 H22B 108.2(15) . . ?
H22A C22 H22B 110(2) . . ?
N1 C22 H22C 110.7(15) . . ?
H22A C22 H22C 107(2) . . ?
H22B C22 H22C 112(2) . . ?
N2 C23 H23A 108.7(14) . . ?
N2 C23 H23B 105.8(16) . . ?
H23A C23 H23B 112(2) . . ?
N2 C23 H23C 108.6(15) . . ?
H23A C23 H23C 111(2) . . ?
H23B C23 H23C 110(2) . . ?
O3S2 S2 O2S2 115.53(10) . . ?
O3S2 S2 O1S2 114.41(10) . . ?
O2S2 S2 O1S2 114.49(10) . . ?
O3S2 S2 C2S 103.65(11) . . ?
O2S2 S2 C2S 103.47(11) . . ?
O1S2 S2 C2S 103.03(11) . . ?
S2 O1S2 Cu2 131.04(10) . . ?
F3S2 C2S F2S2 107.6(2) . . ?
F3S2 C2S F1S2 108.1(2) . . ?
F2S2 C2S F1S2 107.9(2) . . ?
F3S2 C2S S2 111.08(18) . . ?
F2S2 C2S S2 110.83(19) . . ?
F1S2 C2S S2 111.23(17) . . ?
O2S3 S3 O3S3 116.29(15) . . ?
O2S3 S3 O1S3 114.48(11) . . ?
O3S3 S3 O1S3 113.97(13) . . ?
O2S3 S3 C3S 103.46(13) . . ?
O3S3 S3 C3S 103.45(14) . . ?
O1S3 S3 C3S 102.81(12) . . ?
F1S3 C3S F3S3 107.4(2) . . ?
F1S3 C3S F2S3 107.5(2) . . ?
F3S3 C3S F2S3 107.7(2) . . ?
F1S3 C3S S3 112.27(18) . . ?
F3S3 C3S S3 111.2(2) . . ?
F2S3 C3S S3 110.53(18) . . ?

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
O1 H1O O1S3 0.80(3) 1.99(3) 2.786(3) 174(3) 1_655
O1 H2O O2S2 0.68(3) 2.13(3) 2.801(3) 167(3) .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.077
_database_code_depnum_ccdc_archive 'CCDC 948574'
#######################################################################
#
#                 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_ec99

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H28 Cu2 F6 N4 O7 S3'
_chemical_formula_weight         833.77

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6497(5)
_cell_length_b                   10.7181(5)
_cell_length_c                   16.8890(8)
_cell_angle_alpha                73.733(4)
_cell_angle_beta                 86.706(4)
_cell_angle_gamma                69.619(4)
_cell_volume                     1570.30(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3309
_cell_measurement_theta_min      3.2957
_cell_measurement_theta_max      32.4360

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_absorpt_coefficient_mu    1.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_T_max  0.8351
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19076
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         30.51
_reflns_number_total             9486
_reflns_number_gt                5735
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -43.00   10.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -57.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega  -82.00    1.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  127.0000  129.0000 83

#__ type_ start__ end____ width___ exp.time_
  3 omega  -51.00   41.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
  4 omega  -93.00   -1.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
  5 omega  -43.00    3.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000   30.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega   32.00   68.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051 -179.0000    0.0000 36

#__ type_ start__ end____ width___ exp.time_
  7 omega  -96.00   -6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000  120.0000 90

;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0377P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9486
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.0952
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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
Cu1 Cu 0.28432(5) 0.33701(4) 0.81128(3) 0.02305(11) Uani 1 1 d . . .
Cu2 Cu 0.16499(5) 0.60862(4) 0.68821(3) 0.02156(11) Uani 1 1 d . . .
S1 S 0.19657(9) 0.55714(9) 0.83073(5) 0.02070(18) Uani 1 1 d . . .
O3 O 0.3000(3) 0.4236(3) 0.69706(16) 0.0376(7) Uani 1 1 d . . .
H3O H 0.3580 0.3860 0.6563 0.045 Uiso 1 1 calc R . .
