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

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

data_snwllj
_database_code_depnum_ccdc_archive 'CCDC 1507034'
_audit_update_record             
;
2016-09-27 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_nottingham_internal_coll_name   SNWLLJ
_nottingham_internal_coll_number 14537
_nottingham_internal_coll_client SN/WL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '2.0000, 8.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   30/03/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 27/05/2015
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 27/5/2015
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 3/6/2015
_nottingham_internal_refinement_user pczwl
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 3/6/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 3/6/2015
_refine_special_details          ?
_audit_creation_date             2015-06-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H7 Cl N2 O S'
_chemical_formula_sum            'C10 H7 Cl N2 O S'
_chemical_formula_weight         238.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H7 N2 O Cl S'
_chemical_oxdiff_usercomment     
'SNWLLJ #14537 GVB-479 on micromount in fomblin film FOR SN/WL'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.7035(4)
_cell_length_b                   3.79321(9)
_cell_length_c                   17.8136(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.866(3)
_cell_angle_gamma                90
_cell_volume                     992.28(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.8210
_cell_measurement_theta_min      4.9590
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.145
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.3147
_exptl_crystal_size_mid          0.0747
_exptl_crystal_size_min          0.0481
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4575
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.048
_diffrn_reflns_theta_min         4.972
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega -124.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000    0.0000    0.0000 171

#__ type_ start__ end____ width___ exp.time_
  3 omega   33.00  135.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -180.0000 102

#__ type_ start__ end____ width___ exp.time_
  4 omega   31.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000    0.0000 59

#__ type_ start__ end____ width___ exp.time_
  5 omega   35.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -120.0000 63

#__ type_ start__ end____ width___ exp.time_
  6 omega   35.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -30.0000 63

#__ type_ start__ end____ width___ exp.time_
  7 omega   82.00  174.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
  8 omega   82.00  174.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
  9 omega   36.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  150.0000 73
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0938315000
_diffrn_orient_matrix_UB_12      -0.1519192000
_diffrn_orient_matrix_UB_13      0.0249436000
_diffrn_orient_matrix_UB_21      -0.0441136000
_diffrn_orient_matrix_UB_22      -0.2120328000
_diffrn_orient_matrix_UB_23      0.0623228000
_diffrn_orient_matrix_UB_31      -0.0157193000
_diffrn_orient_matrix_UB_32      -0.3115991000
_diffrn_orient_matrix_UB_33      -0.0546658000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1768
_reflns_number_total             1965
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0757P)²+0.4323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1145
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.96661(3) 0.74940(13) 0.58055(3) 0.02448(19) Uani 1 1 d . . . . .
C2 C 0.85101(13) 0.6829(5) 0.57412(11) 0.0191(4) Uani 1 1 d . . . . .
N3 N 0.80550(12) 0.7820(4) 0.63610(10) 0.0219(4) Uani 1 1 d . . . . .
C4 C 0.87035(16) 0.9039(6) 0.68810(12) 0.0275(5) Uani 1 1 d . . . . .
H4 H 0.8540 0.9825 0.7362 0.033 Uiso 1 1 calc R . . . .
C5 C 0.95804(15) 0.9086(6) 0.66866(12) 0.0261(4) Uani 1 1 d . . . . .
H5 H 1.0078 0.9899 0.7000 0.031 Uiso 1 1 calc R . . . .
N6 N 0.81334(12) 0.5385(4) 0.50743(10) 0.0199(4) Uani 1 1 d . . . . .
C7 C 0.72740(14) 0.4648(5) 0.50364(11) 0.0194(4) Uani 1 1 d . . . . .
H7 H 0.6921 0.5105 0.5458 0.023 Uiso 1 1 calc R . . . .
C8 C 0.68384(13) 0.3133(5) 0.43617(11) 0.0186(4) Uani 1 1 d . . . . .
C9 C 0.73329(14) 0.2330(5) 0.37207(11) 0.0203(4) Uani 1 1 d . . . . .
C10 C 0.68811(14) 0.0841(6) 0.30893(11) 0.0230(4) Uani 1 1 d . . . . .
H10 H 0.7211 0.0283 0.2660 0.028 Uiso 1 1 calc R . . . .
C11 C 0.59574(15) 0.0175(5) 0.30864(11) 0.0206(4) Uani 1 1 d . . . . .
H11 H 0.5654 -0.0843 0.2656 0.025 Uiso 1 1 calc R . . . .
C12 C 0.54682(13) 0.0995(5) 0.37148(11) 0.0195(4) Uani 1 1 d . . . . .
C13 C 0.59029(14) 0.2441(5) 0.43471(11) 0.0193(4) Uani 1 1 d . . . . .
H13 H 0.5565 0.2969 0.4774 0.023 Uiso 1 1 calc R . . . .
O14 O 0.82340(10) 0.2972(5) 0.36989(9) 0.0271(4) Uani 1 1 d . . . . .
H14 H 0.840(2) 0.375(9) 0.413(2) 0.041 Uiso 1 1 d R . . . .
Cl15 Cl 0.43016(3) 0.01827(12) 0.36964(3) 0.02326(18) 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
S1 C2 1.717(2) . ?
S1 C5 1.692(2) . ?
C2 N3 1.372(3) . ?
C2 N6 1.397(3) . ?
N3 C4 1.376(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.352(3) . ?
C5 H5 0.9500 . ?
N6 C7 1.293(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.452(3) . ?
C8 C9 1.417(3) . ?
C8 C13 1.399(3) . ?
C9 C10 1.397(3) . ?
C9 O14 1.350(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(3) . ?
C12 C13 1.381(3) . ?
C12 Cl15 1.741(2) . ?
C13 H13 0.9500 . ?
O14 H14 0.84(4) . ?

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
C5 S1 C2 89.71(10) . . ?
N3 C2 S1 115.29(14) . . ?
N3 C2 N6 127.09(17) . . ?
N6 C2 S1 117.61(14) . . ?
C2 N3 C4 106.53(17) . . ?
N3 C4 H4 121.0 . . ?
C5 C4 N3 118.02(19) . . ?
C5 C4 H4 121.0 . . ?
S1 C5 H5 124.8 . . ?
C4 C5 S1 110.43(16) . . ?
C4 C5 H5 124.8 . . ?
C7 N6 C2 118.30(18) . . ?
N6 C7 H7 119.4 . . ?
N6 C7 C8 121.23(19) . . ?
C8 C7 H7 119.4 . . ?
C9 C8 C7 121.95(18) . . ?
C13 C8 C7 118.82(18) . . ?
C13 C8 C9 119.22(18) . . ?
C10 C9 C8 119.55(19) . . ?
O14 C9 C8 121.90(18) . . ?
O14 C9 C10 118.55(18) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.34(19) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.16(18) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 Cl15 119.49(15) . . ?
C13 C12 C11 120.45(19) . . ?
C13 C12 Cl15 120.06(15) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.28(18) . . ?
C12 C13 H13 119.9 . . ?
C9 O14 H14 106(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
O14 H14 N6 0.84(4) 1.86(4) 2.627(2) 151(3) .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C2 N3 C4 -1.4(2) . . . . ?
S1 C2 N6 C7 175.40(15) . . . . ?
C2 S1 C5 C4 -0.12(17) . . . . ?
C2 N3 C4 C5 1.4(3) . . . . ?
C2 N6 C7 C8 -179.81(17) . . . . ?
N3 C2 N6 C7 -5.1(3) . . . . ?
N3 C4 C5 S1 -0.7(3) . . . . ?
C5 S1 C2 N3 0.93(17) . . . . ?
C5 S1 C2 N6 -179.53(17) . . . . ?
N6 C2 N3 C4 179.1(2) . . . . ?
N6 C7 C8 C9 1.2(3) . . . . ?
N6 C7 C8 C13 -178.95(17) . . . . ?
C7 C8 C9 C10 179.32(18) . . . . ?
C7 C8 C9 O14 -0.9(3) . . . . ?
C7 C8 C13 C12 -179.86(18) . . . . ?
C8 C9 C10 C11 0.5(3) . . . . ?
C9 C8 C13 C12 0.0(3) . . . . ?
C9 C10 C11 C12 0.1(3) . . . . ?
C10 C11 C12 C13 -0.7(3) . . . . ?
C10 C11 C12 Cl15 179.27(15) . . . . ?
C11 C12 C13 C8 0.6(3) . . . . ?
C13 C8 C9 C10 -0.5(3) . . . . ?
C13 C8 C9 O14 179.32(17) . . . . ?
O14 C9 C10 C11 -179.37(18) . . . . ?
Cl15 C12 C13 C8 -179.32(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 0.0350 -0.9994 0.0000 0.0004 -0.0938 0.0441 0.0157
1 0 0 0.0130 0.9994 -0.0000 -0.0004 0.0938 -0.0441 -0.0157
-2 0 -5 0.0325 -2.0003 0.0000 -4.9960 -0.3123 -0.2231 0.3046
2 0 5 0.0325 2.0003 -0.0000 4.9960 0.3123 0.2231 -0.3046
-2 2 -1 0.1633 -1.9999 1.9993 -0.9958 -0.5162 -0.3978 -0.5371
1 -1 0 0.1252 0.9998 -0.9997 -0.0018 0.2456 0.1677 0.2959
-5 0 10 0.0418 -4.9938 0.0002 9.9953 -0.2193 0.8432 -0.4680
4 0 -10 0.0264 3.9944 -0.0002 -9.9949 0.1255 -0.7991 0.4836

_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_skwllc_sq
_database_code_depnum_ccdc_archive 'CCDC 1507035'
_audit_update_record             
;
2016-09-27 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_nottingham_internal_coll_name   SKWLLC
_nottingham_internal_coll_number 14025
_nottingham_internal_coll_client SN/WL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '20.0000, 80.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   30/09/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 02/10/2014
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 2/10/2014
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 12/11/2014
_nottingham_internal_refinement_user pczwl
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 15/1/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 15/1/2015
_refine_special_details          
;
A region of disordered solvent could not be modelled as a sensible chemical 
entity, so the structure was treated with PLATON SQUEEZE. As the nature of the 
removed solvent could not be determeined they were not included in the formula. 
The removed solvent molecule(s) would likely have been a hydrogen bond acceptor 
for N46.

DMSO molecule S81-C84 exhibited disorder of one of the methyl groups over two 
postions. The occupancies of the two components were refined competitively, 
converging at a ratio of 0.77:0.23.

DMSO molecule S85-C88 exhibited disorder of the central sulphur atom. The 
occupancies of the two components were refined competitively, converging 
at a ratio of 0.57:0.43.
;
_vrf_PLAT306_skwllc_sq           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O89 Check 
RESPONSE: Positions for the hydrogen atoms of water molecules O89 and O90 
could not be determined, and so these were not included on the model, although 
they were included in the formula, and calculation of dreived parameters.
;
_vrf_PLAT430_skwllc_sq           
;
PROBLEM: Short Inter D...A Contact  O75    ..  O90     ..       2.69 Ang.  
RESPONSE: As the hydrogen atoms positions of water molecules O89 and O90 could 
not be determined, and so hydrogen bonds cannot be calculated for these molecules.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 32 7 ' '
2 0.500 0.500 0.500 339 93 ' '

_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_audit_creation_date             2015-01-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H28 Cl4 Cu4 N8 O8 S4, 2(C2 H6 O S), 2(O)'
_chemical_formula_sum            'C44 H44 Cl4 Cu4 N8 O12 S6'
_chemical_formula_weight         1465.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H52 N8 O12 S8 Cl4 Cu4'
_chemical_oxdiff_usercomment     
'SKWLLC #14025 GVA-331 IN FOMBLIN FIML ON A MICROMOUNT FOR SN/WL'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.5168(9)
_cell_length_b                   14.9751(10)
_cell_length_c                   15.6509(10)
_cell_angle_alpha                81.622(5)
_cell_angle_beta                 71.061(6)
_cell_angle_gamma                71.633(6)
_cell_volume                     3050.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8077
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1320
_cell_measurement_theta_min      2.9990
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.617
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.2084
_exptl_crystal_size_mid          0.1962
_exptl_crystal_size_min          0.0433
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.272
_diffrn_reflns_theta_min         2.989
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3271
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   33.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.2573  -57.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega   34.00   68.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  3 omega   72.00  129.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000    0.0000 57

#__ type_ start__ end____ width___ exp.time_
  4 omega   65.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   30.0000 113

#__ type_ start__ end____ width___ exp.time_
  5 omega  140.00  166.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  127.00  171.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   60.0000 44

#__ type_ start__ end____ width___ exp.time_
  7 omega   82.00  129.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 47

#__ type_ start__ end____ width___ exp.time_
  8 omega   82.00  114.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   60.0000 32

#__ type_ start__ end____ width___ exp.time_
  9 omega   64.00   97.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  150.0000 33

#__ type_ start__ end____ width___ exp.time_
 10 omega   42.00   72.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
 11 omega   31.00   91.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
 12 omega   63.00  103.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000    0.0000 40

#__ type_ start__ end____ width___ exp.time_
 13 omega   55.00  108.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -90.0000 53

#__ type_ start__ end____ width___ exp.time_
 14 omega   62.00  120.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -180.0000 58

#__ type_ start__ end____ width___ exp.time_
 15 omega   35.00  118.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -120.0000 83

#__ type_ start__ end____ width___ exp.time_
 16 omega   37.00   95.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -150.0000 58

#__ type_ start__ end____ width___ exp.time_
 17 omega   35.00   87.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -90.0000 52

#__ type_ start__ end____ width___ exp.time_
 18 omega   15.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.2573   77.0000 -120.0000 99

#__ type_ start__ end____ width___ exp.time_
 19 omega  -68.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   77.0000  150.0000 101

