# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1417645'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O6 S2 Zn, 2(C3 H10 N)'
_chemical_formula_sum            'C6 H20 N2 O6 S2 Zn'
_chemical_formula_weight         345.73

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           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   22.1708(7)
_cell_length_b                   8.7244(2)
_cell_length_c                   7.7214(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1493.53(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2278
_cell_measurement_theta_min      3.6
_cell_measurement_theta_max      30.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12389
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         30.50
_reflns_number_total             2278
_reflns_number_gt                1879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0278P)²+0.5151P] 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         2278
_refine_ls_number_parameters     91
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
C1 C 0.36906(10) 0.2934(2) 1.0362(3) 0.0552(5) Uani 1 1 d . . .
H1E H 0.3698 0.3001 1.1615 0.066 Uiso 1 1 calc R . .
H1F H 0.3665 0.1860 1.0046 0.066 Uiso 1 1 calc R . .
C2 C 0.31486(11) 0.3768(4) 0.9683(4) 0.0781(8) Uani 1 1 d . . .
H2A H 0.3131 0.3643 0.8435 0.094 Uiso 1 1 calc R . .
H2B H 0.3193 0.4853 0.9925 0.094 Uiso 1 1 calc R . .
C3 C 0.25674(17) 0.3215(6) 1.0455(7) 0.1450(18) Uani 1 1 d . . .
H3A H 0.2546 0.2119 1.0364 0.218 Uiso 1 1 calc R . .
H3B H 0.2235 0.3664 0.9842 0.218 Uiso 1 1 calc R . .
H3C H 0.2549 0.3508 1.1652 0.218 Uiso 1 1 calc R . .
N1 N 0.42476(8) 0.3594(2) 0.9651(2) 0.0394(3) Uani 1 1 d D . .
O1 O 0.57497(5) 0.08401(14) 0.81158(17) 0.0396(3) Uani 1 1 d . . .
O2 O 0.52019(6) 0.16536(13) 1.06587(15) 0.0371(3) Uani 1 1 d . . .
O3 O 0.57514(7) 0.34758(13) 0.89803(17) 0.0509(4) Uani 1 1 d . . .
S1 S 0.580403(18) 0.18778(5) 0.96929(5) 0.03147(10) Uani 1 1 d . . .
Zn1 Zn 0.5000 -0.01801(3) 0.7500 0.02928(8) Uani 1 2 d S . .
H1A H 0.4253(9) 0.356(3) 0.852(2) 0.054(6) Uiso 1 1 d D . .
H1B H 0.4553(10) 0.309(3) 1.001(3) 0.049(7) Uiso 1 1 d . . .
H1C H 0.4292(11) 0.456(3) 0.995(3) 0.052(7) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0647(13) 0.0456(11) 0.0553(12) 0.0040(10) 0.0138(11) -0.0054(10)
C2 0.0492(13) 0.091(2) 0.094(2) -0.0055(17) 0.0024(13) -0.0093(13)
C3 0.069(2) 0.181(5) 0.186(4) -0.026(4) 0.035(2) -0.037(2)
N1 0.0460(9) 0.0335(8) 0.0386(8) -0.0065(7) 0.0016(7) 0.0069(7)
O1 0.0464(7) 0.0338(6) 0.0386(6) -0.0119(5) 0.0099(5) -0.0077(5)
O2 0.0437(6) 0.0342(6) 0.0334(6) 0.0122(5) 0.0124(5) 0.0044(5)
O3 0.0891(11) 0.0248(6) 0.0386(7) -0.0017(5) 0.0177(7) -0.0155(6)
S1 0.0357(2) 0.0319(2) 0.02681(18) -0.00036(16) 0.00107(15) -0.00600(16)
Zn1 0.04049(15) 0.02160(12) 0.02573(13) 0.000 0.00685(10) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.469(3) . ?
C1 C2 1.499(4) . ?
C2 C3 1.499(4) . ?
O1 S1 1.5221(12) . ?
O1 Zn1 1.9445(12) . ?
O2 S1 1.5417(12) . ?
O2 Zn1 1.9683(11) 5_657 ?
O3 S1 1.5034(13) . ?
Zn1 O1 1.9445(12) 3_656 ?
Zn1 O2 1.9683(11) 5_657 ?
Zn1 O2 1.9683(11) 7 ?

