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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H14 N4 S4'
_chemical_formula_sum            'C16 H14 N4 S4'
_chemical_formula_weight         390.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

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

_cell_length_a                   11.0637(9)
_cell_length_b                   7.2056(6)
_cell_length_c                   22.927(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.564(8)
_cell_angle_gamma                90.00
_cell_volume                     1790.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3865
_cell_measurement_theta_min      3.69
_cell_measurement_theta_max      26.99

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20966
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_sigmaI/netI    0.1166
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.69
_diffrn_reflns_theta_max         26.99
_reflns_number_total             3865
_reflns_number_gt                1899
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/1sq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0298P)²+1.9248P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3865
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.1178
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4738(3) 0.5110(6) 0.08189(16) 0.0438(10) Uani 1 1 d . . .
C2 C 0.5172(3) 0.3395(6) 0.08961(16) 0.0426(10) Uani 1 1 d . . .
C3 C 0.6923(4) 0.5475(5) 0.15002(16) 0.0417(10) Uani 1 1 d . . .
C4 C 0.7928(4) 0.6117(5) 0.18692(16) 0.0379(10) Uani 1 1 d . . .
C5 C 0.9340(3) 0.8066(5) 0.26832(16) 0.0368(9) Uani 1 1 d . . .
C6 C 0.9792(3) 0.6345(5) 0.27356(16) 0.0404(10) Uani 1 1 d . . .
H6 H 1.0433 0.6033 0.3049 0.049 Uiso 1 1 calc R . .
C7 C 0.9689(4) 0.9658(5) 0.30806(16) 0.0369(9) Uani 1 1 d . . .
C8 C 0.8981(4) 1.0968(6) 0.32830(18) 0.0503(11) Uani 1 1 d . . .
H8 H 0.8123 1.0998 0.3196 0.060 Uiso 1 1 calc R . .
C9 C 0.3511(4) 0.5712(7) 0.04598(18) 0.0586(12) Uani 1 1 d . . .
H9A H 0.3440 0.7037 0.0481 0.088 Uiso 1 1 calc R . .
H9B H 0.2861 0.5139 0.0617 0.088 Uiso 1 1 calc R . .
H9C H 0.3449 0.5344 0.0052 0.088 Uiso 1 1 calc R . .
C10 C 0.4551(4) 0.1651(6) 0.06275(19) 0.0600(12) Uani 1 1 d . . .
H10A H 0.5071 0.0604 0.0757 0.090 Uiso 1 1 calc R . .
H10B H 0.4406 0.1736 0.0201 0.090 Uiso 1 1 calc R . .
H10C H 0.3778 0.1502 0.0752 0.090 Uiso 1 1 calc R . .
C11 C 1.2051(3) 0.9365(5) 0.32817(17) 0.0436(10) Uani 1 1 d . . .
H11A H 1.2634 1.0339 0.3243 0.052 Uiso 1 1 calc R . .
H11B H 1.1949 0.8593 0.2929 0.052 Uiso 1 1 calc R . .
C12 C 1.2563(3) 0.8204(5) 0.38216(16) 0.0376(9) Uani 1 1 d . . .
C13 C 1.3674(4) 0.8618(6) 0.41906(19) 0.0506(11) Uani 1 1 d . . .
H13 H 1.4135 0.9635 0.4114 0.061 Uiso 1 1 calc R . .
C14 C 1.4091(4) 0.7490(7) 0.4678(2) 0.0584(13) Uani 1 1 d . . .
H14 H 1.4842 0.7734 0.4931 0.070 Uiso 1 1 calc R . .
C15 C 1.3389(4) 0.6017(6) 0.47835(19) 0.0539(12) Uani 1 1 d . . .
H15 H 1.3641 0.5254 0.5112 0.065 Uiso 1 1 calc R . .
C16 C 1.2301(4) 0.5697(6) 0.4390(2) 0.0584(12) Uani 1 1 d . . .
H16 H 1.1829 0.4682 0.4459 0.070 Uiso 1 1 calc R . .
N3 N 0.9706(4) 1.2209(5) 0.36270(15) 0.0572(10) Uani 1 1 d . . .
N2 N 1.0869(4) 1.1755(5) 0.36473(15) 0.0538(9) Uani 1 1 d . . .
N1 N 1.0866(3) 1.0201(4) 0.33173(13) 0.0408(8) Uani 1 1 d . . .
N4 N 1.1877(3) 0.6752(5) 0.39146(14) 0.0510(9) Uani 1 1 d . . .
S1 S 0.57086(10) 0.69212(16) 0.11562(5) 0.0538(3) Uani 1 1 d . . .
S2 S 0.81104(10) 0.84862(14) 0.20757(5) 0.0468(3) Uani 1 1 d . . .
S3 S 0.66729(10) 0.31105(15) 0.13212(5) 0.0500(3) Uani 1 1 d . . .
S4 S 0.91660(10) 0.47014(14) 0.22093(5) 0.0459(3) 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
C1 C2 1.325(5) . ?
C1 C9 1.504(5) . ?
C1 S1 1.767(4) . ?
C2 C10 1.504(5) . ?
C2 S3 1.760(4) . ?
C3 C4 1.337(5) . ?
C3 S1 1.758(4) . ?
C3 S3 1.761(4) . ?
C4 S4 1.760(4) . ?
C4 S2 1.772(4) . ?
C5 C6 1.333(5) . ?
C5 C7 1.468(5) . ?
C5 S2 1.767(4) . ?
C6 S4 1.733(4) . ?
C7 N1 1.364(4) . ?
C7 C8 1.366(5) . ?
C8 N3 1.346(5) . ?
C11 N1 1.460(4) . ?
C11 C12 1.507(5) . ?
C12 N4 1.334(5) . ?
C12 C13 1.378(5) . ?
C13 C14 1.384(6) . ?
C14 C15 1.365(6) . ?
C15 C16 1.371(6) . ?
C16 N4 1.335(5) . ?
N3 N2 1.319(5) . ?
N2 N1 1.351(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
C2 C1 C9 127.3(4) . . ?
C2 C1 S1 117.3(3) . . ?
C9 C1 S1 115.4(3) . . ?
C1 C2 C10 126.9(4) . . ?
C1 C2 S3 117.3(3) . . ?
C10 C2 S3 115.6(3) . . ?
C4 C3 S1 122.8(3) . . ?
C4 C3 S3 123.7(3) . . ?
S1 C3 S3 113.5(2) . . ?
C3 C4 S4 123.6(3) . . ?
C3 C4 S2 122.5(3) . . ?
S4 C4 S2 113.8(2) . . ?
C6 C5 C7 128.6(3) . . ?
C6 C5 S2 116.5(3) . . ?
C7 C5 S2 114.8(3) . . ?
C5 C6 S4 118.8(3) . . ?
N1 C7 C8 103.5(3) . . ?
N1 C7 C5 125.6(3) . . ?
C8 C7 C5 130.8(4) . . ?
N3 C8 C7 110.1(4) . . ?
N1 C11 C12 112.2(3) . . ?
N4 C12 C13 122.5(4) . . ?
N4 C12 C11 115.7(3) . . ?
C13 C12 C11 121.8(4) . . ?
C12 C13 C14 118.7(4) . . ?
C15 C14 C13 119.3(4) . . ?
C14 C15 C16 118.1(4) . . ?
N4 C16 C15 124.0(4) . . ?
N2 N3 C8 108.6(3) . . ?
N3 N2 N1 107.0(3) . . ?
N2 N1 C7 110.8(3) . . ?
N2 N1 C11 118.1(3) . . ?
C7 N1 C11 131.0(3) . . ?
C12 N4 C16 117.3(4) . . ?
C3 S1 C1 95.8(2) . . ?
C5 S2 C4 94.23(18) . . ?
C2 S3 C3 95.9(2) . . ?
C6 S4 C4 94.55(19) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 990597'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H23 N7 S8'
_chemical_formula_sum            'C27 H23 N7 S8'
_chemical_formula_weight         702.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   11.2780(12)
_cell_length_b                   31.812(3)
_cell_length_c                   8.790(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.853(14)
_cell_angle_gamma                90.00
_cell_volume                     3116.1(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3034
_cell_measurement_theta_min      3.66
_cell_measurement_theta_max      25.99

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16122
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.66
_diffrn_reflns_theta_max         25.99
_reflns_number_total             3034
_reflns_number_gt                1721
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/1sq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0407P)²+8.9855P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3034
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1107
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.37521(12) 0.02795(4) 0.39461(16) 0.0632(4) Uani 1 1 d . . .
S2 S 0.16681(12) 0.05156(4) 0.16688(14) 0.0544(4) Uani 1 1 d . . .
S3 S 0.43189(14) 0.12467(4) 0.47529(17) 0.0757(5) Uani 1 1 d . . .
S4 S 0.23777(11) 0.15195(4) 0.23189(13) 0.0501(4) Uani 1 1 d . . .
N1 N 0.5159(3) 0.24496(10) 0.5488(4) 0.0351(8) Uani 1 1 d . . .
N2 N 0.6150(3) 0.25720(12) 0.6447(4) 0.0460(10) Uani 1 1 d . . .
N3 N 0.6816(3) 0.22360(12) 0.6800(4) 0.0513(10) Uani 1 1 d . . .
N4 N 0.5000 0.28151(13) 0.2500 0.0302(11) Uani 1 2 d S . .
C1 C 0.2928(4) -0.01290(14) 0.2966(5) 0.0482(12) Uani 1 1 d . . .
C2 C 0.1983(4) -0.00252(14) 0.1927(5) 0.0489(12) Uani 1 1 d . . .
C3 C 0.2907(4) 0.06877(14) 0.2985(5) 0.0464(12) Uani 1 1 d . . .
C4 C 0.3161(4) 0.10976(14) 0.3279(5) 0.0482(12) Uani 1 1 d . . .
C5 C 0.4272(4) 0.17832(13) 0.4274(5) 0.0386(10) Uani 1 1 d . . .
C6 C 0.3392(4) 0.18951(13) 0.3155(5) 0.0413(11) Uani 1 1 d . . .
H6 H 0.3321 0.2173 0.2825 0.050 Uiso 1 1 calc R . .
C7 C 0.5190(4) 0.20318(13) 0.5202(4) 0.0362(10) Uani 1 1 d . . .
C8 C 0.6247(4) 0.19060(15) 0.6055(5) 0.0508(12) Uani 1 1 d . . .
H8 H 0.6533 0.1631 0.6112 0.061 Uiso 1 1 calc R . .
