# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1058262'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H18 Cd Cl0 N6 O0 S4'
_chemical_formula_weight         462.99

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   5.9229(12)
_cell_length_b                   8.1307(16)
_cell_length_c                   10.051(2)
_cell_angle_alpha                107.23(3)
_cell_angle_beta                 97.19(3)
_cell_angle_gamma                93.76(3)
_cell_volume                     455.97(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             232
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4145
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.1310
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         27.42
_reflns_number_total             2039
_reflns_number_gt                1670
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1135P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2039
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.2145
_refine_ls_wR_factor_gt          0.1448
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Cd1 Cd 0.5000 1.0000 0.0000 0.0264(3) Uani 1 2 d S . .
S1 S 0.7156(3) 0.7011(2) -0.0588(2) 0.0371(5) Uani 1 1 d . . .
S2 S 0.6776(4) 1.0583(3) 0.2740(2) 0.0457(6) Uani 1 1 d . . .
N1 N 1.1721(12) 0.8426(10) 0.0135(8) 0.0371(16) Uani 1 1 d . . .
N2 N 0.3136(19) 1.1685(12) 0.4184(10) 0.061(3) Uani 1 1 d . . .
N3 N 0.0508(12) 0.3527(8) 0.6146(7) 0.0297(14) Uani 1 1 d . . .
C1 C 0.9832(14) 0.7843(10) -0.0186(8) 0.0310(16) Uani 1 1 d . . .
C2 C 0.4550(16) 1.1192(9) 0.3574(9) 0.0344(18) Uani 1 1 d . . .
C3 C -0.0692(15) 0.4731(10) 0.5515(8) 0.0345(18) Uani 1 1 d . . .
H3A H -0.0918 0.5754 0.6259 0.041 Uiso 1 1 calc R . .
H3B H -0.2185 0.4170 0.5019 0.041 Uiso 1 1 calc R . .
C4 C 0.2644(15) 0.4415(12) 0.7163(10) 0.041(2) Uani 1 1 d . . .
H4A H 0.3363 0.3590 0.7539 0.061 Uiso 1 1 calc R . .
H4B H 0.2241 0.5331 0.7918 0.061 Uiso 1 1 calc R . .
H4C H 0.3685 0.4888 0.6677 0.061 Uiso 1 1 calc R . .
C5 C -0.1046(17) 0.2636(12) 0.6802(10) 0.042(2) Uani 1 1 d . . .
H5A H -0.2380 0.2088 0.6130 0.063 Uiso 1 1 calc R . .
H5B H -0.1493 0.3461 0.7600 0.063 Uiso 1 1 calc R . .
H5C H -0.0279 0.1775 0.7106 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0198(4) 0.0326(4) 0.0259(4) 0.0081(3) 0.0030(3) 0.0022(3)
S1 0.0272(10) 0.0293(9) 0.0463(13) 0.0025(8) -0.0024(8) 0.0012(8)
S2 0.0411(12) 0.0656(15) 0.0295(11) 0.0105(10) 0.0027(9) 0.0242(12)
N1 0.028(3) 0.045(4) 0.048(4) 0.020(3) 0.023(3) 0.007(3)
N2 0.080(7) 0.049(5) 0.051(5) 0.008(4) 0.000(5) 0.028(5)
N3 0.039(4) 0.026(3) 0.023(3) 0.007(2) -0.004(3) 0.006(3)
C1 0.032(4) 0.028(3) 0.031(4) 0.010(3) -0.002(3) 0.003(3)
C2 0.046(5) 0.023(3) 0.030(4) 0.004(3) -0.003(4) 0.009(4)
C3 0.042(4) 0.037(4) 0.027(4) 0.012(3) 0.003(3) 0.019(4)
C4 0.035(4) 0.046(4) 0.037(5) 0.014(4) -0.009(3) -0.006(4)
C5 0.049(5) 0.042(4) 0.041(5) 0.024(4) 0.004(4) 0.000(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.296(7) 2_775 ?
Cd1 N1 2.296(7) 1_455 ?
Cd1 S2 2.711(2) 2_675 ?
Cd1 S2 2.711(2) . ?
Cd1 S1 2.763(2) 2_675 ?
Cd1 S1 2.763(2) . ?
S1 C1 1.634(8) . ?
S2 C2 1.675(10) . ?
N1 C1 1.153(11) . ?
N1 Cd1 2.296(7) 1_655 ?
N2 C2 1.124(14) . ?
N3 C5 1.468(12) . ?
N3 C3 1.487(9) . ?
N3 C4 1.512(10) . ?
C3 C3 1.540(17) 2_566 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 180.0 2_775 1_455 ?
N1 Cd1 S2 94.2(2) 2_775 2_675 ?
N1 Cd1 S2 85.8(2) 1_455 2_675 ?
N1 Cd1 S2 85.8(2) 2_775 . ?
N1 Cd1 S2 94.2(2) 1_455 . ?
S2 Cd1 S2 180.00(12) 2_675 . ?
N1 Cd1 S1 89.49(18) 2_775 2_675 ?
N1 Cd1 S1 90.51(18) 1_455 2_675 ?
S2 Cd1 S1 86.97(7) 2_675 2_675 ?
S2 Cd1 S1 93.03(7) . 2_675 ?
N1 Cd1 S1 90.51(18) 2_775 . ?
N1 Cd1 S1 89.49(18) 1_455 . ?
S2 Cd1 S1 93.03(7) 2_675 . ?
S2 Cd1 S1 86.97(7) . . ?
S1 Cd1 S1 180.0 2_675 . ?
C1 S1 Cd1 100.2(3) . . ?
C2 S2 Cd1 102.5(3) . . ?
C1 N1 Cd1 156.0(7) . 1_655 ?
C5 N3 C3 111.2(7) . . ?
C5 N3 C4 111.6(7) . . ?
C3 N3 C4 112.4(6) . . ?
N1 C1 S1 178.1(8) . . ?
N2 C2 S2 175.9(9) . . ?
N3 C3 C3 111.2(8) . 2_566 ?
N3 C3 H3A 109.4 . . ?
C3 C3 H3A 109.4 2_566 . ?
N3 C3 H3B 109.4 . . ?
C3 C3 H3B 109.4 2_566 . ?
H3A C3 H3B 108.0 . . ?
N3 C4 H4A 109.5 . . ?
N3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.114
_refine_diff_density_min         -2.074
_refine_diff_density_rms         0.347
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1058263'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H22 Cd2 N8 O0 S6'
_chemical_formula_weight         719.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   5.9186(12)
_cell_length_b                   10.709(2)
_cell_length_c                   10.863(2)
_cell_angle_alpha                73.96(3)
_cell_angle_beta                 76.92(3)
_cell_angle_gamma                81.30(3)
_cell_volume                     641.6(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             354
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6297
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.47
_reflns_number_total             2912
_reflns_number_gt                2699
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2912
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1058
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.147
_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
Cd1 Cd 0.89543(3) 0.31375(2) 0.09800(2) 0.03402(13) Uani 1 1 d . . .
S1 S 0.93476(14) 0.48768(8) -0.15855(8) 0.03267(19) Uani 1 1 d . . .
S2 S 0.73780(14) 0.14134(8) 0.00628(9) 0.0390(2) Uani 1 1 d . . .
S3 S 0.8426(2) 0.15545(10) 0.33339(10) 0.0521(3) Uani 1 1 d . . .
N1 N 0.4592(5) 0.5728(3) -0.1517(3) 0.0377(6) Uani 1 1 d . . .
N2 N 0.2687(5) 0.2359(3) 0.0299(4) 0.0477(7) Uani 1 1 d . . .
N3 N 1.2174(7) 0.2003(4) 0.4265(4) 0.0581(9) Uani 1 1 d . . .
N4 N 0.4442(5) 0.2014(3) 0.6305(3) 0.0336(5) Uani 1 1 d . . .
H00 H 0.436(7) 0.195(4) 0.564(4) 0.039(10) Uiso 1 1 d . . .
C1 C 0.6546(5) 0.5390(3) -0.1543(3) 0.0306(6) Uani 1 1 d . . .
