# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_lk
_database_code_depnum_ccdc_archive 'CCDC 1028855'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H8 N6 O9 S Zn'
_chemical_formula_sum            'C6 H8 N6 O9 S Zn'
_chemical_formula_weight         405.61

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'
Zn Zn 0.2839 1.4301 '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
_symmetry_space_group_name_Hall  -C2yc

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                   16.337(3)
_cell_length_b                   11.925(2)
_cell_length_c                   14.007(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.84(3)
_cell_angle_gamma                90.00
_cell_volume                     2680.1(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3050
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_T_max  0.602
_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            12773
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         27.43
_reflns_number_total             3050
_reflns_number_gt                2514
_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    'Bruker SHELXTL'
_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)+(0.0298P)²+4.1770P] 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         3050
_refine_ls_number_parameters     216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0830
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Zn1 Zn 0.28366(2) 0.02044(3) 0.22162(2) 0.01525(11) Uani 1 1 d . . .
S1 S 0.02524(4) 0.13483(6) -0.09637(5) 0.01547(16) Uani 1 1 d . . .
O1 O -0.06085(12) 0.13558(17) -0.09534(14) 0.0195(4) Uani 1 1 d . . .
O2 O 0.06536(12) 0.06263(17) -0.15262(14) 0.0192(4) Uani 1 1 d . . .
O3 O 0.28562(15) 0.1554(2) 0.32230(16) 0.0208(5) Uani 1 1 d . . .
H3A H 0.262(2) 0.210(3) 0.318(2) 0.018(9) Uiso 1 1 d . . .
H3C H 0.289(2) 0.132(3) 0.381(3) 0.042(11) Uiso 1 1 d . . .
O4 O 0.30044(14) -0.14005(17) 0.15711(14) 0.0225(5) Uani 1 1 d . . .
O5 O 0.34650(15) -0.24272(19) 0.05049(16) 0.0304(5) Uani 1 1 d . . .
O6 O 0.29953(14) -0.07504(17) 0.01137(14) 0.0244(5) Uani 1 1 d . . .
O7 O 0.24725(12) -0.08394(17) 0.32444(14) 0.0192(4) Uani 1 1 d . . .
O8 O 0.31983(13) -0.17508(17) 0.44610(14) 0.0215(5) Uani 1 1 d . . .
O9 O 0.38163(13) -0.06521(18) 0.35653(15) 0.0232(5) Uani 1 1 d . . .
N1 N 0.17402(15) 0.07586(19) 0.14069(17) 0.0168(5) Uani 1 1 d . . .
N2 N 0.07400(14) 0.11753(19) 0.01806(16) 0.0157(5) Uani 1 1 d . . .
N3 N 0.04974(14) 0.26484(19) -0.12338(16) 0.0148(5) Uani 1 1 d . . .
N4 N 0.12333(15) 0.4031(2) -0.16748(16) 0.0158(5) Uani 1 1 d . . .
N5 N 0.31579(16) -0.1541(2) 0.07121(17) 0.0202(5) Uani 1 1 d . . .
N6 N 0.31802(15) -0.1098(2) 0.37787(16) 0.0175(5) Uani 1 1 d . . .
C1 C 0.15216(18) 0.0739(2) 0.0460(2) 0.0164(6) Uani 1 1 d . . .
H1B H 0.1851 0.0468 0.0037 0.020 Uiso 1 1 calc R . .
C2 C 0.10741(18) 0.1238(2) 0.1761(2) 0.0196(6) Uani 1 1 d . . .
H2B H 0.1061 0.1354 0.2414 0.024 Uiso 1 1 calc R . .
C3 C 0.04590(19) 0.1506(2) 0.1023(2) 0.0197(6) Uani 1 1 d . . .
H3B H -0.0048 0.1842 0.1061 0.024 Uiso 1 1 calc R . .
C4 C 0.12008(17) 0.2937(2) -0.15771(19) 0.0154(6) Uani 1 1 d . . .
H4A H 0.1596 0.2434 -0.1720 0.018 Uiso 1 1 calc R . .
C5 C 0.05273(18) 0.4471(2) -0.1371(2) 0.0174(6) Uani 1 1 d . . .
H5A H 0.0393 0.5228 -0.1368 0.021 Uiso 1 1 calc R . .
C6 C 0.00739(18) 0.3635(2) -0.1087(2) 0.0188(6) Uani 1 1 d . . .
H6A H -0.0416 0.3700 -0.0844 0.023 Uiso 1 1 calc R . .


_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
Zn1 N4 2.037(2) 7 ?
Zn1 N1 2.041(2) . ?
Zn1 O7 2.0734(19) . ?
Zn1 O3 2.136(2) . ?
Zn1 O4 2.156(2) . ?
Zn1 O9 2.457(2) . ?
S1 O1 1.409(2) . ?
S1 O2 1.409(2) . ?
S1 N3 1.663(2) . ?
S1 N2 1.663(2) . ?
O3 H3A 0.75(4) . ?
O3 H3C 0.86(4) . ?
O4 N5 1.285(3) . ?
O5 N5 1.228(3) . ?
O6 N5 1.256(3) . ?
O7 N6 1.291(3) . ?
O8 N6 1.229(3) . ?
O9 N6 1.252(3) . ?
N1 C1 1.307(3) . ?
N1 C2 1.400(4) . ?
N2 C1 1.366(4) . ?
N2 C3 1.401(3) . ?
N3 C4 1.370(3) . ?
N3 C6 1.400(4) . ?
N4 C4 1.315(4) . ?
N4 C5 1.404(4) . ?
N4 Zn1 2.037(2) 7 ?
C1 H1B 0.9300 . ?
C2 C3 1.338(4) . ?
C2 H2B 0.9300 . ?
C3 H3B 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.346(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?

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
N4 Zn1 N1 106.65(9) 7 . ?
N4 Zn1 O7 149.18(9) 7 . ?
N1 Zn1 O7 104.11(9) . . ?
N4 Zn1 O3 89.36(9) 7 . ?
N1 Zn1 O3 91.45(10) . . ?
O7 Zn1 O3 87.97(8) . . ?
N4 Zn1 O4 94.51(9) 7 . ?
N1 Zn1 O4 102.83(9) . . ?
O7 Zn1 O4 80.44(8) . . ?
O3 Zn1 O4 163.40(9) . . ?
N4 Zn1 O9 92.79(8) 7 . ?
N1 Zn1 O9 159.77(8) . . ?
O7 Zn1 O9 56.41(7) . . ?
O3 Zn1 O9 83.05(9) . . ?
O4 Zn1 O9 80.65(8) . . ?
O1 S1 O2 125.43(13) . . ?
O1 S1 N3 106.25(12) . . ?
O2 S1 N3 106.57(12) . . ?
O1 S1 N2 106.80(12) . . ?
O2 S1 N2 105.91(12) . . ?
N3 S1 N2 104.05(12) . . ?
Zn1 O3 H3A 131(3) . . ?
Zn1 O3 H3C 112(3) . . ?
H3A O3 H3C 107(3) . . ?
N5 O4 Zn1 124.79(17) . . ?
N6 O7 Zn1 101.73(15) . . ?
N6 O9 Zn1 84.85(15) . . ?
C1 N1 C2 106.5(2) . . ?
C1 N1 Zn1 127.0(2) . . ?
C2 N1 Zn1 126.52(19) . . ?
C1 N2 C3 107.6(2) . . ?
C1 N2 S1 125.16(19) . . ?
C3 N2 S1 127.1(2) . . ?
C4 N3 C6 108.1(2) . . ?
C4 N3 S1 124.6(2) . . ?
C6 N3 S1 127.13(19) . . ?
C4 N4 C5 106.7(2) . . ?
C4 N4 Zn1 122.05(19) . 7 ?
C5 N4 Zn1 131.20(19) . 7 ?
O5 N5 O6 122.2(2) . . ?
O5 N5 O4 119.6(2) . . ?
O6 N5 O4 118.2(2) . . ?
O8 N6 O9 123.7(2) . . ?
O8 N6 O7 119.4(2) . . ?
O9 N6 O7 117.0(2) . . ?
N1 C1 N2 110.3(2) . . ?
N1 C1 H1B 124.9 . . ?
N2 C1 H1B 124.9 . . ?
C3 C2 N1 110.2(2) . . ?
C3 C2 H2B 124.9 . . ?
N1 C2 H2B 124.9 . . ?
C2 C3 N2 105.4(2) . . ?
C2 C3 H3B 127.3 . . ?
N2 C3 H3B 127.3 . . ?
N4 C4 N3 109.8(2) . . ?
N4 C4 H4A 125.1 . . ?
N3 C4 H4A 125.1 . . ?
C6 C5 N4 110.0(3) . . ?
C6 C5 H5A 125.0 . . ?
N4 C5 H5A 125.0 . . ?
C5 C6 N3 105.3(2) . . ?
C5 C6 H6A 127.3 . . ?
N3 C6 H6A 127.3 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.100
####################################################################### 
# 
# 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_p1
_database_code_depnum_ccdc_archive 'CCDC 1028856'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H6 N5 O5 S Zn0.50'
_chemical_formula_sum            'C6 H6 N5 O5 S Zn0.50'
_chemical_formula_weight         292.92

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'
Zn Zn 0.2839 1.4301 '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
_symmetry_space_group_name_Hall  -P1

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

_cell_length_a                   6.6953(13)
_cell_length_b                   8.7758(18)
_cell_length_c                   10.028(2)
_cell_angle_alpha                64.41(3)
_cell_angle_beta                 76.36(3)
_cell_angle_gamma                82.37(3)
_cell_volume                     516.11(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2349
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             296
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_T_max  0.679
_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            5161
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2349
_reflns_number_gt                2293
_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  ?

_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)+(0.0277P)²+0.3776P] 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         2349
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0560
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
Zn1 Zn 0.5000 0.0000 0.5000 0.00930(7) Uani 1 2 d S . .
S1 S 0.00659(5) 0.40580(4) 0.78261(4) 0.01036(8) Uani 1 1 d . . .
O1 O -0.08772(16) 0.48230(13) 0.65585(12) 0.0152(2) Uani 1 1 d . . .
O2 O -0.10223(16) 0.35315(13) 0.93307(12) 0.0159(2) Uani 1 1 d . . .
O3 O 0.22384(16) 0.07968(14) 0.40778(12) 0.0142(2) Uani 1 1 d . . .
O4 O 0.16272(19) 0.19685(15) 0.18075(13) 0.0224(2) Uani 1 1 d . . .
O5 O 0.18363(18) -0.07637(14) 0.29645(13) 0.0209(2) Uani 1 1 d . . .
N1 N 0.34180(18) 0.07982(15) 0.67024(13) 0.0112(2) Uani 1 1 d . . .
N2 N 0.14590(18) 0.23892(15) 0.77162(13) 0.0103(2) Uani 1 1 d . . .
N3 N 0.18950(18) 0.53392(15) 0.75361(13) 0.0116(2) Uani 1 1 d . . .
N4 N 0.39221(18) 0.74958(15) 0.64220(13) 0.0121(2) Uani 1 1 d . . .
N5 N 0.18990(18) 0.06519(16) 0.29341(14) 0.0125(2) Uani 1 1 d . . .
C1 C 0.2305(2) 0.21994(17) 0.64110(15) 0.0116(3) Uani 1 1 d . . .
H1B H 0.2114 0.2961 0.5454 0.014 Uiso 1 1 calc R . .
C2 C 0.2121(2) 0.10022(18) 0.89083(16) 0.0125(3) Uani 1 1 d . . .
H2B H 0.1813 0.0789 0.9926 0.015 Uiso 1 1 calc R . .
C3 C 0.3304(2) 0.00418(18) 0.82574(16) 0.0135(3) Uani 1 1 d . . .
H3A H 0.3952 -0.0982 0.8774 0.016 Uiso 1 1 calc R . .
C4 C 0.2303(2) 0.68841(17) 0.63422(16) 0.0126(3) Uani 1 1 d . . .
H4B H 0.1539 0.7415 0.5589 0.015 Uiso 1 1 calc R . .
C5 C 0.3379(2) 0.49799(18) 0.84115(16) 0.0141(3) Uani 1 1 d . . .
H5A H 0.3493 0.4026 0.9294 0.017 Uiso 1 1 calc R . .
C6 C 0.4614(2) 0.63123(18) 0.77036(16) 0.0135(3) Uani 1 1 d . . .
H6A H 0.5759 0.6426 0.8023 0.016 Uiso 1 1 calc R . .