C9 C 0.3393(5) -0.05633(15) 0.3364(6) 0.0682(15) Uani 1 1 d . . .
H9A H 0.4083 -0.0547 0.4152 0.102 Uiso 1 1 calc R . .
H9B H 0.3614 -0.0694 0.2465 0.102 Uiso 1 1 calc R . .
H9C H 0.2780 -0.0727 0.3731 0.102 Uiso 1 1 calc R . .
C10 C 0.1155(5) -0.03212(16) 0.0955(6) 0.0686(15) Uani 1 1 d . . .
H10A H 0.0553 -0.0163 0.0304 0.103 Uiso 1 1 calc R . .
H10B H 0.0777 -0.0503 0.1609 0.103 Uiso 1 1 calc R . .
H10C H 0.1605 -0.0487 0.0331 0.103 Uiso 1 1 calc R . .
C11 C 0.4282(4) 0.27737(13) 0.4948(5) 0.0409(11) Uani 1 1 d . . .
H11A H 0.4185 0.2959 0.5797 0.049 Uiso 1 1 calc R . .
H11B H 0.3513 0.2643 0.4591 0.049 Uiso 1 1 calc R . .
C12 C 0.4658(4) 0.30285(13) 0.3663(5) 0.0376(10) Uani 1 1 d . . .
C13 C 0.4652(7) 0.34569(15) 0.3698(7) 0.090(2) Uani 1 1 d . . .
H13 H 0.4416 0.3600 0.4525 0.108 Uiso 1 1 calc R . .
C14 C 0.5000 0.3673(2) 0.2500 0.144(6) Uani 1 2 d S . .
H14 H 0.5000 0.3965 0.2500 0.173 Uiso 1 2 calc SR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.746(5) . ?
S1 C3 1.749(4) . ?
S2 C3 1.759(4) . ?
S2 C2 1.764(5) . ?
S3 C5 1.757(4) . ?
S3 C4 1.757(4) . ?
S4 C6 1.737(4) . ?
S4 C4 1.751(5) . ?
N1 N2 1.349(5) . ?
N1 C7 1.354(5) . ?
N1 C11 1.457(5) . ?
N2 N3 1.316(5) . ?
N3 C8 1.347(6) . ?
N4 C12 1.333(5) . ?
N4 C12 1.333(5) 2_655 ?
C1 C2 1.334(6) . ?
C1 C9 1.500(6) . ?
C2 C10 1.498(6) . ?
C3 C4 1.351(6) . ?
C5 C6 1.334(5) . ?
C5 C7 1.450(6) . ?
C7 C8 1.366(6) . ?
C11 C12 1.503(6) . ?
C12 C13 1.363(6) . ?
C13 C14 1.364(6) . ?
C14 C13 1.364(6) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C3 96.0(2) . . ?
C3 S2 C2 95.4(2) . . ?
C5 S3 C4 95.4(2) . . ?
C6 S4 C4 94.2(2) . . ?
N2 N1 C7 110.9(3) . . ?
N2 N1 C11 117.0(3) . . ?
C7 N1 C11 132.1(3) . . ?
N3 N2 N1 107.5(3) . . ?
N2 N3 C8 107.8(3) . . ?
C12 N4 C12 118.8(5) . 2_655 ?
C2 C1 C9 127.0(4) . . ?
C2 C1 S1 117.5(4) . . ?
C9 C1 S1 115.5(3) . . ?
C1 C2 C10 126.7(4) . . ?
C1 C2 S2 117.0(4) . . ?
C10 C2 S2 116.4(4) . . ?
C4 C3 S1 122.7(3) . . ?
C4 C3 S2 123.3(3) . . ?
S1 C3 S2 113.9(2) . . ?
C3 C4 S4 124.8(3) . . ?
C3 C4 S3 120.9(3) . . ?
S4 C4 S3 114.3(2) . . ?
C6 C5 C7 130.9(4) . . ?
C6 C5 S3 115.3(3) . . ?
C7 C5 S3 113.7(3) . . ?
C5 C6 S4 119.7(3) . . ?
N1 C7 C8 103.3(4) . . ?
N1 C7 C5 127.1(4) . . ?
C8 C7 C5 129.5(4) . . ?
N3 C8 C7 110.4(4) . . ?
N1 C11 C12 111.8(3) . . ?
N4 C12 C13 122.0(4) . . ?
N4 C12 C11 116.8(4) . . ?
C13 C12 C11 121.3(4) . . ?
C12 C13 C14 118.9(5) . . ?
C13 C14 C13 119.6(7) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 990598'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H16 Co F12 N4 O4 S4'
_chemical_formula_sum            'C26 H16 Co F12 N4 O4 S4'
_chemical_formula_weight         863.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.2830(13)
_cell_length_b                   12.8980(15)
_cell_length_c                   22.171(4)
_cell_angle_alpha                80.437(12)
_cell_angle_beta                 87.138(11)
_cell_angle_gamma                89.403(8)
_cell_volume                     3459.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10774
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      23.99

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1724
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6658
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43470
_diffrn_reflns_av_R_equivalents  0.1527
_diffrn_reflns_av_sigmaI/netI    0.1680
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         23.99
_reflns_number_total             10774
_reflns_number_gt                4771
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/1sq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0485P)²+16.4000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10774
_refine_ls_number_parameters     919
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2174
_refine_ls_R_factor_gt           0.0896
_refine_ls_wR_factor_ref         0.2078
_refine_ls_wR_factor_gt          0.1577
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.12612(11) -0.37892(11) 0.27030(6) 0.0497(4) Uani 1 1 d . . .
Co2 Co 0.59781(11) 1.08629(11) 0.14034(6) 0.0501(4) Uani 1 1 d . . .
F1 F 0.4866(6) -0.4670(8) 0.3211(5) 0.136(4) Uani 1 1 d . . .
F2 F 0.4727(6) -0.6246(6) 0.3107(5) 0.137(4) Uani 1 1 d . . .
F3 F 0.4882(6) -0.5067(8) 0.2363(4) 0.142(4) Uani 1 1 d . . .
F4 F 0.1549(8) -0.7807(8) 0.2622(9) 0.268(10) Uani 1 1 d . . .
F5 F 0.0268(13) -0.6989(9) 0.2302(7) 0.213(7) Uani 1 1 d . . .
F6 F 0.0289(14) -0.7459(10) 0.3170(6) 0.238(9) Uani 1 1 d . . .
F7 F 0.2523(10) -0.4347(14) 0.0747(5) 0.213(8) Uani 1 1 d . . .
F8 F 0.148(2) -0.5567(13) 0.1020(8) 0.310(13) Uani 1 1 d . . .
F9 F 0.1052(11) -0.4312(15) 0.0382(5) 0.235(9) Uani 1 1 d . . .
F10 F -0.2298(8) -0.3539(12) 0.1506(9) 0.253(9) Uani 1 1 d . . .
F11 F -0.1863(7) -0.2156(9) 0.1567(7) 0.206(7) Uani 1 1 d . . .
F12 F -0.2344(8) -0.3145(14) 0.2304(5) 0.226(8) Uani 1 1 d . . .
F13 F 0.7140(14) 1.4301(10) 0.0674(7) 0.262(10) Uani 1 1 d . . .
F14 F 0.6615(13) 1.4415(10) 0.1525(6) 0.207(6) Uani 1 1 d . . .
F15 F 0.5705(14) 1.5011(9) 0.0840(10) 0.264(9) Uani 1 1 d . . .
F16 F 0.2333(7) 1.1964(10) 0.0981(4) 0.170(5) Uani 1 1 d . . .
F17 F 0.2823(8) 1.3107(8) 0.0240(5) 0.161(4) Uani 1 1 d . . .
F18 F 0.2989(7) 1.1532(9) 0.0187(5) 0.147(4) Uani 1 1 d . . .
F19 F 0.9993(9) 0.9633(13) 0.1702(5) 0.209(7) Uani 1 1 d . . .
F20 F 0.9077(9) 0.9847(17) 0.2405(5) 0.257(10) Uani 1 1 d . . .
F21 F 0.9869(14) 1.0959(9) 0.1948(10) 0.288(12) Uani 1 1 d . . .
F22 F 0.821(3) 1.0370(14) -0.0433(7) 0.353(17) Uani 1 1 d . . .
F23 F 0.9086(10) 1.1488(16) -0.0355(4) 0.223(8) Uani 1 1 d . . .
F24 F 0.7581(12) 1.170(2) -0.0578(5) 0.307(16) Uani 1 1 d . . .
S1 S 0.1974(2) 0.1144(2) 0.58868(12) 0.0649(8) Uani 1 1 d . . .
S2 S 0.2623(3) 0.1516(3) 0.45834(13) 0.0757(9) Uani 1 1 d . . .
S3 S 0.0843(2) -0.1058(2) 0.57694(12) 0.0617(8) Uani 1 1 d . . .
S4 S 0.1654(2) -0.0833(2) 0.44767(12) 0.0619(8) Uani 1 1 d . . .
S5 S 0.4702(2) 0.8886(2) 0.44429(11) 0.0577(8) Uani 1 1 d . . .
S6 S 0.3980(3) 0.6795(2) 0.42336(13) 0.0700(9) Uani 1 1 d . . .
S7 S 0.3877(2) 0.8231(2) 0.59024(12) 0.0594(8) Uani 1 1 d . . .
S8 S 0.3224(2) 0.6167(2) 0.56578(12) 0.0609(8) Uani 1 1 d . . .
O1 O 0.2834(5) -0.4275(5) 0.2919(3) 0.0560(18) Uani 1 1 d . . .
O2 O 0.0807(5) -0.5360(6) 0.2842(3) 0.062(2) Uani 1 1 d . . .
O3 O -0.0243(5) -0.3323(5) 0.2410(3) 0.0551(18) Uani 1 1 d . . .
O4 O 0.1703(6) -0.3979(6) 0.1812(3) 0.069(2) Uani 1 1 d . . .
O5 O 0.7458(5) 1.0500(6) 0.1769(3) 0.0575(19) Uani 1 1 d . . .
O6 O 0.6778(6) 1.1010(6) 0.0531(3) 0.0588(19) Uani 1 1 d . . .
O7 O 0.4502(5) 1.1265(6) 0.1042(3) 0.062(2) Uani 1 1 d . . .
O8 O 0.6265(7) 1.2429(7) 0.1377(4) 0.079(2) Uani 1 1 d . . .
N1 N 0.0772(6) -0.2709(6) 0.3804(3) 0.047(2) Uani 1 1 d . . .