C2 C 0.4619(5) 0.1986(3) 0.0208(3) 0.0315(6) Uani 1 1 d . . .
C3 C 1.0665(6) 0.1832(3) 0.3855(3) 0.0381(7) Uani 1 1 d . . .
C4 C 0.2105(6) 0.2005(4) 0.7186(4) 0.0476(8) Uani 1 1 d . . .
H4A H 0.1479 0.1194 0.7307 0.071 Uiso 1 1 calc R . .
H4B H 0.1077 0.2714 0.6801 0.071 Uiso 1 1 calc R . .
H4C H 0.2258 0.2102 0.8015 0.071 Uiso 1 1 calc R . .
C5 C 0.5997(7) 0.0862(3) 0.6833(3) 0.0442(7) Uani 1 1 d . . .
H5A H 0.5246 0.0082 0.6995 0.066 Uiso 1 1 calc R . .
H5B H 0.6321 0.0938 0.7635 0.066 Uiso 1 1 calc R . .
H5C H 0.7428 0.0821 0.6212 0.066 Uiso 1 1 calc R . .
C6 C 0.5559(6) 0.3250(3) 0.6040(3) 0.0413(7) Uani 1 1 d . . .
H6A H 0.7165 0.3131 0.5598 0.050 Uiso 1 1 calc R . .
H6B H 0.5566 0.3437 0.6863 0.050 Uiso 1 1 calc R . .
C7 C 0.4298(7) 0.4413(3) 0.5200(4) 0.0451(8) Uani 1 1 d . . .
H7A H 0.4094 0.4190 0.4428 0.054 Uiso 1 1 calc R . .
H7B H 0.2768 0.4624 0.5691 0.054 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.02331(17) 0.03902(18) 0.04047(17) -0.01055(11) -0.00984(11) 0.00132(11)
S1 0.0236(4) 0.0340(4) 0.0398(4) -0.0118(3) -0.0049(3) 0.0023(3)
S2 0.0251(4) 0.0448(4) 0.0515(5) -0.0219(4) -0.0081(3) 0.0022(3)
S3 0.0531(6) 0.0566(5) 0.0475(5) 0.0047(4) -0.0235(4) -0.0201(5)
N1 0.0264(13) 0.0436(14) 0.0411(13) -0.0093(11) -0.0075(10) 0.0019(11)
N2 0.0299(14) 0.0532(17) 0.070(2) -0.0303(15) -0.0159(14) 0.0043(13)
N3 0.063(2) 0.066(2) 0.0543(18) -0.0106(16) -0.0324(16) -0.0103(18)
N4 0.0397(14) 0.0334(12) 0.0299(12) -0.0111(10) -0.0085(11) -0.0015(11)
C1 0.0318(15) 0.0307(13) 0.0293(12) -0.0078(10) -0.0058(11) -0.0020(12)
C2 0.0285(15) 0.0334(13) 0.0356(14) -0.0121(11) -0.0078(11) -0.0036(12)
C3 0.0441(18) 0.0362(16) 0.0345(14) -0.0074(12) -0.0131(14) 0.0004(14)
C4 0.0397(18) 0.0495(19) 0.0496(18) -0.0154(15) 0.0013(15) -0.0018(15)
C5 0.0495(19) 0.0362(15) 0.0445(16) -0.0073(13) -0.0135(15) 0.0048(14)
C6 0.0468(19) 0.0344(15) 0.0453(16) -0.0096(13) -0.0133(14) -0.0058(14)
C7 0.052(2) 0.0332(16) 0.0495(18) -0.0066(14) -0.0128(16) -0.0037(15)

_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 N2 2.273(3) 1_655 ?
Cd1 N1 2.300(3) 2_665 ?
Cd1 S3 2.6292(13) . ?
Cd1 S2 2.6889(11) . ?
Cd1 S1 2.7719(11) 2_765 ?
Cd1 S1 2.8739(13) . ?
S1 C1 1.661(3) . ?
S1 Cd1 2.7719(11) 2_765 ?
S2 C2 1.643(3) . ?
S3 C3 1.648(4) . ?
N1 C1 1.155(4) . ?
N1 Cd1 2.300(3) 2_665 ?
N2 C2 1.145(4) . ?
N2 Cd1 2.273(3) 1_455 ?
N3 C3 1.142(5) . ?
N4 C5 1.484(4) . ?
N4 C4 1.493(4) . ?
N4 C6 1.497(4) . ?
N4 H00 0.76(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.529(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C7 1.520(7) 2_666 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?

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
N2 Cd1 N1 170.17(11) 1_655 2_665 ?
N2 Cd1 S3 95.83(10) 1_655 . ?
N1 Cd1 S3 90.97(8) 2_665 . ?
N2 Cd1 S2 90.18(9) 1_655 . ?
N1 Cd1 S2 96.82(8) 2_665 . ?
S3 Cd1 S2 90.87(4) . . ?
N2 Cd1 S1 88.92(9) 1_655 2_765 ?
N1 Cd1 S1 83.22(8) 2_665 2_765 ?
S3 Cd1 S1 96.82(4) . 2_765 ?
S2 Cd1 S1 172.31(3) . 2_765 ?
N2 Cd1 S1 86.09(10) 1_655 . ?
N1 Cd1 S1 87.23(8) 2_665 . ?
S3 Cd1 S1 177.88(3) . . ?
S2 Cd1 S1 88.24(3) . . ?
S1 Cd1 S1 84.08(4) 2_765 . ?
C1 S1 Cd1 102.89(11) . 2_765 ?
C1 S1 Cd1 98.55(11) . . ?
Cd1 S1 Cd1 95.92(4) 2_765 . ?
C2 S2 Cd1 98.97(11) . . ?
C3 S3 Cd1 101.27(12) . . ?
C1 N1 Cd1 157.7(3) . 2_665 ?
C2 N2 Cd1 165.5(3) . 1_455 ?
C5 N4 C4 110.2(3) . . ?
C5 N4 C6 110.9(3) . . ?
C4 N4 C6 113.6(3) . . ?
C5 N4 H00 105(3) . . ?
C4 N4 H00 111(3) . . ?
C6 N4 H00 105(3) . . ?
N1 C1 S1 178.9(3) . . ?
N2 C2 S2 178.3(3) . . ?
N3 C3 S3 177.3(4) . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 C7 112.4(3) . . ?
N4 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
N4 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C7 C7 C6 109.9(4) 2_666 . ?
C7 C7 H7A 109.7 2_666 . ?
C6 C7 H7A 109.7 . . ?
C7 C7 H7B 109.7 2_666 . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.196
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1058264'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H26 Cd2 Cl0 N8 O0 S6'
_chemical_formula_weight         747.63

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   10.5331(6)
_cell_length_b                   11.2159(6)
_cell_length_c                   15.0643(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.416(3)
_cell_angle_gamma                90.00
_cell_volume                     1394.41(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_T_max  0.787
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7690
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2457
_reflns_number_gt                2274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0500P)²+0.5033P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2457
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0833
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.198
_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
Cd1 Cd 0.35102(2) -0.023491(19) -0.385698(16) 0.03035(13) Uani 1 1 d . . .
S1 S 0.26970(9) -0.16596(7) -0.55789(7) 0.0379(2) Uani 1 1 d . . .
S2 S 0.62157(10) -0.13513(7) -0.20751(7) 0.0414(2) Uani 1 1 d . . .
S3 S 0.19663(11) -0.17133(9) -0.34047(8) 0.0499(2) Uani 1 1 d . . .
N1 N 0.4825(3) -0.0880(3) -0.5982(2) 0.0421(6) Uani 1 1 d . . .
N2 N 0.5865(4) -0.3786(2) -0.2597(2) 0.0400(6) Uani 1 1 d . . .
N3 N -0.1239(3) -0.0914(3) -0.4958(2) 0.0450(6) Uani 1 1 d . . .
N4 N -0.2834(3) -0.4459(2) -0.38475(19) 0.0278(5) Uani 1 1 d . . .