_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
Zn1 N1 2.1237(13) . ?
Zn1 N1 2.1237(13) 2_656 ?
Zn1 N4 2.1477(15) 1_545 ?
Zn1 N4 2.1477(15) 2_666 ?
Zn1 O3 2.1604(12) . ?
Zn1 O3 2.1604(12) 2_656 ?
S1 O2 1.4105(12) . ?
S1 O1 1.4121(12) . ?
S1 N2 1.6598(13) . ?
S1 N3 1.6625(13) . ?
O3 N5 1.2806(16) . ?
O4 N5 1.2482(17) . ?
O5 N5 1.2356(17) . ?
N1 C1 1.3044(19) . ?
N1 C3 1.3932(18) . ?
N2 C1 1.3694(18) . ?
N2 C2 1.3988(18) . ?
N3 C4 1.3741(19) . ?
N3 C5 1.3953(18) . ?
N4 C4 1.3045(19) . ?
N4 C6 1.3945(19) . ?
N4 Zn1 2.1477(15) 1_565 ?
C1 H1B 0.9300 . ?
C2 C3 1.348(2) . ?
C2 H2B 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4B 0.9300 . ?
C5 C6 1.348(2) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?

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 Zn1 N1 180 . 2_656 ?
N1 Zn1 N4 89.18(5) . 1_545 ?
N1 Zn1 N4 90.82(5) 2_656 1_545 ?
N1 Zn1 N4 90.82(5) . 2_666 ?
N1 Zn1 N4 89.18(5) 2_656 2_666 ?
N4 Zn1 N4 180 1_545 2_666 ?
N1 Zn1 O3 85.98(5) . . ?
N1 Zn1 O3 94.02(5) 2_656 . ?
N4 Zn1 O3 92.53(5) 1_545 . ?
N4 Zn1 O3 87.47(5) 2_666 . ?
N1 Zn1 O3 94.02(5) . 2_656 ?
N1 Zn1 O3 85.98(5) 2_656 2_656 ?
N4 Zn1 O3 87.47(5) 1_545 2_656 ?
N4 Zn1 O3 92.53(5) 2_666 2_656 ?
O3 Zn1 O3 180 . 2_656 ?
O2 S1 O1 123.84(7) . . ?
O2 S1 N2 106.54(7) . . ?
O1 S1 N2 107.82(7) . . ?
O2 S1 N3 108.86(7) . . ?
O1 S1 N3 106.31(7) . . ?
N2 S1 N3 101.22(6) . . ?
N5 O3 Zn1 126.77(9) . . ?
C1 N1 C3 106.57(12) . . ?
C1 N1 Zn1 122.80(10) . . ?
C3 N1 Zn1 130.62(10) . . ?
C1 N2 C2 107.85(12) . . ?
C1 N2 S1 125.47(10) . . ?
C2 N2 S1 126.48(10) . . ?
C4 N3 C5 107.81(12) . . ?
C4 N3 S1 126.30(11) . . ?
C5 N3 S1 125.76(10) . . ?
C4 N4 C6 106.94(12) . . ?
C4 N4 Zn1 125.07(10) . 1_565 ?
C6 N4 Zn1 127.49(10) . 1_565 ?
O5 N5 O4 121.57(13) . . ?
O5 N5 O3 120.13(12) . . ?
O4 N5 O3 118.30(13) . . ?
N1 C1 N2 110.27(12) . . ?
N1 C1 H1B 124.9 . . ?
N2 C1 H1B 124.9 . . ?
C3 C2 N2 104.81(12) . . ?
C3 C2 H2B 127.6 . . ?
N2 C2 H2B 127.6 . . ?
C2 C3 N1 110.50(13) . . ?
C2 C3 H3A 124.8 . . ?
N1 C3 H3A 124.8 . . ?
N4 C4 N3 109.94(13) . . ?
N4 C4 H4B 125.0 . . ?
N3 C4 H4B 125.0 . . ?
C6 C5 N3 105.22(13) . . ?
C6 C5 H5A 127.4 . . ?
N3 C5 H5A 127.4 . . ?
C5 C6 N4 110.09(13) . . ?
C5 C6 H6A 125.0 . . ?
N4 C6 H6A 125.0 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 1028857'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H6 Co0.50 N5 O5 S'
_chemical_formula_sum            'C6 H6 Co0.50 N5 O5 S'
_chemical_formula_weight         289.69

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'
Co Co 0.3494 0.9721 '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
_symmetry_space_group_name_Hall  -P1

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

_cell_length_a                   6.7656(6)
_cell_length_b                   8.7886(7)
_cell_length_c                   10.0635(8)
_cell_angle_alpha                64.603(5)
_cell_angle_beta                 76.394(5)
_cell_angle_gamma                82.581(5)
_cell_volume                     525.11(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1845
_cell_measurement_theta_min      25.05
_cell_measurement_theta_max      2.29

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             293
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_T_max  0.757
_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            2980
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.05
_reflns_number_total             1845
_reflns_number_gt                1379
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0246P)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         1845
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_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
Co1 Co 0.5000 0.0000 0.5000 0.02147(18) Uani 1 2 d S . .
S1 S 0.01053(11) 0.40608(9) 0.78219(9) 0.0262(2) Uani 1 1 d . . .
N1 N 0.3406(4) 0.0812(3) 0.6689(3) 0.0246(6) Uani 1 1 d . . .
N2 N 0.1473(3) 0.2397(3) 0.7707(3) 0.0228(6) Uani 1 1 d . . .
N3 N 0.1928(4) 0.5342(3) 0.7524(3) 0.0253(6) Uani 1 1 d . . .
N4 N 0.3925(4) 0.7507(3) 0.6422(3) 0.0264(6) Uani 1 1 d . . .
N5 N 0.8041(4) -0.0612(4) 0.7052(3) 0.0319(6) Uani 1 1 d . . .
O1 O -0.0835(3) 0.4825(3) 0.6569(2) 0.0338(5) Uani 1 1 d . . .
O2 O -0.0949(3) 0.3537(3) 0.9319(2) 0.0376(6) Uani 1 1 d . . .
O3 O 0.7668(3) -0.0768(3) 0.5928(2) 0.0323(5) Uani 1 1 d . . .
O4 O 0.8110(4) 0.0798(3) 0.7012(3) 0.0505(7) Uani 1 1 d . . .
O5 O 0.8332(4) -0.1909(3) 0.8156(3) 0.0544(7) Uani 1 1 d . . .
C1 C 0.2324(4) 0.2201(4) 0.6411(4) 0.0256(7) Uani 1 1 d . . .
H1B H 0.2148 0.2964 0.5458 0.031 Uiso 1 1 calc R . .
C2 C 0.3286(5) 0.0074(4) 0.8228(3) 0.0305(7) Uani 1 1 d . . .
H2B H 0.3929 -0.0942 0.8744 0.037 Uiso 1 1 calc R . .
C3 C 0.2121(5) 0.1020(4) 0.8871(3) 0.0286(7) Uani 1 1 d . . .
H3A H 0.1811 0.0800 0.9886 0.034 Uiso 1 1 calc R . .
C4 C 0.2327(5) 0.6880(4) 0.6345(4) 0.0288(7) Uani 1 1 d . . .
H4B H 0.1569 0.7403 0.5597 0.035 Uiso 1 1 calc R . .
C5 C 0.4608(5) 0.6319(4) 0.7678(4) 0.0312(8) Uani 1 1 d . . .
H5A H 0.5753 0.6427 0.7988 0.037 Uiso 1 1 calc R . .
C6 C 0.3397(5) 0.4994(4) 0.8384(4) 0.0342(8) Uani 1 1 d . . .
H6A H 0.3514 0.4046 0.9261 0.041 Uiso 1 1 calc R . .


_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 2.127(2) . ?
Co1 O3 2.127(2) 2_656 ?
Co1 N1 2.131(2) 2_656 ?
Co1 N1 2.131(2) . ?
Co1 N4 2.147(2) 1_545 ?
Co1 N4 2.147(2) 2_666 ?
S1 O2 1.405(2) . ?
S1 O1 1.410(2) . ?
S1 N2 1.660(2) . ?
S1 N3 1.665(2) . ?
N1 C1 1.295(4) . ?
N1 C2 1.386(4) . ?
N2 C1 1.370(3) . ?
N2 C3 1.385(4) . ?
N3 C4 1.370(4) . ?
N3 C6 1.388(4) . ?
N4 C4 1.307(4) . ?
N4 C5 1.385(4) . ?
N4 Co1 2.147(2) 1_565 ?
N5 O4 1.229(3) . ?
N5 O5 1.238(3) . ?
N5 O3 1.280(3) . ?
C1 H1B 0.9300 . ?
C2 C3 1.335(4) . ?
C2 H2B 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4B 0.9300 . ?
C5 C6 1.340(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?

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 O3 180 . 2_656 ?
O3 Co1 N1 86.17(8) . 2_656 ?
O3 Co1 N1 93.83(8) 2_656 2_656 ?
O3 Co1 N1 93.83(8) . . ?
O3 Co1 N1 86.17(8) 2_656 . ?
N1 Co1 N1 180.000(1) 2_656 . ?
O3 Co1 N4 87.34(9) . 1_545 ?
O3 Co1 N4 92.66(9) 2_656 1_545 ?
N1 Co1 N4 90.98(9) 2_656 1_545 ?
N1 Co1 N4 89.02(9) . 1_545 ?
O3 Co1 N4 92.66(9) . 2_666 ?
O3 Co1 N4 87.34(9) 2_656 2_666 ?
N1 Co1 N4 89.02(9) 2_656 2_666 ?
N1 Co1 N4 90.98(9) . 2_666 ?
N4 Co1 N4 180 1_545 2_666 ?
O2 S1 O1 124.09(13) . . ?
O2 S1 N2 106.35(13) . . ?
O1 S1 N2 108.02(12) . . ?
O2 S1 N3 108.76(13) . . ?
O1 S1 N3 106.15(13) . . ?
N2 S1 N3 101.16(12) . . ?
C1 N1 C2 105.8(2) . . ?
C1 N1 Co1 123.7(2) . . ?
C2 N1 Co1 130.48(19) . . ?
C1 N2 C3 106.9(2) . . ?
C1 N2 S1 125.9(2) . . ?
C3 N2 S1 126.94(19) . . ?
C4 N3 C6 107.6(2) . . ?
C4 N3 S1 126.4(2) . . ?
C6 N3 S1 125.9(2) . . ?
C4 N4 C5 106.1(3) . . ?
C4 N4 Co1 125.4(2) . 1_565 ?
C5 N4 Co1 128.2(2) . 1_565 ?
O4 N5 O5 121.8(3) . . ?
O4 N5 O3 120.0(3) . . ?
O5 N5 O3 118.2(3) . . ?
N5 O3 Co1 128.42(18) . . ?
N1 C1 N2 111.0(3) . . ?
N1 C1 H1B 124.5 . . ?
N2 C1 H1B 124.5 . . ?
C3 C2 N1 110.8(3) . . ?
C3 C2 H2B 124.6 . . ?
N1 C2 H2B 124.6 . . ?
C2 C3 N2 105.4(3) . . ?
C2 C3 H3A 127.3 . . ?
N2 C3 H3A 127.3 . . ?
N4 C4 N3 110.3(3) . . ?
N4 C4 H4B 124.9 . . ?
N3 C4 H4B 124.9 . . ?
C6 C5 N4 110.8(3) . . ?
C6 C5 H5A 124.6 . . ?
N4 C5 H5A 124.6 . . ?
C5 C6 N3 105.2(3) . . ?
C5 C6 H6A 127.4 . . ?
N3 C6 H6A 127.4 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.066
####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 1028858'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C9 H12 Cu0.50 N5 O6 S'
_chemical_formula_sum            'C9 H12 Cu0.50 N5 O6 S'
_chemical_formula_weight         350.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   13.8786(8)
_cell_length_b                   13.6808(6)
_cell_length_c                   16.6792(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.229(3)
_cell_angle_gamma                90.00
_cell_volume                     2931.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2578
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      24.97