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 C1 C2 110.66(19) . . ?
C1 C2 C3 113.2(3) . . ?
S1 O1 Zn1 122.38(7) . . ?
S1 O2 Zn1 128.99(7) . 5_657 ?
O3 S1 O1 104.63(7) . . ?
O3 S1 O2 103.14(7) . . ?
O1 S1 O2 104.07(7) . . ?
O1 Zn1 O1 125.52(8) . 3_656 ?
O1 Zn1 O2 108.46(6) . 5_657 ?
O1 Zn1 O2 106.33(5) 3_656 5_657 ?
O1 Zn1 O2 106.33(5) . 7 ?
O1 Zn1 O2 108.46(6) 3_656 7 ?
O2 Zn1 O2 98.44(7) 5_657 7 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_complex2
_database_code_depnum_ccdc_archive 'CCDC 1417646'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O6 S2 Zn, C3 H12 N2'
_chemical_formula_sum            'C3 H12 N2 O6 S2 Zn'
_chemical_formula_weight         301.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Orthorhombic
_symmetry_space_group_name_H-M   Pbcm

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

_cell_length_a                   8.6326(3)
_cell_length_b                   7.6916(3)
_cell_length_c                   16.5072(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1096.05(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1732
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      30.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18464
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         30.53
_reflns_number_total             1732
_reflns_number_gt                1282
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0333P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0076(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1732
_refine_ls_number_parameters     79
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0737
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
C1 C 0.2198(3) 0.0363(3) 0.67453(13) 0.0372(5) Uani 1 1 d . . .
H1D H 0.2147 0.1623 0.6742 0.045 Uiso 1 1 calc R . .
H1E H 0.3281 0.0027 0.6746 0.045 Uiso 1 1 calc R . .
C2 C 0.1418(4) -0.0328(5) 0.7500 0.0338(7) Uani 1 2 d S . .
H2A H 0.0337 0.0015 0.7500 0.041 Uiso 1 2 calc SR . .
H2B H 0.1462 -0.1588 0.7500 0.041 Uiso 1 2 calc SR . .
N1 N 0.1435(3) -0.0329(3) 0.60096(12) 0.0332(5) Uani 1 1 d D . .
O1 O 0.58259(19) 0.1888(2) 0.60062(9) 0.0367(4) Uani 1 1 d . . .
O2 O 0.84912(19) 0.1035(2) 0.60476(11) 0.0460(5) Uani 1 1 d . . .
O3 O 0.66908(18) -0.0668(2) 0.52929(9) 0.0357(4) Uani 1 1 d . . .
S1 S 0.68750(7) 0.03120(7) 0.61013(3) 0.02839(15) Uani 1 1 d . . .
Zn1 Zn 0.47998(4) 0.2500 0.5000 0.02758(13) Uani 1 2 d S . .
H1A H 0.139(3) -0.146(5) 0.6040(15) 0.050(9) Uiso 1 1 d . . .
H1B H 0.189(3) 0.005(3) 0.5595(17) 0.046(8) Uiso 1 1 d . . .
H1C H 0.047(2) 0.001(3) 0.5989(18) 0.055(10) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0357(13) 0.0389(14) 0.0368(12) -0.0018(10) 0.0040(10) -0.0050(11)
C2 0.0322(17) 0.0363(19) 0.0328(15) 0.000 0.000 -0.0036(14)
N1 0.0318(12) 0.0359(13) 0.0319(10) 0.0018(9) 0.0054(8) 0.0054(10)
O1 0.0320(9) 0.0376(9) 0.0406(9) -0.0071(7) -0.0060(7) 0.0097(8)
O2 0.0248(9) 0.0369(10) 0.0763(12) -0.0153(9) -0.0127(8) 0.0019(8)
O3 0.0353(9) 0.0355(9) 0.0363(8) -0.0115(7) 0.0064(7) -0.0126(8)
S1 0.0301(3) 0.0262(3) 0.0289(3) -0.0006(2) -0.0036(2) -0.0002(2)
Zn1 0.0218(2) 0.0257(2) 0.0352(2) -0.00600(14) 0.000 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.481(3) . ?
C1 C2 1.513(3) . ?
C2 C1 1.513(3) 6_557 ?
O1 S1 1.5214(17) . ?
O1 Zn1 1.9403(15) . ?
O2 S1 1.5046(18) . ?
O3 S1 1.5408(15) . ?
O3 Zn1 1.9687(15) 5_656 ?
Zn1 O1 1.9403(15) 4_556 ?
Zn1 O3 1.9687(15) 5_656 ?
Zn1 O3 1.9687(15) 8_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
N1 C1 C2 110.6(2) . . ?
C1 C2 C1 110.9(3) 6_557 . ?
S1 O1 Zn1 123.60(9) . . ?
S1 O3 Zn1 129.07(9) . 5_656 ?
O2 S1 O1 104.56(10) . . ?
O2 S1 O3 103.03(9) . . ?
O1 S1 O3 103.82(9) . . ?
O1 Zn1 O1 125.67(10) 4_556 . ?
O1 Zn1 O3 105.18(6) 4_556 5_656 ?
O1 Zn1 O3 109.57(7) . 5_656 ?
O1 Zn1 O3 109.57(7) 4_556 8_665 ?
O1 Zn1 O3 105.18(6) . 8_665 ?
O3 Zn1 O3 98.37(10) 5_656 8_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.53
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.083
####################################################################### 
# 
# 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_complex3
_database_code_depnum_ccdc_archive 'CCDC 1417647'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O6 S2 Zn, C4 H14 N2'
_chemical_formula_sum            'C4 H14 N2 O6 S2 Zn'
_chemical_formula_weight         315.66