H4 H -0.2973 -0.4514 -0.3310 0.080 Uiso 1 1 calc R . .
C1 C 0.3932(3) -0.1178(2) -0.5828(2) 0.0296(6) Uani 1 1 d . . .
C2 C 0.5962(3) -0.2773(3) -0.2397(2) 0.0317(6) Uani 1 1 d . . .
C3 C 0.0081(4) -0.1233(3) -0.4334(3) 0.0363(7) Uani 1 1 d . . .
C4 C -0.4193(4) -0.5154(3) -0.4859(3) 0.0347(7) Uani 1 1 d . . .
H4A H -0.3989 -0.6001 -0.4702 0.042 Uiso 1 1 calc R . .
H4B H -0.4234 -0.4978 -0.5507 0.042 Uiso 1 1 calc R . .
C5 C -0.1206(4) -0.5033(3) -0.3349(3) 0.0387(7) Uani 1 1 d . . .
H5A H -0.0367 -0.4627 -0.2650 0.046 Uiso 1 1 calc R . .
H5B H -0.1229 -0.5857 -0.3163 0.046 Uiso 1 1 calc R . .
C6 C -0.0768(5) -0.5002(4) -0.4132(4) 0.0571(10) Uani 1 1 d . . .
H6A H 0.0268 -0.5374 -0.3768 0.086 Uiso 1 1 calc R . .
H6B H -0.0718 -0.4189 -0.4307 0.086 Uiso 1 1 calc R . .
H6C H -0.1575 -0.5422 -0.4818 0.086 Uiso 1 1 calc R . .
C7 C -0.2916(4) -0.3149(3) -0.4113(2) 0.0332(6) Uani 1 1 d . . .
H7A H -0.2892 -0.3062 -0.4743 0.040 Uiso 1 1 calc R . .
H7B H -0.3939 -0.2828 -0.4348 0.040 Uiso 1 1 calc R . .
C8 C -0.1552(4) -0.2435(3) -0.3125(3) 0.0443(7) Uani 1 1 d . . .
H8A H -0.1665 -0.1613 -0.3343 0.066 Uiso 1 1 calc R . .
H8B H -0.0536 -0.2736 -0.2898 0.066 Uiso 1 1 calc R . .
H8C H -0.1585 -0.2499 -0.2504 0.066 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.03654(18) 0.02911(19) 0.03360(18) 0.00171(7) 0.02584(14) 0.00165(7)
S1 0.0410(4) 0.0385(4) 0.0436(4) -0.0113(3) 0.0309(4) -0.0115(3)
S2 0.0428(4) 0.0311(4) 0.0366(4) -0.0040(3) 0.0179(4) 0.0030(3)
S3 0.0406(5) 0.0566(5) 0.0610(5) 0.0295(4) 0.0358(4) 0.0129(4)
N1 0.0530(16) 0.0411(15) 0.0470(15) -0.0079(12) 0.0385(14) -0.0091(12)
N2 0.0614(18) 0.0288(15) 0.0414(14) 0.0031(11) 0.0376(14) -0.0001(11)
N3 0.0402(16) 0.0439(16) 0.0522(16) 0.0101(13) 0.0294(14) 0.0056(13)
N4 0.0268(12) 0.0271(11) 0.0266(11) -0.0006(9) 0.0151(10) -0.0019(10)
C1 0.0368(15) 0.0249(13) 0.0273(13) -0.0001(11) 0.0200(12) 0.0022(11)
C2 0.0383(15) 0.0360(18) 0.0268(13) 0.0029(11) 0.0231(12) 0.0014(12)
C3 0.0428(18) 0.0321(16) 0.0443(16) 0.0087(13) 0.0323(15) 0.0016(13)
C4 0.0298(16) 0.0316(16) 0.0372(16) -0.0106(12) 0.0180(14) -0.0056(11)
C5 0.0310(17) 0.0367(15) 0.0388(18) 0.0087(13) 0.0169(15) 0.0076(13)
C6 0.050(2) 0.068(2) 0.067(3) 0.014(2) 0.043(2) 0.0189(19)
C7 0.0341(15) 0.0290(14) 0.0345(14) 0.0020(11) 0.0203(13) 0.0007(11)
C8 0.0465(18) 0.0393(18) 0.0516(18) -0.0114(15) 0.0328(16) -0.0137(14)

_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 N1 2.286(3) 3_654 ?
Cd1 N3 2.295(3) 3_554 ?
Cd1 N2 2.466(3) 2_654 ?
Cd1 S3 2.6898(9) . ?
Cd1 S1 2.6934(8) . ?
Cd1 S2 2.7181(8) . ?
S1 C1 1.652(3) . ?
S2 C2 1.640(3) . ?
S3 C3 1.654(3) . ?
N1 C1 1.150(4) . ?
N1 Cd1 2.286(3) 3_654 ?
N2 C2 1.163(4) . ?
N2 Cd1 2.466(3) 2_644 ?
N3 C3 1.149(4) . ?
N3 Cd1 2.295(3) 3_554 ?
N4 C4 1.506(4) . ?
N4 C7 1.511(4) . ?
N4 C5 1.523(4) . ?
N4 H4 0.9100 . ?
C4 C4 1.513(6) 3_444 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.510(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.505(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N3 96.19(10) 3_654 3_554 ?
N1 Cd1 N2 86.27(9) 3_654 2_654 ?
N3 Cd1 N2 83.95(10) 3_554 2_654 ?
N1 Cd1 S3 171.28(8) 3_654 . ?
N3 Cd1 S3 92.36(7) 3_554 . ?
N2 Cd1 S3 92.92(7) 2_654 . ?
N1 Cd1 S1 91.61(7) 3_654 . ?
N3 Cd1 S1 91.72(8) 3_554 . ?
N2 Cd1 S1 174.94(7) 2_654 . ?
S3 Cd1 S1 89.87(3) . . ?
N1 Cd1 S2 87.37(8) 3_654 . ?
N3 Cd1 S2 166.83(8) 3_554 . ?
N2 Cd1 S2 83.64(7) 2_654 . ?
S3 Cd1 S2 83.90(3) . . ?
S1 Cd1 S2 100.87(3) . . ?
C1 S1 Cd1 101.57(10) . . ?
C2 S2 Cd1 106.12(10) . . ?
C3 S3 Cd1 100.48(10) . . ?
C1 N1 Cd1 163.4(3) . 3_654 ?
C2 N2 Cd1 118.8(2) . 2_644 ?
C3 N3 Cd1 163.3(3) . 3_554 ?
C4 N4 C7 111.9(2) . . ?
C4 N4 C5 110.5(2) . . ?
C7 N4 C5 113.8(2) . . ?
C4 N4 H4 106.7 . . ?
C7 N4 H4 106.7 . . ?
C5 N4 H4 106.7 . . ?
N1 C1 S1 177.5(3) . . ?
N2 C2 S2 176.6(3) . . ?
N3 C3 S3 177.8(3) . . ?
N4 C4 C4 111.2(3) . 3_444 ?
N4 C4 H4A 109.4 . . ?
C4 C4 H4A 109.4 3_444 . ?
N4 C4 H4B 109.4 . . ?
C4 C4 H4B 109.4 3_444 . ?
H4A C4 H4B 108.0 . . ?
C6 C5 N4 113.7(3) . . ?
C6 C5 H5A 108.8 . . ?
N4 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
N4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N4 113.2(2) . . ?
C8 C7 H7A 108.9 . . ?
N4 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
N4 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.500
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.213
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1058265'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H12 Cd Cl0 N4 O2 S2'
_chemical_formula_weight         396.76

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   11.1025(7)
_cell_length_b                   10.9745(5)
_cell_length_c                   12.9968(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.624(4)
_cell_angle_gamma                90.00
_cell_volume                     1539.03(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    1.692
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  0.859
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            8461
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2713
_reflns_number_gt                2273
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0202P)²+1.0174P] 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         2713
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0547
_refine_ls_wR_factor_gt          0.0502
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
Cd1 Cd 0.728405(17) -0.494552(17) 0.425748(16) 0.04766(8) Uani 1 1 d . . .