N2 N 0.0779(7) -0.3646(7) 0.3626(4) 0.052(2) Uani 1 1 d . . .
N3 N 0.0891(8) -0.4381(7) 0.4116(5) 0.069(3) Uani 1 1 d . . .
N4 N 0.1784(6) -0.2170(6) 0.2561(3) 0.045(2) Uani 1 1 d . . .
N5 N 0.5260(6) 0.9635(6) 0.2674(3) 0.045(2) Uani 1 1 d . . .
N6 N 0.5246(6) 1.0607(7) 0.2324(3) 0.050(2) Uani 1 1 d . . .
N7 N 0.4635(6) 1.1233(6) 0.2613(4) 0.053(2) Uani 1 1 d . . .
N8 N 0.5599(6) 0.9238(6) 0.1394(3) 0.045(2) Uani 1 1 d . . .
C1 C 0.2713(9) 0.2581(9) 0.4973(5) 0.062(3) Uani 1 1 d . . .
C2 C 0.2404(8) 0.2414(8) 0.5571(5) 0.055(3) Uani 1 1 d . . .
C3 C 0.1987(8) 0.0669(9) 0.5192(4) 0.053(3) Uani 1 1 d . . .
C4 C 0.1544(8) -0.0267(9) 0.5149(4) 0.050(3) Uani 1 1 d . . .
C5 C 0.0896(8) -0.1962(8) 0.4781(4) 0.052(3) Uani 1 1 d . . .
C6 C 0.0552(8) -0.2049(8) 0.5365(4) 0.057(3) Uani 1 1 d . . .
H6 H 0.0158 -0.2637 0.5554 0.068 Uiso 1 1 calc R . .
C7 C 0.0844(7) -0.2827(9) 0.4429(4) 0.049(3) Uani 1 1 d . . .
C8 C 0.0903(9) -0.3891(9) 0.4605(5) 0.063(3) Uani 1 1 d . . .
H8 H 0.0946 -0.4229 0.5008 0.075 Uiso 1 1 calc R . .
C9 C 0.3167(12) 0.3582(10) 0.4593(6) 0.104(5) Uani 1 1 d . . .
H9A H 0.3314 0.3473 0.4179 0.155 Uiso 1 1 calc R . .
H9B H 0.3829 0.3768 0.4761 0.155 Uiso 1 1 calc R . .
H9C H 0.2644 0.4140 0.4599 0.155 Uiso 1 1 calc R . .
C10 C 0.2452(11) 0.3182(11) 0.6012(6) 0.097(4) Uani 1 1 d . . .
H10A H 0.2181 0.2852 0.6411 0.146 Uiso 1 1 calc R . .
H10B H 0.2014 0.3786 0.5873 0.146 Uiso 1 1 calc R . .
H10C H 0.3194 0.3396 0.6034 0.146 Uiso 1 1 calc R . .
C11 C 0.0494(7) -0.1780(7) 0.3352(4) 0.044(2) Uani 1 1 d . . .
H11A H 0.0303 -0.1202 0.3567 0.053 Uiso 1 1 calc R . .
H11B H -0.0139 -0.1941 0.3141 0.053 Uiso 1 1 calc R . .
C12 C 0.1406(7) -0.1446(8) 0.2892(4) 0.040(2) Uani 1 1 d . . .
C13 C 0.1735(7) -0.0397(8) 0.2757(4) 0.047(3) Uani 1 1 d . . .
H13 H 0.1467 0.0088 0.2994 0.057 Uiso 1 1 calc R . .
C14 C 0.2461(8) -0.0090(9) 0.2269(5) 0.057(3) Uani 1 1 d . . .
H14 H 0.2698 0.0603 0.2173 0.069 Uiso 1 1 calc R . .
C15 C 0.2823(8) -0.0816(10) 0.1931(5) 0.056(3) Uani 1 1 d . . .
H15 H 0.3299 -0.0619 0.1592 0.067 Uiso 1 1 calc R . .
C16 C 0.2493(8) -0.1841(9) 0.2085(5) 0.053(3) Uani 1 1 d . . .
H16 H 0.2768 -0.2330 0.1852 0.064 Uiso 1 1 calc R . .
C17 C 0.1045(12) -0.4065(10) 0.1415(6) 0.074(4) Uani 1 1 d . . .
C18 C -0.0075(10) -0.3806(10) 0.1427(5) 0.076(4) Uani 1 1 d . . .
H18 H -0.0471 -0.3886 0.1091 0.091 Uiso 1 1 calc R . .
C19 C -0.0606(9) -0.3444(8) 0.1907(5) 0.059(3) Uani 1 1 d . . .
C20 C 0.153(2) -0.456(2) 0.0865(10) 0.133(7) Uani 1 1 d . . .
C21 C -0.1760(11) -0.3071(14) 0.1825(8) 0.084(4) Uani 1 1 d . . .
C22 C 0.3189(8) -0.5186(9) 0.2876(4) 0.049(3) Uani 1 1 d . . .
C23 C 0.2610(9) -0.6089(9) 0.2820(5) 0.062(3) Uani 1 1 d . . .
H23 H 0.2995 -0.6706 0.2792 0.074 Uiso 1 1 calc R . .
C24 C 0.1462(9) -0.6099(9) 0.2802(5) 0.059(3) Uani 1 1 d . . .
C25 C 0.4392(10) -0.5319(10) 0.2905(7) 0.072(4) Uani 1 1 d . . .
C26 C 0.0917(17) -0.7098(11) 0.2746(9) 0.104(5) Uani 1 1 d . . .
C27 C 0.2812(9) 0.7907(10) 0.7049(5) 0.075(4) Uani 1 1 d . . .
H27A H 0.3128 0.8594 0.7004 0.113 Uiso 1 1 calc R . .
H27B H 0.3114 0.7459 0.7390 0.113 Uiso 1 1 calc R . .
H27C H 0.2037 0.7957 0.7119 0.113 Uiso 1 1 calc R . .
C28 C 0.2111(11) 0.5660(10) 0.6783(5) 0.089(4) Uani 1 1 d . . .
H28A H 0.2017 0.5073 0.6576 0.134 Uiso 1 1 calc R . .
H28B H 0.1411 0.5933 0.6890 0.134 Uiso 1 1 calc R . .
H28C H 0.2496 0.5435 0.7149 0.134 Uiso 1 1 calc R . .
C29 C 0.3056(8) 0.7451(9) 0.6473(4) 0.052(3) Uani 1 1 d . . .
C30 C 0.2762(8) 0.6513(9) 0.6366(4) 0.055(3) Uani 1 1 d . . .
C31 C 0.3777(8) 0.7400(8) 0.5352(5) 0.051(3) Uani 1 1 d . . .
C32 C 0.4121(8) 0.7677(8) 0.4761(4) 0.057(3) Uani 1 1 d . . .
C33 C 0.4145(8) 0.7774(9) 0.3603(4) 0.055(3) Uani 1 1 d . . .
H33 H 0.4009 0.7641 0.3214 0.066 Uiso 1 1 calc R . .
C34 C 0.4474(8) 0.8734(10) 0.3684(4) 0.055(3) Uani 1 1 d . . .
C35 C 0.4681(7) 0.9656(8) 0.3207(4) 0.041(2) Uani 1 1 d . . .
C36 C 0.4298(8) 1.0667(9) 0.3161(5) 0.056(3) Uani 1 1 d . . .
H36 H 0.3870 1.0926 0.3460 0.068 Uiso 1 1 calc R . .
C37 C 0.5946(7) 0.8795(8) 0.2481(4) 0.050(3) Uani 1 1 d . . .
H37A H 0.5925 0.8188 0.2804 0.060 Uiso 1 1 calc R . .
H37B H 0.6695 0.9037 0.2416 0.060 Uiso 1 1 calc R . .
C38 C 0.5570(7) 0.8473(9) 0.1894(4) 0.047(3) Uani 1 1 d . . .
C39 C 0.5237(8) 0.7476(9) 0.1869(5) 0.060(3) Uani 1 1 d . . .
H39 H 0.5241 0.6959 0.2216 0.072 Uiso 1 1 calc R . .
C40 C 0.4895(10) 0.7242(11) 0.1324(7) 0.078(4) Uani 1 1 d . . .
H40 H 0.4647 0.6572 0.1302 0.094 Uiso 1 1 calc R . .
C41 C 0.4927(9) 0.8008(11) 0.0816(6) 0.071(3) Uani 1 1 d . . .
H41 H 0.4717 0.7864 0.0441 0.085 Uiso 1 1 calc R . .
C42 C 0.5275(8) 0.8998(10) 0.0872(5) 0.061(3) Uani 1 1 d . . .
H42 H 0.5283 0.9522 0.0528 0.073 Uiso 1 1 calc R . .
C43 C 0.8367(8) 1.0534(8) 0.1486(5) 0.051(3) Uani 1 1 d . . .
C44 C 0.8588(8) 1.0737(10) 0.0857(5) 0.071(4) Uani 1 1 d . . .
H44 H 0.9308 1.0710 0.0709 0.085 Uiso 1 1 calc R . .
C45 C 0.7789(9) 1.0976(9) 0.0441(5) 0.063(3) Uani 1 1 d . . .
C46 C 0.8167(14) 1.132(3) -0.0251(8) 0.149(10) Uani 1 1 d . . .
C47 C 0.9315(10) 1.0182(19) 0.1897(7) 0.106(6) Uani 1 1 d . . .
C48 C 0.5729(13) 1.3149(10) 0.1084(6) 0.073(4) Uani 1 1 d . . .
C49 C 0.4734(12) 1.3084(11) 0.0813(5) 0.078(4) Uani 1 1 d . . .
H49 H 0.4435 1.3702 0.0609 0.094 Uiso 1 1 calc R . .
C50 C 0.4182(9) 1.2181(10) 0.0831(5) 0.057(3) Uani 1 1 d . . .
C51 C 0.635(2) 1.4222(13) 0.1023(9) 0.141(9) Uani 1 1 d . . .
C52 C 0.3087(13) 1.2238(13) 0.0557(7) 0.095(5) 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
Co1 O3 2.041(6) . ?
Co1 O4 2.075(7) . ?
Co1 O2 2.075(7) . ?
Co1 O1 2.079(6) . ?
Co1 N2 2.138(8) . ?
Co1 N4 2.160(8) . ?
Co2 O8 2.045(8) . ?
Co2 O5 2.046(6) . ?
Co2 O7 2.046(7) . ?
Co2 O6 2.106(6) . ?
Co2 N8 2.155(8) . ?