#__ type_ start__ end____ width___ exp.time_
 20 omega -101.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -77.0000   30.0000 89
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0163348000
_diffrn_orient_matrix_UB_12      -0.0733937000
_diffrn_orient_matrix_UB_13      0.0790780000
_diffrn_orient_matrix_UB_21      0.0951506000
_diffrn_orient_matrix_UB_22      0.0047511000
_diffrn_orient_matrix_UB_23      0.0205465000
_diffrn_orient_matrix_UB_31      -0.0662632000
_diffrn_orient_matrix_UB_32      0.0798011000
_diffrn_orient_matrix_UB_33      0.0646516000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9591
_reflns_number_total             11993
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.796
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11993
_refine_ls_number_restraints     786
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0704
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0957P)²+8.0445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1941
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(S85A)=Sof(H87D)=Sof(H87E)=Sof(H87F)=Sof(H88D)=Sof(H88E)=Sof(H88F)=1-FVAR(1)
 Sof(S85)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(1)
 Sof(C84A)=Sof(H84D)=Sof(H84E)=Sof(H84F)=1-FVAR(2)
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C27(H27), C47(H47), C67(H67)
4.b Me refined with riding coordinates:
 C87(H87A,H87B,H87C), C87(H87D,H87E,H87F), C88(H88A,H88B,H88C), C88(H88D,H88E,
 H88F)
4.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N26(H26), N46(H46), N66(H66), C4(H4), C5(H5), C11(H11), C12(H12),
 C14(H14), C24(H24), C25(H25), C31(H31), C32(H32), C34(H34), C44(H44), C45(H45),
  C51(H51), C52(H52), C54(H54), C64(H64), C65(H65), C71(H71), C72(H72), C74(H74)
4.d Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C84A(H84D,H84E,H84F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.14774(5) 0.64403(5) 0.18961(5) 0.03599(18) Uani 1 1 d . U . . .
Cu2 Cu 0.26577(5) 0.80103(5) 0.14041(5) 0.03550(18) Uani 1 1 d . U . . .
Cu3 Cu 0.05525(5) 0.83771(5) 0.29671(5) 0.03530(18) Uani 1 1 d . U . . .
Cu4 Cu 0.24593(5) 0.68037(5) 0.33253(5) 0.03932(19) Uani 1 1 d . U . . .
Cl16 Cl -0.25879(12) 0.96884(19) 0.04119(17) 0.0918(7) Uani 1 1 d . U . . .
Cl36 Cl 0.49330(15) 0.9440(2) 0.42041(17) 0.1073(10) Uani 1 1 d . U . . .
Cl56 Cl 0.73465(15) 0.5265(2) 0.0024(2) 0.1137(9) Uani 1 1 d . U . . .
Cl76 Cl -0.23678(15) 0.50718(14) 0.46269(17) 0.0815(6) Uani 1 1 d . U . . .
S3 S 0.34427(10) 0.69053(11) -0.13339(10) 0.0495(3) Uani 1 1 d . U . . .
S23 S 0.03937(10) 1.13000(10) 0.17364(9) 0.0427(3) Uani 1 1 d . U . . .
S43 S 0.23572(11) 0.35789(10) 0.32668(11) 0.0530(4) Uani 1 1 d . U . . .
S63 S 0.0844(2) 0.8080(3) 0.60118(18) 0.1153(11) Uani 1 1 d . U . . .
O8 O 0.1362(2) 0.7757(2) 0.1509(2) 0.0365(7) Uani 1 1 d . U . . .
O15 O 0.0346(3) 0.6409(3) 0.1544(3) 0.0482(9) Uani 1 1 d . U . . .
O28 O 0.2002(2) 0.8350(2) 0.2658(2) 0.0365(7) Uani 1 1 d . U . . .
O35 O 0.3813(3) 0.8411(3) 0.1278(3) 0.0460(9) Uani 1 1 d . U . . .
O48 O 0.2754(2) 0.6454(2) 0.2089(3) 0.0382(7) Uani 1 1 d . U . . .
O55 O 0.3853(3) 0.6413(3) 0.3298(3) 0.0591(11) Uani 1 1 d . U . . .
O68 O 0.1024(2) 0.7064(2) 0.3354(2) 0.0355(7) Uani 1 1 d . U . . .
O75 O -0.0852(2) 0.8400(3) 0.3423(3) 0.0446(8) Uani 1 1 d . U . . .
N1 N 0.3201(3) 0.7616(3) 0.0148(3) 0.0385(9) Uani 1 1 d . U . . .
N6 N 0.1684(3) 0.7518(3) -0.0031(3) 0.0415(10) Uani 1 1 d . U . . .
H6 H 0.1420 0.7254 -0.0322 0.050 Uiso 1 1 calc R . . . .
N21 N 0.0213(3) 0.9712(3) 0.2558(3) 0.0380(9) Uani 1 1 d . U . . .
N26 N 0.1816(3) 0.9957(3) 0.2324(3) 0.0403(9) Uani 1 1 d . U . . .
H26 H 0.2237 1.0283 0.2013 0.048 Uiso 1 1 calc R . . . .
N41 N 0.1713(3) 0.5113(3) 0.2375(3) 0.0426(9) Uani 1 1 d . U . . .
N46 N 0.3370(3) 0.4854(3) 0.2473(3) 0.0449(10) Uani 1 1 d . U . . .
H46 H 0.3823 0.4536 0.2750 0.054 Uiso 1 1 calc R . . . .
N61 N 0.1976(4) 0.7223(4) 0.4572(3) 0.0507(11) Uani 1 1 d . U . . .
N66 N 0.0234(4) 0.7328(4) 0.4903(3) 0.0507(11) Uani 1 1 d . U . . .
H66 H -0.0389 0.7571 0.5248 0.061 Uiso 1 1 calc R . . . .
C2 C 0.2691(4) 0.7399(3) -0.0310(4) 0.0374(10) Uani 1 1 d . U . . .
C4 C 0.4499(4) 0.6987(5) -0.1095(5) 0.0567(15) Uani 1 1 d . U . . .
H4 H 0.5177 0.6784 -0.1479 0.068 Uiso 1 1 calc R . . . .
C5 C 0.4237(4) 0.7366(4) -0.0313(4) 0.0472(12) Uani 1 1 d . U . . .
H5 H 0.4723 0.7463 -0.0078 0.057 Uiso 1 1 calc R . . . .
C7 C 0.1021(3) 0.8073(4) 0.0740(3) 0.0375(10) Uani 1 1 d . U . . .
H7 H 0.1016 0.8746 0.0588 0.045 Uiso 1 1 calc R . . . .
C9 C -0.0043(3) 0.8000(4) 0.0911(4) 0.0413(11) Uani 1 1 d . U . . .
C10 C -0.0294(4) 0.7165(4) 0.1291(4) 0.0437(11) Uani 1 1 d . U . . .
C11 C -0.1277(4) 0.7131(6) 0.1363(4) 0.0576(15) Uani 1 1 d . U . . .
H11 H -0.1464 0.6571 0.1602 0.069 Uiso 1 1 calc R . . . .
C12 C -0.1977(4) 0.7898(6) 0.1092(4) 0.0613(15) Uani 1 1 d . U . . .
H12 H -0.2634 0.7858 0.1145 0.074 Uiso 1 1 calc R . . . .
C13 C -0.1721(4) 0.8716(6) 0.0748(4) 0.0590(15) Uani 1 1 d . U . . .
C14 C -0.0752(4) 0.8766(5) 0.0654(4) 0.0484(13) Uani 1 1 d . U . . .
H14 H -0.0574 0.9330 0.0412 0.058 Uiso 1 1 calc R . . . .
C22 C 0.0865(4) 1.0219(4) 0.2261(3) 0.0362(10) Uani 1 1 d . U . . .
C24 C -0.0742(4) 1.1028(4) 0.1941(4) 0.0451(12) Uani 1 1 d . U . . .
H24 H -0.1315 1.1426 0.1772 0.054 Uiso 1 1 calc R . . . .
C25 C -0.0698(4) 1.0192(4) 0.2364(4) 0.0435(11) Uani 1 1 d . U . . .
H25 H -0.1253 0.9932 0.2528 0.052 Uiso 1 1 calc R . . . .
C27 C 0.2170(4) 0.9140(3) 0.2899(4) 0.0378(10) Uani 1 1 d . U . . .
H27 H 0.1777 0.9266 0.3546 0.045 Uiso 1 1 calc R . . . .
C29 C 0.3281(4) 0.8998(4) 0.2772(4) 0.0399(10) Uani 1 1 d . U . . .
C30 C 0.4026(4) 0.8635(4) 0.1967(4) 0.0400(10) Uani 1 1 d . U . . .
C31 C 0.5052(4) 0.8542(4) 0.1886(4) 0.0465(12) Uani 1 1 d . U . . .
H31 H 0.5565 0.8311 0.1346 0.056 Uiso 1 1 calc R . . . .
C32 C 0.5328(4) 0.8774(5) 0.2561(5) 0.0573(15) Uani 1 1 d . U . . .
H32 H 0.6022 0.8705 0.2489 0.069 Uiso 1 1 calc R . . . .
C33 C 0.4580(5) 0.9116(5) 0.3358(5) 0.0610(16) Uani 1 1 d . U . . .
C34 C 0.3566(4) 0.9220(5) 0.3465(4) 0.0506(13) Uani 1 1 d . U . . .
H34 H 0.3064 0.9443 0.4013 0.061 Uiso 1 1 calc R . . . .
C42 C 0.2509(4) 0.4612(4) 0.2644(4) 0.0416(11) Uani 1 1 d . U . . .
C44 C 0.1164(5) 0.3852(5) 0.3158(5) 0.0616(16) Uani 1 1 d . U . . .
H44 H 0.0713 0.3475 0.3405 0.074 Uiso 1 1 calc R . . . .
C45 C 0.0942(4) 0.4679(4) 0.2674(5) 0.0527(14) Uani 1 1 d . U . . .
H45 H 0.0309 0.4939 0.2550 0.063 Uiso 1 1 calc R . . . .
C47 C 0.3566(3) 0.5636(4) 0.1837(4) 0.0408(11) Uani 1 1 d . U . . .
H47 H 0.3622 0.5479 0.1219 0.049 Uiso 1 1 calc R . . . .
C49 C 0.4554(4) 0.5780(4) 0.1820(5) 0.0476(12) Uani 1 1 d . U . . .
C50 C 0.4619(4) 0.6170(4) 0.2558(5) 0.0545(13) Uani 1 1 d . U . . .
C51 C 0.5578(5) 0.6272(6) 0.2477(6) 0.0729(19) Uani 1 1 d . U . . .
H51 H 0.5667 0.6523 0.2958 0.087 Uiso 1 1 calc R . . . .
C52 C 0.6400(5) 0.6008(6) 0.1699(7) 0.0757(19) Uani 1 1 d . U . . .
H52 H 0.7036 0.6087 0.1661 0.091 Uiso 1 1 calc R . . . .
C53 C 0.6307(5) 0.5645(6) 0.1007(6) 0.0739(19) Uani 1 1 d . U . . .
C54 C 0.5377(4) 0.5539(5) 0.1053(5) 0.0583(15) Uani 1 1 d . U . . .
H54 H 0.5304 0.5299 0.0556 0.070 Uiso 1 1 calc R . . . .
C62 C 0.1019(5) 0.7495(5) 0.5072(4) 0.0578(15) Uani 1 1 d . U . . .
C64 C 0.2136(8) 0.7967(9) 0.5675(7) 0.107(4) Uani 1 1 d . U . . .
H64 H 0.2463 0.8210 0.5985 0.128 Uiso 1 1 calc R . . . .
C65 C 0.2601(7) 0.7502(7) 0.4934(5) 0.075(2) Uani 1 1 d . U . . .
H65 H 0.3315 0.7363 0.4660 0.090 Uiso 1 1 calc R . . . .
C67 C 0.0394(4) 0.6759(4) 0.4165(4) 0.0391(10) Uani 1 1 d . U . . .
H67 H 0.0737 0.6090 0.4314 0.047 Uiso 1 1 calc R . . . .
C69 C -0.0619(4) 0.6810(4) 0.4058(4) 0.0408(11) Uani 1 1 d . U . . .
C70 C -0.1161(4) 0.7625(4) 0.3675(4) 0.0447(11) Uani 1 1 d . U . . .
C71 C -0.2090(4) 0.7623(5) 0.3575(5) 0.0563(15) Uani 1 1 d . U . . .
H71 H -0.2475 0.8165 0.3315 0.068 Uiso 1 1 calc R . . . .
C72 C -0.2456(5) 0.6837(5) 0.3853(5) 0.0630(16) Uani 1 1 d . U . . .
H72 H -0.3084 0.6846 0.3780 0.076 Uiso 1 1 calc R . . . .
C73 C -0.1904(5) 0.6050(5) 0.4232(5) 0.0573(14) Uani 1 1 d . U . . .
C74 C -0.0988(4) 0.6036(4) 0.4327(4) 0.0462(12) Uani 1 1 d . U . . .
H74 H -0.0605 0.5487 0.4581 0.055 Uiso 1 1 calc R . . . .
S81 S 0.35127(11) 1.17841(10) 0.15611(10) 0.0497(3) Uani 1 1 d . U . . .
O82 O 0.2614(4) 1.1474(4) 0.2159(3) 0.0731(14) Uani 1 1 d . U . . .
C83 C 0.4256(6) 1.0878(6) 0.0783(5) 0.077(2) Uani 1 1 d . U . . .
H83A H 0.4490 1.0288 0.1117 0.116 Uiso 1 1 calc GR . . . .
H83B H 0.4845 1.1060 0.0369 0.116 Uiso 1 1 calc GR . . . .
H83C H 0.3841 1.0789 0.0435 0.116 Uiso 1 1 calc GR . . . .
C84 C 0.2965(10) 1.2478(11) 0.0769(10) 0.079(4) Uani 0.567(14) 1 d . U P A 1
H84A H 0.2684 1.2106 0.0508 0.119 Uiso 0.567(14) 1 calc GR . P A 1
H84B H 0.3482 1.2703 0.0288 0.119 Uiso 0.567(14) 1 calc GR . P A 1
H84C H 0.2419 1.3019 0.1061 0.119 Uiso 0.567(14) 1 calc GR . P A 1
C84A C 0.4304(12) 1.1352(10) 0.2248(11) 0.059(4) Uani 0.433(14) 1 d . U P A 2
H84D H 0.4030 1.1717 0.2792 0.089 Uiso 0.433(14) 1 calc GR . P A 2
H84E H 0.4985 1.1408 0.1917 0.089 Uiso 0.433(14) 1 calc GR . P A 2
H84F H 0.4343 1.0689 0.2422 0.089 Uiso 0.433(14) 1 calc GR . P A 2
S85 S 0.0925(3) 0.5925(2) -0.1235(3) 0.1015(14) Uani 0.769(7) 1 d . U P B 1
S85A S 0.0449(5) 0.6387(5) -0.1600(5) 0.050(2) Uani 0.231(7) 1 d . U P B 2
O86 O 0.1033(4) 0.6898(3) -0.1238(4) 0.0662(12) Uani 1 1 d . U . . .
C87 C -0.0319(11) 0.6039(12) -0.0946(9) 0.152(5) Uani 1 1 d . U . . .
H87A H -0.0422 0.5421 -0.0936 0.228 Uiso 0.769(7) 1 calc R . P B 1
H87B H -0.0653 0.6296 -0.0345 0.228 Uiso 0.769(7) 1 calc R . P B 1
H87C H -0.0613 0.6466 -0.1388 0.228 Uiso 0.769(7) 1 calc R . P B 1
H87D H -0.0625 0.5737 -0.1253 0.228 Uiso 0.231(7) 1 calc R . P B 2
H87E H -0.0017 0.5577 -0.0529 0.228 Uiso 0.231(7) 1 calc R . P B 2
H87F H -0.0845 0.6562 -0.0606 0.228 Uiso 0.231(7) 1 calc R . P B 2
C88 C 0.1353(8) 0.5653(8) -0.2357(9) 0.112(3) Uani 1 1 d . U . . .
H88A H 0.1304 0.5026 -0.2404 0.168 Uiso 0.769(7) 1 calc R . P B 1
H88B H 0.0934 0.6120 -0.2690 0.168 Uiso 0.769(7) 1 calc R . P B 1
H88C H 0.2062 0.5661 -0.2614 0.168 Uiso 0.769(7) 1 calc R . P B 1
H88D H 0.1824 0.5988 -0.2760 0.168 Uiso 0.231(7) 1 calc R . P B 2
H88E H 0.1725 0.5120 -0.2042 0.168 Uiso 0.231(7) 1 calc R . P B 2
H88F H 0.1038 0.5422 -0.2714 0.168 Uiso 0.231(7) 1 calc R . P B 2
O89 O -0.1641(5) 0.8378(4) 0.5999(4) 0.0922(19) Uani 1 1 d . U . . .
O90 O -0.2297(7) 0.9648(5) 0.4579(5) 0.135(4) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O8 1.947(4) . ?
Cu1 O15 1.910(4) . ?
Cu1 O48 1.979(3) . ?
Cu1 O68 2.403(3) . ?
Cu1 N41 1.983(5) . ?
Cu2 O8 1.985(3) . ?
Cu2 O28 1.947(4) . ?
Cu2 O35 1.897(3) . ?
Cu2 O48 2.401(4) . ?
Cu2 N1 1.968(5) . ?
Cu3 O8 2.375(4) . ?
Cu3 O28 1.989(3) . ?
Cu3 O68 1.944(4) . ?
Cu3 O75 1.920(3) . ?
Cu3 N21 1.965(4) . ?
Cu4 O28 2.381(4) . ?
Cu4 O48 1.953(4) . ?
Cu4 O55 1.909(4) . ?
Cu4 O68 1.982(3) . ?
Cu4 N61 1.971(5) . ?
Cl16 C13 1.742(7) . ?
Cl36 C33 1.743(7) . ?
Cl56 C53 1.782(9) . ?
Cl76 C73 1.751(6) . ?
S3 C2 1.734(5) . ?
S3 C4 1.734(6) . ?
S23 C22 1.744(5) . ?
S23 C24 1.740(5) . ?
S43 C42 1.740(5) . ?
S43 C44 1.710(7) . ?
S63 C62 1.728(7) . ?
S63 C64 1.735(10) . ?
O8 C7 1.410(6) . ?
O15 C10 1.323(7) . ?
O28 C27 1.404(6) . ?
O35 C30 1.326(7) . ?
O48 C47 1.405(6) . ?
O55 C50 1.320(8) . ?
O68 C67 1.412(6) . ?
O75 C70 1.335(7) . ?
N1 C2 1.316(7) . ?
N1 C5 1.394(6) . ?
N6 H6 0.8800 . ?
N6 C2 1.344(6) . ?
N6 C7 1.451(7) . ?
N21 C22 1.325(6) . ?
N21 C25 1.397(6) . ?
N26 H26 0.8800 . ?
N26 C22 1.344(6) . ?
N26 C27 1.467(7) . ?
N41 C42 1.323(7) . ?
N41 C45 1.388(6) . ?
N46 H46 0.8800 . ?
N46 C42 1.345(7) . ?
N46 C47 1.460(7) . ?
N61 C62 1.318(9) . ?
N61 C65 1.399(8) . ?
N66 H66 0.8800 . ?
N66 C62 1.352(8) . ?
N66 C67 1.450(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.316(9) . ?
C5 H5 0.9500 . ?
C7 H7 1.0000 . ?
C7 C9 1.516(6) . ?
C9 C10 1.408(8) . ?
C9 C14 1.388(8) . ?
C10 C11 1.410(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.392(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.375(11) . ?
C13 C14 1.391(7) . ?
C14 H14 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.321(8) . ?
C25 H25 0.9500 . ?
C27 H27 1.0000 . ?
C27 C29 1.507(6) . ?
C29 C30 1.414(8) . ?
C29 C34 1.393(8) . ?
C30 C31 1.416(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.365(9) . ?
C32 H32 0.9500 . ?
C32 C33 1.398(10) . ?
C33 C34 1.386(8) . ?
C34 H34 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.357(10) . ?
C45 H45 0.9500 . ?
C47 H47 1.0000 . ?
C47 C49 1.507(6) . ?
C49 C50 1.411(10) . ?
C49 C54 1.387(9) . ?
C50 C51 1.409(8) . ?
C51 H51 0.9500 . ?
C51 C52 1.401(13) . ?
C52 H52 0.9500 . ?
C52 C53 1.341(13) . ?
C53 C54 1.387(9) . ?
C54 H54 0.9500 . ?
C64 H64 0.9500 . ?
C64 C65 1.310(13) . ?
C65 H65 0.9500 . ?
C67 H67 1.0000 . ?
C67 C69 1.511(7) . ?
C69 C70 1.398(8) . ?
C69 C74 1.383(7) . ?
C70 C71 1.408(8) . ?
C71 H71 0.9500 . ?
C71 C72 1.396(9) . ?
C72 H72 0.9500 . ?
C72 C73 1.375(10) . ?
C73 C74 1.380(8) . ?
C74 H74 0.9500 . ?
S81 O82 1.502(4) . ?
S81 C83 1.787(7) . ?
S81 C84 1.731(14) . ?
S81 C84A 1.739(17) . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C84A H84D 0.9800 . ?
C84A H84E 0.9800 . ?
C84A H84F 0.9800 . ?
S85 O86 1.513(5) . ?
S85 C87 1.672(13) . ?
S85 C88 1.726(12) . ?
S85A O86 1.570(7) . ?
S85A C87 1.427(13) . ?
S85A C88 1.672(12) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C87 H87D 0.9800 . ?
C87 H87E 0.9800 . ?
C87 H87F 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C88 H88D 0.9800 . ?
C88 H88E 0.9800 . ?
C88 H88F 0.9800 . ?