N1 N 0.2246(3) 0.2427(3) 0.92267(17) 0.0238(6) Uani 1 1 d . . .
N2 N -0.0167(3) 0.7856(3) 0.67686(17) 0.0206(6) Uani 1 1 d . . .
N3 N 0.3009(3) 0.1569(3) 0.78927(19) 0.0323(8) Uani 1 1 d . . .
N4 N 0.0952(3) 0.6292(3) 0.57391(19) 0.0273(7) Uani 1 1 d . . .
C1 C 0.0122(4) 0.5602(3) 0.8522(2) 0.0195(7) Uani 1 1 d . . .
C2 C -0.0110(4) 0.4478(3) 0.9111(2) 0.0215(7) Uani 1 1 d . . .
C3 C -0.1551(4) 0.4468(4) 0.9215(2) 0.0264(8) Uani 1 1 d . . .
H3 H -0.1711 0.3691 0.9591 0.032 Uiso 1 1 calc R . .
C4 C -0.2756(4) 0.5556(4) 0.8785(2) 0.0276(8) Uani 1 1 d . . .
C5 C -0.2503(4) 0.6693(4) 0.8248(2) 0.0236(8) Uani 1 1 d . . .
H5 H -0.3322 0.7463 0.7966 0.028 Uiso 1 1 calc R . .
C6 C -0.1079(4) 0.6736(4) 0.8113(2) 0.0213(7) Uani 1 1 d . . .
C7 C 0.1161(4) 0.3375(4) 0.9653(2) 0.0265(8) Uani 1 1 d . . .
H7A H 0.1693 0.3829 0.9897 0.032 Uiso 1 1 calc R . .
H7B H 0.0761 0.2813 1.0112 0.032 Uiso 1 1 calc R . .
C8 C -0.0867(4) 0.8020(3) 0.7566(2) 0.0228(7) Uani 1 1 d . . .
H8A H -0.1842 0.8773 0.7442 0.027 Uiso 1 1 calc R . .
H8B H -0.0242 0.8307 0.7872 0.027 Uiso 1 1 calc R . .
C9 C -0.4305(4) 0.5500(4) 0.8893(3) 0.0378(10) Uani 1 1 d . . .
H9A H -0.4924 0.6264 0.9108 0.057 Uiso 1 1 calc R . .
H9B H -0.4264 0.4615 0.9282 0.057 Uiso 1 1 calc R . .
H9C H -0.4729 0.5585 0.8359 0.057 Uiso 1 1 calc R . .
C10 C 0.1603(4) 0.1429(4) 0.9095(3) 0.0354(10) Uani 1 1 d . . .
H10A H 0.0552 0.1918 0.8904 0.042 Uiso 1 1 calc R . .
H10B H 0.1648 0.0714 0.9622 0.042 Uiso 1 1 calc R . .
C11 C 0.2443(4) 0.0755(4) 0.8464(3) 0.0336(9) Uani 1 1 d . . .
C12 C 0.2571(5) -0.0550(4) 0.8431(3) 0.0429(11) Uani 1 1 d . . .
H12 H 0.2162 -0.1110 0.8845 0.051 Uiso 1 1 calc R . .
C13 C 0.3287(5) -0.1033(5) 0.7800(3) 0.0493(12) Uani 1 1 d . . .
H13 H 0.3385 -0.1931 0.7769 0.059 Uiso 1 1 calc R . .
C14 C 0.3861(5) -0.0206(5) 0.7213(3) 0.0446(12) Uani 1 1 d . . .
H14 H 0.4342 -0.0519 0.6762 0.053 Uiso 1 1 calc R . .
C15 C 0.3746(4) 0.1093(5) 0.7273(3) 0.0388(10) Uani 1 1 d . . .
H15 H 0.4187 0.1647 0.6876 0.047 Uiso 1 1 calc R . .
C16 C -0.1236(4) 0.7709(4) 0.6227(2) 0.0241(8) Uani 1 1 d . . .
H16A H -0.2020 0.8619 0.6000 0.029 Uiso 1 1 calc R . .
H16B H -0.1711 0.7058 0.6555 0.029 Uiso 1 1 calc R . .