Co2 N6 2.165(8) . ?
F1 C25 1.319(14) . ?
F2 C25 1.276(12) . ?
F3 C25 1.311(13) . ?
F4 C26 1.249(17) . ?
F5 C26 1.286(17) . ?
F6 C26 1.219(18) . ?
F7 C20 1.26(2) . ?
F8 C20 1.29(3) . ?
F9 C20 1.24(2) . ?
F10 C21 1.223(15) . ?
F11 C21 1.232(16) . ?
F12 C21 1.242(16) . ?
F13 C51 1.20(2) . ?
F14 C51 1.24(2) . ?
F15 C51 1.31(2) . ?
F16 C52 1.294(16) . ?
F17 C52 1.269(14) . ?
F18 C52 1.333(16) . ?
F19 C47 1.199(16) . ?
F20 C47 1.160(16) . ?
F21 C47 1.24(2) . ?
F22 C46 1.35(3) . ?
F23 C46 1.156(16) . ?
F24 C46 1.10(2) . ?
S1 C2 1.747(11) . ?
S1 C3 1.749(10) . ?
S2 C3 1.745(11) . ?
S2 C1 1.748(11) . ?
S3 C6 1.729(11) . ?
S3 C4 1.763(11) . ?
S4 C5 1.757(11) . ?
S4 C4 1.764(9) . ?
S5 C32 1.745(11) . ?
S5 C34 1.762(10) . ?
S6 C33 1.726(10) . ?
S6 C32 1.778(11) . ?
S7 C29 1.761(11) . ?
S7 C31 1.763(10) . ?
S8 C31 1.752(10) . ?
S8 C30 1.767(10) . ?
O1 C22 1.265(11) . ?
O2 C24 1.252(11) . ?
O3 C19 1.255(11) . ?
O4 C17 1.243(13) . ?
O5 C43 1.251(11) . ?
O6 C45 1.249(11) . ?
O7 C50 1.263(12) . ?
O8 C48 1.244(15) . ?
N1 N2 1.333(10) . ?
N1 C7 1.376(11) . ?
N1 C11 1.476(11) . ?
N2 N3 1.330(10) . ?
N3 C8 1.344(12) . ?
N4 C12 1.345(11) . ?
N4 C16 1.349(12) . ?
N5 C35 1.352(10) . ?
N5 N6 1.360(10) . ?
N5 C37 1.473(11) . ?
N6 N7 1.317(10) . ?
N7 C36 1.356(12) . ?
N8 C42 1.328(12) . ?
N8 C38 1.355(11) . ?
C1 C2 1.343(13) . ?
C1 C9 1.515(16) . ?
C2 C10 1.507(14) . ?
C3 C4 1.349(13) . ?
C5 C6 1.328(12) . ?
C5 C7 1.468(13) . ?
C7 C8 1.365(13) . ?
C11 C12 1.494(12) . ?
C12 C13 1.395(13) . ?
C13 C14 1.375(13) . ?
C14 C15 1.352(13) . ?
C15 C16 1.370(14) . ?
C17 C18 1.413(16) . ?
C17 C20 1.552(19) . ?
C18 C19 1.364(14) . ?
C19 C21 1.502(15) . ?
C22 C23 1.398(14) . ?
C22 C25 1.489(14) . ?
C23 C24 1.414(14) . ?
C24 C26 1.484(17) . ?
C27 C29 1.508(13) . ?
C28 C30 1.521(14) . ?
C29 C30 1.328(14) . ?
C31 C32 1.346(12) . ?
C33 C34 1.350(14) . ?
C34 C35 1.469(13) . ?
C35 C36 1.371(13) . ?
C37 C38 1.524(13) . ?
C38 C39 1.365(14) . ?
C39 C40 1.380(15) . ?
C40 C41 1.369(16) . ?
C41 C42 1.377(15) . ?
C43 C44 1.389(13) . ?
C43 C47 1.533(16) . ?
C44 C45 1.377(14) . ?
C45 C46 1.57(2) . ?
C48 C49 1.398(17) . ?
C48 C51 1.57(2) . ?
C49 C50 1.349(16) . ?
C50 C52 1.499(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O4 88.2(3) . . ?
O3 Co1 O2 91.5(3) . . ?
O4 Co1 O2 86.1(3) . . ?
O3 Co1 O1 174.7(3) . . ?
O4 Co1 O1 86.6(3) . . ?
O2 Co1 O1 88.3(3) . . ?
O3 Co1 N2 91.5(3) . . ?
O4 Co1 N2 178.0(3) . . ?
O2 Co1 N2 91.9(3) . . ?
O1 Co1 N2 93.7(3) . . ?
O3 Co1 N4 90.1(3) . . ?
O4 Co1 N4 93.6(3) . . ?
O2 Co1 N4 178.3(3) . . ?
O1 Co1 N4 89.9(3) . . ?
N2 Co1 N4 88.4(3) . . ?
O8 Co2 O5 90.4(3) . . ?
O8 Co2 O7 88.2(3) . . ?
O5 Co2 O7 178.5(3) . . ?
O8 Co2 O6 87.7(3) . . ?
O5 Co2 O6 87.8(3) . . ?
O7 Co2 O6 92.5(3) . . ?
O8 Co2 N8 176.6(3) . . ?
O5 Co2 N8 92.9(3) . . ?
O7 Co2 N8 88.6(3) . . ?
O6 Co2 N8 91.5(3) . . ?
O8 Co2 N6 95.1(3) . . ?
O5 Co2 N6 88.4(3) . . ?
O7 Co2 N6 91.4(3) . . ?
O6 Co2 N6 175.3(3) . . ?
N8 Co2 N6 85.9(3) . . ?
C2 S1 C3 95.8(5) . . ?
C3 S2 C1 95.8(5) . . ?
C6 S3 C4 95.1(5) . . ?
C5 S4 C4 95.3(5) . . ?
C32 S5 C34 94.0(5) . . ?
C33 S6 C32 93.4(5) . . ?
C29 S7 C31 95.5(5) . . ?
C31 S8 C30 95.8(5) . . ?
C22 O1 Co1 122.8(6) . . ?
C24 O2 Co1 123.7(7) . . ?
C19 O3 Co1 125.2(6) . . ?
C17 O4 Co1 124.4(7) . . ?
C43 O5 Co2 126.9(6) . . ?
C45 O6 Co2 124.1(6) . . ?
C50 O7 Co2 126.5(8) . . ?
C48 O8 Co2 124.3(9) . . ?
N2 N1 C7 110.2(8) . . ?
N2 N1 C11 118.0(7) . . ?
C7 N1 C11 130.7(8) . . ?
N3 N2 N1 108.3(8) . . ?
N3 N2 Co1 125.9(7) . . ?
N1 N2 Co1 120.3(6) . . ?
N2 N3 C8 107.4(9) . . ?
C12 N4 C16 117.3(9) . . ?
C12 N4 Co1 124.7(6) . . ?
C16 N4 Co1 117.9(7) . . ?
C35 N5 N6 109.4(8) . . ?
C35 N5 C37 129.9(8) . . ?
N6 N5 C37 120.3(7) . . ?
N7 N6 N5 108.7(7) . . ?
N7 N6 Co2 130.3(6) . . ?
N5 N6 Co2 120.5(6) . . ?
N6 N7 C36 107.2(8) . . ?
C42 N8 C38 118.0(9) . . ?
C42 N8 Co2 117.0(7) . . ?
C38 N8 Co2 124.6(7) . . ?
C2 C1 C9 127.8(10) . . ?
C2 C1 S2 116.9(9) . . ?
C9 C1 S2 115.2(8) . . ?
C1 C2 C10 127.2(11) . . ?
C1 C2 S1 116.8(8) . . ?
C10 C2 S1 115.9(8) . . ?
C4 C3 S2 124.9(8) . . ?
C4 C3 S1 121.7(8) . . ?
S2 C3 S1 113.4(6) . . ?
C3 C4 S3 123.0(7) . . ?
C3 C4 S4 123.1(8) . . ?
S3 C4 S4 113.9(7) . . ?
C6 C5 C7 123.2(10) . . ?
C6 C5 S4 116.5(8) . . ?
C7 C5 S4 119.4(7) . . ?
C5 C6 S3 119.2(9) . . ?
C8 C7 N1 103.5(9) . . ?
C8 C7 C5 131.2(10) . . ?
N1 C7 C5 125.2(9) . . ?
N3 C8 C7 110.5(9) . . ?
N1 C11 C12 112.8(7) . . ?
N4 C12 C13 122.0(9) . . ?
N4 C12 C11 116.5(9) . . ?
C13 C12 C11 120.9(9) . . ?
C14 C13 C12 119.2(9) . . ?
C15 C14 C13 118.7(10) . . ?
C14 C15 C16 120.2(10) . . ?
N4 C16 C15 122.6(9) . . ?
O4 C17 C18 127.1(10) . . ?
O4 C17 C20 114.8(14) . . ?
C18 C17 C20 118.1(14) . . ?
C19 C18 C17 123.4(11) . . ?
O3 C19 C18 128.7(10) . . ?
O3 C19 C21 113.7(10) . . ?
C18 C19 C21 117.5(11) . . ?
F9 C20 F7 107(2) . . ?
F9 C20 F8 108(2) . . ?
F7 C20 F8 105(2) . . ?
F9 C20 C17 115.3(18) . . ?
F7 C20 C17 112.8(17) . . ?
F8 C20 C17 107.7(19) . . ?
F10 C21 F11 101.1(14) . . ?
F10 C21 F12 102.1(15) . . ?
F11 C21 F12 105.4(16) . . ?
F10 C21 C19 115.8(14) . . ?
F11 C21 C19 115.4(13) . . ?
F12 C21 C19 115.2(12) . . ?
O1 C22 C23 129.2(9) . . ?
O1 C22 C25 115.3(10) . . ?
C23 C22 C25 115.5(10) . . ?
C22 C23 C24 122.4(9) . . ?
O2 C24 C23 128.2(10) . . ?
O2 C24 C26 113.3(12) . . ?
C23 C24 C26 118.5(12) . . ?
F2 C25 F3 105.1(11) . . ?
F2 C25 F1 107.6(12) . . ?
F3 C25 F1 101.1(11) . . ?
F2 C25 C22 115.9(11) . . ?
F3 C25 C22 111.3(11) . . ?
F1 C25 C22 114.5(11) . . ?
F6 C26 F4 109.2(16) . . ?
F6 C26 F5 100.1(18) . . ?
F4 C26 F5 102.7(16) . . ?