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
O8 Cu1 O48 84.03(14) . . ?
O8 Cu1 O68 81.55(13) . . ?
O8 Cu1 N41 172.61(16) . . ?
O15 Cu1 O8 94.68(16) . . ?
O15 Cu1 O48 172.41(17) . . ?
O15 Cu1 O68 114.23(15) . . ?
O15 Cu1 N41 92.48(18) . . ?
O48 Cu1 O68 73.03(13) . . ?
O48 Cu1 N41 89.10(16) . . ?
N41 Cu1 O68 93.86(16) . . ?
O8 Cu2 O48 72.93(13) . . ?
O28 Cu2 O8 84.29(14) . . ?
O28 Cu2 O48 81.66(13) . . ?
O28 Cu2 N1 174.05(15) . . ?
O35 Cu2 O8 172.90(17) . . ?
O35 Cu2 O28 94.70(15) . . ?
O35 Cu2 O48 113.93(15) . . ?
O35 Cu2 N1 91.24(17) . . ?
N1 Cu2 O8 89.85(15) . . ?
N1 Cu2 O48 95.68(16) . . ?
O28 Cu3 O8 73.80(13) . . ?
O68 Cu3 O8 82.34(13) . . ?
O68 Cu3 O28 84.72(14) . . ?
O68 Cu3 N21 174.30(15) . . ?
O75 Cu3 O8 112.85(15) . . ?
O75 Cu3 O28 172.73(17) . . ?
O75 Cu3 O68 93.14(15) . . ?
O75 Cu3 N21 92.40(16) . . ?
N21 Cu3 O8 96.72(16) . . ?
N21 Cu3 O28 89.62(15) . . ?
O48 Cu4 O28 82.05(14) . . ?
O48 Cu4 O68 83.86(14) . . ?
O48 Cu4 N61 172.54(18) . . ?
O55 Cu4 O28 111.36(17) . . ?
O55 Cu4 O48 94.10(18) . . ?
O55 Cu4 O68 173.84(18) . . ?
O55 Cu4 N61 93.3(2) . . ?
O68 Cu4 O28 74.18(13) . . ?
N61 Cu4 O28 94.68(18) . . ?
N61 Cu4 O68 88.81(18) . . ?
C2 S3 C4 88.8(3) . . ?
C24 S23 C22 89.0(2) . . ?
C44 S43 C42 89.2(3) . . ?
C62 S63 C64 89.3(4) . . ?
Cu1 O8 Cu2 108.69(16) . . ?
Cu1 O8 Cu3 96.78(14) . . ?
Cu2 O8 Cu3 93.18(13) . . ?
C7 O8 Cu1 115.6(3) . . ?
C7 O8 Cu2 113.6(3) . . ?
C7 O8 Cu3 125.8(3) . . ?
C10 O15 Cu1 123.9(3) . . ?
Cu2 O28 Cu3 107.73(16) . . ?
Cu2 O28 Cu4 96.88(14) . . ?
Cu3 O28 Cu4 92.49(13) . . ?
C27 O28 Cu2 116.0(3) . . ?
C27 O28 Cu3 115.4(3) . . ?
C27 O28 Cu4 124.6(3) . . ?
C30 O35 Cu2 123.7(3) . . ?
Cu1 O48 Cu2 93.20(14) . . ?
Cu4 O48 Cu1 108.97(16) . . ?
Cu4 O48 Cu2 96.07(14) . . ?
C47 O48 Cu1 114.5(3) . . ?
C47 O48 Cu2 126.6(3) . . ?
C47 O48 Cu4 114.3(3) . . ?
C50 O55 Cu4 123.8(4) . . ?
Cu3 O68 Cu1 95.99(14) . . ?
Cu3 O68 Cu4 107.65(15) . . ?
Cu4 O68 Cu1 93.29(13) . . ?
C67 O68 Cu1 125.5(3) . . ?
C67 O68 Cu3 116.1(3) . . ?
C67 O68 Cu4 114.7(3) . . ?
C70 O75 Cu3 123.4(3) . . ?
C2 N1 Cu2 125.9(3) . . ?
C2 N1 C5 110.6(5) . . ?
C5 N1 Cu2 122.6(4) . . ?
C2 N6 H6 119.2 . . ?
C2 N6 C7 121.6(4) . . ?
C7 N6 H6 119.2 . . ?
C22 N21 Cu3 125.1(3) . . ?
C22 N21 C25 110.3(4) . . ?
C25 N21 Cu3 123.3(3) . . ?
C22 N26 H26 119.2 . . ?
C22 N26 C27 121.6(4) . . ?
C27 N26 H26 119.2 . . ?
C42 N41 Cu1 125.5(3) . . ?
C42 N41 C45 110.6(5) . . ?
C45 N41 Cu1 122.2(4) . . ?
C42 N46 H46 119.5 . . ?
C42 N46 C47 121.1(5) . . ?
C47 N46 H46 119.5 . . ?
C62 N61 Cu4 125.8(4) . . ?
C62 N61 C65 110.9(6) . . ?
C65 N61 Cu4 121.3(5) . . ?
C62 N66 H66 119.3 . . ?
C62 N66 C67 121.5(5) . . ?
C67 N66 H66 119.3 . . ?
N1 C2 S3 114.0(4) . . ?
N1 C2 N6 125.0(5) . . ?
N6 C2 S3 121.0(4) . . ?
S3 C4 H4 124.5 . . ?
C5 C4 S3 111.0(4) . . ?
C5 C4 H4 124.5 . . ?
N1 C5 H5 122.2 . . ?
C4 C5 N1 115.6(5) . . ?
C4 C5 H5 122.2 . . ?
O8 C7 N6 111.1(4) . . ?
O8 C7 H7 108.9 . . ?
O8 C7 C9 111.3(4) . . ?
N6 C7 H7 108.9 . . ?
N6 C7 C9 107.8(4) . . ?
C9 C7 H7 108.9 . . ?
C10 C9 C7 120.7(5) . . ?
C14 C9 C7 118.3(5) . . ?
C14 C9 C10 120.9(5) . . ?
O15 C10 C9 124.0(4) . . ?
O15 C10 C11 118.8(6) . . ?
C9 C10 C11 117.2(6) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 C10 121.4(7) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 Cl16 120.9(4) . . ?
C12 C13 C14 119.8(6) . . ?
C14 C13 Cl16 119.3(6) . . ?
C9 C14 C13 120.5(6) . . ?
C9 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
N21 C22 S23 113.8(4) . . ?
N21 C22 N26 125.6(5) . . ?
N26 C22 S23 120.6(4) . . ?
S23 C24 H24 124.6 . . ?
C25 C24 S23 110.7(4) . . ?
C25 C24 H24 124.6 . . ?
N21 C25 H25 121.9 . . ?
C24 C25 N21 116.2(5) . . ?
C24 C25 H25 121.9 . . ?
O28 C27 N26 108.8(4) . . ?
O28 C27 H27 109.3 . . ?
O28 C27 C29 111.8(4) . . ?
N26 C27 H27 109.3 . . ?
N26 C27 C29 108.4(4) . . ?
C29 C27 H27 109.3 . . ?
C30 C29 C27 120.7(5) . . ?
C34 C29 C27 119.1(5) . . ?
C34 C29 C30 120.2(5) . . ?
O35 C30 C29 123.7(4) . . ?
O35 C30 C31 118.7(5) . . ?
C29 C30 C31 117.5(5) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 C30 122.1(6) . . ?
C32 C31 H31 119.0 . . ?
C31 C32 H32 120.3 . . ?
C31 C32 C33 119.4(5) . . ?
C33 C32 H32 120.3 . . ?
C32 C33 Cl36 119.2(4) . . ?
C34 C33 Cl36 120.3(5) . . ?
C34 C33 C32 120.5(6) . . ?
C29 C34 H34 119.9 . . ?
C33 C34 C29 120.2(6) . . ?
C33 C34 H34 119.9 . . ?
N41 C42 S43 114.2(4) . . ?
N41 C42 N46 124.9(5) . . ?
N46 C42 S43 121.0(4) . . ?
S43 C44 H44 124.4 . . ?
C45 C44 S43 111.3(4) . . ?
C45 C44 H44 124.4 . . ?
N41 C45 H45 122.6 . . ?
C44 C45 N41 114.8(6) . . ?
C44 C45 H45 122.6 . . ?
O48 C47 N46 109.6(4) . . ?
O48 C47 H47 108.9 . . ?
O48 C47 C49 111.1(4) . . ?
N46 C47 H47 108.9 . . ?
N46 C47 C49 109.4(4) . . ?
C49 C47 H47 108.9 . . ?
C50 C49 C47 120.3(5) . . ?
C54 C49 C47 118.0(6) . . ?
C54 C49 C50 121.6(5) . . ?
O55 C50 C49 123.6(5) . . ?
O55 C50 C51 120.5(7) . . ?
C51 C50 C49 115.9(7) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 C50 121.1(8) . . ?
C52 C51 H51 119.4 . . ?
C51 C52 H52 119.3 . . ?
C53 C52 C51 121.4(6) . . ?
C53 C52 H52 119.3 . . ?
C52 C53 Cl56 122.6(5) . . ?
C52 C53 C54 119.6(7) . . ?
C54 C53 Cl56 117.7(7) . . ?
C49 C54 H54 119.8 . . ?
C53 C54 C49 120.3(8) . . ?
C53 C54 H54 119.8 . . ?
N61 C62 S63 113.4(5) . . ?
N61 C62 N66 125.0(6) . . ?
N66 C62 S63 121.5(5) . . ?
S63 C64 H64 124.6 . . ?
C65 C64 S63 110.8(6) . . ?
C65 C64 H64 124.6 . . ?
N61 C65 H65 122.2 . . ?
C64 C65 N61 115.6(8) . . ?
C64 C65 H65 122.2 . . ?
O68 C67 N66 110.6(4) . . ?
O68 C67 H67 108.6 . . ?
O68 C67 C69 110.8(4) . . ?
N66 C67 H67 108.6 . . ?
N66 C67 C69 109.5(4) . . ?
C69 C67 H67 108.6 . . ?
C70 C69 C67 120.1(5) . . ?
C74 C69 C67 119.0(5) . . ?
C74 C69 C70 120.8(5) . . ?
O75 C70 C69 123.3(5) . . ?
O75 C70 C71 119.2(5) . . ?
C69 C70 C71 117.5(5) . . ?
C70 C71 H71 119.4 . . ?
C72 C71 C70 121.1(6) . . ?
C72 C71 H71 119.4 . . ?
C71 C72 H72 120.1 . . ?
C73 C72 C71 119.8(6) . . ?
C73 C72 H72 120.1 . . ?
C72 C73 Cl76 120.8(5) . . ?
C72 C73 C74 119.9(6) . . ?
C74 C73 Cl76 119.3(5) . . ?
C69 C74 H74 119.6 . . ?
C73 C74 C69 120.9(6) . . ?
C73 C74 H74 119.6 . . ?
O82 S81 C83 106.8(3) . . ?
O82 S81 C84 99.0(5) . . ?
O82 S81 C84A 98.0(5) . . ?
C84 S81 C83 92.3(6) . . ?
C84A S81 C83 91.5(6) . . ?
S81 C83 H83A 109.5 . . ?
S81 C83 H83B 109.5 . . ?
S81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
S81 C84 H84A 109.5 . . ?
S81 C84 H84B 109.5 . . ?
S81 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
S81 C84A H84D 109.5 . . ?
S81 C84A H84E 109.5 . . ?
S81 C84A H84F 109.5 . . ?
H84D C84A H84E 109.5 . . ?
H84D C84A H84F 109.5 . . ?
H84E C84A H84F 109.5 . . ?
O86 S85 C87 106.9(6) . . ?
O86 S85 C88 105.2(5) . . ?
C87 S85 C88 103.4(6) . . ?
O86 S85A C88 105.1(5) . . ?
C87 S85A O86 117.2(7) . . ?
C87 S85A C88 118.6(9) . . ?
S85 C87 H87A 109.5 . . ?
S85 C87 H87B 109.5 . . ?
S85 C87 H87C 109.5 . . ?
S85A C87 H87D 109.5 . . ?
S85A C87 H87E 109.5 . . ?
S85A C87 H87F 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
H87D C87 H87E 109.5 . . ?
H87D C87 H87F 109.5 . . ?
H87E C87 H87F 109.5 . . ?
S85 C88 H88A 109.5 . . ?
S85 C88 H88B 109.5 . . ?
S85 C88 H88C 109.5 . . ?
S85A C88 H88D 109.5 . . ?
S85A C88 H88E 109.5 . . ?
S85A C88 H88F 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
H88D C88 H88E 109.5 . . ?
H88D C88 H88F 109.5 . . ?
H88E C88 H88F 109.5 . . ?