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

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                   17.3344(9)
_cell_length_b                   8.4890(3)
_cell_length_c                   8.1660(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.855(5)
_cell_angle_gamma                90.00
_cell_volume                     1150.02(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1482
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      28.7

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    2.509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8711
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         28.71
_reflns_number_total             1482
_reflns_number_gt                1275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0336P)²+0.7231P] 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         1482
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0737
_refine_ls_wR_factor_gt          0.0701
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.18549(15) -0.2901(4) 0.1513(3) 0.0383(6) Uani 1 1 d . . .
H1D H 0.2250 -0.3488 0.2384 0.046 Uiso 1 1 calc R . .
H1E H 0.1855 -0.1826 0.1915 0.046 Uiso 1 1 calc R . .
C2 C 0.21002(15) -0.2900(3) -0.0099(3) 0.0348(6) Uani 1 1 d . . .
H2A H 0.1688 -0.2368 -0.0990 0.042 Uiso 1 1 calc R . .
H2B H 0.2132 -0.3979 -0.0463 0.042 Uiso 1 1 calc R . .
N1 N 0.10524(13) -0.3595(3) 0.1296(3) 0.0273(4) Uani 1 1 d . . .
O1 O 0.02378(10) 0.1692(2) 0.0796(2) 0.0295(4) Uani 1 1 d . . .
O2 O 0.09566(11) 0.0832(2) -0.1204(2) 0.0350(4) Uani 1 1 d . . .
O3 O 0.09912(13) 0.3528(2) -0.0331(3) 0.0486(6) Uani 1 1 d . . .
S1 S 0.10374(3) 0.18788(7) 0.03485(7) 0.02592(15) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.02890(4) 0.2500 0.02379(13) Uani 1 2 d S . .
H1A H 0.0661(18) -0.310(3) 0.061(4) 0.036(8) Uiso 1 1 d . . .
H1B H 0.0926(17) -0.367(4) 0.226(4) 0.040(8) Uiso 1 1 d . . .
H1C H 0.104(2) -0.456(4) 0.090(5) 0.052(10) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0336(13) 0.0526(18) 0.0315(14) -0.0087(12) 0.0140(11) -0.0104(12)
C2 0.0374(14) 0.0431(16) 0.0276(13) -0.0060(11) 0.0153(11) -0.0086(11)
N1 0.0301(11) 0.0272(11) 0.0270(11) -0.0034(9) 0.0122(9) -0.0015(9)
O1 0.0338(9) 0.0288(9) 0.0299(9) 0.0074(7) 0.0159(7) 0.0022(7)
O2 0.0418(10) 0.0311(9) 0.0381(10) -0.0131(8) 0.0213(8) -0.0098(8)
O3 0.0915(16) 0.0242(10) 0.0459(12) -0.0065(8) 0.0450(12) -0.0181(10)
S1 0.0282(3) 0.0291(3) 0.0207(3) -0.0014(2) 0.0075(2) -0.0059(2)
Zn1 0.0325(2) 0.01853(19) 0.0238(2) 0.000 0.01365(16) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.473(3) . ?
C1 C2 1.497(3) . ?
C2 C2 1.509(5) 7_545 ?
O1 S1 1.5406(17) . ?
O1 Zn1 1.9641(16) . ?
O2 S1 1.5214(18) . ?
O2 Zn1 1.9383(17) 5 ?
O3 S1 1.500(2) . ?
Zn1 O2 1.9383(17) 5 ?
Zn1 O2 1.9383(17) 6_556 ?
Zn1 O1 1.9641(16) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 113.2(2) . . ?
C1 C2 C2 113.1(3) . 7_545 ?
S1 O1 Zn1 128.21(10) . . ?
S1 O2 Zn1 126.81(10) . 5 ?
O3 S1 O2 104.78(11) . . ?
O3 S1 O1 103.21(11) . . ?
O2 S1 O1 105.40(10) . . ?
O2 Zn1 O2 121.21(12) 5 6_556 ?
O2 Zn1 O1 111.24(7) 5 2 ?
O2 Zn1 O1 103.46(7) 6_556 2 ?
O2 Zn1 O1 103.46(7) 5 . ?
O2 Zn1 O1 111.24(7) 6_556 . ?
O1 Zn1 O1 105.36(10) 2 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.71
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.080
####################################################################### 
# 
# 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_complex4
_database_code_depnum_ccdc_archive 'CCDC 1417648'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O6 S2 Zn, C6 H18 N2'
_chemical_formula_sum            'C6 H18 N2 O6 S2 Zn'
_chemical_formula_weight         343.71