S1 S 0.65817(8) -0.30161(7) 0.51266(8) 0.0753(3) Uani 1 1 d . . .
S2 S 0.84021(7) -0.66194(8) 0.55940(6) 0.0623(2) Uani 1 1 d . . .
O1 O 0.75130(19) -0.61546(17) 0.27468(16) 0.0592(5) Uani 1 1 d . . .
O2 O 0.64487(18) -0.44709(19) 0.24714(16) 0.0588(5) Uani 1 1 d . . .
N1 N 0.4517(2) -0.3924(2) 0.5751(2) 0.0631(7) Uani 1 1 d . . .
N2 N 1.0892(2) -0.6033(2) 0.5795(2) 0.0616(7) Uani 1 1 d . . .
N3 N 0.1910(2) -0.36186(19) 0.17900(17) 0.0477(5) Uani 1 1 d . . .
H3A H 0.1900 -0.2835 0.1808 0.057 Uiso 1 1 calc R . .
C1 C 0.5356(3) -0.3569(2) 0.5478(2) 0.0507(7) Uani 1 1 d . . .
C2 C 0.9859(3) -0.6249(2) 0.5701(2) 0.0466(6) Uani 1 1 d . . .
C3 C 0.6870(2) -0.5401(2) 0.2123(2) 0.0484(6) Uani 1 1 d . . .
C4 C 0.6592(3) -0.5610(3) 0.0952(2) 0.0741(9) Uani 1 1 d . . .
H4A H 0.7215 -0.6130 0.0785 0.111 Uiso 1 1 calc R . .
H4B H 0.6588 -0.4843 0.0596 0.111 Uiso 1 1 calc R . .
H4C H 0.5794 -0.5990 0.0725 0.111 Uiso 1 1 calc R . .
C5 C 0.0802(3) -0.4205(3) 0.1624(2) 0.0575(7) Uani 1 1 d . . .
C6 C 0.0822(4) -0.5445(3) 0.1610(3) 0.0810(11) Uani 1 1 d . . .
H6A H 0.0086 -0.5885 0.1491 0.097 Uiso 1 1 calc R . .
C7 C 0.1952(4) -0.6049(3) 0.1774(3) 0.0855(11) Uani 1 1 d . . .
H7A H 0.1961 -0.6896 0.1782 0.103 Uiso 1 1 calc R . .
C8 C 0.3041(3) -0.5441(3) 0.1923(3) 0.0662(8) Uani 1 1 d . . .
H8A H 0.3787 -0.5862 0.2019 0.079 Uiso 1 1 calc R . .
C9 C 0.3018(3) -0.4168(2) 0.1929(2) 0.0492(6) Uani 1 1 d . . .
N4 N 0.4022(2) -0.3479(2) 0.2062(2) 0.0734(8) Uani 1 1 d . . .
H4D H 0.3956 -0.2699 0.2058 0.088 Uiso 1 1 calc R . .
H4E H 0.4740 -0.3813 0.2151 0.088 Uiso 1 1 calc R . .
C10 C -0.0324(3) -0.3431(3) 0.1469(3) 0.0767(10) Uani 1 1 d . . .
H10A H -0.0086 -0.2588 0.1516 0.115 Uiso 1 1 calc R . .
H10B H -0.0759 -0.3614 0.2007 0.115 Uiso 1 1 calc R . .
H10C H -0.0853 -0.3590 0.0784 0.115 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.03674(12) 0.05109(13) 0.05766(14) -0.00085(9) 0.01617(9) -0.00066(9)
S1 0.0685(5) 0.0547(5) 0.1196(8) -0.0260(5) 0.0562(5) -0.0220(4)
S2 0.0450(4) 0.0739(5) 0.0678(5) 0.0224(4) 0.0127(4) -0.0146(4)
O1 0.0671(13) 0.0465(11) 0.0638(12) 0.0087(9) 0.0152(11) 0.0148(10)
O2 0.0512(12) 0.0574(12) 0.0670(13) -0.0008(10) 0.0123(10) 0.0169(10)
N1 0.0456(14) 0.0615(16) 0.0896(19) -0.0174(13) 0.0307(14) -0.0116(12)
N2 0.0429(14) 0.0591(15) 0.0839(18) 0.0199(13) 0.0169(13) 0.0004(12)
N3 0.0483(13) 0.0391(11) 0.0549(13) 0.0023(10) 0.0108(11) -0.0001(10)
C1 0.0435(15) 0.0435(15) 0.0670(18) -0.0132(13) 0.0167(14) -0.0024(12)
C2 0.0470(17) 0.0439(15) 0.0485(15) 0.0104(12) 0.0104(13) -0.0008(12)
C3 0.0416(15) 0.0428(14) 0.0615(17) 0.0034(13) 0.0132(13) 0.0009(12)
C4 0.082(2) 0.074(2) 0.060(2) -0.0079(17) 0.0063(17) 0.0165(19)
C5 0.0542(18) 0.0643(19) 0.0514(16) 0.0024(14) 0.0074(14) -0.0093(15)
C6 0.070(2) 0.067(2) 0.100(3) -0.005(2) 0.008(2) -0.024(2)
C7 0.103(3) 0.0440(18) 0.109(3) -0.0046(18) 0.023(3) -0.015(2)
C8 0.075(2) 0.0452(16) 0.078(2) 0.0006(15) 0.0170(18) 0.0097(16)
C9 0.0503(16) 0.0428(15) 0.0534(16) 0.0014(12) 0.0099(13) 0.0031(13)
N4 0.0464(15) 0.0503(15) 0.122(2) 0.0042(15) 0.0157(15) 0.0058(12)
C10 0.0465(18) 0.097(3) 0.085(2) 0.009(2) 0.0118(17) 0.0004(18)

_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 N2 2.307(2) 3_746 ?
Cd1 O2 2.346(2) . ?
Cd1 N1 2.351(2) 3_646 ?
Cd1 O1 2.432(2) . ?
Cd1 S1 2.6043(8) . ?
Cd1 S2 2.6300(8) . ?
Cd1 C3 2.749(3) . ?
S1 C1 1.649(3) . ?
S2 C2 1.641(3) . ?
O1 C3 1.256(3) . ?
O2 C3 1.252(3) . ?
N1 C1 1.141(3) . ?
N1 Cd1 2.351(2) 3_646 ?
N2 C2 1.150(3) . ?
N2 Cd1 2.307(2) 3_746 ?
N3 C9 1.344(3) . ?
N3 C5 1.360(4) . ?
C3 C4 1.497(4) . ?
C5 C6 1.361(5) . ?
C5 C10 1.485(4) . ?
C6 C7 1.390(5) . ?
C7 C8 1.354(5) . ?
C8 C9 1.398(4) . ?
C9 N4 1.323(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
N2 Cd1 O2 90.72(8) 3_746 . ?
N2 Cd1 N1 175.48(9) 3_746 3_646 ?
O2 Cd1 N1 88.57(9) . 3_646 ?
N2 Cd1 O1 88.32(9) 3_746 . ?
O2 Cd1 O1 54.17(6) . . ?
N1 Cd1 O1 87.64(8) 3_646 . ?
N2 Cd1 S1 89.37(7) 3_746 . ?
O2 Cd1 S1 99.18(5) . . ?
N1 Cd1 S1 95.15(6) 3_646 . ?
O1 Cd1 S1 153.20(5) . . ?
N2 Cd1 S2 93.64(6) 3_746 . ?
O2 Cd1 S2 145.44(5) . . ?
N1 Cd1 S2 84.44(7) 3_646 . ?
O1 Cd1 S2 91.68(5) . . ?
S1 Cd1 S2 115.11(3) . . ?
N2 Cd1 C3 89.67(9) 3_746 . ?
O2 Cd1 C3 26.99(7) . . ?
N1 Cd1 C3 87.67(9) 3_646 . ?
O1 Cd1 C3 27.19(7) . . ?
S1 Cd1 C3 126.14(6) . . ?
S2 Cd1 C3 118.69(6) . . ?