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
N6 H6 O86 0.88 1.89 2.748(6) 163.1 .
N26 H26 O82 0.88 2.09 2.804(6) 138.3 .
N66 H66 O89 0.88 1.95 2.807(7) 165.5 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O8 C7 N6 -58.0(4) . . . . ?
Cu1 O8 C7 C9 62.2(5) . . . . ?
Cu1 O15 C10 C9 25.9(7) . . . . ?
Cu1 O15 C10 C11 -157.1(4) . . . . ?
Cu1 O48 C47 N46 -70.8(5) . . . . ?
Cu1 O48 C47 C49 168.1(4) . . . . ?
Cu1 O68 C67 N66 -176.5(3) . . . . ?
Cu1 O68 C67 C69 -54.9(5) . . . . ?
Cu1 N41 C42 S43 165.8(3) . . . . ?
Cu1 N41 C42 N46 -13.6(8) . . . . ?
Cu1 N41 C45 C44 -166.3(5) . . . . ?
Cu2 O8 C7 N6 68.7(4) . . . . ?
Cu2 O8 C7 C9 -171.2(3) . . . . ?
Cu2 O28 C27 N26 58.4(4) . . . . ?
Cu2 O28 C27 C29 -61.3(5) . . . . ?
Cu2 O35 C30 C29 -28.6(7) . . . . ?
Cu2 O35 C30 C31 153.9(4) . . . . ?
Cu2 O48 C47 N46 174.7(3) . . . . ?
Cu2 O48 C47 C49 53.6(6) . . . . ?
Cu2 N1 C2 S3 -170.4(3) . . . . ?
Cu2 N1 C2 N6 8.4(8) . . . . ?
Cu2 N1 C5 C4 170.3(5) . . . . ?
Cu3 O8 C7 N6 -178.4(3) . . . . ?
Cu3 O8 C7 C9 -58.3(5) . . . . ?
Cu3 O28 C27 N26 -69.0(4) . . . . ?
Cu3 O28 C27 C29 171.3(3) . . . . ?
Cu3 O68 C67 N66 -57.1(5) . . . . ?
Cu3 O68 C67 C69 64.5(5) . . . . ?
Cu3 O75 C70 C69 32.6(7) . . . . ?
Cu3 O75 C70 C71 -149.1(5) . . . . ?
Cu3 N21 C22 S23 167.6(3) . . . . ?
Cu3 N21 C22 N26 -11.3(8) . . . . ?
Cu3 N21 C25 C24 -168.0(4) . . . . ?
Cu4 O28 C27 N26 178.3(3) . . . . ?
Cu4 O28 C27 C29 58.6(5) . . . . ?
Cu4 O48 C47 N46 56.0(5) . . . . ?
Cu4 O48 C47 C49 -65.1(5) . . . . ?
Cu4 O55 C50 C49 -28.5(8) . . . . ?
Cu4 O55 C50 C51 153.2(5) . . . . ?
Cu4 O68 C67 N66 69.5(5) . . . . ?
Cu4 O68 C67 C69 -168.8(3) . . . . ?
Cu4 N61 C62 S63 -165.2(3) . . . . ?
Cu4 N61 C62 N66 16.4(10) . . . . ?
Cu4 N61 C65 C64 164.7(8) . . . . ?
Cl16 C13 C14 C9 -179.6(4) . . . . ?
Cl36 C33 C34 C29 177.3(5) . . . . ?
Cl56 C53 C54 C49 176.9(5) . . . . ?
Cl76 C73 C74 C69 -177.3(5) . . . . ?
S3 C4 C5 N1 0.0(8) . . . . ?
S23 C24 C25 N21 0.1(7) . . . . ?
S43 C44 C45 N41 0.2(8) . . . . ?
S63 C64 C65 N61 1.3(13) . . . . ?
O8 C7 C9 C10 -48.8(6) . . . . ?
O8 C7 C9 C14 133.4(5) . . . . ?
O15 C10 C11 C12 -178.9(6) . . . . ?
O28 Cu2 O35 C30 11.4(4) . . . . ?
O28 C27 C29 C30 46.9(7) . . . . ?
O28 C27 C29 C34 -132.4(5) . . . . ?
O35 C30 C31 C32 178.8(6) . . . . ?
O48 Cu2 O35 C30 -71.6(4) . . . . ?
O48 C47 C49 C50 48.8(7) . . . . ?
O48 C47 C49 C54 -129.6(5) . . . . ?
O55 C50 C51 C52 179.3(6) . . . . ?
O68 C67 C69 C70 -48.0(6) . . . . ?
O68 C67 C69 C74 130.7(5) . . . . ?
O75 C70 C71 C72 -178.2(6) . . . . ?
N1 Cu2 O35 C30 -168.4(4) . . . . ?
N6 C7 C9 C10 73.3(6) . . . . ?
N6 C7 C9 C14 -104.6(6) . . . . ?
N26 C27 C29 C30 -73.0(6) . . . . ?
N26 C27 C29 C34 107.7(6) . . . . ?
N46 C47 C49 C50 -72.4(6) . . . . ?
N46 C47 C49 C54 109.2(6) . . . . ?
N66 C67 C69 C70 74.2(6) . . . . ?
N66 C67 C69 C74 -107.1(6) . . . . ?
C2 S3 C4 C5 -0.7(5) . . . . ?
C2 N1 C5 C4 0.9(8) . . . . ?
C2 N6 C7 O8 -53.6(6) . . . . ?
C2 N6 C7 C9 -175.8(5) . . . . ?
C4 S3 C2 N1 1.2(4) . . . . ?
C4 S3 C2 N6 -177.6(5) . . . . ?
C5 N1 C2 S3 -1.4(6) . . . . ?
C5 N1 C2 N6 177.4(5) . . . . ?
C7 N6 C2 S3 -169.2(4) . . . . ?
C7 N6 C2 N1 12.1(8) . . . . ?
C7 C9 C10 O15 1.8(8) . . . . ?
C7 C9 C10 C11 -175.3(5) . . . . ?
C7 C9 C14 C13 176.3(5) . . . . ?
C9 C10 C11 C12 -1.6(9) . . . . ?
C10 C9 C14 C13 -1.5(8) . . . . ?
C10 C11 C12 C13 -0.2(10) . . . . ?
C11 C12 C13 Cl16 -179.6(5) . . . . ?
C11 C12 C13 C14 1.3(10) . . . . ?
C12 C13 C14 C9 -0.5(9) . . . . ?
C14 C9 C10 O15 179.6(5) . . . . ?
C14 C9 C10 C11 2.5(8) . . . . ?
C22 S23 C24 C25 -0.1(5) . . . . ?
C22 N21 C25 C24 -0.2(7) . . . . ?
C22 N26 C27 O28 54.5(6) . . . . ?
C22 N26 C27 C29 176.3(5) . . . . ?
C24 S23 C22 N21 0.0(4) . . . . ?
C24 S23 C22 N26 179.0(5) . . . . ?
C25 N21 C22 S23 0.1(6) . . . . ?
C25 N21 C22 N26 -178.8(5) . . . . ?
C27 N26 C22 S23 168.7(4) . . . . ?
C27 N26 C22 N21 -12.4(8) . . . . ?
C27 C29 C30 O35 1.0(8) . . . . ?
C27 C29 C30 C31 178.5(5) . . . . ?
C27 C29 C34 C33 -178.6(6) . . . . ?
C29 C30 C31 C32 1.2(9) . . . . ?
C30 C29 C34 C33 2.1(9) . . . . ?
C30 C31 C32 C33 0.0(10) . . . . ?
C31 C32 C33 Cl36 -178.3(6) . . . . ?
C31 C32 C33 C34 -0.1(11) . . . . ?
C32 C33 C34 C29 -1.0(11) . . . . ?
C34 C29 C30 O35 -179.7(5) . . . . ?
C34 C29 C30 C31 -2.2(8) . . . . ?
C42 S43 C44 C45 0.1(5) . . . . ?
C42 N41 C45 C44 -0.5(8) . . . . ?
C42 N46 C47 O48 54.8(7) . . . . ?
C42 N46 C47 C49 176.9(5) . . . . ?
C44 S43 C42 N41 -0.3(5) . . . . ?
C44 S43 C42 N46 179.1(5) . . . . ?
C45 N41 C42 S43 0.5(6) . . . . ?
C45 N41 C42 N46 -178.9(5) . . . . ?
C47 N46 C42 S43 170.3(4) . . . . ?
C47 N46 C42 N41 -10.3(8) . . . . ?
C47 C49 C50 O55 1.3(9) . . . . ?
C47 C49 C50 C51 179.8(6) . . . . ?
C47 C49 C54 C53 -179.2(6) . . . . ?
C49 C50 C51 C52 0.8(10) . . . . ?
C50 C49 C54 C53 2.4(10) . . . . ?
C50 C51 C52 C53 -0.3(12) . . . . ?
C51 C52 C53 Cl56 -177.8(6) . . . . ?
C51 C52 C53 C54 0.8(12) . . . . ?
C52 C53 C54 C49 -1.8(11) . . . . ?
C54 C49 C50 O55 179.7(6) . . . . ?
C54 C49 C50 C51 -1.9(9) . . . . ?
C62 S63 C64 C65 -1.7(10) . . . . ?
C62 N61 C65 C64 -0.1(12) . . . . ?
C62 N66 C67 O68 -49.6(7) . . . . ?
C62 N66 C67 C69 -172.0(6) . . . . ?
C64 S63 C62 N61 1.7(7) . . . . ?
C64 S63 C62 N66 -179.9(7) . . . . ?
C65 N61 C62 S63 -1.3(8) . . . . ?
C65 N61 C62 N66 -179.7(7) . . . . ?
C67 N66 C62 S63 -173.9(5) . . . . ?
C67 N66 C62 N61 4.4(10) . . . . ?
C67 C69 C70 O75 -3.0(8) . . . . ?
C67 C69 C70 C71 178.7(5) . . . . ?
C67 C69 C74 C73 -179.2(5) . . . . ?
C69 C70 C71 C72 0.2(10) . . . . ?
C70 C69 C74 C73 -0.6(9) . . . . ?
C70 C71 C72 C73 0.1(11) . . . . ?
C71 C72 C73 Cl76 177.5(6) . . . . ?
C71 C72 C73 C74 -0.7(11) . . . . ?
C72 C73 C74 C69 0.9(10) . . . . ?
C74 C69 C70 O75 178.4(5) . . . . ?
C74 C69 C70 C71 0.0(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
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 -9 -1 0.0827 0.9957 -8.9950 -1.0025 0.5646 0.0314 -0.8486
1 0 -9 0.0800 0.9978 0.0018 -9.0184 -0.7296 -0.0903 -0.6490
0 7 -6 0.0951 0.0017 6.9975 -6.0119 -0.9890 -0.0901 0.1696
-1 8 3 0.0726 -0.9956 7.9953 3.0065 -0.3328 0.0050 0.8984
-2 4 8 0.0603 -1.9969 3.9957 8.0165 0.3733 -0.0063 0.9695
-1 -5 7 0.0956 -1.0011 -4.9993 7.0140 0.9379 0.0251 0.1209
-1 -1 -1 0.0236 -1.0017 -1.0002 -1.0022 0.0105 -0.1207 -0.0782
1 1 1 0.0196 1.0017 1.0002 1.0022 -0.0105 0.1207 0.0782
1 7 7 0.0525 1.0068 6.9969 7.0149 0.0247 0.2732 0.9452
-9 -1 -2 0.0770 -9.0085 -1.0065 -2.0050 0.0625 -0.9031 0.3870
9 3 4 0.0798 9.0102 3.0054 4.0092 -0.0507 0.9540 -0.0980
1 -7 -6 0.0902 0.9951 -6.9954 -6.0126 0.0217 -0.0621 -1.0129