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1436
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.784
_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            8120
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         24.97
_reflns_number_total             2578
_reflns_number_gt                2234
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0471P)²+6.9422P] 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         2578
_refine_ls_number_parameters     200
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.073
_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 0.2500 0.2500 0.5000 0.02794(17) Uani 1 2 d S . .
S1 S 0.19013(5) 0.19578(5) 0.14810(4) 0.0328(2) Uani 1 1 d . . .
O1 O 0.17759(18) 0.09655(15) 0.16486(14) 0.0444(5) Uani 1 1 d . . .
O2 O 0.26311(17) 0.23246(18) 0.11539(14) 0.0447(5) Uani 1 1 d . . .
O3 O 0.20512(18) 0.08476(15) 0.46356(15) 0.0448(5) Uani 1 1 d . . .
O4 O 0.2734(3) -0.0532(3) 0.5133(2) 0.0984(13) Uani 1 1 d . . .
O5 O 0.2773(2) -0.00236(17) 0.39375(16) 0.0575(7) Uani 1 1 d . . .
O6 O 0.0000 0.0566(3) 0.2500 0.0742(11) Uani 1 2 d S . .
O7 O 0.0000 0.3600(4) 0.2500 0.1030(17) Uani 1 2 d S . .
N1 N 0.23035(17) 0.27638(18) 0.37602(14) 0.0296(5) Uani 1 1 d . . .
N2 N 0.21012(18) 0.25397(16) 0.24085(15) 0.0297(5) Uani 1 1 d . . .
N3 N 0.07425(18) 0.23769(17) 0.08289(15) 0.0317(5) Uani 1 1 d . . .
N4 N -0.09439(18) 0.26181(17) 0.02818(15) 0.0318(5) Uani 1 1 d . . .
N5 N 0.2534(2) 0.00921(17) 0.45728(16) 0.0383(6) Uani 1 1 d . . .
C1 C 0.2046(2) 0.2125(2) 0.31356(16) 0.0304(6) Uani 1 1 d . . .
H1A H 0.1853 0.1481 0.3178 0.036 Uiso 1 1 calc R . .
C2 C 0.2407(2) 0.3512(2) 0.26059(19) 0.0354(6) Uani 1 1 d . . .
H2A H 0.2507 0.3978 0.2239 0.043 Uiso 1 1 calc R . .
C3 C 0.2527(2) 0.3632(2) 0.34329(18) 0.0343(6) Uani 1 1 d . . .
H3A H 0.2729 0.4211 0.3744 0.041 Uiso 1 1 calc R . .
C4 C -0.0200(2) 0.2118(2) 0.08507(17) 0.0334(6) Uani 1 1 d . . .
H4B H -0.0295 0.1652 0.1220 0.040 Uiso 1 1 calc R . .
C5 C -0.0471(2) 0.3234(2) -0.01258(19) 0.0403(7) Uani 1 1 d . . .
H5A H -0.0823 0.3674 -0.0563 0.048 Uiso 1 1 calc R . .
C6 C 0.0566(2) 0.3102(2) 0.02017(19) 0.0392(7) Uani 1 1 d . . .
H6A H 0.1058 0.3424 0.0044 0.047 Uiso 1 1 calc R . .
C7 C 0.0000 -0.0310(5) 0.2500 0.0742(18) Uani 1 2 d S . .
C8 C 0.0192(5) -0.0875(5) 0.3309(4) 0.1008(17) Uani 1 1 d U . .
H8A H 0.0874 -0.1162 0.3503 0.121 Uiso 1 1 calc R . .
H8B H -0.0320 -0.1383 0.3197 0.121 Uiso 1 1 calc R . .
H8C H 0.0147 -0.0446 0.3748 0.121 Uiso 1 1 calc R . .
C9 C 0.0000 0.4490(5) 0.2500 0.0698(16) Uani 1 2 d S . .
C10 C 0.0117(6) 0.5071(5) 0.1797(4) 0.117(2) Uani 1 1 d . . .
H10A H 0.0633 0.4774 0.1621 0.141 Uiso 1 1 calc R . .
H10B H 0.0331 0.5723 0.1999 0.141 Uiso 1 1 calc R . .
H10C H -0.0536 0.5095 0.1312 0.141 Uiso 1 1 calc R . .


_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 N1 2.013(2) 7_556 ?
Cu1 N1 2.013(2) . ?
Cu1 N4 2.035(2) 2 ?
Cu1 N4 2.035(2) 8_556 ?
Cu1 O3 2.363(2) . ?
Cu1 O3 2.363(2) 7_556 ?
S1 O1 1.410(2) . ?
S1 O2 1.412(2) . ?
S1 N3 1.666(2) . ?
S1 N2 1.667(2) . ?
O3 N5 1.257(3) . ?
O4 N5 1.218(4) . ?
O5 N5 1.235(3) . ?
O6 C7 1.199(7) . ?
O7 C9 1.219(8) . ?
N1 C1 1.302(4) . ?
N1 C3 1.390(4) . ?
N2 C1 1.367(3) . ?
N2 C2 1.398(4) . ?
N3 C4 1.369(4) . ?
N3 C6 1.395(4) . ?
N4 C4 1.301(4) . ?
N4 C5 1.393(4) . ?
N4 Cu1 2.035(2) 2 ?
C1 H1A 0.9300 . ?
C2 C3 1.336(4) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4B 0.9300 . ?
C5 C6 1.345(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.489(6) 2 ?
C7 C8 1.489(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.476(7) 2 ?
C9 C10 1.476(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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 Cu1 N1 180 7_556 . ?
N1 Cu1 N4 88.34(9) 7_556 2 ?
N1 Cu1 N4 91.66(9) . 2 ?
N1 Cu1 N4 91.66(9) 7_556 8_556 ?
N1 Cu1 N4 88.34(9) . 8_556 ?
N4 Cu1 N4 180 2 8_556 ?
N1 Cu1 O3 90.73(9) 7_556 . ?
N1 Cu1 O3 89.27(9) . . ?
N4 Cu1 O3 82.13(9) 2 . ?
N4 Cu1 O3 97.87(9) 8_556 . ?
N1 Cu1 O3 89.27(9) 7_556 7_556 ?
N1 Cu1 O3 90.73(9) . 7_556 ?
N4 Cu1 O3 97.87(9) 2 7_556 ?
N4 Cu1 O3 82.13(9) 8_556 7_556 ?
O3 Cu1 O3 180 . 7_556 ?
O1 S1 O2 125.39(14) . . ?
O1 S1 N3 107.44(13) . . ?
O2 S1 N3 106.37(13) . . ?
O1 S1 N2 105.40(12) . . ?
O2 S1 N2 107.28(13) . . ?
N3 S1 N2 102.84(12) . . ?
N5 O3 Cu1 135.32(19) . . ?
C1 N1 C3 107.1(2) . . ?
C1 N1 Cu1 126.20(19) . . ?
C3 N1 Cu1 126.35(19) . . ?
C1 N2 C2 107.5(2) . . ?
C1 N2 S1 125.39(19) . . ?
C2 N2 S1 127.03(19) . . ?
C4 N3 C6 107.8(2) . . ?
C4 N3 S1 126.2(2) . . ?
C6 N3 S1 125.9(2) . . ?
C4 N4 C5 106.5(2) . . ?
C4 N4 Cu1 127.35(19) . 2 ?
C5 N4 Cu1 126.2(2) . 2 ?
O4 N5 O5 120.7(3) . . ?
O4 N5 O3 119.2(3) . . ?
O5 N5 O3 120.1(2) . . ?
N1 C1 N2 109.9(2) . . ?
N1 C1 H1A 125.1 . . ?
N2 C1 H1A 125.1 . . ?
C3 C2 N2 105.5(2) . . ?
C3 C2 H2A 127.2 . . ?
N2 C2 H2A 127.2 . . ?
C2 C3 N1 110.0(2) . . ?
C2 C3 H3A 125.0 . . ?
N1 C3 H3A 125.0 . . ?
N4 C4 N3 110.3(2) . . ?
N4 C4 H4B 124.8 . . ?
N3 C4 H4B 124.8 . . ?
C6 C5 N4 110.5(3) . . ?
C6 C5 H5A 124.7 . . ?
N4 C5 H5A 124.7 . . ?
C5 C6 N3 104.9(2) . . ?
C5 C6 H6A 127.5 . . ?
N3 C6 H6A 127.5 . . ?
O6 C7 C8 121.3(3) . 2 ?
O6 C7 C8 121.3(3) . . ?
C8 C7 C8 117.4(7) 2 . ?
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 . . ?
O7 C9 C10 122.6(4) . 2 ?
O7 C9 C10 122.6(4) . . ?
C10 C9 C10 114.8(7) 2 . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_cc
_database_code_depnum_ccdc_archive 'CCDC 1028859'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H8 Mn0.50 N5 O6 S'
_chemical_formula_sum            'C6 H8 Mn0.50 N5 O6 S'
_chemical_formula_weight         305.71

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'
Mn Mn 0.3368 0.7283 '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   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   10.269(2)
_cell_length_b                   15.040(3)
_cell_length_c                   15.004(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.71(3)
_cell_angle_gamma                90.00
_cell_volume                     2276.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2589
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  0.812
_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            11088
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.44
_reflns_number_total             2589
_reflns_number_gt                2362
_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  ?