C1 S1 Cd1 99.91(10) . . ?
C2 S2 Cd1 100.68(9) . . ?
C3 O1 Cd1 90.60(17) . . ?
C3 O2 Cd1 94.73(16) . . ?
C1 N1 Cd1 159.2(2) . 3_646 ?
C2 N2 Cd1 162.6(2) . 3_746 ?
C9 N3 C5 125.1(2) . . ?
N1 C1 S1 177.6(3) . . ?
N2 C2 S2 177.3(3) . . ?
O2 C3 O1 120.5(3) . . ?
O2 C3 C4 119.1(3) . . ?
O1 C3 C4 120.4(3) . . ?
O2 C3 Cd1 58.29(14) . . ?
O1 C3 Cd1 62.22(15) . . ?
C4 C3 Cd1 177.3(2) . . ?
N3 C5 C6 117.3(3) . . ?
N3 C5 C10 116.8(3) . . ?
C6 C5 C10 125.9(3) . . ?
C5 C6 C7 119.4(3) . . ?
C8 C7 C6 122.1(3) . . ?
C7 C8 C9 118.4(3) . . ?
N4 C9 N3 118.6(2) . . ?
N4 C9 C8 123.7(3) . . ?
N3 C9 C8 117.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1058266'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H26 Br4 Cd N12 O5 S5'
_chemical_formula_weight         1154.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 -0.2900 2.4600 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8080 1.2020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.9159(4)
_cell_length_b                   12.9791(8)
_cell_length_c                   16.8359(8)
_cell_angle_alpha                68.545(3)
_cell_angle_beta                 88.854(3)
_cell_angle_gamma                79.115(4)
_cell_volume                     1977.49(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1124
_exptl_absorpt_coefficient_mu    4.908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_T_max  0.612
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11231
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         25.04
_reflns_number_total             6942
_reflns_number_gt                5405
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1192P)²+3.8069P] 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         6942
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1893
_refine_ls_wR_factor_gt          0.1789
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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
Cd1 Cd 0.04640(5) 0.90040(4) 0.36737(3) 0.03854(19) Uani 1 1 d . . .
S1 S -0.0454(3) 0.5665(3) 0.37651(19) 0.0736(7) Uani 1 1 d . . .
S2 S -0.1931(2) 0.9295(2) 0.30009(15) 0.0586(6) Uani 1 1 d . . .
S3 S 0.1047(3) 1.0974(2) 0.34790(15) 0.0655(7) Uani 1 1 d . . .
S4 S 0.4521(2) 0.9651(2) 0.21508(18) 0.0632(6) Uani 1 1 d . . .
N1 N 0.1124(9) 0.7057(6) 0.4104(5) 0.064(2) Uani 1 1 d . . .
N2 N -0.2146(9) 1.1449(8) 0.1734(6) 0.072(2) Uani 1 1 d . . .
N3 N 0.0062(9) 1.1284(6) 0.4952(4) 0.063(2) Uani 1 1 d . . .
N4 N 0.1984(8) 0.9073(7) 0.2616(5) 0.065(2) Uani 1 1 d . . .
C1 C 0.0430(8) 0.6492(7) 0.3934(5) 0.0467(19) Uani 1 1 d . . .
C2 C -0.2045(8) 1.0593(8) 0.2253(6) 0.0494(19) Uani 1 1 d . . .
C3 C 0.0474(9) 1.1134(6) 0.4345(5) 0.0477(19) Uani 1 1 d . . .
C4 C 0.3033(9) 0.9316(7) 0.2428(5) 0.0447(18) Uani 1 1 d . . .
Br1 Br -0.10566(9) 0.76386(7) -0.10389(5) 0.0518(2) Uani 1 1 d . . .
N5 N 0.0200(6) 0.7806(5) 0.0335(4) 0.0382(13) Uani 1 1 d . . .
H5A H 0.0779 0.7247 0.0293 0.046 Uiso 1 1 calc R . .
N9 N 0.1531(7) 0.7666(6) 0.1503(5) 0.0549(18) Uani 1 1 d . . .
H9A H 0.2082 0.7106 0.1440 0.066 Uiso 1 1 calc R . .
H9B H 0.1695 0.7888 0.1908 0.066 Uiso 1 1 calc R . .
C5 C 0.0419(8) 0.8190(6) 0.0970(5) 0.0426(17) Uani 1 1 d . . .
C6 C -0.0542(9) 0.9090(7) 0.1023(5) 0.054(2) Uani 1 1 d . . .
H6A H -0.0428 0.9369 0.1448 0.064 Uiso 1 1 calc R . .
C7 C -0.1621(10) 0.9551(8) 0.0472(6) 0.062(2) Uani 1 1 d . . .
H7A H -0.2244 1.0159 0.0514 0.075 Uiso 1 1 calc R . .
C8 C -0.1858(8) 0.9154(7) -0.0176(6) 0.054(2) Uani 1 1 d . . .
H8A H -0.2631 0.9471 -0.0551 0.064 Uiso 1 1 calc R . .
C9 C -0.0902(8) 0.8282(6) -0.0226(5) 0.0411(16) Uani 1 1 d . . .
Br2 Br -0.57031(8) 0.76581(7) -0.02147(6) 0.0545(3) Uani 1 1 d . . .
N6 N -0.3263(6) 0.6264(5) 0.0534(3) 0.0342(12) Uani 1 1 d . . .
H6B H -0.3386 0.6019 0.0135 0.041 Uiso 1 1 calc R . .
N10 N -0.1194(6) 0.4999(6) 0.0924(4) 0.0461(15) Uani 1 1 d . . .
H10A H -0.1346 0.4768 0.0523 0.055 Uiso 1 1 calc R . .
H10B H -0.0453 0.4703 0.1247 0.055 Uiso 1 1 calc R . .
C10 C -0.2098(7) 0.5805(6) 0.1046(4) 0.0396(16) Uani 1 1 d . . .
C11 C -0.1932(9) 0.6229(8) 0.1687(5) 0.051(2) Uani 1 1 d . . .
H11A H -0.1135 0.5960 0.2041 0.061 Uiso 1 1 calc R . .
C12 C -0.2941(10) 0.7036(8) 0.1789(5) 0.057(2) Uani 1 1 d . . .
H12A H -0.2843 0.7294 0.2229 0.068 Uiso 1 1 calc R . .
C13 C -0.4132(10) 0.7486(8) 0.1236(6) 0.057(2) Uani 1 1 d . . .
H13A H -0.4819 0.8043 0.1299 0.068 Uiso 1 1 calc R . .
C14 C -0.4239(8) 0.7089(6) 0.0623(5) 0.0417(17) Uani 1 1 d . . .
Br3 Br 0.59937(10) 0.40778(9) 0.65156(6) 0.0654(3) Uani 1 1 d . . .
N7 N 0.4585(6) 0.5399(5) 0.7356(4) 0.0431(15) Uani 1 1 d . . .
H7B H 0.5304 0.5104 0.7698 0.052 Uiso 1 1 calc R . .
N11 N 0.3744(7) 0.6336(6) 0.8232(5) 0.0519(17) Uani 1 1 d . . .
H11B H 0.4464 0.6007 0.8569 0.062 Uiso 1 1 calc R . .
H11C H 0.3114 0.6804 0.8350 0.062 Uiso 1 1 calc R . .
C15 C 0.3604(7) 0.6121(6) 0.7523(5) 0.0448(18) Uani 1 1 d . . .
C16 C 0.2421(9) 0.6613(7) 0.6952(6) 0.060(2) Uani 1 1 d . . .
H16A H 0.1716 0.7127 0.7052 0.072 Uiso 1 1 calc R . .
C17 C 0.2327(10) 0.6326(8) 0.6261(7) 0.068(3) Uani 1 1 d . . .
H17A H 0.1546 0.6641 0.5893 0.081 Uiso 1 1 calc R . .
C18 C 0.3393(10) 0.5560(8) 0.6088(6) 0.065(3) Uani 1 1 d . . .