F6 C26 C24 116.0(15) . . ?
F4 C26 C24 114.6(16) . . ?
F5 C26 C24 112.5(14) . . ?
C30 C29 C27 127.0(10) . . ?
C30 C29 S7 117.3(8) . . ?
C27 C29 S7 115.6(8) . . ?
C29 C30 C28 128.7(10) . . ?
C29 C30 S8 116.8(8) . . ?
C28 C30 S8 114.5(9) . . ?
C32 C31 S8 123.7(8) . . ?
C32 C31 S7 123.2(8) . . ?
S8 C31 S7 113.0(6) . . ?
C31 C32 S5 125.1(8) . . ?
C31 C32 S6 120.4(8) . . ?
S5 C32 S6 114.5(6) . . ?
C34 C33 S6 118.9(8) . . ?
C33 C34 C35 127.0(9) . . ?
C33 C34 S5 116.2(8) . . ?
C35 C34 S5 116.8(8) . . ?
N5 C35 C36 104.6(8) . . ?
N5 C35 C34 124.5(9) . . ?
C36 C35 C34 130.6(9) . . ?
N7 C36 C35 110.0(9) . . ?
N5 C37 C38 111.9(7) . . ?
N8 C38 C39 122.0(10) . . ?
N8 C38 C37 115.7(9) . . ?
C39 C38 C37 122.3(10) . . ?
C38 C39 C40 119.2(11) . . ?
C41 C40 C39 119.3(12) . . ?
C40 C41 C42 118.5(11) . . ?
N8 C42 C41 123.0(11) . . ?
O5 C43 C44 128.0(9) . . ?
O5 C43 C47 113.6(10) . . ?
C44 C43 C47 117.9(10) . . ?
C45 C44 C43 123.0(9) . . ?
O6 C45 C44 129.5(9) . . ?
O6 C45 C46 112.9(11) . . ?
C44 C45 C46 117.5(11) . . ?
F24 C46 F23 119(3) . . ?
F24 C46 F22 98.0(19) . . ?
F23 C46 F22 95(2) . . ?
F24 C46 C45 119.5(15) . . ?
F23 C46 C45 116.7(15) . . ?
F22 C46 C45 100(2) . . ?
F20 C47 F19 110(2) . . ?
F20 C47 F21 101.9(16) . . ?
F19 C47 F21 100.9(15) . . ?
F20 C47 C43 116.1(12) . . ?
F19 C47 C43 116.5(12) . . ?
F21 C47 C43 109.3(17) . . ?
O8 C48 C49 128.5(12) . . ?
O8 C48 C51 110.2(16) . . ?
C49 C48 C51 121.3(17) . . ?
C50 C49 C48 123.9(12) . . ?
O7 C50 C49 126.7(11) . . ?
O7 C50 C52 115.0(12) . . ?
C49 C50 C52 118.2(12) . . ?
F13 C51 F14 109(3) . . ?
F13 C51 F15 107.3(17) . . ?
F14 C51 F15 101.8(16) . . ?
F13 C51 C48 114.6(14) . . ?
F14 C51 C48 112.3(14) . . ?
F15 C51 C48 111(2) . . ?
F17 C52 F16 109.0(13) . . ?
F17 C52 F18 104.7(14) . . ?
F16 C52 F18 103.1(16) . . ?
F17 C52 C50 117.1(15) . . ?
F16 C52 C50 110.1(12) . . ?
F18 C52 C50 111.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        23.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.094
_database_code_depnum_ccdc_archive 'CCDC 990599'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C108 H92 Cd N28 O2 S32 2(Cl O4), 2(O)'
_chemical_formula_sum            'C108 H92 Cd Cl2 N28 O12 S32'
_chemical_formula_weight         3183.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4cc

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

_cell_length_a                   21.102(3)
_cell_length_b                   21.102(2)
_cell_length_c                   15.6110(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6951.5(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5749
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      24.99

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'dark orange'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3154
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36180
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         24.99
_reflns_number_total             5749
_reflns_number_gt                4030
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/1sq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0242P)²+9.5477P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_number_reflns         5749
_refine_ls_number_parameters     431
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1030
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 0.5000 0.70017(6) 0.03622(19) Uani 1 4 d S . .
O1 O 0.5000 0.5000 0.5510(5) 0.059(2) Uani 1 4 d S . .
O2 O 0.5000 0.5000 0.8454(6) 0.066(3) Uani 1 4 d S . .
S1 S 0.67002(9) 0.91902(9) 0.77128(16) 0.0801(6) Uani 1 1 d . . .
S2 S 0.80497(9) 0.91077(8) 0.81601(15) 0.0693(6) Uani 1 1 d . . .
S3 S 0.80478(8) 0.76106(8) 0.77507(14) 0.0620(5) Uani 1 1 d . . .
S4 S 0.66763(8) 0.76613(7) 0.73388(13) 0.0620(5) Uani 1 1 d . . .
S5 S 0.71678(8) 0.69366(8) 0.97886(12) 0.0660(6) Uani 1 1 d . . .
S6 S 0.85280(8) 0.69067(10) 1.02355(15) 0.0762(6) Uani 1 1 d . . .
S7 S 0.84685(11) 0.84238(11) 1.06627(15) 0.0873(6) Uani 1 1 d . . .
S8 S 0.71174(10) 0.84398(10) 1.01918(15) 0.0797(6) Uani 1 1 d . . .
N1 N 0.6834(2) 0.5865(2) 0.6687(3) 0.0364(11) Uani 1 1 d . . .
N2 N 0.6374(2) 0.5436(2) 0.6594(3) 0.0410(11) Uani 1 1 d . . .
N3 N 0.58786(19) 0.56688(18) 0.7018(4) 0.0424(11) Uani 1 1 d . . .
N4 N 0.7709(2) 0.5265(2) 0.7685(3) 0.0425(12) Uani 1 1 d . . .
N5 N 0.7281(2) 0.5074(2) 0.9329(3) 0.0517(14) Uani 1 1 d . . .
N6 N 0.6753(3) 0.4721(3) 0.9226(4) 0.076(2) Uani 1 1 d . . .
N7 N 0.6275(3) 0.5073(3) 0.9422(7) 0.099(2) Uani 1 1 d . . .
C1 C 0.7060(4) 0.9871(3) 0.8158(5) 0.072(2) Uani 1 1 d . . .
C2 C 0.7660(4) 0.9830(3) 0.8366(5) 0.067(2) Uani 1 1 d . . .
C3 C 0.7368(3) 0.8701(3) 0.7806(5) 0.0584(18) Uani 1 1 d . . .
C4 C 0.7363(3) 0.8079(3) 0.7657(4) 0.0513(17) Uani 1 1 d . . .
C5 C 0.7046(3) 0.6915(3) 0.7361(4) 0.0442(15) Uani 1 1 d . . .
C6 C 0.7665(3) 0.6900(3) 0.7558(4) 0.0544(18) Uani 1 1 d . . .
H6 H 0.7882 0.6517 0.7590 0.065 Uiso 1 1 calc R . .
C7 C 0.6647(2) 0.6363(2) 0.7157(4) 0.0375(14) Uani 1 1 d . . .
C8 C 0.6027(3) 0.6233(3) 0.7352(4) 0.0464(16) Uani 1 1 d . . .
H8 H 0.5755 0.6493 0.7663 0.056 Uiso 1 1 calc R . .
C9 C 0.6622(5) 1.0433(4) 0.8237(7) 0.112(3) Uani 1 1 d . . .
H9A H 0.6209 1.0320 0.8026 0.168 Uiso 1 1 calc R . .
H9B H 0.6786 1.0780 0.7907 0.168 Uiso 1 1 calc R . .
H9C H 0.6590 1.0556 0.8827 0.168 Uiso 1 1 calc R . .
C10 C 0.8080(4) 1.0329(4) 0.8773(6) 0.098(3) Uani 1 1 d . . .
H10A H 0.8498 1.0159 0.8854 0.147 Uiso 1 1 calc R . .
H10B H 0.7906 1.0450 0.9318 0.147 Uiso 1 1 calc R . .
H10C H 0.8102 1.0693 0.8406 0.147 Uiso 1 1 calc R . .
C11 C 0.7444(2) 0.5729(3) 0.6300(4) 0.0454(15) Uani 1 1 d . . .
H11A H 0.7623 0.6120 0.6082 0.054 Uiso 1 1 calc R . .
H11B H 0.7380 0.5447 0.5818 0.054 Uiso 1 1 calc R . .
C12 C 0.7912(2) 0.5431(2) 0.6906(4) 0.0417(14) Uani 1 1 d . . .
C13 C 0.8529(3) 0.5353(3) 0.6643(5) 0.0618(19) Uani 1 1 d . . .
H13 H 0.8658 0.5477 0.6099 0.074 Uiso 1 1 calc R . .
C14 C 0.8946(3) 0.5086(4) 0.7214(6) 0.087(3) Uani 1 1 d . . .
H14 H 0.9365 0.5017 0.7051 0.105 Uiso 1 1 calc R . .
C15 C 0.8753(3) 0.4923(4) 0.8011(5) 0.069(2) Uani 1 1 d . . .
H15 H 0.9038 0.4757 0.8407 0.083 Uiso 1 1 calc R . .
C16 C 0.8125(3) 0.5009(3) 0.8221(4) 0.0459(15) Uani 1 1 d . . .
C17 C 0.7447(5) 0.9139(4) 1.0637(6) 0.086(3) Uani 1 1 d . . .
C18 C 0.8043(5) 0.9118(4) 1.0843(6) 0.088(3) Uani 1 1 d . . .
C19 C 0.7820(3) 0.7978(3) 1.0314(5) 0.068(2) Uani 1 1 d . . .
C20 C 0.7828(3) 0.7365(3) 1.0153(5) 0.0598(18) Uani 1 1 d . . .
C21 C 0.7547(3) 0.6190(3) 0.9782(4) 0.0475(16) Uani 1 1 d . . .
C22 C 0.8164(3) 0.6201(3) 0.9975(4) 0.0620(19) Uani 1 1 d . . .
H22 H 0.8397 0.5827 0.9969 0.074 Uiso 1 1 calc R . .
C23 C 0.7125(3) 0.5666(3) 0.9588(5) 0.0496(15) Uani 1 1 d . . .
C24 C 0.6483(3) 0.5654(3) 0.9641(6) 0.071(2) Uani 1 1 d . . .
H24 H 0.6227 0.5992 0.9803 0.086 Uiso 1 1 calc R . .