C17 C -0.0436(4) 0.7174(4) 0.5530(2) 0.0274(8) Uani 1 1 d . . .
C18 C -0.1064(5) 0.7494(4) 0.4750(2) 0.0348(9) Uani 1 1 d . . .
H18 H -0.2039 0.8141 0.4607 0.042 Uiso 1 1 calc R . .
C19 C -0.0247(5) 0.6858(5) 0.4181(3) 0.0401(10) Uani 1 1 d . . .
H19 H -0.0662 0.7049 0.3645 0.048 Uiso 1 1 calc R . .
C20 C 0.1166(5) 0.5949(4) 0.4399(2) 0.0370(10) Uani 1 1 d . . .
H20 H 0.1742 0.5507 0.4014 0.044 Uiso 1 1 calc R . .
C21 C 0.1747(4) 0.5682(4) 0.5181(2) 0.0306(9) Uani 1 1 d . . .
H21 H 0.2728 0.5053 0.5330 0.037 Uiso 1 1 calc R . .
C22 C 0.3606(4) 0.1675(4) 0.9772(2) 0.0362(10) Uani 1 1 d . . .
H22A H 0.3341 0.1261 1.0327 0.054 Uiso 1 1 calc R . .
H22B H 0.4096 0.2325 0.9799 0.054 Uiso 1 1 calc R . .
H22C H 0.4279 0.0944 0.9549 0.054 Uiso 1 1 calc R . .
C23 C 0.0196(4) 0.9111(3) 0.6349(2) 0.0270(8) Uani 1 1 d . . .
H23A H 0.0590 0.9041 0.5809 0.041 Uiso 1 1 calc R . .
H23B H 0.0938 0.9188 0.6687 0.041 Uiso 1 1 calc R . .
H23C H -0.0701 0.9933 0.6274 0.041 Uiso 1 1 calc R . .
S11 S 0.67395(11) 0.16972(10) 0.84896(6) 0.0284(2) Uani 1 1 d . . .
F1S1 F 0.9199(3) 0.1240(3) 0.77047(18) 0.0572(7) Uani 1 1 d . . .
F2S1 F 0.7229(3) 0.2287(3) 0.69170(14) 0.0505(7) Uani 1 1 d . . .
F3S1 F 0.7994(3) 0.3393(3) 0.75786(14) 0.0478(7) Uani 1 1 d . . .
O1S1 O 0.5357(3) 0.2857(3) 0.83037(17) 0.0373(7) Uani 1 1 d . . .
O2S1 O 0.7567(3) 0.1595(3) 0.92031(16) 0.0447(7) Uani 1 1 d . . .
O3S1 O 0.6666(3) 0.0419(3) 0.84060(17) 0.0403(7) Uani 1 1 d . . .
C1S C 0.7838(4) 0.2190(4) 0.7631(2) 0.0329(9) Uani 1 1 d . . .
S12 S 0.47497(10) 0.67243(10) 0.61224(6) 0.0266(2) Uani 1 1 d . . .
F1S2 F 0.5345(3) 0.7755(3) 0.46068(17) 0.0729(9) Uani 1 1 d . . .
F2S2 F 0.3072(3) 0.7926(3) 0.47588(15) 0.0523(7) Uani 1 1 d . . .
F3S2 F 0.3888(3) 0.9256(3) 0.51623(18) 0.0649(8) Uani 1 1 d . . .
O1S2 O 0.3392(3) 0.7105(3) 0.65592(15) 0.0273(6) Uani 1 1 d . . .
O2S2 O 0.5927(3) 0.7029(3) 0.64116(18) 0.0464(8) Uani 1 1 d . . .
O3S2 O 0.5127(3) 0.5405(3) 0.59619(18) 0.0392(7) Uani 1 1 d . . .
C2S C 0.4240(5) 0.7966(5) 0.5113(3) 0.0371(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 1.915(3) . ?
Cu1 N3 2.017(3) . ?
Cu1 N1 2.027(3) . ?
Cu1 O1S1 2.313(3) . ?
Cu1 S1 2.3242(9) . ?
Cu1 Cu2 2.9447(6) . ?
Cu2 O3 1.926(3) . ?