H18A H 0.3340 0.5375 0.5607 0.079 Uiso 1 1 calc R . .
C19 C 0.4507(8) 0.5100(7) 0.6658(5) 0.0482(18) Uani 1 1 d . . .
Br4 Br -0.64013(13) 0.92583(11) 0.57880(9) 0.0927(4) Uani 1 1 d . . .
N12 N -0.1946(11) 0.6369(7) 0.6475(6) 0.078(2) Uani 1 1 d . . .
H12B H -0.2045 0.6489 0.6945 0.094 Uiso 1 1 calc R . .
H12C H -0.1244 0.5900 0.6424 0.094 Uiso 1 1 calc R . .
S5 S 0.25086(17) 0.49899(15) 0.11395(11) 0.0350(4) Uani 1 1 d . . .
O1 O 0.1584(6) 0.4327(5) 0.1705(4) 0.0550(14) Uani 1 1 d . . .
O2 O 0.3574(5) 0.4227(5) 0.0891(3) 0.0486(13) Uani 1 1 d . . .
O3 O 0.1725(6) 0.5840(4) 0.0366(3) 0.0489(13) Uani 1 1 d . . .
O4 O 0.3158(5) 0.5570(4) 0.1588(4) 0.0499(14) Uani 1 1 d . . .
C24 C -0.5074(5) 0.8314(5) 0.5427(4) 0.067(3) Uani 1 1 d G . .
C23 C -0.5127(6) 0.8260(6) 0.4619(4) 0.083(3) Uiso 1 1 d G . .
H23A H -0.5855 0.8699 0.4230 0.100 Uiso 1 1 calc R . .
C22 C -0.4092(8) 0.7551(7) 0.4392(3) 0.098(4) Uiso 1 1 d G . .
H22A H -0.4127 0.7515 0.3851 0.118 Uiso 1 1 calc R . .
C21 C -0.3004(7) 0.6896(6) 0.4973(4) 0.078(3) Uiso 1 1 d G . .
H21A H -0.2311 0.6421 0.4821 0.094 Uiso 1 1 calc R . .
C20 C -0.2951(5) 0.6949(5) 0.5781(4) 0.067(3) Uani 1 1 d G . .
N8 N -0.3986(6) 0.7658(5) 0.6008(3) 0.0532(17) Uani 1 1 d G . .
H8B H -0.3953 0.7692 0.6508 0.064 Uiso 1 1 calc R . .
OW1 O 0.3955(8) 1.2114(6) 0.2460(5) 0.0721(18) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0408(3) 0.0422(3) 0.0345(3) -0.0195(2) 0.0010(2) -0.0015(2)
S1 0.0757(16) 0.0852(18) 0.0731(16) -0.0478(15) -0.0048(13) -0.0082(14)
S2 0.0420(11) 0.0713(15) 0.0560(13) -0.0160(11) -0.0042(9) -0.0104(10)
S3 0.1026(19) 0.0659(14) 0.0488(12) -0.0348(11) 0.0318(12) -0.0404(14)
S4 0.0462(12) 0.0762(16) 0.0830(17) -0.0474(14) 0.0099(11) -0.0129(11)
N1 0.086(6) 0.050(4) 0.070(5) -0.039(4) 0.015(4) -0.012(4)
N2 0.065(5) 0.069(5) 0.065(5) -0.019(5) -0.023(4) 0.019(4)
N3 0.108(7) 0.047(4) 0.037(4) -0.020(3) 0.011(4) -0.011(4)
N4 0.064(5) 0.079(5) 0.072(5) -0.048(4) 0.032(4) -0.027(4)
C1 0.054(5) 0.040(4) 0.037(4) -0.013(3) 0.001(3) 0.011(4)
C2 0.040(4) 0.058(5) 0.048(5) -0.026(4) -0.007(4) 0.009(4)
C3 0.070(5) 0.038(4) 0.041(4) -0.020(3) 0.007(4) -0.014(4)
C4 0.056(5) 0.048(4) 0.037(4) -0.028(3) 0.002(4) -0.001(4)
Br1 0.0563(5) 0.0596(5) 0.0414(4) -0.0246(4) -0.0104(4) -0.0022(4)
N5 0.042(3) 0.037(3) 0.037(3) -0.020(3) -0.001(3) 0.005(3)
N9 0.058(4) 0.057(4) 0.056(4) -0.038(4) -0.017(3) 0.011(3)
C5 0.051(4) 0.039(4) 0.040(4) -0.020(3) 0.000(3) -0.003(3)
C6 0.064(5) 0.050(5) 0.049(5) -0.029(4) 0.003(4) 0.007(4)
C7 0.060(5) 0.058(5) 0.060(5) -0.029(4) 0.001(4) 0.022(4)
C8 0.044(4) 0.051(5) 0.054(5) -0.016(4) -0.002(4) 0.011(4)
C9 0.048(4) 0.045(4) 0.032(4) -0.016(3) -0.004(3) -0.008(3)
Br2 0.0478(5) 0.0527(5) 0.0541(5) -0.0205(4) -0.0032(4) 0.0133(4)
N6 0.038(3) 0.039(3) 0.028(3) -0.017(2) 0.001(2) -0.003(2)
N10 0.031(3) 0.068(4) 0.042(3) -0.029(3) -0.007(3) 0.004(3)
C10 0.038(4) 0.049(4) 0.032(4) -0.015(3) 0.005(3) -0.011(3)
C11 0.057(5) 0.066(5) 0.037(4) -0.024(4) -0.005(4) -0.016(4)
C12 0.077(6) 0.059(5) 0.042(4) -0.029(4) 0.011(4) -0.012(4)
C13 0.068(6) 0.055(5) 0.049(5) -0.030(4) 0.007(4) 0.002(4)
C14 0.044(4) 0.039(4) 0.038(4) -0.011(3) 0.006(3) -0.003(3)
Br3 0.0644(6) 0.0760(6) 0.0651(6) -0.0408(5) -0.0063(5) -0.0044(5)
N7 0.038(3) 0.039(3) 0.046(4) -0.008(3) -0.014(3) -0.008(3)
N11 0.037(3) 0.050(4) 0.071(5) -0.029(4) -0.007(3) 0.002(3)
C15 0.035(4) 0.031(4) 0.064(5) -0.012(4) -0.014(3) -0.004(3)
C16 0.048(5) 0.043(5) 0.071(6) -0.005(4) -0.015(4) 0.001(4)
C17 0.056(5) 0.063(6) 0.069(6) -0.007(5) -0.031(5) -0.006(5)
C18 0.067(6) 0.070(6) 0.060(6) -0.020(5) -0.024(5) -0.019(5)
C19 0.050(4) 0.047(4) 0.044(4) -0.013(4) -0.002(4) -0.009(4)
Br4 0.0808(8) 0.0795(8) 0.0990(9) -0.0163(7) 0.0119(7) -0.0059(6)
N12 0.112(7) 0.064(5) 0.067(5) -0.034(4) 0.019(5) -0.021(5)
S5 0.0307(8) 0.0390(9) 0.0364(9) -0.0214(7) -0.0112(7) 0.0074(7)
O1 0.046(3) 0.072(4) 0.044(3) -0.017(3) -0.004(2) -0.011(3)
O2 0.041(3) 0.059(3) 0.050(3) -0.036(3) -0.011(2) 0.013(2)
O3 0.053(3) 0.044(3) 0.045(3) -0.019(2) -0.021(2) 0.010(2)
O4 0.047(3) 0.044(3) 0.064(3) -0.035(3) -0.023(3) 0.010(2)
C24 0.082(7) 0.064(6) 0.051(5) -0.010(5) 0.009(5) -0.025(5)
C20 0.084(7) 0.063(6) 0.052(5) -0.013(5) 0.003(5) -0.028(5)
N8 0.071(5) 0.047(4) 0.043(4) -0.016(3) 0.006(3) -0.016(3)
OW1 0.084(5) 0.062(4) 0.070(4) -0.026(3) 0.002(4) -0.011(3)

_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 N3 2.271(7) 2_576 ?
Cd1 N4 2.298(7) . ?