C25 C 0.6962(5) 0.9678(4) 1.0692(7) 0.125(4) Uani 1 1 d . . .
H25A H 0.6559 0.9532 1.0486 0.188 Uiso 1 1 calc R . .
H25B H 0.7103 1.0028 1.0346 0.188 Uiso 1 1 calc R . .
H25C H 0.6921 0.9813 1.1276 0.188 Uiso 1 1 calc R . .
C26 C 0.8439(6) 0.9655(5) 1.1230(7) 0.142(5) Uani 1 1 d . . .
H26A H 0.8866 0.9513 1.1314 0.213 Uiso 1 1 calc R . .
H26B H 0.8261 0.9779 1.1771 0.213 Uiso 1 1 calc R . .
H26C H 0.8438 1.0012 1.0848 0.213 Uiso 1 1 calc R . .
C27 C 0.7885(3) 0.4795(3) 0.9075(4) 0.0581(19) Uani 1 1 d . . .
H27A H 0.7839 0.4337 0.9064 0.070 Uiso 1 1 calc R . .
H27B H 0.8200 0.4897 0.9506 0.070 Uiso 1 1 calc R . .
Cl1 Cl 1.0000 0.5000 0.5011(2) 0.0978(10) Uani 1 2 d S . .
O3 O 0.9562(10) 0.4600(7) 0.5230(16) 0.180(11) Uani 0.50 1 d P . .
O4 O 1.0570(6) 0.4709(16) 0.4925(11) 0.200(12) Uani 0.50 1 d P . .
O5 O 0.9864(11) 0.520(5) 0.4337(17) 0.56(6) Uani 0.50 1 d P . .
O6 O 1.0000 0.5000 0.5783(17) 0.68(5) Uani 1 2 d S . .
O7 O 0.0000 0.0000 0.787(3) 0.291(15) Uani 1 4 d S . .
O8 O 0.0000 0.0000 0.445(3) 0.299(12) Uani 1 4 d S . .


_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
Cd1 O2 2.267(9) . ?
Cd1 O1 2.328(8) . ?
Cd1 N3 2.330(4) 3_665 ?
Cd1 N3 2.330(4) 7_655 ?
Cd1 N3 2.330(4) 6_565 ?
Cd1 N3 2.330(4) . ?
S1 C3 1.753(7) . ?
S1 C1 1.768(7) . ?
S2 C2 1.761(7) . ?
S2 C3 1.763(6) . ?
S3 C6 1.730(6) . ?
S3 C4 1.756(6) . ?
S4 C5 1.758(6) . ?
S4 C4 1.768(6) . ?
S5 C20 1.755(7) . ?
S5 C21 1.767(6) . ?
S6 C22 1.724(7) . ?
S6 C20 1.771(7) . ?
S7 C18 1.740(10) . ?
S7 C19 1.747(7) . ?
S8 C17 1.772(9) . ?
S8 C19 1.785(8) . ?
N1 N2 1.337(6) . ?
N1 C7 1.340(7) . ?
N1 C11 1.450(7) . ?
N2 N3 1.331(6) . ?
N3 C8 1.336(7) . ?
N4 C16 1.328(7) . ?
N4 C12 1.335(7) . ?
N5 N6 1.349(7) . ?
N5 C23 1.354(8) . ?
N5 C27 1.460(8) . ?
N6 N7 1.290(9) . ?
N7 C24 1.346(9) . ?
C1 C2 1.309(10) . ?
C1 C9 1.508(10) . ?
C2 C10 1.516(10) . ?
C3 C4 1.334(8) . ?
C5 C6 1.341(8) . ?
C5 C7 1.472(7) . ?
C7 C8 1.373(7) . ?
C11 C12 1.505(8) . ?
C12 C13 1.375(8) . ?
C13 C14 1.374(10) . ?
C14 C15 1.354(11) . ?
C15 C16 1.378(9) . ?
C16 C27 1.495(8) . ?
C17 C18 1.299(12) . ?
C17 C25 1.533(12) . ?
C18 C26 1.534(12) . ?
C19 C20 1.318(9) . ?
C21 C22 1.337(8) . ?
C21 C23 1.451(8) . ?
C23 C24 1.358(8) . ?
Cl1 O5 1.17(4) . ?
Cl1 O5 1.17(4) 3_765 ?
Cl1 O6 1.21(3) . ?
Cl1 O3 1.298(14) . ?
Cl1 O3 1.298(14) 3_765 ?
Cl1 O4 1.356(14) 3_765 ?
Cl1 O4 1.356(15) . ?
O3 O6 1.52(3) . ?
O3 O4 1.56(3) 3_765 ?
O4 O5 1.31(3) 3_765 ?
O4 O3 1.56(3) 3_765 ?
O5 O5 1.03(17) 3_765 ?
O5 O4 1.31(3) 3_765 ?
O6 O3 1.52(3) 3_765 ?

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
O2 Cd1 O1 180.000(3) . . ?
O2 Cd1 N3 89.36(15) . 3_665 ?
O1 Cd1 N3 90.64(15) . 3_665 ?
O2 Cd1 N3 89.36(15) . 7_655 ?
O1 Cd1 N3 90.64(15) . 7_655 ?
N3 Cd1 N3 89.993(4) 3_665 7_655 ?
O2 Cd1 N3 89.36(15) . 6_565 ?
O1 Cd1 N3 90.64(15) . 6_565 ?
N3 Cd1 N3 89.993(4) 3_665 6_565 ?
N3 Cd1 N3 178.7(3) 7_655 6_565 ?
O2 Cd1 N3 89.36(15) . . ?
O1 Cd1 N3 90.64(15) . . ?
N3 Cd1 N3 178.7(3) 3_665 . ?
N3 Cd1 N3 89.993(5) 7_655 . ?
N3 Cd1 N3 89.993(5) 6_565 . ?
C3 S1 C1 95.7(3) . . ?
C2 S2 C3 95.6(3) . . ?
C6 S3 C4 95.1(3) . . ?
C5 S4 C4 94.4(3) . . ?
C20 S5 C21 95.9(3) . . ?
C22 S6 C20 94.7(3) . . ?
C18 S7 C19 95.7(4) . . ?
C17 S8 C19 94.9(4) . . ?
N2 N1 C7 112.1(4) . . ?
N2 N1 C11 117.7(5) . . ?
C7 N1 C11 130.1(5) . . ?
N3 N2 N1 105.4(4) . . ?
N2 N3 C8 109.9(4) . . ?
N2 N3 Cd1 113.3(3) . . ?
C8 N3 Cd1 136.9(4) . . ?
C16 N4 C12 118.0(5) . . ?
N6 N5 C23 110.2(5) . . ?
N6 N5 C27 117.7(6) . . ?
C23 N5 C27 131.7(5) . . ?
N7 N6 N5 107.4(6) . . ?
N6 N7 C24 109.2(6) . . ?
C2 C1 C9 128.7(7) . . ?
C2 C1 S1 117.3(6) . . ?
C9 C1 S1 114.0(6) . . ?
C1 C2 C10 128.5(7) . . ?
C1 C2 S2 117.6(6) . . ?
C10 C2 S2 113.9(6) . . ?
C4 C3 S1 124.0(5) . . ?
C4 C3 S2 122.7(5) . . ?
S1 C3 S2 113.3(3) . . ?
C3 C4 S3 122.2(5) . . ?
C3 C4 S4 123.1(5) . . ?
S3 C4 S4 114.7(3) . . ?
C6 C5 C7 125.9(5) . . ?
C6 C5 S4 117.3(4) . . ?
C7 C5 S4 116.8(4) . . ?
C5 C6 S3 118.3(5) . . ?
N1 C7 C8 104.2(5) . . ?
N1 C7 C5 124.8(5) . . ?
C8 C7 C5 131.0(5) . . ?
N3 C8 C7 108.4(5) . . ?
N1 C11 C12 113.8(5) . . ?
N4 C12 C13 122.9(6) . . ?
N4 C12 C11 118.2(5) . . ?
C13 C12 C11 118.9(6) . . ?
C14 C13 C12 117.5(7) . . ?
C15 C14 C13 120.5(7) . . ?
C14 C15 C16 118.4(7) . . ?
N4 C16 C15 122.6(6) . . ?
N4 C16 C27 117.5(5) . . ?
C15 C16 C27 119.9(6) . . ?
C18 C17 C25 131.1(9) . . ?
C18 C17 S8 116.7(7) . . ?
C25 C17 S8 112.2(8) . . ?
C17 C18 C26 126.8(10) . . ?
C17 C18 S7 119.2(7) . . ?
C26 C18 S7 113.9(9) . . ?
C20 C19 S7 125.4(6) . . ?
C20 C19 S8 121.7(6) . . ?
S7 C19 S8 112.9(4) . . ?
C19 C20 S5 124.0(6) . . ?
C19 C20 S6 122.1(6) . . ?
S5 C20 S6 113.8(4) . . ?
C22 C21 C23 131.1(6) . . ?
C22 C21 S5 115.1(5) . . ?
C23 C21 S5 113.7(4) . . ?
C21 C22 S6 120.2(6) . . ?
N5 C23 C24 104.0(5) . . ?
N5 C23 C21 128.1(6) . . ?
C24 C23 C21 127.9(6) . . ?
N7 C24 C23 109.1(6) . . ?
N5 C27 C16 114.6(5) . . ?
O5 Cl1 O5 52(8) . 3_765 ?
O5 Cl1 O6 154(4) . . ?
O5 Cl1 O6 154(4) 3_765 . ?
O5 Cl1 O3 107(4) . . ?
O5 Cl1 O3 100(4) 3_765 . ?
O6 Cl1 O3 74.7(12) . . ?
O5 Cl1 O3 100(4) . 3_765 ?
O5 Cl1 O3 107(4) 3_765 3_765 ?
O6 Cl1 O3 74.7(12) . 3_765 ?
O3 Cl1 O3 149(2) . 3_765 ?
O5 Cl1 O4 61.9(17) . 3_765 ?
O5 Cl1 O4 107(2) 3_765 3_765 ?
O6 Cl1 O4 95.7(7) . 3_765 ?
O3 Cl1 O4 71.9(12) . 3_765 ?
O3 Cl1 O4 111.3(11) 3_765 3_765 ?
O5 Cl1 O4 107(2) . . ?
O5 Cl1 O4 61.9(17) 3_765 . ?
O6 Cl1 O4 95.7(7) . . ?
O3 Cl1 O4 111.3(11) . . ?
O3 Cl1 O4 71.9(12) 3_765 . ?