Cu2 N4 2.009(3) . ?
Cu2 N2 2.056(3) . ?
Cu2 O1S2 2.271(2) . ?
Cu2 S1 2.3268(9) . ?
S1 C1 1.786(3) . ?
O3 H3O 0.9500 . ?
N1 C10 1.480(5) . ?
N1 C22 1.485(5) . ?
N1 C7 1.493(4) . ?
N2 C23 1.483(4) . ?
N2 C16 1.493(4) . ?
N2 C8 1.499(4) . ?
N3 C11 1.338(5) . ?
N3 C15 1.350(4) . ?
N4 C17 1.341(5) . ?
N4 C21 1.347(4) . ?
C1 C6 1.393(5) . ?
C1 C2 1.408(5) . ?
C2 C3 1.396(5) . ?
C2 C7 1.500(5) . ?
C3 C4 1.385(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(5) . ?
C4 C9 1.515(5) . ?
C5 C6 1.394(5) . ?
C5 H5 0.9500 . ?
C6 C8 1.500(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.496(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.378(5) . ?
C12 C13 1.362(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.365(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.508(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.384(5) . ?
C18 C19 1.384(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.369(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
S11 O2S1 1.442(3) . ?
S11 O3S1 1.442(3) . ?
S11 O1S1 1.449(3) . ?
S11 C1S 1.813(4) . ?
F1S1 C1S 1.339(4) . ?
F2S1 C1S 1.335(4) . ?
F3S1 C1S 1.327(4) . ?
S12 O2S2 1.430(3) . ?
S12 O3S2 1.432(3) . ?
S12 O1S2 1.453(2) . ?
S12 C2S 1.814(4) . ?
F1S2 C2S 1.324(4) . ?
F2S2 C2S 1.324(4) . ?
F3S2 C2S 1.329(5) . ?

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
O3 Cu1 N3 92.60(12) . . ?
O3 Cu1 N1 166.78(12) . . ?
N3 Cu1 N1 81.45(12) . . ?
O3 Cu1 O1S1 88.64(11) . . ?
N3 Cu1 O1S1 96.11(11) . . ?
N1 Cu1 O1S1 103.67(11) . . ?
O3 Cu1 S1 87.60(8) . . ?
N3 Cu1 S1 164.28(9) . . ?
N1 Cu1 S1 94.95(8) . . ?
O1S1 Cu1 S1 99.60(7) . . ?
O3 Cu1 Cu2 40.07(8) . . ?
N3 Cu1 Cu2 123.38(9) . . ?
N1 Cu1 Cu2 136.11(8) . . ?
O1S1 Cu1 Cu2 108.06(7) . . ?
S1 Cu1 Cu2 50.76(2) . . ?
O3 Cu2 N4 91.58(12) . . ?
O3 Cu2 N2 166.29(11) . . ?
N4 Cu2 N2 82.31(11) . . ?
O3 Cu2 O1S2 95.24(11) . . ?
N4 Cu2 O1S2 99.52(11) . . ?
N2 Cu2 O1S2 97.87(10) . . ?
O3 Cu2 S1 87.28(8) . . ?
N4 Cu2 S1 164.32(9) . . ?
N2 Cu2 S1 95.29(8) . . ?
O1S2 Cu2 S1 96.16(7) . . ?
O3 Cu2 Cu1 39.81(8) . . ?
N4 Cu2 Cu1 122.33(9) . . ?
N2 Cu2 Cu1 136.10(8) . . ?
O1S2 Cu2 Cu1 111.01(7) . . ?
S1 Cu2 Cu1 50.68(2) . . ?
C1 S1 Cu1 95.85(11) . . ?
C1 S1 Cu2 95.32(11) . . ?
Cu1 S1 Cu2 78.56(3) . . ?
Cu1 O3 Cu2 100.12(11) . . ?
Cu1 O3 H3O 129.9 . . ?
Cu2 O3 H3O 129.9 . . ?
C10 N1 C22 109.9(3) . . ?
C10 N1 C7 109.0(3) . . ?
C22 N1 C7 107.7(3) . . ?
C10 N1 Cu1 107.3(2) . . ?