_nottingham_internal_coll_instrument 'GVA, PL13110002'
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_skwllh_sq
_database_code_depnum_ccdc_archive 'CCDC 1507036'
_audit_update_record             
;
2016-09-27 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_nottingham_internal_coll_name   SKWLLH
_nottingham_internal_coll_number 14030
_nottingham_internal_coll_client SN/WL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '60.0000, 240.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   02/10/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 15/01/2015
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 3/10/2014
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 15/1/2015
_nottingham_internal_refinement_user pczwl
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 15/1/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 15/1/2015
_refine_special_details          
;
A region of disordered solvent could not be modelled as a sensible chemical 
entity, so the structure was treated with PLATON SQUEEZE. As the nature of the 
removed solvent could not be determeined they were not included in the formula. 
The removed solvent molecule(s) would likely have been a hydrogen bond acceptor 
for N46.

DMSO molecule S81-C84 exhibited disorder of one of the methyl groups over two 
postions. The occupancies of the two components were refined competitively, 
converging at a ratio of 0.50:0.50.

DMSO molecule S85-C88 exhibited disorder of the central sulphur atom. The 
occupancies of the two components were refined competitively, converging 
at a ratio of 0.76:0.24.
;
_vrf_PLAT084_skwllh_sq           
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: This is indicative of the weak/poor quality dataset.
;
_vrf_PLAT306_skwllh_sq           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O89 Check 
RESPONSE: Positions for the hydrogen atoms of water molecules O89 and O90 
could not be determined, and so these were not included on the model, although 
they were included in the formula, and calculation of dreived parameters.
;
_vrf_PLAT341_skwllh_sq           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0237 Ang.  
RESPONSE: This is indicative of the weak/poor quality dataset.
;
_vrf_PLAT430_skwllh_sq           
;
PROBLEM: Short Inter D...A Contact  O75    ..  O90     ..       2.71 Ang.  
RESPONSE: As the hydrogen atoms positions of water molecules O89 and O90 could 
not be determined, and so hydrogen bonds cannot be calculated for these molecules.
;
_vrf_PLAT973_skwllh_sq           
;
PROBLEM: Check Calcd Positive Residual Density on     Cu1       2.21 eA-3  
RESPONSE: This large residual density feature could not be sensibly assigned 
as disorder, and no twinning is present in the structure. It is in a chemically 
nonsensical position, and is an indicator of the low quality of the dataset.
;
_vrf_RFACR01_skwllh_sq           
;
PROBLEM: The value of the weighted R factor is > 0.35
RESPONSE: This is due to the relative poor quality of the datset.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.033 0.033 0.528 16 0 ' '
2 -0.041 0.960 0.466 14 -1 ' '
3 0.500 0.500 0.500 347 145 ' '

_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_audit_creation_date             2015-01-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H28 Br4 Cu4 N8 O8 S4, 2(C2 H6 O S), 2(O)'
_chemical_formula_sum            'C44 H44 Br4 Cu4 N8 O12 S6'
_chemical_formula_weight         1643.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H44 Br4 Cu4 N8 O12 S6'
_chemical_oxdiff_usercomment     
'SKWLLH #14030 SN-314 IN FOMBLIN FILM ON A MICROMOUNT FOR SN/WL'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.5404(14)
_cell_length_b                   15.0453(15)
_cell_length_c                   15.6677(16)
_cell_angle_alpha                81.325(9)
_cell_angle_beta                 70.620(9)
_cell_angle_gamma                71.468(9)
_cell_volume                     3061.7(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7686
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6040
_cell_measurement_theta_min      4.1080
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.049
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.0662
_exptl_crystal_size_min          0.0264
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32366
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.364
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -91.00  -64.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -164.0000 -101.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega -108.00  -16.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -180.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega  -90.00  -54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega -109.00  -13.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000   60.0000 96

#__ type_ start__ end____ width___ exp.time_
  5 omega  -64.00   32.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
  6 omega   87.00  114.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277  164.0000  -76.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00   70.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -30.0000  -30.0000 33

#__ type_ start__ end____ width___ exp.time_
  8 omega   42.00   98.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -95.0000 -180.0000 56

#__ type_ start__ end____ width___ exp.time_
  9 omega   89.00  171.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822   45.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00   72.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -30.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
 11 omega   36.00   87.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -30.0000    0.0000 51

#__ type_ start__ end____ width___ exp.time_
 12 omega   61.00  119.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822 -125.0000   90.0000 58

#__ type_ start__ end____ width___ exp.time_
 13 omega   41.00   91.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -30.0000   90.0000 50

#__ type_ start__ end____ width___ exp.time_
 14 omega   64.00   91.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -95.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 15 omega   44.00   92.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -45.0000  150.0000 48

#__ type_ start__ end____ width___ exp.time_
 16 omega   27.00  151.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -15.0000 -180.0000 124

#__ type_ start__ end____ width___ exp.time_
 17 omega   56.00   87.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -30.0000 -120.0000 31

#__ type_ start__ end____ width___ exp.time_
 18 omega   36.00   89.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -45.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 19 omega   47.00  121.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822 -125.0000  -60.0000 74

#__ type_ start__ end____ width___ exp.time_
 20 omega   39.00  132.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -77.0000  -90.0000 93

#__ type_ start__ end____ width___ exp.time_
 21 omega   50.00  105.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822  -95.0000   90.0000 55

#__ type_ start__ end____ width___ exp.time_
 22 omega -109.00  -12.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000  -60.0000 97

#__ type_ start__ end____ width___ exp.time_
 23 omega   12.00  117.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277   77.0000   30.0000 105

#__ type_ start__ end____ width___ exp.time_
 24 omega   12.00  117.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277   77.0000  120.0000 105

#__ type_ start__ end____ width___ exp.time_
 25 omega   23.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277 -125.0000   60.0000 75