_refine_special_details          
; 
The maximum residual electron density 2.235 belongs to Q1 (0.1450 0.0602 0.4678). 
The distance of Q1 and N5 from one free nitrate anion is 0.1254nm.
The distance of Q1 and O5 from the same free nitrate anion is 0.1462nm.
 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)+(0.1225P)²+6.1136P] 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         2589
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1906
_refine_ls_wR_factor_gt          0.1867
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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
Mn1 Mn 1.0000 0.36117(4) 0.2500 0.0277(2) Uani 1 2 d S . .
S1 S 0.43745(8) 0.28132(6) 0.09828(5) 0.0355(3) Uani 1 1 d . . .
N1 N 0.7810(3) 0.36873(19) 0.19644(19) 0.0325(6) Uani 1 1 d . . .
N2 N 0.5723(3) 0.33855(19) 0.14224(18) 0.0309(6) Uani 1 1 d . . .
N3 N 0.4336(3) 0.28447(19) -0.01278(18) 0.0325(6) Uani 1 1 d . . .
N4 N 0.4672(3) 0.2415(2) -0.14626(19) 0.0375(6) Uani 1 1 d . . .
N5 N 0.2513(3) 0.0709(3) 0.4394(2) 0.0492(8) Uani 1 1 d . . .
O1 O 0.4622(3) 0.1926(2) 0.1253(2) 0.0542(8) Uani 1 1 d . . .
O2 O 0.3283(3) 0.3312(2) 0.11470(19) 0.0520(7) Uani 1 1 d . . .
O3 O 0.9903(4) 0.4664(2) 0.3499(2) 0.0599(9) Uani 1 1 d . . .
H3A H 1.0501 0.4594 0.3939 0.090 Uiso 1 1 calc R . .
O4 O 0.2350(8) 0.0754(4) 0.3592(3) 0.125(2) Uani 1 1 d . . .
O5 O 0.2190(7) 0.1438(4) 0.4759(4) 0.118(2) Uani 1 1 d . . .
O6 O 0.3255(5) 0.0176(3) 0.4863(3) 0.0942(14) Uani 1 1 d . . .
C1 C 0.6987(3) 0.3056(2) 0.1650(2) 0.0327(7) Uani 1 1 d . . .
H1B H 0.7222 0.2465 0.1589 0.039 Uiso 1 1 calc R . .
C2 C 0.5788(4) 0.4297(2) 0.1588(3) 0.0418(8) Uani 1 1 d . . .
H2B H 0.5094 0.4703 0.1492 0.050 Uiso 1 1 calc R . .
C3 C 0.7077(4) 0.4460(2) 0.1920(3) 0.0409(8) Uani 1 1 d . . .
H3B H 0.7425 0.5017 0.2094 0.049 Uiso 1 1 calc R . .
C4 C 0.4854(3) 0.2206(2) -0.0609(2) 0.0390(8) Uani 1 1 d . . .
H4B H 0.5278 0.1692 -0.0360 0.047 Uiso 1 1 calc R . .
C5 C 0.4012(4) 0.3227(2) -0.1546(2) 0.0396(8) Uani 1 1 d . . .
H5A H 0.3753 0.3536 -0.2087 0.048 Uiso 1 1 calc R . .
C6 C 0.3801(4) 0.3498(2) -0.0734(2) 0.0397(8) Uani 1 1 d . . .
H6A H 0.3382 0.4018 -0.0606 0.048 Uiso 1 1 calc R . .
H3C H 0.916(6) 0.484(4) 0.364(4) 0.081(19) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 2.196(3) . ?
Mn1 O3 2.196(3) 2_755 ?
Mn1 N1 2.246(3) . ?
Mn1 N1 2.246(3) 2_755 ?
Mn1 N4 2.262(3) 7_655 ?
Mn1 N4 2.262(3) 8_556 ?
S1 O1 1.404(3) . ?
S1 O2 1.409(3) . ?
S1 N2 1.660(3) . ?
S1 N3 1.660(3) . ?
N1 C1 1.300(4) . ?
N1 C3 1.379(4) . ?
N2 C1 1.372(4) . ?
N2 C2 1.392(4) . ?
N3 C4 1.368(4) . ?
N3 C6 1.382(4) . ?
N4 C4 1.298(5) . ?
N4 C5 1.391(5) . ?
N4 Mn1 2.262(3) 7_655 ?
N5 O4 1.186(5) . ?
N5 O6 1.232(6) . ?
N5 O5 1.295(6) . ?
O3 H3A 0.8200 . ?
O3 H3C 0.87(7) . ?
C1 H1B 0.9300 . ?
C2 C3 1.347(5) . ?
C2 H2B 0.9300 . ?
C3 H3B 0.9300 . ?
C4 H4B 0.9300 . ?
C5 C6 1.339(5) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?

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 Mn1 O3 87.71(19) . 2_755 ?
O3 Mn1 N1 92.19(12) . . ?
O3 Mn1 N1 83.61(12) 2_755 . ?
O3 Mn1 N1 83.61(12) . 2_755 ?
O3 Mn1 N1 92.19(13) 2_755 2_755 ?
N1 Mn1 N1 174.20(15) . 2_755 ?
O3 Mn1 N4 173.63(13) . 7_655 ?
O3 Mn1 N4 89.48(13) 2_755 7_655 ?
N1 Mn1 N4 93.18(10) . 7_655 ?
N1 Mn1 N4 90.78(10) 2_755 7_655 ?
O3 Mn1 N4 89.48(13) . 8_556 ?
O3 Mn1 N4 173.63(13) 2_755 8_556 ?
N1 Mn1 N4 90.78(10) . 8_556 ?
N1 Mn1 N4 93.18(10) 2_755 8_556 ?
N4 Mn1 N4 93.87(17) 7_655 8_556 ?
O1 S1 O2 124.3(2) . . ?
O1 S1 N2 106.56(16) . . ?
O2 S1 N2 106.66(17) . . ?
O1 S1 N3 106.63(17) . . ?
O2 S1 N3 106.80(16) . . ?
N2 S1 N3 104.28(14) . . ?
C1 N1 C3 106.6(3) . . ?
C1 N1 Mn1 129.2(2) . . ?
C3 N1 Mn1 124.1(2) . . ?
C1 N2 C2 107.4(3) . . ?
C1 N2 S1 126.3(2) . . ?
C2 N2 S1 126.2(2) . . ?
C4 N3 C6 107.3(3) . . ?
C4 N3 S1 124.8(2) . . ?
C6 N3 S1 127.9(2) . . ?
C4 N4 C5 106.3(3) . . ?
C4 N4 Mn1 120.0(2) . 7_655 ?
C5 N4 Mn1 132.1(2) . 7_655 ?
O4 N5 O6 124.8(5) . . ?
O4 N5 O5 112.4(5) . . ?
O6 N5 O5 119.3(4) . . ?
Mn1 O3 H3A 109.5 . . ?
Mn1 O3 H3C 122(4) . . ?
H3A O3 H3C 114.0 . . ?
N1 C1 N2 110.3(3) . . ?
N1 C1 H1B 124.8 . . ?
N2 C1 H1B 124.8 . . ?
C3 C2 N2 104.9(3) . . ?
C3 C2 H2B 127.6 . . ?
N2 C2 H2B 127.6 . . ?
C2 C3 N1 110.7(3) . . ?
C2 C3 H3B 124.6 . . ?
N1 C3 H3B 124.6 . . ?
N4 C4 N3 110.6(3) . . ?
N4 C4 H4B 124.7 . . ?
N3 C4 H4B 124.7 . . ?
C6 C5 N4 110.1(3) . . ?
C6 C5 H5A 124.9 . . ?
N4 C5 H5A 124.9 . . ?
C5 C6 N3 105.7(3) . . ?
C5 C6 H6A 127.1 . . ?
N3 C6 H6A 127.1 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.235
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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_c2c
_database_code_depnum_ccdc_archive 'CCDC 1028860'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H8 Cl Co0.50 N4 O7 S'
_chemical_formula_sum            'C6 H8 Cl Co0.50 N4 O7 S'
_chemical_formula_weight         345.14

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'
Co Co 0.3494 0.9721 '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
_symmetry_space_group_name_Hall  -C2yc

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                   10.184(2)
_cell_length_b                   16.442(3)
_cell_length_c                   14.923(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.55(3)
_cell_angle_gamma                90.00
_cell_volume                     2464.2(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2801
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.750
_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            11194
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         27.42
_reflns_number_total             2801
_reflns_number_gt                1974
_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  ?

_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)+(0.0383P)²+5.5054P] 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         2801
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Co1 Co 0.5000 0.34623(4) 0.2500 0.0310(2) Uani 1 2 d S . .
Cl1 Cl 0.76174(9) 0.56914(6) 0.06246(6) 0.0418(3) Uani 1 1 d . . .
S1 S 0.55552(9) 0.22057(7) -0.09823(6) 0.0413(3) Uani 1 1 d . . .
O1 O 0.6643(2) 0.1733(2) -0.11601(18) 0.0567(9) Uani 1 1 d . . .
O2 O 0.5325(3) 0.30215(19) -0.12409(17) 0.0542(8) Uani 1 1 d . . .
O3 O 0.8705(4) 0.5228(2) 0.0409(3) 0.0888(12) Uani 1 1 d . . .
O4 O 0.7590(4) 0.5686(3) 0.1574(2) 0.1009(14) Uani 1 1 d . . .
O5 O 0.6402(3) 0.5347(2) 0.0158(2) 0.0863(12) Uani 1 1 d . . .
O6 O 0.7726(3) 0.65066(17) 0.0322(2) 0.0560(8) Uani 1 1 d . . .
O7 O 0.5201(3) 0.4439(2) 0.15741(19) 0.0557(9) Uani 1 1 d . . .
H7A H 0.4642 0.4387 0.1114 0.084 Uiso 1 1 calc R . .
N1 N 0.5320(3) 0.2584(2) 0.14980(18) 0.0355(7) Uani 1 1 d . . .
N2 N 0.5591(3) 0.21695(19) 0.01384(18) 0.0350(7) Uani 1 1 d . . .
N3 N 0.4184(3) 0.1696(2) -0.14220(18) 0.0362(7) Uani 1 1 d . . .
N4 N 0.2083(3) 0.14458(19) -0.19654(18) 0.0341(7) Uani 1 1 d . . .
C1 C 0.5108(3) 0.2767(2) 0.0634(2) 0.0381(9) Uani 1 1 d . . .
H1B H 0.4687 0.3238 0.0389 0.046 Uiso 1 1 calc R . .
C2 C 0.6131(4) 0.1565(2) 0.0739(2) 0.0422(9) Uani 1 1 d . . .
H2B H 0.6528 0.1082 0.0601 0.051 Uiso 1 1 calc R . .
C3 C 0.5953(4) 0.1832(2) 0.1563(2) 0.0402(9) Uani 1 1 d . . .
H3A H 0.6217 0.1551 0.2104 0.048 Uiso 1 1 calc R . .
C4 C 0.2927(3) 0.2016(2) -0.1660(2) 0.0363(8) Uani 1 1 d . . .
H4C H 0.2710 0.2561 -0.1610 0.044 Uiso 1 1 calc R . .
C5 C 0.2803(4) 0.0727(3) -0.1912(3) 0.0439(9) Uani 1 1 d . . .
H5B H 0.2444 0.0219 -0.2079 0.053 Uiso 1 1 calc R . .
C6 C 0.4092(4) 0.0867(3) -0.1585(2) 0.0438(9) Uani 1 1 d . . .
H6B H 0.4778 0.0488 -0.1489 0.053 Uiso 1 1 calc R . .
H7B H 0.578(6) 0.469(4) 0.151(4) 0.12(3) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 2.142(3) . ?
Co1 N1 2.142(3) 2_655 ?
Co1 N4 2.144(3) 8_556 ?
Co1 N4 2.144(3) 7 ?
Co1 O7 2.150(3) 2_655 ?
Co1 O7 2.150(3) . ?
Cl1 O4 1.422(3) . ?
Cl1 O6 1.424(3) . ?
Cl1 O3 1.425(3) . ?
Cl1 O5 1.433(3) . ?
S1 O2 1.405(3) . ?
S1 O1 1.414(3) . ?
S1 N3 1.667(3) . ?
S1 N2 1.668(3) . ?
O7 H7A 0.8200 . ?
O7 H7B 0.74(6) . ?
N1 C1 1.307(4) . ?
N1 C3 1.391(5) . ?
N2 C1 1.369(4) . ?
N2 C2 1.389(5) . ?
N3 C4 1.375(4) . ?
N3 C6 1.385(5) . ?
N4 C4 1.301(4) . ?
N4 C5 1.386(5) . ?
N4 Co1 2.144(3) 7 ?
C1 H1B 0.9300 . ?
C2 C3 1.346(5) . ?
C2 H2B 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4C 0.9300 . ?
C5 C6 1.342(5) . ?
C5 H5B 0.9300 . ?
C6 H6B 0.9300 . ?