C22 N1 Cu1 107.7(2) . . ?
C7 N1 Cu1 115.2(2) . . ?
C23 N2 C16 108.9(3) . . ?
C23 N2 C8 109.0(2) . . ?
C16 N2 C8 109.2(3) . . ?
C23 N2 Cu2 111.2(2) . . ?
C16 N2 Cu2 103.68(19) . . ?
C8 N2 Cu2 114.6(2) . . ?
C11 N3 C15 119.2(3) . . ?
C11 N3 Cu1 115.1(2) . . ?
C15 N3 Cu1 125.4(3) . . ?
C17 N4 C21 119.3(3) . . ?
C17 N4 Cu2 114.0(2) . . ?
C21 N4 Cu2 126.7(3) . . ?
C6 C1 C2 120.2(3) . . ?
C6 C1 S1 120.1(3) . . ?
C2 C1 S1 119.7(3) . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 C7 121.3(3) . . ?
C1 C2 C7 120.0(3) . . ?
C4 C3 C2 122.0(3) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 118.1(3) . . ?
C3 C4 C9 120.8(4) . . ?
C5 C4 C9 121.1(4) . . ?
C4 C5 C6 121.8(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 119.0(3) . . ?
C1 C6 C8 121.0(3) . . ?
C5 C6 C8 119.9(3) . . ?
N1 C7 C2 114.9(3) . . ?
N1 C7 H7A 108.5 . . ?
C2 C7 H7A 108.5 . . ?
N1 C7 H7B 108.5 . . ?
C2 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
N2 C8 C6 114.3(3) . . ?
N2 C8 H8A 108.7 . . ?
C6 C8 H8A 108.7 . . ?
N2 C8 H8B 108.7 . . ?
C6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 109.9(3) . . ?
N1 C10 H10A 109.7 . . ?
C11 C10 H10A 109.7 . . ?
N1 C10 H10B 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N3 C11 C12 121.8(4) . . ?
N3 C11 C10 113.7(3) . . ?
C12 C11 C10 124.3(4) . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 118.9(4) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C13 C14 C15 120.2(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N3 C15 C14 120.2(4) . . ?
N3 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
N2 C16 C17 109.8(3) . . ?
N2 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
N2 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N4 C17 C18 121.6(3) . . ?
N4 C17 C16 113.9(3) . . ?
C18 C17 C16 124.5(3) . . ?
C19 C18 C17 118.9(4) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C20 C19 C18 119.3(4) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 119.4(4) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
N4 C21 C20 121.5(4) . . ?
N4 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2S1 S11 O3S1 116.43(17) . . ?
O2S1 S11 O1S1 114.34(17) . . ?
O3S1 S11 O1S1 114.77(17) . . ?
O2S1 S11 C1S 103.74(18) . . ?
O3S1 S11 C1S 102.83(17) . . ?
O1S1 S11 C1S 102.05(18) . . ?
S11 O1S1 Cu1 141.51(17) . . ?
F3S1 C1S F2S1 108.1(3) . . ?
F3S1 C1S F1S1 107.2(3) . . ?
F2S1 C1S F1S1 106.9(3) . . ?
F3S1 C1S S11 112.4(3) . . ?
F2S1 C1S S11 110.9(3) . . ?
F1S1 C1S S11 111.0(3) . . ?
O2S2 S12 O3S2 116.82(18) . . ?
O2S2 S12 O1S2 114.06(16) . . ?
O3S2 S12 O1S2 113.93(15) . . ?
O2S2 S12 C2S 103.05(19) . . ?
O3S2 S12 C2S 104.30(18) . . ?
O1S2 S12 C2S 102.26(18) . . ?
S12 O1S2 Cu2 130.50(14) . . ?
F1S2 C2S F2S2 108.0(3) . . ?
F1S2 C2S F3S2 107.2(3) . . ?
F2S2 C2S F3S2 106.2(4) . . ?
F1S2 C2S S12 111.3(3) . . ?
F2S2 C2S S12 112.7(3) . . ?
F3S2 C2S S12 111.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.104
_database_code_depnum_ccdc_archive 'CCDC 948577'