O4 Cl1 O4 168.6(14) 3_765 . ?
Cl1 O3 O6 49.9(12) . . ?
Cl1 O3 O4 55.8(7) . 3_765 ?
O6 O3 O4 76.2(10) . 3_765 ?
O5 O4 Cl1 52(2) 3_765 . ?
O5 O4 O3 88(5) 3_765 3_765 ?
Cl1 O4 O3 52.3(10) . 3_765 ?
O5 O5 Cl1 64(4) 3_765 . ?
O5 O5 O4 120(9) 3_765 3_765 ?
Cl1 O5 O4 66.0(17) . 3_765 ?
Cl1 O6 O3 55.4(12) . . ?
Cl1 O6 O3 55.4(12) . 3_765 ?
O3 O6 O3 111(2) . 3_765 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 990600'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H52 Cd5 Cl10 N16 S16'
_chemical_formula_sum            'C58 H52 Cd5 Cl10 N16 S16'
_chemical_formula_weight         2402.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   16.796(4)
_cell_length_b                   9.9569(12)
_cell_length_c                   25.493(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.108(9)
_cell_angle_gamma                90.00
_cell_volume                     4152.3(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8046
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      26.00

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark orange'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2356
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6074
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42521
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8046
_reflns_number_gt                6326
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/1sq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0360P)²+9.0413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8046
_refine_ls_number_parameters     476
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0837
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd3 Cd -0.019151(19) 0.64305(3) -0.054122(13) 0.03615(9) Uani 1 1 d . . .
Cd2 Cd 0.0000 1.0000 0.0000 0.04168(13) Uani 1 2 d S . .
Cd1 Cd 0.065376(19) 0.71754(3) 0.106904(13) 0.03596(9) Uani 1 1 d . . .
S1 S 0.67633(7) 0.36442(12) 0.16556(5) 0.0437(3) Uani 1 1 d . . .
S2 S 0.60604(8) 0.60904(13) 0.10957(6) 0.0514(3) Uani 1 1 d . . .
S3 S 0.52718(7) 0.35107(13) 0.22798(5) 0.0432(3) Uani 1 1 d . . .
S4 S 0.45800(8) 0.59947(13) 0.17231(5) 0.0492(3) Uani 1 1 d . . .
S5 S 0.40470(7) 0.23102(13) 0.09732(5) 0.0490(3) Uani 1 1 d . . .
S6 S 0.47084(8) -0.03652(15) 0.13519(6) 0.0578(4) Uani 1 1 d . . .
S7 S 0.54495(9) 0.25502(15) 0.02644(6) 0.0590(4) Uani 1 1 d . . .
S8 S 0.60979(8) -0.00886(15) 0.06750(5) 0.0523(3) Uani 1 1 d . . .
C10 C 0.7910(3) 0.3420(6) 0.1039(2) 0.0608(14) Uani 1 1 d . . .
H10A H 0.8002 0.2669 0.1281 0.091 Uiso 1 1 calc R . .
H10B H 0.8389 0.3976 0.1103 0.091 Uiso 1 1 calc R . .
H10C H 0.7794 0.3101 0.0674 0.091 Uiso 1 1 calc R . .
C9 C 0.7149(4) 0.6071(6) 0.0432(2) 0.0694(17) Uani 1 1 d . . .
H9A H 0.6807 0.6842 0.0327 0.104 Uiso 1 1 calc R . .
H9B H 0.7105 0.5481 0.0129 0.104 Uiso 1 1 calc R . .
H9C H 0.7707 0.6354 0.0554 0.104 Uiso 1 1 calc R . .
C2 C 0.7195(3) 0.4227(5) 0.11307(19) 0.0425(11) Uani 1 1 d . . .
C1 C 0.6880(3) 0.5339(5) 0.08802(19) 0.0451(11) Uani 1 1 d . . .
C3 C 0.5971(2) 0.4832(4) 0.15557(17) 0.0368(10) Uani 1 1 d . . .
C4 C 0.5370(3) 0.4781(5) 0.18203(18) 0.0390(10) Uani 1 1 d . . .
C6 C 0.4266(3) 0.3913(5) 0.22899(18) 0.0402(10) Uani 1 1 d . . .
H6 H 0.3961 0.3363 0.2465 0.048 Uiso 1 1 calc R . .
C5 C 0.3940(3) 0.5037(5) 0.20381(17) 0.0400(10) Uani 1 1 d . . .
C7 C 0.3108(3) 0.5572(5) 0.19760(17) 0.0383(10) Uani 1 1 d . . .
C8 C 0.2582(3) 0.6105(5) 0.15304(18) 0.0449(11) Uani 1 1 d . . .
H8 H 0.2691 0.6193 0.1190 0.054 Uiso 1 1 calc R . .
C11 C 0.2882(3) 0.5198(5) 0.29288(16) 0.0419(11) Uani 1 1 d . . .
H11A H 0.2685 0.5842 0.3156 0.050 Uiso 1 1 calc R . .
H11B H 0.3470 0.5124 0.3055 0.050 Uiso 1 1 calc R . .
C12 C 0.2492(3) 0.3853(5) 0.29690(16) 0.0371(10) Uani 1 1 d . . .
C13 C 0.2027(3) 0.3590(5) 0.33451(18) 0.0456(11) Uani 1 1 d . . .
H13 H 0.1956 0.4244 0.3590 0.055 Uiso 1 1 calc R . .
C14 C 0.1675(3) 0.2341(5) 0.33472(19) 0.0480(12) Uani 1 1 d . . .
H14 H 0.1372 0.2131 0.3599 0.058 Uiso 1 1 calc R . .
C15 C 0.1780(3) 0.1406(5) 0.29684(19) 0.0442(11) Uani 1 1 d . . .
H15 H 0.1539 0.0562 0.2957 0.053 Uiso 1 1 calc R . .
C16 C 0.2247(3) 0.1741(4) 0.26070(17) 0.0366(10) Uani 1 1 d . . .
C27 C 0.2387(3) 0.0824(5) 0.21660(17) 0.0420(11) Uani 1 1 d . . .
H27A H 0.2955 0.0548 0.2241 0.050 Uiso 1 1 calc R . .
H27B H 0.2051 0.0026 0.2151 0.050 Uiso 1 1 calc R . .
C24 C 0.2127(3) 0.2590(5) 0.09076(18) 0.0404(10) Uani 1 1 d . . .
H24 H 0.2257 0.2960 0.0603 0.049 Uiso 1 1 calc R . .
C23 C 0.2628(2) 0.1788(4) 0.12799(17) 0.0349(9) Uani 1 1 d . . .
C21 C 0.3438(3) 0.1266(5) 0.12774(17) 0.0376(10) Uani 1 1 d . . .
C22 C 0.3745(3) 0.0051(5) 0.14442(19) 0.0474(12) Uani 1 1 d . . .
H22 H 0.3449 -0.0550 0.1605 0.057 Uiso 1 1 calc R . .
C20 C 0.4780(3) 0.1055(5) 0.09490(18) 0.0434(11) Uani 1 1 d . . .
C19 C 0.5356(3) 0.1168(5) 0.06690(18) 0.0440(11) Uani 1 1 d . . .
C17 C 0.6289(3) 0.1898(6) 0.0037(2) 0.0567(14) Uani 1 1 d . . .
C18 C 0.6584(3) 0.0702(6) 0.0224(2) 0.0540(13) Uani 1 1 d . . .
C25 C 0.6617(5) 0.2782(7) -0.0347(2) 0.085(2) Uani 1 1 d . . .
H25A H 0.6292 0.3583 -0.0419 0.128 Uiso 1 1 calc R . .
H25B H 0.6593 0.2307 -0.0678 0.128 Uiso 1 1 calc R . .
H25C H 0.7173 0.3019 -0.0188 0.128 Uiso 1 1 calc R . .
C26 C 0.7313(4) -0.0011(7) 0.0102(2) 0.0725(17) Uani 1 1 d . . .
H26A H 0.7393 -0.0851 0.0292 0.109 Uiso 1 1 calc R . .
H26B H 0.7791 0.0538 0.0215 0.109 Uiso 1 1 calc R . .
H26C H 0.7219 -0.0174 -0.0278 0.109 Uiso 1 1 calc R . .
C28 C 0.0088(4) 0.9527(9) 0.1920(3) 0.088(2) Uani 1 1 d . . .
C29 C -0.0230(5) 1.0841(8) 0.2116(3) 0.107(3) Uani 1 1 d . . .
H29A H -0.0738 1.1085 0.1877 0.160 Uiso 1 1 calc R . .
H29B H 0.0164 1.1542 0.2120 0.160 Uiso 1 1 calc R . .
H29C H -0.0313 1.0716 0.2473 0.160 Uiso 1 1 calc R . .
Cl4 Cl -0.06860(6) 0.78250(10) 0.02978(4) 0.0362(2) Uani 1 1 d . . .
Cl2 Cl 0.10434(6) 0.56148(10) 0.02579(4) 0.0343(2) Uani 1 1 d . . .
Cl3 Cl 0.13200(7) 0.92100(11) 0.07621(5) 0.0432(3) Uani 1 1 d . . .
Cl5 Cl -0.05498(7) 1.14381(11) 0.06977(5) 0.0425(3) Uani 1 1 d . . .
Cl1 Cl -0.00874(7) 0.50929(11) 0.13054(5) 0.0429(3) Uani 1 1 d . . .
N3 N 0.1888(2) 0.6476(4) 0.16646(15) 0.0420(9) Uani 1 1 d . . .
N2 N 0.1940(2) 0.6217(4) 0.21803(15) 0.0427(9) Uani 1 1 d . . .
N1 N 0.2686(2) 0.5673(4) 0.23703(14) 0.0360(8) Uani 1 1 d . . .
N4 N 0.2609(2) 0.2944(4) 0.26119(14) 0.0374(8) Uani 1 1 d . . .
N5 N 0.2177(2) 0.1529(4) 0.16485(14) 0.0357(8) Uani 1 1 d . . .
N6 N 0.1437(2) 0.2103(4) 0.15127(15) 0.0402(9) Uani 1 1 d . . .
N7 N 0.1414(2) 0.2749(4) 0.10598(15) 0.0390(8) Uani 1 1 d . . .
N8 N 0.0283(3) 0.8557(6) 0.1739(2) 0.0777(16) 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
Cd3 N7 2.323(4) 3_565 ?
Cd3 Cl5 2.5374(12) 3_575 ?
Cd3 Cl1 2.5942(11) 3_565 ?