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 Co1 N1 95.26(17) . 2_655 ?
N1 Co1 N4 92.96(11) . 8_556 ?
N1 Co1 N4 92.49(11) 2_655 8_556 ?
N1 Co1 N4 92.49(11) . 7 ?
N1 Co1 N4 92.96(11) 2_655 7 ?
N4 Co1 N4 171.92(17) 8_556 7 ?
N1 Co1 O7 173.55(12) . 2_655 ?
N1 Co1 O7 90.74(12) 2_655 2_655 ?
N4 Co1 O7 84.38(12) 8_556 2_655 ?
N4 Co1 O7 89.58(12) 7 2_655 ?
N1 Co1 O7 90.74(12) . . ?
N1 Co1 O7 173.55(12) 2_655 . ?
N4 Co1 O7 89.58(12) 8_556 . ?
N4 Co1 O7 84.38(12) 7 . ?
O7 Co1 O7 83.37(18) 2_655 . ?
O4 Cl1 O6 109.7(2) . . ?
O4 Cl1 O3 111.5(3) . . ?
O6 Cl1 O3 109.2(2) . . ?
O4 Cl1 O5 108.9(2) . . ?
O6 Cl1 O5 108.9(2) . . ?
O3 Cl1 O5 108.7(2) . . ?
O2 S1 O1 125.02(19) . . ?
O2 S1 N3 106.34(17) . . ?
O1 S1 N3 106.30(17) . . ?
O2 S1 N2 106.53(16) . . ?
O1 S1 N2 106.31(16) . . ?
N3 S1 N2 104.74(14) . . ?
Co1 O7 H7A 109.5 . . ?
Co1 O7 H7B 132(5) . . ?
H7A O7 H7B 113.9 . . ?
C1 N1 C3 105.8(3) . . ?
C1 N1 Co1 121.0(3) . . ?
C3 N1 Co1 132.3(2) . . ?
C1 N2 C2 107.7(3) . . ?
C1 N2 S1 124.5(3) . . ?
C2 N2 S1 127.8(3) . . ?
C4 N3 C6 107.3(3) . . ?
C4 N3 S1 126.4(3) . . ?
C6 N3 S1 126.3(3) . . ?
C4 N4 C5 106.3(3) . . ?
C4 N4 Co1 129.4(3) . 7 ?
C5 N4 Co1 124.3(2) . 7 ?
N1 C1 N2 110.7(3) . . ?
N1 C1 H1B 124.7 . . ?
N2 C1 H1B 124.7 . . ?
C3 C2 N2 104.9(3) . . ?
C3 C2 H2B 127.5 . . ?
N2 C2 H2B 127.5 . . ?
C2 C3 N1 110.9(3) . . ?
C2 C3 H3A 124.5 . . ?
N1 C3 H3A 124.5 . . ?
N4 C4 N3 110.4(3) . . ?
N4 C4 H4C 124.8 . . ?
N3 C4 H4C 124.8 . . ?
C6 C5 N4 110.5(4) . . ?
C6 C5 H5B 124.7 . . ?
N4 C5 H5B 124.7 . . ?
C5 C6 N3 105.5(3) . . ?
C5 C6 H6B 127.3 . . ?
N3 C6 H6B 127.3 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.078
####################################################################### 
# 
# 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_c2c
_database_code_depnum_ccdc_archive 'CCDC 1028861'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C11 H15 Cl N4 O11 S Zn'
_chemical_formula_sum            'C11 H13 Cl N4 O11 S Zn'
_chemical_formula_weight         512.13

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   9.6762(5)
_cell_length_b                   23.2403(15)
_cell_length_c                   16.8723(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.630(4)
_cell_angle_gamma                90.00
_cell_volume                     3716.3(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3318
_cell_measurement_theta_min      1.75
_cell_measurement_theta_max      25.18

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.644
_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            10469
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.18
_reflns_number_total             3318
_reflns_number_gt                2591
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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+3.5123P] 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         3318
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0873
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Zn1 Zn -0.5000 -0.35020(2) 0.2500 0.02473(15) Uani 1 2 d S . .
Zn2 Zn -0.5000 0.02514(2) 0.2500 0.02674(15) Uani 1 2 d S . .
S1 S -0.76960(10) -0.16550(3) 0.06146(5) 0.0393(2) Uani 1 1 d . . .
O1 O -0.9115(3) -0.16552(10) 0.01962(17) 0.0597(8) Uani 1 1 d . . .
O2 O -0.6518(3) -0.16488(10) 0.02410(16) 0.0540(7) Uani 1 1 d . . .
O3 O -0.5613(2) -0.39262(9) 0.33814(12) 0.0278(5) Uani 1 1 d . . .
O4 O -0.3535(2) -0.43128(10) 0.33810(14) 0.0417(6) Uani 1 1 d . . .
O5 O -0.4105(2) 0.02933(11) 0.14379(14) 0.0402(6) Uani 1 1 d . . .
O6 O -0.6453(2) 0.09035(10) 0.20013(17) 0.0368(6) Uani 1 1 d . . .
H6A H -0.6971 0.0976 0.2317 0.055 Uiso 1 1 calc R . .
H6D H -0.641(4) 0.1081(17) 0.165(2) 0.042(13) Uiso 1 1 d . . .
O7 O 0.6412(3) 0.16571(11) 0.70073(17) 0.0530(7) Uani 1 1 d . . .
O8 O 0.6813(3) 0.11738(14) 0.5877(2) 0.0827(10) Uani 1 1 d . . .
O9 O 0.6779(3) 0.21785(14) 0.5896(2) 0.0772(10) Uani 1 1 d . . .
O10 O 0.8654(3) 0.16777(14) 0.6690(2) 0.0754(10) Uani 1 1 d . . .
O11 O -0.6530(4) 0.17707(14) 0.0901(2) 0.0784(10) Uani 1 1 d . . .
N1 N -0.6505(3) -0.03786(11) 0.19912(16) 0.0308(6) Uani 1 1 d . . .
N2 N -0.7498(3) -0.10997(10) 0.12535(16) 0.0326(6) Uani 1 1 d . . .
N3 N -0.7513(3) -0.22274(10) 0.12213(16) 0.0306(6) Uani 1 1 d . . .
N4 N -0.6519(3) -0.29403(11) 0.19685(15) 0.0286(6) Uani 1 1 d . . .
C1 C -0.6294(3) -0.07818(13) 0.1498(2) 0.0322(7) Uani 1 1 d . . .
H1B H -0.5446 -0.0846 0.1334 0.039 Uiso 1 1 calc R . .
C2 C -0.8517(3) -0.08800(14) 0.1646(2) 0.0386(8) Uani 1 1 d . . .
H2B H -0.9435 -0.1011 0.1609 0.046 Uiso 1 1 calc R . .
C3 C -0.7890(3) -0.04391(14) 0.2088(2) 0.0371(8) Uani 1 1 d . . .
H3A H -0.8322 -0.0206 0.2414 0.044 Uiso 1 1 calc R . .
C4 C -0.6286(3) -0.25130(13) 0.15204(19) 0.0313(7) Uani 1 1 d . . .
H4A H -0.5408 -0.2415 0.1417 0.038 Uiso 1 1 calc R . .
C5 C -0.7955(4) -0.29359(16) 0.1960(2) 0.0467(9) Uani 1 1 d . . .
H5A H -0.8420 -0.3199 0.2229 0.056 Uiso 1 1 calc R . .
C6 C -0.8573(4) -0.24991(15) 0.1511(3) 0.0490(10) Uani 1 1 d . . .
H6B H -0.9523 -0.2399 0.1413 0.059 Uiso 1 1 calc R . .
C7 C -0.4616(3) -0.42755(13) 0.36710(17) 0.0253(6) Uani 1 1 d . . .
C8 C -0.4812(3) -0.46433(12) 0.43678(17) 0.0240(6) Uani 1 1 d . . .
C9 C -0.5903(3) -0.45364(13) 0.47701(18) 0.0276(7) Uani 1 1 d . . .
H9 H -0.6507 -0.4227 0.4617 0.080 Uiso 1 1 calc . . .
C10 C -0.3909(3) -0.51109(13) 0.46039(18) 0.0290(7) Uani 1 1 d . . .
H10 H -0.3177 -0.5184 0.4336 0.080 Uiso 1 1 calc . . .
C11 C -0.4770(6) 0.0514(3) 0.0679(3) 0.121(3) Uani 1 1 d . . .
H11A H -0.4144 0.0481 0.0307 0.181 Uiso 1 1 calc R . .
H11B H -0.5004 0.0911 0.0736 0.181 Uiso 1 1 calc R . .
H11C H -0.5616 0.0300 0.0478 0.181 Uiso 1 1 calc R . .
Cl1 Cl 0.71879(9) 0.16702(4) 0.63711(6) 0.0427(2) 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
Zn1 O3 1.9724(19) 2_455 ?
Zn1 O3 1.9724(19) . ?
Zn1 N4 2.034(3) 2_455 ?
Zn1 N4 2.034(3) . ?
Zn2 N1 2.121(3) . ?
Zn2 N1 2.121(3) 2_455 ?
Zn2 O6 2.122(2) 2_455 ?
Zn2 O6 2.122(2) . ?
Zn2 O5 2.144(2) 2_455 ?
Zn2 O5 2.144(2) . ?
S1 O2 1.409(3) . ?
S1 O1 1.412(3) . ?
S1 N3 1.666(3) . ?
S1 N2 1.668(3) . ?
O3 C7 1.280(3) . ?
O4 C7 1.244(3) . ?
O5 C11 1.408(6) . ?
O6 H6A 0.8200 . ?
O6 H6D 0.73(4) . ?
O7 Cl1 1.429(3) . ?
O8 Cl1 1.427(3) . ?
O9 Cl1 1.438(3) . ?
O10 Cl1 1.412(3) . ?
N1 C1 1.296(4) . ?
N1 C3 1.390(4) . ?
N2 C1 1.371(4) . ?
N2 C2 1.390(4) . ?
N3 C4 1.365(4) . ?
N3 C6 1.375(4) . ?
N4 C4 1.295(4) . ?
N4 C5 1.387(4) . ?
C1 H1B 0.9300 . ?
C2 C3 1.339(5) . ?
C2 H2B 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.334(5) . ?
C5 H5A 0.9300 . ?
C6 H6B 0.9300 . ?
C7 C8 1.496(4) . ?
C8 C9 1.388(4) . ?
C8 C10 1.400(4) . ?
C9 C10 1.378(4) 5_446 ?
C9 H9 0.9300 . ?
C10 C9 1.378(4) 5_446 ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 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
O3 Zn1 O3 120.02(12) 2_455 . ?
O3 Zn1 N4 110.67(9) 2_455 2_455 ?
O3 Zn1 N4 106.78(9) . 2_455 ?
O3 Zn1 N4 106.78(9) 2_455 . ?
O3 Zn1 N4 110.67(9) . . ?
N4 Zn1 N4 100.15(14) 2_455 . ?
N1 Zn2 N1 92.68(14) . 2_455 ?
N1 Zn2 O6 178.07(9) . 2_455 ?
N1 Zn2 O6 89.23(9) 2_455 2_455 ?
N1 Zn2 O6 89.23(9) . . ?
N1 Zn2 O6 178.07(10) 2_455 . ?
O6 Zn2 O6 88.86(13) 2_455 . ?
N1 Zn2 O5 90.56(10) . 2_455 ?
N1 Zn2 O5 93.04(10) 2_455 2_455 ?
O6 Zn2 O5 89.02(10) 2_455 2_455 ?
O6 Zn2 O5 87.26(10) . 2_455 ?
N1 Zn2 O5 93.04(10) . . ?
N1 Zn2 O5 90.56(10) 2_455 . ?
O6 Zn2 O5 87.26(10) 2_455 . ?
O6 Zn2 O5 89.02(10) . . ?
O5 Zn2 O5 174.79(14) 2_455 . ?
O2 S1 O1 124.69(18) . . ?
O2 S1 N3 106.72(15) . . ?
O1 S1 N3 106.21(15) . . ?
O2 S1 N2 106.47(15) . . ?
O1 S1 N2 107.26(15) . . ?
N3 S1 N2 103.68(14) . . ?
C7 O3 Zn1 106.69(17) . . ?
C11 O5 Zn2 126.1(3) . . ?
Zn2 O6 H6A 109.5 . . ?
Zn2 O6 H6D 125(3) . . ?
H6A O6 H6D 123.7 . . ?
C1 N1 C3 106.4(3) . . ?
C1 N1 Zn2 125.1(2) . . ?
C3 N1 Zn2 128.5(2) . . ?
C1 N2 C2 107.4(3) . . ?
C1 N2 S1 126.3(2) . . ?
C2 N2 S1 126.3(2) . . ?
C4 N3 C6 107.5(3) . . ?
C4 N3 S1 126.3(2) . . ?
C6 N3 S1 126.2(2) . . ?
C4 N4 C5 106.3(3) . . ?
C4 N4 Zn1 123.7(2) . . ?
C5 N4 Zn1 130.0(2) . . ?
N1 C1 N2 110.4(3) . . ?
N1 C1 H1B 124.8 . . ?
N2 C1 H1B 124.8 . . ?
C3 C2 N2 105.2(3) . . ?
C3 C2 H2B 127.4 . . ?
N2 C2 H2B 127.4 . . ?
C2 C3 N1 110.6(3) . . ?
C2 C3 H3A 124.7 . . ?
N1 C3 H3A 124.7 . . ?
N4 C4 N3 110.4(3) . . ?
N4 C4 H4A 124.8 . . ?
N3 C4 H4A 124.8 . . ?
C6 C5 N4 110.2(3) . . ?
C6 C5 H5A 124.9 . . ?
N4 C5 H5A 124.9 . . ?
C5 C6 N3 105.7(3) . . ?
C5 C6 H6B 127.2 . . ?
N3 C6 H6B 127.2 . . ?
O4 C7 O3 121.5(3) . . ?
O4 C7 C8 121.2(3) . . ?
O3 C7 C8 117.2(3) . . ?
C9 C8 C10 119.5(3) . . ?
C9 C8 C7 120.7(3) . . ?
C10 C8 C7 119.8(3) . . ?
C10 C9 C8 120.0(3) 5_446 . ?
C10 C9 H9 120.0 5_446 . ?
C8 C9 H9 120.0 . . ?
C9 C10 C8 120.6(3) 5_446 . ?
C9 C10 H10 119.7 5_446 . ?
C8 C10 H10 119.7 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O10 Cl1 O8 110.5(2) . . ?
O10 Cl1 O7 110.7(2) . . ?
O8 Cl1 O7 108.17(19) . . ?
O10 Cl1 O9 110.1(2) . . ?
O8 Cl1 O9 109.2(2) . . ?
O7 Cl1 O9 108.04(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6A O3 0.82 2.41 2.810(3) 111.2 4_355