#__ type_ start__ end____ width___ exp.time_
 26 omega    1.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277  -99.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
 27 omega   16.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277   57.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
 28 omega   21.00  168.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3822    0.0000  -60.0000 147
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0428575000
_diffrn_orient_matrix_UB_12      0.1076500000
_diffrn_orient_matrix_UB_13      0.0020253000
_diffrn_orient_matrix_UB_21      0.0180375000
_diffrn_orient_matrix_UB_22      0.0064053000
_diffrn_orient_matrix_UB_23      -0.1030574000
_diffrn_orient_matrix_UB_31      -0.1076382000
_diffrn_orient_matrix_UB_32      -0.0079647000
_diffrn_orient_matrix_UB_33      0.0163575000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6385
_reflns_number_total             10828
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.629
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         10828
_refine_ls_number_restraints     1351
_refine_ls_R_factor_all          0.1781
_refine_ls_R_factor_gt           0.1273
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3317
_refine_ls_wR_factor_ref         0.3879
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S85-O86 \\sim S85A-O86
 with sigma of 0.02
 S85A-C88 \\sim S85-C88 \\sim S85-C87 \\sim S85A-C87
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S85A)=Sof(H87D)=Sof(H87E)=Sof(H87F)=Sof(H88D)=Sof(H88E)=Sof(H88F)=1-FVAR(1)
 Sof(S85)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(1)
 Sof(C84A)=Sof(H84D)=Sof(H84E)=Sof(H84F)=1-FVAR(2)
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(2)
6.a Riding coordinates:
 C84A(H84D,H84E,H84F)
6.b Ternary CH refined with riding coordinates:
 C7(H7), C27(H27), C47(H47), C67(H67)
6.c Me refined with riding coordinates:
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C87(H87A,H87B,H87C), C87(H87D,H87E,
 H87F), C88(H88A,H88B,H88C), C88(H88D,H88E,H88F)
6.d Aromatic/amide H refined with riding coordinates:
 N6(H6), N26(H26), N46(H46), N66(H66), C12(H12), C4(H4), C5(H5), C11(H11),
 C14(H14), C24(H24), C25(H25), C31(H31), C32(H32), C34(H34), C44(H44), C45(H45),
  C51(H51), C52(H52), C54(H54), C64(H64), C65(H65), C71(H71), C72(H72), C74(H74)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br16 Br -0.26373(14) 0.98180(17) 0.03891(17) 0.0907(7) Uani 1 1 d . U . . .
Br36 Br 0.49754(18) 0.9390(3) 0.4225(2) 0.1240(11) Uani 1 1 d . U . . .
Br56 Br 0.73784(17) 0.5332(3) -0.0032(2) 0.1244(11) Uani 1 1 d . U . . .
Br76 Br -0.24732(18) 0.50572(16) 0.47491(18) 0.0953(7) Uani 1 1 d . U . . .
Cu1 Cu 0.14633(13) 0.64381(13) 0.18984(14) 0.0488(5) Uani 1 1 d . U . . .
Cu2 Cu 0.26491(13) 0.79985(13) 0.13901(13) 0.0471(5) Uani 1 1 d . U . . .
Cu3 Cu 0.05327(13) 0.83925(13) 0.29432(13) 0.0490(5) Uani 1 1 d . U . . .
Cu4 Cu 0.24175(14) 0.68160(14) 0.33335(14) 0.0504(5) Uani 1 1 d . U . . .
S3 S 0.3467(3) 0.6879(3) -0.1343(3) 0.0633(9) Uani 1 1 d . U . . .
S23 S 0.0385(3) 1.1311(3) 0.1727(3) 0.0578(8) Uani 1 1 d . U . . .
S43 S 0.2334(3) 0.3573(3) 0.3268(3) 0.0682(10) Uani 1 1 d . U . . .
S63 S 0.0722(5) 0.8213(6) 0.5969(5) 0.126(2) Uani 1 1 d . U . . .
O8 O 0.1360(6) 0.7757(6) 0.1489(6) 0.0480(15) Uani 1 1 d . U . . .
O15 O 0.0335(7) 0.6420(7) 0.1543(7) 0.0590(19) Uani 1 1 d . U . . .
O28 O 0.1977(6) 0.8369(6) 0.2650(6) 0.0446(15) Uani 1 1 d . U . . .
O35 O 0.3796(6) 0.8415(7) 0.1255(7) 0.0543(18) Uani 1 1 d . U . . .
O48 O 0.2720(6) 0.6452(6) 0.2101(6) 0.0491(16) Uani 1 1 d . U . . .
O55 O 0.3804(8) 0.6395(8) 0.3335(8) 0.065(2) Uani 1 1 d . U . . .
O68 O 0.1002(6) 0.7069(6) 0.3350(6) 0.0484(15) Uani 1 1 d . U . . .
O75 O -0.0879(7) 0.8421(7) 0.3394(7) 0.061(2) Uani 1 1 d . U . . .
N1 N 0.3231(8) 0.7571(8) 0.0129(8) 0.0521(19) Uani 1 1 d . U . . .
N6 N 0.1695(8) 0.7502(8) -0.0038(8) 0.051(2) Uani 1 1 d . U . . .
H6 H 0.1426 0.7255 -0.0335 0.062 Uiso 1 1 calc R . . . .
N21 N 0.0201(8) 0.9752(8) 0.2502(8) 0.051(2) Uani 1 1 d . U . . .
N26 N 0.1798(9) 0.9963(8) 0.2332(8) 0.053(2) Uani 1 1 d . U . . .
H26 H 0.2210 1.0306 0.2050 0.064 Uiso 1 1 calc R . . . .
N41 N 0.1714(8) 0.5103(8) 0.2383(8) 0.054(2) Uani 1 1 d . U . . .
N46 N 0.3335(9) 0.4850(8) 0.2505(9) 0.057(2) Uani 1 1 d . U . . .
H46 H 0.3777 0.4531 0.2790 0.068 Uiso 1 1 calc R . . . .
N61 N 0.1905(11) 0.7282(10) 0.4580(9) 0.067(2) Uani 1 1 d . U . . .
N66 N 0.0177(10) 0.7390(10) 0.4880(9) 0.067(2) Uani 1 1 d . U . . .
H66 H -0.0450 0.7631 0.5223 0.081 Uiso 1 1 calc R . . . .
C13 C -0.1701(11) 0.8729(13) 0.0725(11) 0.064(3) Uani 1 1 d . U . . .
C9 C 0.0000(10) 0.7999(11) 0.0880(10) 0.055(2) Uani 1 1 d . U . . .
C2 C 0.2714(10) 0.7352(10) -0.0321(10) 0.052(2) Uani 1 1 d . U . . .
C12 C -0.1966(11) 0.7911(13) 0.1060(11) 0.066(3) Uani 1 1 d . U . . .
H12 H -0.2621 0.7874 0.1106 0.079 Uiso 1 1 calc R . . . .
C4 C 0.4522(11) 0.6943(11) -0.1102(11) 0.060(3) Uani 1 1 d . U . . .
H4 H 0.5205 0.6731 -0.1479 0.072 Uiso 1 1 calc R . . . .
C10 C -0.0290(10) 0.7159(11) 0.1271(10) 0.056(2) Uani 1 1 d . U . . .
C5 C 0.4241(10) 0.7331(10) -0.0320(11) 0.058(2) Uani 1 1 d . U . . .
H5 H 0.4720 0.7435 -0.0084 0.070 Uiso 1 1 calc R . . . .
C7 C 0.1020(10) 0.8053(11) 0.0736(9) 0.053(2) Uani 1 1 d . U . . .
H7 H 0.1019 0.8723 0.0576 0.063 Uiso 1 1 calc R . . . .
C11 C -0.1263(11) 0.7139(12) 0.1330(11) 0.061(3) Uani 1 1 d . U . . .
H11 H -0.1455 0.6582 0.1561 0.074 Uiso 1 1 calc R . . . .
C14 C -0.0730(10) 0.8778(12) 0.0654(10) 0.057(2) Uani 1 1 d . U . . .
H14 H -0.0566 0.9352 0.0448 0.068 Uiso 1 1 calc R . . . .
C22 C 0.0856(10) 1.0235(10) 0.2245(10) 0.054(2) Uani 1 1 d . U . . .
C24 C -0.0764(11) 1.1059(11) 0.1906(11) 0.060(3) Uani 1 1 d . U . . .
H24 H -0.1337 1.1461 0.1740 0.072 Uiso 1 1 calc R . . . .
C25 C -0.0697(10) 1.0207(10) 0.2314(10) 0.054(2) Uani 1 1 d . U . . .
H25 H -0.1238 0.9931 0.2466 0.065 Uiso 1 1 calc R . . . .
C27 C 0.2170(10) 0.9136(9) 0.2864(9) 0.049(2) Uani 1 1 d . U . . .
H27 H 0.1790 0.9253 0.3517 0.059 Uiso 1 1 calc R . . . .
C29 C 0.3260(10) 0.8985(10) 0.2740(10) 0.054(2) Uani 1 1 d . U . . .
C30 C 0.4005(10) 0.8643(10) 0.1917(10) 0.053(2) Uani 1 1 d . U . . .
C31 C 0.5036(11) 0.8509(11) 0.1827(11) 0.062(3) Uani 1 1 d . U . . .
H31 H 0.5546 0.8270 0.1286 0.074 Uiso 1 1 calc R . . . .
C32 C 0.5312(11) 0.8724(11) 0.2525(11) 0.063(3) Uani 1 1 d . U . . .
H32 H 0.6008 0.8634 0.2463 0.075 Uiso 1 1 calc R . . . .
C33 C 0.4586(12) 0.9059(12) 0.3284(12) 0.067(3) Uani 1 1 d . U . . .
C34 C 0.3567(11) 0.9165(11) 0.3422(11) 0.060(3) Uani 1 1 d . U . . .
H34 H 0.3079 0.9362 0.3987 0.072 Uiso 1 1 calc R . . . .
C42 C 0.2480(11) 0.4628(10) 0.2652(11) 0.057(2) Uani 1 1 d . U . . .
C44 C 0.1121(12) 0.3853(11) 0.3153(12) 0.070(3) Uani 1 1 d . U . . .
H44 H 0.0665 0.3481 0.3394 0.083 Uiso 1 1 calc R . . . .
C45 C 0.0922(11) 0.4696(11) 0.2659(11) 0.062(3) Uani 1 1 d . U . . .
H45 H 0.0299 0.4972 0.2521 0.074 Uiso 1 1 calc R . . . .
C47 C 0.3535(9) 0.5634(9) 0.1860(10) 0.049(2) Uani 1 1 d . U . . .
H47 H 0.3608 0.5473 0.1240 0.059 Uiso 1 1 calc R . . . .
C49 C 0.4509(10) 0.5787(10) 0.1854(11) 0.055(2) Uani 1 1 d . U . . .
C50 C 0.4566(11) 0.6135(11) 0.2622(12) 0.062(2) Uani 1 1 d . U . . .
C51 C 0.5521(11) 0.6253(12) 0.2538(13) 0.070(3) Uani 1 1 d . U . . .
H51 H 0.5598 0.6500 0.3026 0.084 Uiso 1 1 calc R . . . .
C52 C 0.6331(12) 0.6024(13) 0.1784(13) 0.074(3) Uani 1 1 d . U . . .
H52 H 0.6960 0.6105 0.1762 0.089 Uiso 1 1 calc R . . . .
C53 C 0.6261(13) 0.5678(14) 0.1052(14) 0.076(3) Uani 1 1 d . U . . .
C54 C 0.5332(11) 0.5534(11) 0.1099(12) 0.064(3) Uani 1 1 d . U . . .
H54 H 0.5277 0.5265 0.0613 0.077 Uiso 1 1 calc R . . . .
C62 C 0.0964(14) 0.7563(15) 0.5045(13) 0.082(3) Uani 1 1 d . U . . .
C64 C 0.2064(18) 0.807(2) 0.5612(16) 0.109(4) Uani 1 1 d . U . . .
H64 H 0.2401 0.8332 0.5893 0.131 Uiso 1 1 calc R . . . .
C65 C 0.2495(15) 0.7571(15) 0.4923(13) 0.085(3) Uani 1 1 d . U . . .
H65 H 0.3213 0.7405 0.4657 0.102 Uiso 1 1 calc R . . . .
C67 C 0.0364(11) 0.6806(11) 0.4135(10) 0.056(2) Uani 1 1 d . U . . .
H67 H 0.0703 0.6144 0.4306 0.068 Uiso 1 1 calc R . . . .
C69 C -0.0658(11) 0.6834(11) 0.4056(10) 0.059(2) Uani 1 1 d . U . . .
C70 C -0.1191(11) 0.7656(11) 0.3637(11) 0.062(2) Uani 1 1 d . U . . .
C71 C -0.2096(12) 0.7629(12) 0.3553(13) 0.070(3) Uani 1 1 d . U . . .
H71 H -0.2466 0.8149 0.3259 0.084 Uiso 1 1 calc R . . . .
C72 C -0.2487(13) 0.6870(12) 0.3880(13) 0.072(3) Uani 1 1 d . U . . .
H72 H -0.3125 0.6890 0.3825 0.086 Uiso 1 1 calc R . . . .
C73 C -0.1980(12) 0.6124(12) 0.4265(12) 0.069(3) Uani 1 1 d . U . . .
C74 C -0.1039(11) 0.6096(11) 0.4336(11) 0.061(3) Uani 1 1 d . U . . .
H74 H -0.0659 0.5544 0.4586 0.074 Uiso 1 1 calc R . . . .
S81 S 0.3515(3) 1.1786(3) 0.1583(3) 0.0727(11) Uani 1 1 d . U . . .
O82 O 0.2626(10) 1.1485(8) 0.2124(9) 0.083(3) Uani 1 1 d . U . . .
C83 C 0.4226(16) 1.0956(15) 0.0822(16) 0.093(4) Uani 1 1 d . U . . .
H83A H 0.4837 1.1128 0.0440 0.140 Uiso 1 1 calc R . . . .
H83B H 0.4426 1.0349 0.1143 0.140 Uiso 1 1 calc R . . . .
H83C H 0.3828 1.0911 0.0442 0.140 Uiso 1 1 calc R . . . .
C84 C 0.434(3) 1.136(2) 0.227(2) 0.074(6) Uani 0.50(3) 1 d . U P A 1
H84A H 0.4980 1.1526 0.1966 0.111 Uiso 0.50(3) 1 calc R . P A 1
H84B H 0.4016 1.1647 0.2857 0.111 Uiso 0.50(3) 1 calc R . P A 1
H84C H 0.4492 1.0677 0.2358 0.111 Uiso 0.50(3) 1 calc R . P A 1
C84A C 0.299(3) 1.238(3) 0.077(3) 0.088(7) Uani 0.50(3) 1 d . U P A 2
H84D H 0.3532 1.2372 0.0199 0.131 Uiso 0.50(3) 1 d R . P A 2
H84E H 0.2521 1.2064 0.0712 0.131 Uiso 0.50(3) 1 d R . P A 2
H84F H 0.2606 1.3040 0.0917 0.131 Uiso 0.50(3) 1 d R . P A 2
S85 S 0.1057(8) 0.5900(6) -0.1374(8) 0.120(3) Uani 0.755(13) 1 d D U P B 1
S85A S 0.0560(16) 0.6459(16) -0.1724(15) 0.123(4) Uani 0.245(13) 1 d D U P B 2
O86 O 0.1147(13) 0.6855(10) -0.1314(13) 0.112(3) Uani 1 1 d D U . . .
C87 C -0.0143(19) 0.5937(18) -0.093(2) 0.135(4) Uani 1 1 d D U . . .
H87A H -0.0223 0.5321 -0.0961 0.202 Uiso 0.755(13) 1 calc R . P B 1
H87B H -0.0376 0.6102 -0.0297 0.202 Uiso 0.755(13) 1 calc R . P B 1
H87C H -0.0547 0.6411 -0.1269 0.202 Uiso 0.755(13) 1 calc R . P B 1
H87D H -0.0527 0.5678 -0.1187 0.202 Uiso 0.245(13) 1 calc R . P B 2
H87E H 0.0287 0.5428 -0.0642 0.202 Uiso 0.245(13) 1 calc R . P B 2
H87F H -0.0617 0.6387 -0.0478 0.202 Uiso 0.245(13) 1 calc R . P B 2
C88 C 0.136(2) 0.5678(18) -0.2427(18) 0.133(4) Uani 1 1 d D U . . .
H88A H 0.1300 0.5056 -0.2466 0.200 Uiso 0.755(13) 1 calc R . P B 1
H88B H 0.0898 0.6153 -0.2715 0.200 Uiso 0.755(13) 1 calc R . P B 1
H88C H 0.2061 0.5692 -0.2738 0.200 Uiso 0.755(13) 1 calc R . P B 1
H88D H 0.0986 0.5418 -0.2696 0.200 Uiso 0.245(13) 1 calc R . P B 2
H88E H 0.1820 0.5970 -0.2907 0.200 Uiso 0.245(13) 1 calc R . P B 2
H88F H 0.1753 0.5174 -0.2105 0.200 Uiso 0.245(13) 1 calc R . P B 2
O89 O -0.1699(12) 0.8405(10) 0.6001(12) 0.114(6) Uani 1 1 d . U . . .
O90 O -0.2341(14) 0.9689(11) 0.4555(11) 0.115(5) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br16 C13 1.901(17) . ?
Br36 C33 1.922(15) . ?
Br56 C53 1.921(19) . ?
Br76 C73 1.916(15) . ?
Cu1 O8 1.965(9) . ?
Cu1 O15 1.909(9) . ?
Cu1 O48 1.963(8) . ?
Cu1 O68 2.400(9) . ?
Cu1 N41 2.000(12) . ?
Cu2 O8 1.973(8) . ?
Cu2 O28 1.966(9) . ?
Cu2 O35 1.900(8) . ?
Cu2 O48 2.409(9) . ?
Cu2 N1 1.990(12) . ?
Cu3 O8 2.378(9) . ?
Cu3 O28 1.985(8) . ?
Cu3 O68 1.969(9) . ?
Cu3 O75 1.925(9) . ?
Cu3 N21 2.015(11) . ?
Cu4 O28 2.401(9) . ?
Cu4 O48 1.955(9) . ?
Cu4 O55 1.912(10) . ?
Cu4 O68 1.962(8) . ?
Cu4 N61 1.995(13) . ?
S3 C2 1.718(14) . ?
S3 C4 1.731(14) . ?
S23 C22 1.736(15) . ?
S23 C24 1.754(14) . ?
S43 C42 1.764(14) . ?
S43 C44 1.743(17) . ?
S63 C62 1.745(17) . ?
S63 C64 1.79(2) . ?
O8 C7 1.388(16) . ?
O15 C10 1.309(18) . ?
O28 C27 1.382(14) . ?
O35 C30 1.292(16) . ?
O48 C47 1.406(16) . ?
O55 C50 1.290(19) . ?
O68 C67 1.364(17) . ?
O75 C70 1.326(17) . ?
N1 C2 1.323(17) . ?
N1 C5 1.356(18) . ?
N6 H6 0.8800 . ?
N6 C2 1.351(17) . ?
N6 C7 1.454(19) . ?
N21 C22 1.303(17) . ?
N21 C25 1.373(18) . ?
N26 H26 0.8800 . ?
N26 C22 1.346(18) . ?
N26 C27 1.447(18) . ?
N41 C42 1.281(19) . ?
N41 C45 1.389(17) . ?
N46 H46 0.8800 . ?
N46 C42 1.326(18) . ?
N46 C47 1.470(18) . ?
N61 C62 1.28(2) . ?
N61 C65 1.35(2) . ?
N66 H66 0.8800 . ?
N66 C62 1.36(2) . ?
N66 C67 1.468(19) . ?
C13 C12 1.38(2) . ?
C13 C14 1.403(19) . ?
C9 C10 1.44(2) . ?
C9 C7 1.452(18) . ?
C9 C14 1.40(2) . ?
C12 H12 0.9500 . ?
C12 C11 1.40(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.32(2) . ?
C10 C11 1.397(19) . ?
C5 H5 0.9500 . ?
C7 H7 1.0000 . ?
C11 H11 0.9500 . ?
C14 H14 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.33(2) . ?
C25 H25 0.9500 . ?
C27 H27 1.0000 . ?
C27 C29 1.477(18) . ?
C29 C30 1.42(2) . ?
C29 C34 1.38(2) . ?
C30 C31 1.407(19) . ?
C31 H31 0.9500 . ?
C31 C32 1.40(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.34(2) . ?
C33 C34 1.38(2) . ?
C34 H34 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.38(2) . ?
C45 H45 0.9500 . ?
C47 H47 1.0000 . ?
C47 C49 1.502(16) . ?
C49 C50 1.42(2) . ?
C49 C54 1.37(2) . ?
C50 C51 1.417(19) . ?
C51 H51 0.9500 . ?
C51 C52 1.36(3) . ?
C52 H52 0.9500 . ?
C52 C53 1.37(3) . ?
C53 C54 1.41(2) . ?
C54 H54 0.9500 . ?
C64 H64 0.9500 . ?
C64 C65 1.27(3) . ?
C65 H65 0.9500 . ?
C67 H67 1.0000 . ?
C67 C69 1.52(2) . ?
C69 C70 1.43(2) . ?
C69 C74 1.35(2) . ?
C70 C71 1.38(2) . ?
C71 H71 0.9500 . ?
C71 C72 1.39(2) . ?
C72 H72 0.9500 . ?
C72 C73 1.32(2) . ?
C73 C74 1.40(2) . ?
C74 H74 0.9500 . ?
S81 O82 1.457(12) . ?
S81 C83 1.69(2) . ?
S81 C84 1.78(4) . ?
S81 C84A 1.70(4) . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C84A H84D 0.9722 . ?
C84A H84E 0.9731 . ?
C84A H84F 0.9947 . ?
S85 O86 1.503(15) . ?
S85 C87 1.63(2) . ?
S85 C88 1.62(2) . ?
S85A O86 1.516(19) . ?
S85A C87 1.61(2) . ?
S85A C88 1.62(2) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C87 H87D 0.9800 . ?
C87 H87E 0.9800 . ?
C87 H87F 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C88 H88D 0.9800 . ?
C88 H88E 0.9800 . ?
C88 H88F 0.9800 . ?