Cd3 Cl2 2.6805(11) 3_565 ?
Cd3 Cl2 2.6824(11) . ?
Cd3 Cl4 2.8281(11) . ?
Cd2 Cl5 2.6099(11) 3_575 ?
Cd2 Cl5 2.6099(11) . ?
Cd2 Cl4 2.6439(11) 3_575 ?
Cd2 Cl4 2.6439(11) . ?
Cd2 Cl3 2.7121(12) . ?
Cd2 Cl3 2.7121(12) 3_575 ?
Cd1 N3 2.379(4) . ?
Cd1 N8 2.384(5) . ?
Cd1 Cl3 2.5230(12) . ?
Cd1 Cl1 2.5598(12) . ?
Cd1 Cl4 2.7094(12) . ?
Cd1 Cl2 2.7807(11) . ?
S1 C3 1.755(4) . ?
S1 C2 1.759(5) . ?
S2 C3 1.746(4) . ?
S2 C1 1.760(5) . ?
S3 C6 1.742(4) . ?
S3 C4 1.757(5) . ?
S4 C5 1.760(4) . ?
S4 C4 1.770(5) . ?
S5 C21 1.757(4) . ?
S5 C20 1.765(5) . ?
S6 C22 1.737(5) . ?
S6 C20 1.768(5) . ?
S7 C19 1.748(5) . ?
S7 C17 1.767(6) . ?
S8 C18 1.741(5) . ?
S8 C19 1.763(5) . ?
C10 C2 1.506(6) . ?
C9 C1 1.508(7) . ?
C2 C1 1.327(7) . ?
C3 C4 1.337(6) . ?
C6 C5 1.344(6) . ?
C5 C7 1.471(6) . ?
C7 N1 1.359(5) . ?
C7 C8 1.378(6) . ?
C8 N3 1.339(6) . ?
C11 N1 1.465(5) . ?
C11 C12 1.504(6) . ?
C12 N4 1.330(6) . ?
C12 C13 1.392(6) . ?
C13 C14 1.377(7) . ?
C14 C15 1.381(7) . ?
C15 C16 1.380(6) . ?
C16 N4 1.341(6) . ?
C16 C27 1.508(6) . ?
C27 N5 1.465(5) . ?
C24 N7 1.350(6) . ?
C24 C23 1.373(6) . ?
C23 N5 1.359(5) . ?
C23 C21 1.457(6) . ?
C21 C22 1.346(6) . ?
C20 C19 1.331(6) . ?
C17 C18 1.336(8) . ?
C17 C25 1.509(7) . ?
C18 C26 1.508(8) . ?
C28 N8 1.149(9) . ?
C28 C29 1.538(11) . ?
Cl2 Cd3 2.6805(11) 3_565 ?
Cl5 Cd3 2.5374(12) 3_575 ?
Cl1 Cd3 2.5942(11) 3_565 ?
N3 N2 1.323(5) . ?
N2 N1 1.350(5) . ?
N5 N6 1.341(5) . ?
N6 N7 1.315(5) . ?
N7 Cd3 2.323(4) 3_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Cd3 Cl5 91.04(10) 3_565 3_575 ?
N7 Cd3 Cl1 93.72(10) 3_565 3_565 ?
Cl5 Cd3 Cl1 101.09(4) 3_575 3_565 ?
N7 Cd3 Cl2 87.92(9) 3_565 3_565 ?
Cl5 Cd3 Cl2 171.40(3) 3_575 3_565 ?
Cl1 Cd3 Cl2 87.50(3) 3_565 3_565 ?
N7 Cd3 Cl2 165.90(9) 3_565 . ?
Cl5 Cd3 Cl2 92.88(4) 3_575 . ?
Cl1 Cd3 Cl2 98.81(4) 3_565 . ?
Cl2 Cd3 Cl2 86.18(3) 3_565 . ?
N7 Cd3 Cl4 83.38(9) 3_565 . ?
Cl5 Cd3 Cl4 86.96(3) 3_575 . ?
Cl1 Cd3 Cl4 171.52(3) 3_565 . ?
Cl2 Cd3 Cl4 84.43(3) 3_565 . ?
Cl2 Cd3 Cl4 83.30(3) . . ?
Cl5 Cd2 Cl5 180.00(5) 3_575 . ?
Cl5 Cd2 Cl4 90.52(3) 3_575 3_575 ?
Cl5 Cd2 Cl4 89.48(3) . 3_575 ?
Cl5 Cd2 Cl4 89.48(3) 3_575 . ?
Cl5 Cd2 Cl4 90.52(3) . . ?
Cl4 Cd2 Cl4 180.00(4) 3_575 . ?
Cl5 Cd2 Cl3 88.34(4) 3_575 . ?
Cl5 Cd2 Cl3 91.66(4) . . ?
Cl4 Cd2 Cl3 96.00(3) 3_575 . ?
Cl4 Cd2 Cl3 84.00(3) . . ?
Cl5 Cd2 Cl3 91.66(4) 3_575 3_575 ?
Cl5 Cd2 Cl3 88.34(4) . 3_575 ?
Cl4 Cd2 Cl3 84.00(3) 3_575 3_575 ?
Cl4 Cd2 Cl3 96.00(3) . 3_575 ?
Cl3 Cd2 Cl3 180.0 . 3_575 ?
N3 Cd1 N8 92.46(17) . . ?
N3 Cd1 Cl3 92.84(9) . . ?
N8 Cd1 Cl3 88.01(14) . . ?
N3 Cd1 Cl1 90.71(10) . . ?
N8 Cd1 Cl1 94.51(14) . . ?
Cl3 Cd1 Cl1 175.56(4) . . ?
N3 Cd1 Cl4 173.25(10) . . ?
N8 Cd1 Cl4 94.22(15) . . ?
Cl3 Cd1 Cl4 86.39(4) . . ?
Cl1 Cd1 Cl4 89.77(4) . . ?
N3 Cd1 Cl2 89.59(10) . . ?
N8 Cd1 Cl2 177.85(15) . . ?
Cl3 Cd1 Cl2 91.28(4) . . ?
Cl1 Cd1 Cl2 86.07(3) . . ?
Cl4 Cd1 Cl2 83.72(3) . . ?
C3 S1 C2 95.6(2) . . ?
C3 S2 C1 95.6(2) . . ?
C6 S3 C4 94.7(2) . . ?
C5 S4 C4 94.7(2) . . ?
C21 S5 C20 94.4(2) . . ?
C22 S6 C20 94.4(2) . . ?
C19 S7 C17 95.1(3) . . ?
C18 S8 C19 96.3(3) . . ?
C1 C2 C10 128.0(5) . . ?
C1 C2 S1 116.9(3) . . ?
C10 C2 S1 115.0(4) . . ?
C2 C1 C9 127.7(5) . . ?
C2 C1 S2 117.4(4) . . ?
C9 C1 S2 114.9(4) . . ?
C4 C3 S2 123.8(3) . . ?
C4 C3 S1 122.4(3) . . ?
S2 C3 S1 113.8(2) . . ?
C3 C4 S3 124.0(3) . . ?
C3 C4 S4 122.1(3) . . ?
S3 C4 S4 113.9(2) . . ?
C5 C6 S3 118.4(3) . . ?
C6 C5 C7 128.8(4) . . ?
C6 C5 S4 116.4(3) . . ?
C7 C5 S4 114.8(3) . . ?
N1 C7 C8 103.7(4) . . ?
N1 C7 C5 126.2(4) . . ?
C8 C7 C5 130.1(4) . . ?
N3 C8 C7 109.1(4) . . ?
N1 C11 C12 110.4(3) . . ?
N4 C12 C13 122.4(4) . . ?
N4 C12 C11 115.2(4) . . ?
C13 C12 C11 122.4(4) . . ?
C14 C13 C12 118.8(5) . . ?
C13 C14 C15 118.9(4) . . ?
C16 C15 C14 119.0(4) . . ?
N4 C16 C15 122.3(4) . . ?
N4 C16 C27 113.6(4) . . ?
C15 C16 C27 124.0(4) . . ?
N5 C27 C16 109.6(4) . . ?
N7 C24 C23 108.4(4) . . ?
N5 C23 C24 103.7(4) . . ?
N5 C23 C21 127.1(4) . . ?
C24 C23 C21 129.1(4) . . ?
C22 C21 C23 127.6(4) . . ?
C22 C21 S5 116.8(3) . . ?
C23 C21 S5 115.4(3) . . ?
C21 C22 S6 118.3(4) . . ?
C19 C20 S5 123.8(4) . . ?
C19 C20 S6 122.2(4) . . ?
S5 C20 S6 114.0(3) . . ?
C20 C19 S7 123.8(4) . . ?
C20 C19 S8 122.2(4) . . ?
S7 C19 S8 114.0(3) . . ?
C18 C17 C25 126.3(6) . . ?
C18 C17 S7 117.9(4) . . ?
C25 C17 S7 115.7(5) . . ?
C17 C18 C26 126.7(5) . . ?
C17 C18 S8 116.6(4) . . ?
C26 C18 S8 116.6(4) . . ?
N8 C28 C29 175.0(8) . . ?
Cd2 Cl4 Cd1 93.42(3) . . ?
Cd2 Cl4 Cd3 87.89(3) . . ?
Cd1 Cl4 Cd3 95.37(3) . . ?
Cd3 Cl2 Cd3 93.82(3) 3_565 . ?
Cd3 Cl2 Cd1 89.66(3) 3_565 . ?
Cd3 Cl2 Cd1 97.11(3) . . ?
Cd1 Cl3 Cd2 96.14(4) . . ?
Cd3 Cl5 Cd2 95.14(4) 3_575 . ?
Cd1 Cl1 Cd3 96.69(4) . 3_565 ?
N2 N3 C8 109.6(4) . . ?
N2 N3 Cd1 122.9(3) . . ?
C8 N3 Cd1 126.9(3) . . ?
N3 N2 N1 106.3(3) . . ?
N2 N1 C7 111.2(3) . . ?
N2 N1 C11 117.6(3) . . ?
C7 N1 C11 130.9(4) . . ?
C12 N4 C16 118.5(4) . . ?
N6 N5 C23 111.8(3) . . ?
N6 N5 C27 117.2(3) . . ?
C23 N5 C27 130.9(4) . . ?
N7 N6 N5 106.0(3) . . ?
N6 N7 C24 110.1(4) . . ?
N6 N7 Cd3 121.2(3) . 3_565 ?
C24 N7 Cd3 127.2(3) . 3_565 ?
C28 N8 Cd1 156.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 990601'