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.18
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 1028862'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H6 Cd N10 O2 S'
_chemical_formula_sum            'C6 H6 Cd N10 O2 S'
_chemical_formula_weight         394.69

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
_symmetry_space_group_name_Hall  -P1

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

_cell_length_a                   6.6171(4)
_cell_length_b                   10.0019(6)
_cell_length_c                   10.9248(7)
_cell_angle_alpha                64.702(3)
_cell_angle_beta                 80.817(4)
_cell_angle_gamma                88.608(4)
_cell_volume                     644.54(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2244
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             384
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_T_max  0.587
_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            3614
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2244
_reflns_number_gt                2136
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0395P)²+0.2341P] 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         2244
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0625
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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 0.76726(3) 0.488235(19) 0.428724(17) 0.02571(10) Uani 1 1 d . . .
S1 S 0.62434(11) 0.79416(8) -0.15541(7) 0.03213(17) Uani 1 1 d . . .
O1 O 0.5754(4) 0.9433(3) -0.2241(2) 0.0478(6) Uani 1 1 d . . .
O2 O 0.4949(3) 0.6708(3) -0.1277(2) 0.0457(6) Uani 1 1 d . . .
N1 N 0.7322(4) 0.6659(3) 0.2072(2) 0.0322(5) Uani 1 1 d . . .
N2 N 0.6849(4) 0.7746(2) -0.0071(2) 0.0287(5) Uani 1 1 d . . .
N3 N 0.8459(4) 0.7716(3) -0.2390(2) 0.0320(5) Uani 1 1 d . . .
N4 N 1.0808(4) 0.6678(3) -0.3307(3) 0.0356(6) Uani 1 1 d . . .
N5 N 0.5591(4) 0.6244(3) 0.5241(3) 0.0391(6) Uani 1 1 d . . .
N6 N 0.6148(4) 0.7422(3) 0.5065(3) 0.0332(6) Uani 1 1 d . . .
N7 N 0.6746(5) 0.8573(3) 0.4901(4) 0.0547(8) Uani 1 1 d . . .
N8 N 0.9185(4) 0.3631(3) 0.6205(3) 0.0381(6) Uani 1 1 d . . .
N9 N 0.8308(4) 0.3114(3) 0.7365(3) 0.0348(6) Uani 1 1 d . . .
N10 N 0.7512(5) 0.2633(4) 0.8489(3) 0.0582(9) Uani 1 1 d . . .
C1 C 0.6911(4) 0.6429(3) 0.1056(3) 0.0315(6) Uani 1 1 d . . .
H1B H 0.6689 0.5500 0.1087 0.038 Uiso 1 1 calc R . .
C2 C 0.7519(5) 0.8182(3) 0.1608(3) 0.0370(7) Uani 1 1 d . . .
H2B H 0.7802 0.8660 0.2132 0.044 Uiso 1 1 calc R . .
C3 C 0.7244(5) 0.8869(3) 0.0294(3) 0.0344(6) Uani 1 1 d . . .
H3A H 0.7307 0.9883 -0.0256 0.041 Uiso 1 1 calc R . .
C4 C 0.9019(5) 0.6456(3) -0.2540(3) 0.0345(6) Uani 1 1 d . . .
H4B H 0.8232 0.5572 -0.2149 0.041 Uiso 1 1 calc R . .
C5 C 1.0023(5) 0.8786(3) -0.3133(3) 0.0397(7) Uani 1 1 d . . .
H5B H 1.0078 0.9755 -0.3232 0.048 Uiso 1 1 calc R . .
C6 C 1.1438(5) 0.8130(4) -0.3679(3) 0.0409(7) Uani 1 1 d . . .
H6A H 1.2673 0.8585 -0.4231 0.049 Uiso 1 1 calc R . .


_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 N8 2.308(2) . ?
Cd1 N5 2.338(3) 2_666 ?
Cd1 N5 2.346(3) . ?
Cd1 N1 2.356(2) . ?
Cd1 N4 2.366(3) 2_765 ?
Cd1 N8 2.436(3) 2_766 ?
Cd1 Cd1 3.6750(4) 2_666 ?
Cd1 Cd1 3.7212(4) 2_766 ?
S1 O1 1.410(2) . ?
S1 O2 1.413(2) . ?
S1 N2 1.661(2) . ?
S1 N3 1.663(2) . ?
N1 C1 1.295(4) . ?
N1 C2 1.387(4) . ?
N2 C1 1.372(4) . ?
N2 C3 1.384(4) . ?
N3 C4 1.374(4) . ?
N3 C5 1.385(4) . ?
N4 C4 1.300(4) . ?
N4 C6 1.385(4) . ?
N4 Cd1 2.366(3) 2_765 ?
N5 N6 1.169(4) . ?
N5 Cd1 2.338(3) 2_666 ?
N6 N7 1.157(4) . ?
N8 N9 1.195(4) . ?
N8 Cd1 2.436(3) 2_766 ?
N9 N10 1.148(4) . ?
C1 H1B 0.9300 . ?
C2 C3 1.342(4) . ?
C2 H2B 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4B 0.9300 . ?
C5 C6 1.338(5) . ?
C5 H5B 0.9300 . ?
C6 H6A 0.9300 . ?

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
N8 Cd1 N5 106.78(10) . 2_666 ?
N8 Cd1 N5 94.83(10) . . ?
N5 Cd1 N5 76.62(11) 2_666 . ?
N8 Cd1 N1 158.39(9) . . ?
N5 Cd1 N1 94.82(10) 2_666 . ?
N5 Cd1 N1 89.71(10) . . ?
N8 Cd1 N4 90.13(10) . 2_765 ?
N5 Cd1 N4 92.96(9) 2_666 2_765 ?
N5 Cd1 N4 169.38(9) . 2_765 ?
N1 Cd1 N4 89.09(9) . 2_765 ?
N8 Cd1 N8 76.69(10) . 2_766 ?
N5 Cd1 N8 171.70(9) 2_666 2_766 ?
N5 Cd1 N8 95.70(9) . 2_766 ?
N1 Cd1 N8 81.85(8) . 2_766 ?
N4 Cd1 N8 94.57(9) 2_765 2_766 ?
N8 Cd1 Cd1 103.74(7) . 2_666 ?
N5 Cd1 Cd1 38.39(7) 2_666 2_666 ?
N5 Cd1 Cd1 38.23(6) . 2_666 ?
N1 Cd1 Cd1 92.88(6) . 2_666 ?
N4 Cd1 Cd1 131.32(7) 2_765 2_666 ?
N8 Cd1 Cd1 133.86(7) 2_766 2_666 ?
N8 Cd1 Cd1 39.57(7) . 2_766 ?
N5 Cd1 Cd1 145.77(7) 2_666 2_766 ?
N5 Cd1 Cd1 96.74(7) . 2_766 ?
N1 Cd1 Cd1 118.93(6) . 2_766 ?
N4 Cd1 Cd1 93.07(7) 2_765 2_766 ?
N8 Cd1 Cd1 37.12(6) 2_766 2_766 ?
Cd1 Cd1 Cd1 126.929(10) 2_666 2_766 ?
O1 S1 O2 124.74(15) . . ?
O1 S1 N2 106.29(13) . . ?
O2 S1 N2 107.40(13) . . ?
O1 S1 N3 107.59(14) . . ?
O2 S1 N3 105.93(13) . . ?
N2 S1 N3 102.90(12) . . ?
C1 N1 C2 106.4(2) . . ?
C1 N1 Cd1 127.8(2) . . ?
C2 N1 Cd1 125.77(19) . . ?
C1 N2 C3 107.3(2) . . ?
C1 N2 S1 125.7(2) . . ?
C3 N2 S1 126.82(19) . . ?
C4 N3 C5 107.3(2) . . ?
C4 N3 S1 126.1(2) . . ?
C5 N3 S1 126.5(2) . . ?
C4 N4 C6 106.4(3) . . ?
C4 N4 Cd1 126.3(2) . 2_765 ?
C6 N4 Cd1 125.9(2) . 2_765 ?
N6 N5 Cd1 132.5(2) . 2_666 ?
N6 N5 Cd1 120.3(2) . . ?
Cd1 N5 Cd1 103.38(11) 2_666 . ?
N7 N6 N5 178.3(3) . . ?
N9 N8 Cd1 125.3(2) . . ?
N9 N8 Cd1 116.7(2) . 2_766 ?
Cd1 N8 Cd1 103.31(10) . 2_766 ?
N10 N9 N8 178.0(3) . . ?
N1 C1 N2 110.5(2) . . ?
N1 C1 H1B 124.7 . . ?
N2 C1 H1B 124.7 . . ?
C3 C2 N1 110.4(3) . . ?
C3 C2 H2B 124.8 . . ?
N1 C2 H2B 124.8 . . ?
C2 C3 N2 105.4(2) . . ?
C2 C3 H3A 127.3 . . ?
N2 C3 H3A 127.3 . . ?
N4 C4 N3 110.3(3) . . ?
N4 C4 H4B 124.9 . . ?
N3 C4 H4B 124.9 . . ?
C6 C5 N3 105.5(3) . . ?
C6 C5 H5B 127.3 . . ?
N3 C5 H5B 127.3 . . ?
C5 C6 N4 110.5(3) . . ?
C5 C6 H6A 124.7 . . ?
N4 C6 H6A 124.7 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 1028863'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C3 H3 Mn0.50 N5 O S0.50'
_chemical_formula_sum            'C3 H3 Mn0.50 N5 O S0.50'
_chemical_formula_weight         168.60

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_Hall  -P2ac2n

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

_cell_length_a                   9.3444(19)
_cell_length_b                   17.647(4)
_cell_length_c                   7.3560(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1213.0(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1439
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_T_max  0.732
_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            11268
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1439
_reflns_number_gt                1317
_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  ?