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
O8 Cu1 O68 81.7(3) . . ?
O8 Cu1 N41 172.2(4) . . ?
O15 Cu1 O8 94.1(4) . . ?
O15 Cu1 O48 172.8(4) . . ?
O15 Cu1 O68 114.3(4) . . ?
O15 Cu1 N41 93.6(4) . . ?
O48 Cu1 O8 84.0(4) . . ?
O48 Cu1 O68 72.4(3) . . ?
O48 Cu1 N41 88.4(4) . . ?
N41 Cu1 O68 94.3(4) . . ?
O8 Cu2 O48 72.9(3) . . ?
O8 Cu2 N1 90.1(4) . . ?
O28 Cu2 O8 84.9(3) . . ?
O28 Cu2 O48 82.1(3) . . ?
O28 Cu2 N1 174.9(4) . . ?
O35 Cu2 O8 171.7(4) . . ?
O35 Cu2 O28 94.1(4) . . ?
O35 Cu2 O48 115.2(4) . . ?
O35 Cu2 N1 91.0(4) . . ?
N1 Cu2 O48 95.2(4) . . ?
O28 Cu3 O8 74.5(3) . . ?
O28 Cu3 N21 89.2(4) . . ?
O68 Cu3 O8 82.2(3) . . ?
O68 Cu3 O28 84.9(3) . . ?
O68 Cu3 N21 174.1(4) . . ?
O75 Cu3 O8 112.6(4) . . ?
O75 Cu3 O28 172.3(4) . . ?
O75 Cu3 O68 93.2(4) . . ?
O75 Cu3 N21 92.6(4) . . ?
N21 Cu3 O8 96.6(4) . . ?
O48 Cu4 O28 82.6(3) . . ?
O48 Cu4 O68 83.2(4) . . ?
O48 Cu4 N61 171.7(5) . . ?
O55 Cu4 O28 112.6(4) . . ?
O55 Cu4 O48 94.9(4) . . ?
O55 Cu4 O68 172.3(4) . . ?
O55 Cu4 N61 93.3(5) . . ?
O68 Cu4 O28 74.6(3) . . ?
O68 Cu4 N61 88.9(5) . . ?
N61 Cu4 O28 93.0(5) . . ?
C2 S3 C4 89.1(7) . . ?
C22 S23 C24 90.6(7) . . ?
C44 S43 C42 88.9(7) . . ?
C62 S63 C64 86.4(9) . . ?
Cu1 O8 Cu2 108.5(4) . . ?
Cu1 O8 Cu3 96.7(4) . . ?
Cu2 O8 Cu3 93.1(3) . . ?
C7 O8 Cu1 114.9(8) . . ?
C7 O8 Cu2 115.0(7) . . ?
C7 O8 Cu3 125.4(8) . . ?
C10 O15 Cu1 125.0(8) . . ?
Cu2 O28 Cu3 106.7(4) . . ?
Cu2 O28 Cu4 96.0(3) . . ?
Cu3 O28 Cu4 92.1(3) . . ?
C27 O28 Cu2 115.5(8) . . ?
C27 O28 Cu3 117.6(8) . . ?
C27 O28 Cu4 124.7(8) . . ?
C30 O35 Cu2 124.4(8) . . ?
Cu1 O48 Cu2 93.4(4) . . ?
Cu4 O48 Cu1 109.7(4) . . ?
Cu4 O48 Cu2 96.0(3) . . ?
C47 O48 Cu1 114.6(7) . . ?
C47 O48 Cu2 126.2(7) . . ?
C47 O48 Cu4 114.1(8) . . ?
C50 O55 Cu4 123.6(10) . . ?
Cu3 O68 Cu1 95.9(4) . . ?
Cu4 O68 Cu1 94.0(3) . . ?
Cu4 O68 Cu3 107.5(4) . . ?
C67 O68 Cu1 125.8(8) . . ?
C67 O68 Cu3 114.5(9) . . ?
C67 O68 Cu4 115.6(9) . . ?
C70 O75 Cu3 123.5(9) . . ?
C2 N1 Cu2 124.6(9) . . ?
C2 N1 C5 111.3(12) . . ?
C5 N1 Cu2 123.3(9) . . ?
C2 N6 H6 118.4 . . ?
C2 N6 C7 123.2(11) . . ?
C7 N6 H6 118.4 . . ?
C22 N21 Cu3 123.8(10) . . ?
C22 N21 C25 113.5(12) . . ?
C25 N21 Cu3 122.0(9) . . ?
C22 N26 H26 118.2 . . ?
C22 N26 C27 123.7(11) . . ?
C27 N26 H26 118.2 . . ?
C42 N41 Cu1 125.6(9) . . ?
C42 N41 C45 113.3(13) . . ?
C45 N41 Cu1 119.4(10) . . ?
C42 N46 H46 120.3 . . ?
C42 N46 C47 119.4(12) . . ?
C47 N46 H46 120.3 . . ?
C62 N61 Cu4 125.0(11) . . ?
C62 N61 C65 111.3(14) . . ?
C65 N61 Cu4 121.5(12) . . ?
C62 N66 H66 119.7 . . ?
C62 N66 C67 120.6(14) . . ?
C67 N66 H66 119.7 . . ?
C12 C13 Br16 121.6(11) . . ?
C12 C13 C14 120.0(15) . . ?
C14 C13 Br16 118.4(13) . . ?
C10 C9 C7 121.3(13) . . ?
C14 C9 C10 118.8(12) . . ?
C14 C9 C7 119.9(13) . . ?
N1 C2 S3 113.2(10) . . ?
N1 C2 N6 124.6(13) . . ?
N6 C2 S3 122.2(10) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.5(13) . . ?
C11 C12 H12 120.2 . . ?
S3 C4 H4 124.9 . . ?
C5 C4 S3 110.2(11) . . ?
C5 C4 H4 124.9 . . ?
O15 C10 C9 122.3(12) . . ?
O15 C10 C11 119.9(14) . . ?
C11 C10 C9 117.8(14) . . ?
N1 C5 H5 121.9 . . ?
C4 C5 N1 116.2(13) . . ?
C4 C5 H5 121.9 . . ?
O8 C7 N6 111.1(11) . . ?
O8 C7 C9 113.6(12) . . ?
O8 C7 H7 108.1 . . ?
N6 C7 H7 108.1 . . ?
C9 C7 N6 107.6(11) . . ?
C9 C7 H7 108.1 . . ?
C12 C11 H11 118.8 . . ?
C10 C11 C12 122.4(15) . . ?
C10 C11 H11 118.8 . . ?
C13 C14 H14 119.3 . . ?
C9 C14 C13 121.3(15) . . ?
C9 C14 H14 119.3 . . ?
N21 C22 S23 111.5(11) . . ?
N21 C22 N26 126.5(13) . . ?
N26 C22 S23 121.9(10) . . ?
S23 C24 H24 125.9 . . ?
C25 C24 S23 108.3(11) . . ?
C25 C24 H24 125.9 . . ?
N21 C25 H25 121.9 . . ?
C24 C25 N21 116.1(12) . . ?
C24 C25 H25 121.9 . . ?
O28 C27 N26 110.4(10) . . ?
O28 C27 H27 107.9 . . ?
O28 C27 C29 112.8(11) . . ?
N26 C27 H27 107.9 . . ?
N26 C27 C29 109.8(11) . . ?
C29 C27 H27 107.9 . . ?
C30 C29 C27 120.3(12) . . ?
C34 C29 C27 120.4(13) . . ?
C34 C29 C30 119.3(13) . . ?
O35 C30 C29 123.7(11) . . ?
O35 C30 C31 117.7(13) . . ?
C31 C30 C29 118.5(13) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.5(15) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 120.4 . . ?
C33 C32 C31 119.2(14) . . ?
C33 C32 H32 120.4 . . ?
C32 C33 Br36 118.7(11) . . ?
C32 C33 C34 122.5(14) . . ?
C34 C33 Br36 118.7(12) . . ?
C29 C34 C33 119.9(15) . . ?
C29 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
N41 C42 S43 113.9(10) . . ?
N41 C42 N46 126.8(13) . . ?
N46 C42 S43 119.4(12) . . ?
S43 C44 H44 125.0 . . ?
C45 C44 S43 110.0(11) . . ?
C45 C44 H44 125.0 . . ?
N41 C45 H45 123.1 . . ?
C44 C45 N41 113.9(14) . . ?
C44 C45 H45 123.1 . . ?
O48 C47 N46 110.0(11) . . ?
O48 C47 H47 108.9 . . ?
O48 C47 C49 110.5(10) . . ?
N46 C47 H47 108.9 . . ?
N46 C47 C49 109.4(11) . . ?
C49 C47 H47 108.9 . . ?
C50 C49 C47 120.2(13) . . ?
C54 C49 C47 117.0(13) . . ?
C54 C49 C50 122.7(13) . . ?
O55 C50 C49 124.3(12) . . ?
O55 C50 C51 120.3(15) . . ?
C51 C50 C49 115.3(15) . . ?
C50 C51 H51 118.9 . . ?
C52 C51 C50 122.2(16) . . ?
C52 C51 H51 118.9 . . ?
C51 C52 H52 119.2 . . ?
C51 C52 C53 121.5(14) . . ?
C53 C52 H52 119.2 . . ?
C52 C53 Br56 123.7(12) . . ?
C52 C53 C54 119.0(17) . . ?
C54 C53 Br56 117.3(14) . . ?
C49 C54 C53 119.2(16) . . ?
C49 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
N61 C62 S63 114.6(13) . . ?
N61 C62 N66 125.9(15) . . ?
N66 C62 S63 119.4(14) . . ?
S63 C64 H64 125.3 . . ?
C65 C64 S63 109.4(15) . . ?
C65 C64 H64 125.3 . . ?
N61 C65 H65 120.9 . . ?
C64 C65 N61 118.3(19) . . ?
C64 C65 H65 120.9 . . ?
O68 C67 N66 111.6(11) . . ?
O68 C67 H67 107.7 . . ?
O68 C67 C69 113.6(12) . . ?
N66 C67 H67 107.7 . . ?
N66 C67 C69 108.2(12) . . ?
C69 C67 H67 107.7 . . ?
C70 C69 C67 118.0(12) . . ?
C74 C69 C67 121.5(15) . . ?
C74 C69 C70 120.5(14) . . ?
O75 C70 C69 123.0(13) . . ?
O75 C70 C71 121.5(15) . . ?
C71 C70 C69 115.4(13) . . ?
C70 C71 H71 118.7 . . ?
C70 C71 C72 122.7(16) . . ?
C72 C71 H71 118.7 . . ?
C71 C72 H72 119.8 . . ?
C73 C72 C71 120.4(15) . . ?
C73 C72 H72 119.8 . . ?
C72 C73 Br76 123.1(12) . . ?
C72 C73 C74 119.5(15) . . ?
C74 C73 Br76 117.4(13) . . ?
C69 C74 C73 121.4(16) . . ?
C69 C74 H74 119.3 . . ?
C73 C74 H74 119.3 . . ?
O82 S81 C83 106.4(9) . . ?
O82 S81 C84 102.2(12) . . ?
O82 S81 C84A 95.0(15) . . ?
C83 S81 C84 92.3(15) . . ?
C83 S81 C84A 86.7(16) . . ?
S81 C83 H83A 109.5 . . ?
S81 C83 H83B 109.5 . . ?
S81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
S81 C84 H84A 109.5 . . ?
S81 C84 H84B 109.5 . . ?
S81 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
S81 C84A H84D 108.4 . . ?
S81 C84A H84E 108.3 . . ?
S81 C84A H84F 111.7 . . ?
H84D C84A H84E 110.7 . . ?
H84D C84A H84F 108.9 . . ?
H84E C84A H84F 108.8 . . ?
O86 S85 C87 107.8(13) . . ?
O86 S85 C88 109.4(13) . . ?
C88 S85 C87 106.0(15) . . ?
O86 S85A C87 108.6(16) . . ?
O86 S85A C88 108.9(16) . . ?
C87 S85A C88 107.4(17) . . ?
S85 C87 H87A 109.5 . . ?
S85 C87 H87B 109.5 . . ?
S85 C87 H87C 109.5 . . ?
S85A C87 H87D 109.5 . . ?
S85A C87 H87E 109.5 . . ?
S85A C87 H87F 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
H87D C87 H87E 109.5 . . ?
H87D C87 H87F 109.5 . . ?
H87E C87 H87F 109.5 . . ?
S85 C88 H88A 109.5 . . ?
S85 C88 H88B 109.5 . . ?
S85 C88 H88C 109.5 . . ?
S85A C88 H88D 109.5 . . ?
S85A C88 H88E 109.5 . . ?
S85A C88 H88F 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
H88D C88 H88E 109.5 . . ?
H88D C88 H88F 109.5 . . ?
H88E C88 H88F 109.5 . . ?