Cd1 N1 2.323(7) . ?
Cd1 S2 2.554(2) . ?
Cd1 S3 2.630(2) . ?
S1 C1 1.609(10) . ?
S2 C2 1.679(10) . ?
S3 C3 1.624(8) . ?
S4 C4 1.628(9) . ?
N1 C1 1.202(11) . ?
N2 C2 1.122(12) . ?
N3 C3 1.160(10) . ?
N3 Cd1 2.271(7) 2_576 ?
N4 C4 1.148(11) . ?
Br1 C9 1.868(7) . ?
N5 C9 1.352(9) . ?
N5 C5 1.370(9) . ?
N5 H5A 0.8600 . ?
N9 C5 1.339(10) . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
C5 C6 1.390(11) . ?
C6 C7 1.325(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.405(13) . ?
C7 H7A 0.9300 . ?
C8 C9 1.359(11) . ?
C8 H8A 0.9300 . ?
Br2 C14 1.886(8) . ?
N6 C14 1.352(9) . ?
N6 C10 1.356(9) . ?
N6 H6B 0.8600 . ?
N10 C10 1.317(10) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
C10 C11 1.404(11) . ?
C11 C12 1.363(12) . ?
C11 H11A 0.9300 . ?
C12 C13 1.410(13) . ?
C12 H12A 0.9300 . ?
C13 C14 1.326(11) . ?
C13 H13A 0.9300 . ?
Br3 C19 1.863(9) . ?
N7 C15 1.319(10) . ?
N7 C19 1.373(10) . ?
N7 H7B 0.8600 . ?
N11 C15 1.336(11) . ?
N11 H11B 0.8600 . ?
N11 H11C 0.8600 . ?
C15 C16 1.422(11) . ?
C16 C17 1.354(15) . ?
C16 H16A 0.9300 . ?
C17 C18 1.412(15) . ?
C17 H17A 0.9300 . ?
C18 C19 1.369(12) . ?
C18 H18A 0.9300 . ?
Br4 C24 1.873(5) . ?
N12 C20 1.430(11) . ?
N12 H12B 0.8600 . ?
N12 H12C 0.8600 . ?
S5 O1 1.466(6) . ?
S5 O2 1.470(5) . ?
S5 O4 1.474(5) . ?
S5 O3 1.477(5) . ?
C24 C23 1.3900 . ?
C24 N8 1.3900 . ?
C23 C22 1.3900 . ?
C23 H23A 0.9300 . ?
C22 C21 1.3900 . ?
C22 H22A 0.9300 . ?
C21 C20 1.3900 . ?
C21 H21A 0.9300 . ?
C20 N8 1.3900 . ?
N8 H8B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cd1 N4 153.0(3) 2_576 . ?
N3 Cd1 N1 87.1(3) 2_576 . ?
N4 Cd1 N1 85.4(3) . . ?
N3 Cd1 S2 100.1(2) 2_576 . ?
N4 Cd1 S2 106.8(2) . . ?
N1 Cd1 S2 100.2(2) . . ?
N3 Cd1 S3 90.7(2) 2_576 . ?
N4 Cd1 S3 83.2(2) . . ?
N1 Cd1 S3 150.1(2) . . ?
S2 Cd1 S3 109.53(9) . . ?
C2 S2 Cd1 100.2(3) . . ?
C3 S3 Cd1 101.2(3) . . ?
C1 N1 Cd1 122.3(7) . . ?
C3 N3 Cd1 162.1(7) . 2_576 ?
C4 N4 Cd1 139.5(7) . . ?
N1 C1 S1 176.1(8) . . ?
N2 C2 S2 177.5(9) . . ?
N3 C3 S3 177.8(7) . . ?
N4 C4 S4 179.1(7) . . ?
C9 N5 C5 121.7(6) . . ?
C9 N5 H5A 119.1 . . ?
C5 N5 H5A 119.1 . . ?
C5 N9 H9A 120.0 . . ?
C5 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
N9 C5 N5 117.9(6) . . ?
N9 C5 C6 124.5(7) . . ?
N5 C5 C6 117.5(7) . . ?
C7 C6 C5 120.3(8) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C6 C7 C8 122.4(8) . . ?
C6 C7 H7A 118.8 . . ?
C8 C7 H7A 118.8 . . ?
C9 C8 C7 116.6(7) . . ?
C9 C8 H8A 121.7 . . ?
C7 C8 H8A 121.7 . . ?
N5 C9 C8 121.4(7) . . ?
N5 C9 Br1 116.1(5) . . ?
C8 C9 Br1 122.5(6) . . ?
C14 N6 C10 122.8(6) . . ?
C14 N6 H6B 118.6 . . ?
C10 N6 H6B 118.6 . . ?
C10 N10 H10A 120.0 . . ?
C10 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
N10 C10 N6 119.4(6) . . ?
N10 C10 C11 123.7(7) . . ?
N6 C10 C11 116.9(7) . . ?
C12 C11 C10 119.9(8) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 120.8(8) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C14 C13 C12 117.8(8) . . ?
C14 C13 H13A 121.1 . . ?
C12 C13 H13A 121.1 . . ?
C13 C14 N6 121.8(7) . . ?
C13 C14 Br2 123.4(6) . . ?
N6 C14 Br2 114.8(5) . . ?
C15 N7 C19 122.8(6) . . ?
C15 N7 H7B 118.6 . . ?
C19 N7 H7B 118.6 . . ?
C15 N11 H11B 120.0 . . ?
C15 N11 H11C 120.0 . . ?
H11B N11 H11C 120.0 . . ?
N7 C15 N11 118.9(6) . . ?
N7 C15 C16 118.4(8) . . ?
N11 C15 C16 122.7(8) . . ?
C17 C16 C15 119.6(9) . . ?
C17 C16 H16A 120.2 . . ?
C15 C16 H16A 120.2 . . ?
C16 C17 C18 121.3(8) . . ?
C16 C17 H17A 119.4 . . ?
C18 C17 H17A 119.4 . . ?
C19 C18 C17 117.2(9) . . ?
C19 C18 H18A 121.4 . . ?
C17 C18 H18A 121.4 . . ?
C18 C19 N7 120.8(8) . . ?
C18 C19 Br3 122.1(7) . . ?
N7 C19 Br3 117.1(6) . . ?
C20 N12 H12B 120.0 . . ?
C20 N12 H12C 120.0 . . ?
H12B N12 H12C 120.0 . . ?
O1 S5 O2 108.9(4) . . ?
O1 S5 O4 109.8(4) . . ?
O2 S5 O4 109.7(3) . . ?
O1 S5 O3 109.9(3) . . ?
O2 S5 O3 109.4(3) . . ?
O4 S5 O3 109.1(3) . . ?
C23 C24 N8 120.0 . . ?
C23 C24 Br4 123.3(3) . . ?
N8 C24 Br4 116.7(3) . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C21 C22 H22A 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
N8 C20 C21 120.0 . . ?
N8 C20 N12 109.9(5) . . ?
C21 C20 N12 130.1(5) . . ?
C20 N8 C24 120.0 . . ?
C20 N8 H8B 120.0 . . ?
C24 N8 H8B 120.0 . . ?

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
N3 Cd1 S2 C2 121.3(3) 2_576 . . . ?
N4 Cd1 S2 C2 -61.7(4) . . . . ?
N1 Cd1 S2 C2 -149.9(4) . . . . ?
S3 Cd1 S2 C2 26.9(3) . . . . ?
N3 Cd1 S3 C3 -10.5(4) 2_576 . . . ?
N4 Cd1 S3 C3 -164.1(4) . . . . ?
N1 Cd1 S3 C3 -95.9(5) . . . . ?
S2 Cd1 S3 C3 90.4(3) . . . . ?
N3 Cd1 N1 C1 104.8(8) 2_576 . . . ?
N4 Cd1 N1 C1 -101.2(7) . . . . ?
S2 Cd1 N1 C1 5.1(7) . . . . ?
S3 Cd1 N1 C1 -168.9(5) . . . . ?