_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)+(0.0229P)²+0.9967P] 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         1439
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0576
_refine_ls_wR_factor_gt          0.0565
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Mn1 Mn 0.5000 0.5000 0.5000 0.00958(10) Uani 1 2 d S . .
S1 S 0.70952(5) 0.7500 0.04243(7) 0.01192(12) Uani 1 2 d S . .
O1 O 0.82946(16) 0.7500 0.1593(2) 0.0173(3) Uani 1 2 d S . .
O2 O 0.71571(17) 0.7500 -0.1489(2) 0.0178(3) Uani 1 2 d S . .
N1 N 0.52557(13) 0.58287(7) 0.26956(17) 0.0125(3) Uani 1 1 d . . .
N2 N 0.60859(13) 0.67643(7) 0.10303(16) 0.0113(2) Uani 1 1 d . . .
N4 N 0.66271(14) 0.56778(8) 0.64472(17) 0.0176(3) Uani 1 1 d . . .
N5 N 0.74516(12) 0.56827(7) 0.76521(16) 0.0117(3) Uani 1 1 d . . .
C1 C 0.61593(15) 0.63912(8) 0.2661(2) 0.0129(3) Uani 1 1 d . . .
H1A H 0.6769 0.6521 0.3611 0.016 Uiso 1 1 calc R . .
C2 C 0.50409(16) 0.64110(9) -0.0018(2) 0.0140(3) Uani 1 1 d . . .
H2A H 0.4744 0.6541 -0.1184 0.017 Uiso 1 1 calc R . .
C3 C 0.45526(15) 0.58378(8) 0.1028(2) 0.0131(3) Uani 1 1 d . . .
H3A H 0.3845 0.5497 0.0682 0.016 Uiso 1 1 calc R . .
N3 N 0.82641(14) 0.57194(7) 0.88618(18) 0.0177(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
Mn1 N4 2.2081(13) 5_666 ?
Mn1 N4 2.2081(13) . ?
Mn1 N3 2.2235(13) 6_557 ?
Mn1 N3 2.2235(13) 2_664 ?
Mn1 N1 2.2515(13) . ?
Mn1 N1 2.2515(13) 5_666 ?
S1 O2 1.4088(16) . ?
S1 O1 1.4125(16) . ?
S1 N2 1.6654(12) 7_575 ?
S1 N2 1.6654(12) . ?
N1 C1 1.3035(19) . ?
N1 C3 1.3918(19) . ?
N2 C1 1.3702(18) . ?
N2 C2 1.3917(19) . ?
N4 N5 1.1744(17) . ?
N5 N3 1.1715(17) . ?
C1 H1A 0.9300 . ?
C2 C3 1.350(2) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
N3 Mn1 2.2235(13) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Mn1 N4 180 5_666 . ?
N4 Mn1 N3 89.34(5) 5_666 6_557 ?
N4 Mn1 N3 90.66(5) . 6_557 ?
N4 Mn1 N3 90.66(5) 5_666 2_664 ?
N4 Mn1 N3 89.34(5) . 2_664 ?
N3 Mn1 N3 180 6_557 2_664 ?
N4 Mn1 N1 93.55(5) 5_666 . ?
N4 Mn1 N1 86.45(5) . . ?
N3 Mn1 N1 89.43(5) 6_557 . ?
N3 Mn1 N1 90.57(5) 2_664 . ?
N4 Mn1 N1 86.45(5) 5_666 5_666 ?
N4 Mn1 N1 93.55(5) . 5_666 ?
N3 Mn1 N1 90.57(5) 6_557 5_666 ?
N3 Mn1 N1 89.43(5) 2_664 5_666 ?
N1 Mn1 N1 180 . 5_666 ?
O2 S1 O1 125.13(10) . . ?
O2 S1 N2 106.90(6) . 7_575 ?
O1 S1 N2 106.65(6) . 7_575 ?
O2 S1 N2 106.90(6) . . ?
O1 S1 N2 106.65(6) . . ?
N2 S1 N2 102.44(9) 7_575 . ?
C1 N1 C3 106.25(12) . . ?
C1 N1 Mn1 125.31(10) . . ?
C3 N1 Mn1 128.40(10) . . ?
C1 N2 C2 107.76(12) . . ?
C1 N2 S1 125.49(10) . . ?
C2 N2 S1 126.75(10) . . ?
N5 N4 Mn1 145.04(11) . . ?
N3 N5 N4 177.21(15) . . ?
N1 C1 N2 110.52(13) . . ?
N1 C1 H1A 124.7 . . ?
N2 C1 H1A 124.7 . . ?
C3 C2 N2 104.90(13) . . ?
C3 C2 H2A 127.6 . . ?
N2 C2 H2A 127.6 . . ?
C2 C3 N1 110.57(13) . . ?
C2 C3 H3A 124.7 . . ?
N1 C3 H3A 124.7 . . ?
N5 N3 Mn1 136.66(11) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.059
####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 1028864'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C6 H6 Cl0 N4 Ni0.50 O4 S1.50'
_chemical_formula_sum            'C6 H6 Cl0 N4 Ni0.50 O4 S1.50'
_chemical_formula_weight         275.59

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   17.052(3)
_cell_length_b                   10.831(2)
_cell_length_c                   12.777(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.06(3)
_cell_angle_gamma                90.00
_cell_volume                     2062.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2344
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_T_max  0.728
_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            9960
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         27.47
_reflns_number_total             2344
_reflns_number_gt                1782
_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  ?

_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)+(0.0357P)²+1.7479P] 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         2344
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0904
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Ni1 Ni 0.5000 0.0000 1.0000 0.02089(14) Uani 1 2 d S . .
S1 S 0.36511(5) -0.49518(7) 0.87877(7) 0.03383(19) Uani 1 1 d . . .
S2 S 0.5000 0.11661(8) 1.2500 0.0244(2) Uani 1 2 d S . .
O1 O 0.33589(15) -0.5760(2) 0.9395(2) 0.0495(6) Uani 1 1 d . . .
O2 O 0.43363(14) -0.52245(19) 0.8510(2) 0.0478(6) Uani 1 1 d . . .
O3 O 0.49529(13) 0.03582(19) 1.15509(17) 0.0363(5) Uani 1 1 d . . .
O4 O 0.41941(17) 0.1912(2) 1.2022(2) 0.0645(8) Uani 1 1 d . . .
N1 N 0.45361(14) -0.1788(2) 1.0098(2) 0.0285(5) Uani 1 1 d . . .
N2 N 0.39413(15) -0.3636(2) 0.9549(2) 0.0306(5) Uani 1 1 d . . .
N3 N 0.27490(14) -0.4572(2) 0.7511(2) 0.0324(6) Uani 1 1 d . . .
N4 N 0.13567(14) -0.4524(2) 0.6064(2) 0.0272(5) Uani 1 1 d . . .
C1 C 0.44669(18) -0.2738(2) 0.9447(2) 0.0286(6) Uani 1 1 d . . .
H1A H 0.4739 -0.2804 0.8970 0.034 Uiso 1 1 calc R . .
C2 C 0.3668(3) -0.3204(3) 1.0330(4) 0.0565(10) Uani 1 1 d . . .
H2A H 0.3302 -0.3605 1.0574 0.068 Uiso 1 1 calc R . .
C3 C 0.4041(2) -0.2079(3) 1.0669(4) 0.0555(10) Uani 1 1 d . . .
H3A H 0.3977 -0.1567 1.1208 0.067 Uiso 1 1 calc R . .
C4 C 0.18833(17) -0.4935(3) 0.7134(2) 0.0303(6) Uani 1 1 d . . .
H4A H 0.1699 -0.5410 0.7581 0.036 Uiso 1 1 calc R . .
C5 C 0.18862(18) -0.3865(3) 0.5713(3) 0.0368(7) Uani 1 1 d . . .
H5A H 0.1676 -0.3463 0.4982 0.044 Uiso 1 1 calc R . .
C6 C 0.27459(19) -0.3889(3) 0.6579(3) 0.0408(8) Uani 1 1 d . . .
H6A H 0.3235 -0.3529 0.6564 0.049 Uiso 1 1 calc R . .


_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
Ni1 O3 2.0586(19) 5_657 ?
Ni1 O3 2.0586(19) . ?
Ni1 N4 2.100(2) 8_546 ?
Ni1 N4 2.100(2) 4_556 ?
Ni1 N1 2.119(2) . ?
Ni1 N1 2.119(2) 5_657 ?
S1 O2 1.408(2) . ?
S1 O1 1.412(2) . ?
S1 N2 1.660(2) . ?
S1 N3 1.661(2) . ?
S2 O4 1.449(2) 2_657 ?
S2 O4 1.449(2) . ?
S2 O3 1.4656(19) . ?
S2 O3 1.4656(19) 2_657 ?
N1 C1 1.292(3) . ?
N1 C3 1.393(4) . ?
N2 C1 1.371(3) . ?
N2 C2 1.373(4) . ?
N3 C4 1.369(3) . ?
N3 C6 1.399(4) . ?
N4 C4 1.296(3) . ?
N4 C5 1.386(3) . ?
N4 Ni1 2.100(2) 4_546 ?
C1 H1A 0.9300 . ?
C2 C3 1.345(5) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.341(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?