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
N6 H6 O86 0.88 1.93 2.779(17) 161.5 .
N26 H26 O82 0.88 2.08 2.841(15) 144.6 .
N66 H66 O89 0.88 1.94 2.800(19) 165.9 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br16 C13 C12 C11 -177.6(12) . . . . ?
Br16 C13 C14 C9 -179.2(11) . . . . ?
Br36 C33 C34 C29 176.2(12) . . . . ?
Br56 C53 C54 C49 -178.9(12) . . . . ?
Br76 C73 C74 C69 -176.5(13) . . . . ?
Cu1 O8 C7 N6 -59.6(11) . . . . ?
Cu1 O8 C7 C9 61.9(14) . . . . ?
Cu1 O15 C10 C9 24.5(19) . . . . ?
Cu1 O15 C10 C11 -157.6(11) . . . . ?
Cu1 O48 C47 N46 -70.9(12) . . . . ?
Cu1 O48 C47 C49 168.2(9) . . . . ?
Cu1 O68 C67 N66 -175.0(9) . . . . ?
Cu1 O68 C67 C69 -52.3(16) . . . . ?
Cu1 N41 C42 S43 166.6(7) . . . . ?
Cu1 N41 C42 N46 -14(2) . . . . ?
Cu1 N41 C45 C44 -167.0(11) . . . . ?
Cu2 O8 C7 N6 67.4(11) . . . . ?
Cu2 O8 C7 C9 -171.1(10) . . . . ?
Cu2 O28 C27 N26 62.4(12) . . . . ?
Cu2 O28 C27 C29 -60.9(13) . . . . ?
Cu2 O35 C30 C29 -27.0(19) . . . . ?
Cu2 O35 C30 C31 150.5(11) . . . . ?
Cu2 O48 C47 N46 174.7(7) . . . . ?
Cu2 O48 C47 C49 53.7(14) . . . . ?
Cu2 N1 C2 S3 -172.8(7) . . . . ?
Cu2 N1 C2 N6 9(2) . . . . ?
Cu2 N1 C5 C4 171.2(11) . . . . ?
Cu3 O8 C7 N6 -178.8(7) . . . . ?
Cu3 O8 C7 C9 -57.3(15) . . . . ?
Cu3 O28 C27 N26 -65.1(12) . . . . ?
Cu3 O28 C27 C29 171.7(9) . . . . ?
Cu3 O68 C67 N66 -57.0(14) . . . . ?
Cu3 O68 C67 C69 65.6(13) . . . . ?
Cu3 O75 C70 C69 35(2) . . . . ?
Cu3 O75 C70 C71 -149.4(14) . . . . ?
Cu3 N21 C22 S23 169.7(6) . . . . ?
Cu3 N21 C22 N26 -9(2) . . . . ?
Cu3 N21 C25 C24 -170.7(11) . . . . ?
Cu4 O28 C27 N26 -179.5(7) . . . . ?
Cu4 O28 C27 C29 57.3(14) . . . . ?
Cu4 O48 C47 N46 56.7(11) . . . . ?
Cu4 O48 C47 C49 -64.3(13) . . . . ?
Cu4 O55 C50 C49 -25(2) . . . . ?
Cu4 O55 C50 C51 150.3(13) . . . . ?
Cu4 O68 C67 N66 68.9(14) . . . . ?
Cu4 O68 C67 C69 -168.5(9) . . . . ?
Cu4 N61 C62 S63 -163.8(10) . . . . ?
Cu4 N61 C62 N66 17(3) . . . . ?
Cu4 N61 C65 C64 163(2) . . . . ?
S3 C4 C5 N1 1.4(18) . . . . ?
S23 C24 C25 N21 0.8(17) . . . . ?
S43 C44 C45 N41 0.0(18) . . . . ?
S63 C64 C65 N61 2(3) . . . . ?
O15 C10 C11 C12 179.3(14) . . . . ?
O28 Cu2 O35 C30 12.4(11) . . . . ?
O28 C27 C29 C30 50.0(18) . . . . ?
O28 C27 C29 C34 -129.4(14) . . . . ?
O35 C30 C31 C32 -178.7(14) . . . . ?
O48 Cu2 O35 C30 -70.8(12) . . . . ?
O48 C47 C49 C50 52.7(18) . . . . ?
O48 C47 C49 C54 -130.2(14) . . . . ?
O55 C50 C51 C52 -177.3(16) . . . . ?
O68 C67 C69 C70 -47.9(19) . . . . ?
O68 C67 C69 C74 129.4(15) . . . . ?
O75 C70 C71 C72 -173.8(16) . . . . ?
N1 Cu2 O35 C30 -167.0(11) . . . . ?
N26 C27 C29 C30 -73.6(16) . . . . ?
N26 C27 C29 C34 107.0(15) . . . . ?
N46 C47 C49 C50 -68.6(17) . . . . ?
N46 C47 C49 C54 108.4(15) . . . . ?
N66 C67 C69 C70 76.7(17) . . . . ?
N66 C67 C69 C74 -106.1(17) . . . . ?
C13 C12 C11 C10 0(2) . . . . ?
C9 C10 C11 C12 -3(2) . . . . ?
C2 S3 C4 C5 -2.2(13) . . . . ?
C2 N1 C5 C4 1(2) . . . . ?
C2 N6 C7 O8 -50.6(17) . . . . ?
C2 N6 C7 C9 -175.5(13) . . . . ?
C12 C13 C14 C9 3(2) . . . . ?
C4 S3 C2 N1 2.6(12) . . . . ?
C4 S3 C2 N6 -179.3(13) . . . . ?
C10 C9 C7 O8 -49.1(18) . . . . ?
C10 C9 C7 N6 74.3(16) . . . . ?
C10 C9 C14 C13 -6(2) . . . . ?
C5 N1 C2 S3 -2.4(16) . . . . ?
C5 N1 C2 N6 179.6(14) . . . . ?
C7 N6 C2 S3 -168.3(11) . . . . ?
C7 N6 C2 N1 10(2) . . . . ?
C7 C9 C10 O15 2(2) . . . . ?
C7 C9 C10 C11 -175.6(14) . . . . ?
C7 C9 C14 C13 175.5(14) . . . . ?
C14 C13 C12 C11 0(2) . . . . ?
C14 C9 C10 O15 -176.4(13) . . . . ?
C14 C9 C10 C11 6(2) . . . . ?
C14 C9 C7 O8 129.6(14) . . . . ?
C14 C9 C7 N6 -107.0(15) . . . . ?
C22 S23 C24 C25 -1.0(12) . . . . ?
C22 N21 C25 C24 -0.1(19) . . . . ?
C22 N26 C27 O28 49.1(17) . . . . ?
C22 N26 C27 C29 174.1(12) . . . . ?
C24 S23 C22 N21 1.0(12) . . . . ?
C24 S23 C22 N26 179.5(13) . . . . ?
C25 N21 C22 S23 -0.7(15) . . . . ?
C25 N21 C22 N26 -179.2(13) . . . . ?
C27 N26 C22 S23 171.2(10) . . . . ?
C27 N26 C22 N21 -10(2) . . . . ?
C27 C29 C30 O35 -3(2) . . . . ?
C27 C29 C30 C31 180.0(13) . . . . ?
C27 C29 C34 C33 -177.2(15) . . . . ?
C29 C30 C31 C32 -1(2) . . . . ?
C30 C29 C34 C33 3(2) . . . . ?
C30 C31 C32 C33 0(2) . . . . ?
C31 C32 C33 Br36 -178.0(12) . . . . ?
C31 C32 C33 C34 3(3) . . . . ?
C32 C33 C34 C29 -5(3) . . . . ?
C34 C29 C30 O35 176.9(14) . . . . ?
C34 C29 C30 C31 -1(2) . . . . ?
C42 S43 C44 C45 0.8(13) . . . . ?
C42 N41 C45 C44 -1(2) . . . . ?
C42 N46 C47 O48 54.8(16) . . . . ?
C42 N46 C47 C49 176.4(13) . . . . ?
C44 S43 C42 N41 -1.5(13) . . . . ?
C44 S43 C42 N46 179.1(14) . . . . ?
C45 N41 C42 S43 1.8(17) . . . . ?
C45 N41 C42 N46 -178.9(15) . . . . ?
C47 N46 C42 S43 169.2(10) . . . . ?
C47 N46 C42 N41 -10(2) . . . . ?
C47 C49 C50 O55 -4(2) . . . . ?
C47 C49 C50 C51 -179.8(14) . . . . ?
C47 C49 C54 C53 178.9(15) . . . . ?
C49 C50 C51 C52 -2(3) . . . . ?
C50 C49 C54 C53 -4(2) . . . . ?
C50 C51 C52 C53 1(3) . . . . ?
C51 C52 C53 Br56 -179.5(14) . . . . ?
C51 C52 C53 C54 -2(3) . . . . ?
C52 C53 C54 C49 3(3) . . . . ?
C54 C49 C50 O55 178.6(15) . . . . ?
C54 C49 C50 C51 3(2) . . . . ?
C62 S63 C64 C65 -2(2) . . . . ?
C62 N61 C65 C64 -1(3) . . . . ?
C62 N66 C67 O68 -48(2) . . . . ?
C62 N66 C67 C69 -173.7(16) . . . . ?
C64 S63 C62 N61 1(2) . . . . ?
C64 S63 C62 N66 -179.0(19) . . . . ?
C65 N61 C62 S63 0(2) . . . . ?
C65 N61 C62 N66 -180(2) . . . . ?
C67 N66 C62 S63 -176.9(13) . . . . ?
C67 N66 C62 N61 3(3) . . . . ?
C67 C69 C70 O75 -6(2) . . . . ?
C67 C69 C70 C71 177.6(15) . . . . ?
C67 C69 C74 C73 179.8(15) . . . . ?
C69 C70 C71 C72 2(3) . . . . ?
C70 C69 C74 C73 -3(3) . . . . ?
C70 C71 C72 C73 -2(3) . . . . ?
C71 C72 C73 Br76 179.1(14) . . . . ?
C71 C72 C73 C74 -1(3) . . . . ?
C72 C73 C74 C69 3(3) . . . . ?
C74 C69 C70 O75 176.3(15) . . . . ?
C74 C69 C70 C71 0(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
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
-2 1 -10 0.0230 -1.9896 0.9959 -10.0064 0.1722 1.0017 0.0426
3 0 10 0.0348 2.9909 0.0042 10.0073 -0.1075 -0.9773 -0.1583
-6 -3 5 0.0800 -6.0079 -2.9892 4.9929 -0.0542 -0.6421 0.7522
8 4 -2 0.0898 8.0065 3.9904 -1.9897 0.0824 0.3750 -0.9261
1 9 2 0.0132 1.0109 9.0188 1.9943 0.9316 -0.1295 -0.1480
-1 -9 -2 0.0132 -1.0109 -9.0188 -1.9943 -0.9316 0.1295 0.1480
-9 -3 -5 0.0883 -8.9988 -2.9934 -5.0143 0.0533 0.3353 0.9104

_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