N3 Cd1 N4 C4 -35.3(15) 2_576 . . . ?
N1 Cd1 N4 C4 -109.6(12) . . . . ?
S2 Cd1 N4 C4 151.1(11) . . . . ?
S3 Cd1 N4 C4 42.7(11) . . . . ?
Cd1 N1 C1 S1 -152(11) . . . . ?
Cd1 S2 C2 N2 145(20) . . . . ?
Cd1 N3 C3 S3 -161(21) 2_576 . . . ?
Cd1 S3 C3 N3 -160(24) . . . . ?
Cd1 N4 C4 S4 167(68) . . . . ?
C9 N5 C5 N9 179.6(7) . . . . ?
C9 N5 C5 C6 0.4(11) . . . . ?
N9 C5 C6 C7 -179.4(9) . . . . ?
N5 C5 C6 C7 -0.3(13) . . . . ?
C5 C6 C7 C8 0.9(15) . . . . ?
C6 C7 C8 C9 -1.6(15) . . . . ?
C5 N5 C9 C8 -1.2(12) . . . . ?
C5 N5 C9 Br1 -179.0(6) . . . . ?
C7 C8 C9 N5 1.7(13) . . . . ?
C7 C8 C9 Br1 179.4(7) . . . . ?
C14 N6 C10 N10 179.6(7) . . . . ?
C14 N6 C10 C11 -0.3(10) . . . . ?
N10 C10 C11 C12 -177.6(8) . . . . ?
N6 C10 C11 C12 2.3(11) . . . . ?
C10 C11 C12 C13 -2.5(13) . . . . ?
C11 C12 C13 C14 0.7(14) . . . . ?
C12 C13 C14 N6 1.4(13) . . . . ?
C12 C13 C14 Br2 -175.9(6) . . . . ?
C10 N6 C14 C13 -1.6(11) . . . . ?
C10 N6 C14 Br2 175.9(5) . . . . ?
C19 N7 C15 N11 177.8(7) . . . . ?
C19 N7 C15 C16 -0.4(11) . . . . ?
N7 C15 C16 C17 0.4(12) . . . . ?
N11 C15 C16 C17 -177.8(8) . . . . ?
C15 C16 C17 C18 -1.0(14) . . . . ?
C16 C17 C18 C19 1.5(15) . . . . ?
C17 C18 C19 N7 -1.5(13) . . . . ?
C17 C18 C19 Br3 -179.9(7) . . . . ?
C15 N7 C19 C18 1.0(12) . . . . ?
C15 N7 C19 Br3 179.5(6) . . . . ?
N8 C24 C23 C22 0.0 . . . . ?
Br4 C24 C23 C22 179.0(5) . . . . ?
C24 C23 C22 C21 0.0 . . . . ?
C23 C22 C21 C20 0.0 . . . . ?
C22 C21 C20 N8 0.0 . . . . ?
C22 C21 C20 N12 -179.6(8) . . . . ?
C21 C20 N8 C24 0.0 . . . . ?
N12 C20 N8 C24 179.7(6) . . . . ?
C23 C24 N8 C20 0.0 . . . . ?
Br4 C24 N8 C20 -179.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         5.492
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.161
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1058267'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H16 Cl4 Cu N2 O0'
_chemical_formula_weight         321.56

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   9.3655(6)
_cell_length_b                   7.2877(5)
_cell_length_c                   8.6164(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.869(4)
_cell_angle_gamma                90.00
_cell_volume                     587.36(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             326
_exptl_absorpt_coefficient_mu    2.728
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_T_max  0.741
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            3235
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         25.18
_reflns_number_total             1056
_reflns_number_gt                995
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0800P)²+0.4064P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1056
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1175
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 -0.5000 0.5000 0.0234(3) Uani 1 2 d S . .
Cl1 Cl 0.50005(7) -0.24411(9) 0.34926(9) 0.0338(3) Uani 1 1 d . . .
Cl2 Cl 0.74552(9) -0.50352(8) 0.50352(10) 0.0275(3) Uani 1 1 d . . .
N1 N 0.2674(3) 0.0731(4) 0.3692(3) 0.0268(6) Uani 1 1 d . . .
C1 C 0.1331(4) -0.0131(3) 0.4195(4) 0.0213(7) Uani 1 1 d . . .
H1C H 0.1283 -0.1396 0.3810 0.026 Uiso 1 1 calc R . .
C2 C 0.0051(3) 0.0934(4) 0.3493(3) 0.0235(6) Uani 1 1 d . . .
H2A H 0.0136 0.2215 0.3791 0.028 Uiso 1 1 calc R . .
H2B H 0.0048 0.0866 0.2369 0.028 Uiso 1 1 calc R . .
C3 C 0.1352(4) -0.0162(4) 0.5955(4) 0.0243(7) Uani 1 1 d . . .
H3A H 0.1491 0.1074 0.6353 0.029 Uiso 1 1 calc R . .
H3B H 0.2142 -0.0912 0.6355 0.029 Uiso 1 1 calc R . .
H03 H 0.263(4) 0.068(6) 0.282(5) 0.033(10) Uiso 1 1 d . . .
H02 H 0.285(5) 0.177(7) 0.415(5) 0.052(11) Uiso 1 1 d . . .
H01 H 0.330(6) 0.014(5) 0.404(6) 0.044(14) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0203(4) 0.0225(4) 0.0276(4) 0.00505(15) 0.0022(2) 0.00064(14)
Cl1 0.0316(5) 0.0284(5) 0.0420(5) 0.0120(3) 0.0083(3) 0.0069(3)
Cl2 0.0218(5) 0.0312(5) 0.0295(5) 0.0029(2) -0.0003(3) 0.0013(2)
N1 0.0231(13) 0.0326(16) 0.0249(14) -0.0018(11) 0.0040(10) 0.0003(11)
C1 0.0190(15) 0.0202(14) 0.0246(16) -0.0010(9) 0.0007(12) 0.0001(9)
C2 0.0235(14) 0.0261(14) 0.0209(12) 0.0060(9) 0.0000(10) 0.0018(10)
C3 0.0222(16) 0.0298(15) 0.0204(15) 0.0018(9) -0.0030(11) 0.0000(10)

_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 Cl1 2.2726(7) . ?
Cu1 Cl1 2.2726(7) 3_646 ?
Cu1 Cl2 2.2983(8) . ?
Cu1 Cl2 2.2983(8) 3_646 ?
N1 C1 1.490(4) . ?
N1 H03 0.75(4) . ?
N1 H02 0.87(5) . ?
N1 H01 0.78(6) . ?
C1 C3 1.516(5) . ?
C1 C2 1.527(4) . ?
C1 H1C 0.9800 . ?
C2 C3 1.527(4) 3_556 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C2 1.527(4) 3_556 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

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
Cl1 Cu1 Cl1 180.00(4) . 3_646 ?
Cl1 Cu1 Cl2 89.31(2) . . ?
Cl1 Cu1 Cl2 90.69(2) 3_646 . ?
Cl1 Cu1 Cl2 90.69(2) . 3_646 ?
Cl1 Cu1 Cl2 89.31(2) 3_646 3_646 ?
Cl2 Cu1 Cl2 180.00(4) . 3_646 ?
C1 N1 H03 105(3) . . ?
C1 N1 H02 113(3) . . ?
H03 N1 H02 120(4) . . ?
C1 N1 H01 107(4) . . ?
H03 N1 H01 111(5) . . ?
H02 N1 H01 100(4) . . ?
N1 C1 C3 109.2(3) . . ?
N1 C1 C2 109.1(2) . . ?
C3 C1 C2 112.0(3) . . ?
N1 C1 H1C 108.8 . . ?
C3 C1 H1C 108.8 . . ?
C2 C1 H1C 108.8 . . ?
C3 C2 C1 111.1(2) 3_556 . ?
C3 C2 H2A 109.4 3_556 . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 3_556 . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C1 C3 C2 110.4(3) . 3_556 ?
C1 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 3_556 . ?
C1 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 3_556 . ?
H3A C3 H3B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.18
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.599
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.261