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 Ni1 O3 180 5_657 . ?
O3 Ni1 N4 91.79(9) 5_657 8_546 ?
O3 Ni1 N4 88.21(9) . 8_546 ?
O3 Ni1 N4 88.21(9) 5_657 4_556 ?
O3 Ni1 N4 91.79(9) . 4_556 ?
N4 Ni1 N4 180 8_546 4_556 ?
O3 Ni1 N1 94.29(9) 5_657 . ?
O3 Ni1 N1 85.71(9) . . ?
N4 Ni1 N1 93.60(9) 8_546 . ?
N4 Ni1 N1 86.40(9) 4_556 . ?
O3 Ni1 N1 85.71(9) 5_657 5_657 ?
O3 Ni1 N1 94.29(9) . 5_657 ?
N4 Ni1 N1 86.40(9) 8_546 5_657 ?
N4 Ni1 N1 93.60(9) 4_556 5_657 ?
N1 Ni1 N1 180 . 5_657 ?
O2 S1 O1 124.50(15) . . ?
O2 S1 N2 106.27(13) . . ?
O1 S1 N2 107.14(14) . . ?
O2 S1 N3 106.88(14) . . ?
O1 S1 N3 106.73(13) . . ?
N2 S1 N3 103.50(12) . . ?
O4 S2 O4 112.2(2) 2_657 . ?
O4 S2 O3 109.94(14) 2_657 . ?
O4 S2 O3 108.95(12) . . ?
O4 S2 O3 108.95(12) 2_657 2_657 ?
O4 S2 O3 109.94(14) . 2_657 ?
O3 S2 O3 106.69(18) . 2_657 ?
S2 O3 Ni1 153.75(14) . . ?
C1 N1 C3 105.5(2) . . ?
C1 N1 Ni1 127.57(18) . . ?
C3 N1 Ni1 125.2(2) . . ?
C1 N2 C2 107.2(2) . . ?
C1 N2 S1 125.2(2) . . ?
C2 N2 S1 127.5(2) . . ?
C4 N3 C6 107.1(2) . . ?
C4 N3 S1 126.9(2) . . ?
C6 N3 S1 125.85(19) . . ?
C4 N4 C5 107.0(2) . . ?
C4 N4 Ni1 125.41(18) . 4_546 ?
C5 N4 Ni1 127.08(18) . 4_546 ?
N1 C1 N2 111.3(2) . . ?
N1 C1 H1A 124.4 . . ?
N2 C1 H1A 124.4 . . ?
C3 C2 N2 105.5(3) . . ?
C3 C2 H2A 127.2 . . ?
N2 C2 H2A 127.2 . . ?
C2 C3 N1 110.4(3) . . ?
C2 C3 H3A 124.8 . . ?
N1 C3 H3A 124.8 . . ?
N4 C4 N3 110.4(2) . . ?
N4 C4 H4A 124.8 . . ?
N3 C4 H4A 124.8 . . ?
C6 C5 N4 110.2(3) . . ?
C6 C5 H5A 124.9 . . ?
N4 C5 H5A 124.9 . . ?
C5 C6 N3 105.3(2) . . ?
C5 C6 H6A 127.3 . . ?
N3 C6 H6A 127.3 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 1028865'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C13 H9 Cd N2 O8 S0.50'
_chemical_formula_sum            'C13 H9 Cd N2 O8 S0.50'
_chemical_formula_weight         449.65

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'
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'
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   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   18.592(4)
_cell_length_b                   8.3621(17)
_cell_length_c                   19.857(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.14(3)
_cell_angle_gamma                90.00
_cell_volume                     3039.0(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3460
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9241
_exptl_absorpt_correction_T_max  1.0000
_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            14563
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.43
_reflns_number_total             3460
_reflns_number_gt                2801
_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  ?

_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)+(0.0312P)²+6.0358P] 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         3460
_refine_ls_number_parameters     222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 -0.070991(14) -0.35556(3) 0.494764(15) 0.02932(10) Uani 1 1 d . . .
S1 S 0.0000 0.02695(18) 0.7500 0.0434(4) Uani 1 2 d S . .
O1 O 0.0527(2) 0.1038(4) 0.71853(16) 0.0638(11) Uani 1 1 d . . .
O2 O -0.10427(16) -0.1155(3) 0.43983(17) 0.0466(8) Uani 1 1 d . . .
O3 O 0.02824(13) -0.3937(3) 0.44707(14) 0.0299(6) Uani 1 1 d . . .
O4 O 0.05500(15) -0.1627(3) 0.50099(15) 0.0395(7) Uani 1 1 d . . .
O5 O 0.30793(14) 0.0537(3) 0.49033(15) 0.0413(7) Uani 1 1 d . . .
O6 O 0.36352(14) -0.0199(3) 0.40627(14) 0.0365(7) Uani 1 1 d . . .
O7 O 0.23626(18) -0.3706(4) 0.22455(18) 0.0604(10) Uani 1 1 d . . .
O8 O 0.12345(15) -0.4566(4) 0.22419(14) 0.0429(7) Uani 1 1 d . . .
N1 N -0.07042(17) -0.2406(4) 0.59771(17) 0.0355(8) Uani 1 1 d . . .
N2 N -0.04457(18) -0.0958(4) 0.69104(16) 0.0345(8) Uani 1 1 d . . .
C1 C -0.0212(2) -0.1487(5) 0.6333(2) 0.0395(10) Uani 1 1 d . . .
H1A H 0.0235 -0.1228 0.6212 0.047 Uiso 1 1 calc R . .
C2 C -0.1136(2) -0.1595(5) 0.6902(2) 0.0468(11) Uani 1 1 d . . .
H2A H -0.1434 -0.1450 0.7227 0.056 Uiso 1 1 calc R . .
C3 C -0.1280(2) -0.2459(6) 0.6329(2) 0.0446(11) Uani 1 1 d . . .
H3A H -0.1711 -0.3022 0.6187 0.054 Uiso 1 1 calc R . .
C4 C -0.1703(3) -0.0851(6) 0.3951(3) 0.0601(14) Uani 1 1 d . . .
H4A H -0.1707 0.0234 0.3793 0.090 Uiso 1 1 calc R . .
H4B H -0.2105 -0.1016 0.4188 0.090 Uiso 1 1 calc R . .
H4C H -0.1748 -0.1565 0.3567 0.090 Uiso 1 1 calc R . .
C5 C 0.12692(19) -0.2426(4) 0.41808(18) 0.0257(8) Uani 1 1 d . . .
C6 C 0.1857(2) -0.1418(4) 0.44301(19) 0.0283(8) Uani 1 1 d . . .
H6A H 0.1860 -0.0855 0.4834 0.034 Uiso 1 1 calc R . .
C7 C 0.24389(19) -0.1251(4) 0.40765(19) 0.0266(8) Uani 1 1 d . . .
C8 C 0.2414(2) -0.2058(5) 0.3466(2) 0.0300(8) Uani 1 1 d . . .
H8A H 0.2801 -0.1955 0.3230 0.036 Uiso 1 1 calc R . .
C9 C 0.18220(19) -0.3025(4) 0.31977(19) 0.0280(8) Uani 1 1 d . . .
C10 C 0.12494(19) -0.3220(4) 0.35623(19) 0.0267(8) Uani 1 1 d . . .
H10A H 0.0856 -0.3879 0.3392 0.032 Uiso 1 1 calc R . .
C11 C 0.30846(19) -0.0231(4) 0.4364(2) 0.0293(8) Uani 1 1 d . . .
C12 C 0.1837(2) -0.3787(5) 0.2522(2) 0.0356(9) Uani 1 1 d . . .
C13 C 0.06652(19) -0.2649(5) 0.45857(19) 0.0288(8) 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
Cd1 O3 2.240(3) . ?
Cd1 N1 2.257(3) . ?
Cd1 O2 2.316(3) . ?
Cd1 O5 2.363(3) 3_445 ?
Cd1 O6 2.388(3) 3_445 ?
Cd1 O3 2.458(3) 5_546 ?
Cd1 C11 2.723(4) 3_445 ?
S1 O1 1.407(3) 2_556 ?
S1 O1 1.407(3) . ?
S1 N2 1.664(3) . ?
S1 N2 1.664(3) 2_556 ?
O2 C4 1.406(5) . ?
O3 C13 1.289(4) . ?
O3 Cd1 2.458(3) 5_546 ?
O4 C13 1.245(4) . ?
O5 C11 1.251(5) . ?
O5 Cd1 2.363(3) 3 ?
O6 C11 1.273(4) . ?
O6 Cd1 2.388(3) 3 ?
O7 C12 1.204(5) . ?
O8 C12 1.330(5) . ?
N1 C1 1.304(5) . ?
N1 C3 1.378(5) . ?
N2 C1 1.369(5) . ?
N2 C2 1.386(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.335(6) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C10 1.391(5) . ?
C5 C6 1.400(5) . ?
C5 C13 1.503(5) . ?
C6 C7 1.396(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.380(5) . ?
C7 C11 1.501(5) . ?
C8 C9 1.394(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.398(5) . ?
C9 C12 1.489(5) . ?
C10 H10A 0.9300 . ?
C11 Cd1 2.723(4) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd1 N1 124.79(11) . . ?
O3 Cd1 O2 95.50(11) . . ?
N1 Cd1 O2 90.91(12) . . ?
O3 Cd1 O5 142.08(9) . 3_445 ?
N1 Cd1 O5 91.32(11) . 3_445 ?
O2 Cd1 O5 94.99(11) . 3_445 ?
O3 Cd1 O6 87.61(9) . 3_445 ?
N1 Cd1 O6 146.28(10) . 3_445 ?
O2 Cd1 O6 95.32(10) . 3_445 ?
O5 Cd1 O6 55.17(9) 3_445 3_445 ?
O3 Cd1 O3 81.66(9) . 5_546 ?
N1 Cd1 O3 89.32(10) . 5_546 ?
O2 Cd1 O3 176.68(9) . 5_546 ?
O5 Cd1 O3 88.32(9) 3_445 5_546 ?
O6 Cd1 O3 86.31(9) 3_445 5_546 ?
O3 Cd1 C11 115.10(11) . 3_445 ?
N1 Cd1 C11 118.49(12) . 3_445 ?
O2 Cd1 C11 96.53(11) . 3_445 ?
O5 Cd1 C11 27.31(10) 3_445 3_445 ?
O6 Cd1 C11 27.88(10) 3_445 3_445 ?
O3 Cd1 C11 86.27(10) 5_546 3_445 ?
O1 S1 O1 125.6(3) 2_556 . ?
O1 S1 N2 107.14(19) 2_556 . ?
O1 S1 N2 105.60(17) . . ?
O1 S1 N2 105.60(17) 2_556 2_556 ?
O1 S1 N2 107.14(19) . 2_556 ?
N2 S1 N2 103.8(2) . 2_556 ?
C4 O2 Cd1 125.8(3) . . ?
C13 O3 Cd1 106.1(2) . . ?
C13 O3 Cd1 120.5(2) . 5_546 ?
Cd1 O3 Cd1 98.34(9) . 5_546 ?
C11 O5 Cd1 92.6(2) . 3 ?
C11 O6 Cd1 90.8(2) . 3 ?
C1 N1 C3 106.1(4) . . ?
C1 N1 Cd1 129.3(3) . . ?
C3 N1 Cd1 124.4(3) . . ?
C1 N2 C2 107.2(3) . . ?
C1 N2 S1 126.6(3) . . ?
C2 N2 S1 126.2(3) . . ?
N1 C1 N2 110.4(4) . . ?
N1 C1 H1A 124.8 . . ?
N2 C1 H1A 124.8 . . ?
C3 C2 N2 105.3(4) . . ?
C3 C2 H2A 127.3 . . ?
N2 C2 H2A 127.3 . . ?
C2 C3 N1 110.9(4) . . ?
C2 C3 H3A 124.5 . . ?
N1 C3 H3A 124.5 . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C10 C5 C6 119.8(3) . . ?
C10 C5 C13 120.5(3) . . ?
C6 C5 C13 119.7(3) . . ?
C7 C6 C5 120.5(3) . . ?
C7 C6 H6A 119.7 . . ?
C5 C6 H6A 119.7 . . ?
C8 C7 C6 118.9(3) . . ?
C8 C7 C11 120.8(3) . . ?
C6 C7 C11 120.3(3) . . ?
C7 C8 C9 121.4(3) . . ?
C7 C8 H8A 119.3 . . ?
C9 C8 H8A 119.3 . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 C12 117.0(3) . . ?
C10 C9 C12 123.6(3) . . ?
C5 C10 C9 119.8(3) . . ?
C5 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
O5 C11 O6 121.3(3) . . ?
O5 C11 C7 119.4(3) . . ?
O6 C11 C7 119.3(3) . . ?
O5 C11 Cd1 60.07(19) . 3 ?
O6 C11 Cd1 61.28(19) . 3 ?
C7 C11 Cd1 175.9(3) . 3 ?
O7 C12 O8 121.8(4) . . ?
O7 C12 C9 122.2(4) . . ?
O8 C12 C9 116.0(3) . . ?
O4 C13 O3 122.5(3) . . ?
O4 C13 C5 120.7(3) . . ?
O3 C13 C5 116.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.105