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'
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

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                   21.1872(13)
_cell_length_b                   8.5354(4)
_cell_length_c                   8.0784(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.333(4)
_cell_angle_gamma                90.00
_cell_volume                     1378.53(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2113
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      30.6

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    2.100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12033
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         30.57
_reflns_number_total             2113
_reflns_number_gt                1833
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0406P)²+1.1480P] 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         2113
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.15204(11) -0.2840(3) -0.1084(3) 0.0378(5) Uani 1 1 d . . .
H1D H -0.1475 -0.1716 -0.0912 0.045 Uiso 1 1 calc R . .
H1E H -0.1858 -0.3199 -0.0604 0.045 Uiso 1 1 calc R . .
C2 C -0.17469(12) -0.3190(3) -0.3013(3) 0.0397(5) Uani 1 1 d . . .
H2A H -0.1846 -0.4299 -0.3189 0.048 Uiso 1 1 calc R . .
H2B H -0.1385 -0.2955 -0.3461 0.048 Uiso 1 1 calc R . .
C3 C -0.23574(12) -0.2265(3) -0.4042(3) 0.0440(5) Uani 1 1 d . . .
H3A H -0.2242 -0.1162 -0.3973 0.053 Uiso 1 1 calc R . .
H3B H -0.2700 -0.2402 -0.3502 0.053 Uiso 1 1 calc R . .
N1 N -0.08763(9) -0.3599(2) -0.0126(2) 0.0292(3) Uani 1 1 d . . .
O1 O -0.01902(7) 0.16821(17) 0.04670(17) 0.0305(3) Uani 1 1 d . . .
O2 O -0.08444(10) 0.34997(18) -0.1654(2) 0.0474(5) Uani 1 1 d . . .
O3 O -0.07989(8) 0.08365(19) -0.25127(18) 0.0364(3) Uani 1 1 d . . .
S1 S -0.08641(2) 0.18517(6) -0.10340(6) 0.02719(12) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.02816(3) 0.2500 0.02507(10) Uani 1 2 d S . .
H1A H -0.0555(17) -0.313(4) -0.026(4) 0.053(9) Uiso 1 1 d . . .
H1B H -0.0874(14) -0.458(4) -0.049(4) 0.041(7) Uiso 1 1 d . . .
H1C H -0.0829(13) -0.358(3) 0.095(4) 0.035(6) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0376(11) 0.0463(13) 0.0250(9) -0.0031(9) 0.0042(8) 0.0093(9)
C2 0.0389(11) 0.0530(14) 0.0229(9) 0.0023(9) 0.0047(8) 0.0085(10)
C3 0.0382(11) 0.0563(15) 0.0299(10) 0.0006(10) 0.0009(9) 0.0107(11)
N1 0.0335(9) 0.0287(9) 0.0208(7) -0.0021(6) 0.0027(6) -0.0003(7)
O1 0.0367(7) 0.0308(7) 0.0196(6) 0.0067(5) 0.0032(5) -0.0018(6)
O2 0.0859(13) 0.0265(8) 0.0235(7) 0.0032(6) 0.0096(8) 0.0186(8)
O3 0.0444(8) 0.0332(8) 0.0244(7) -0.0063(6) 0.0017(6) 0.0108(7)
S1 0.0312(2) 0.0297(2) 0.0202(2) 0.00208(16) 0.00783(17) 0.00685(17)
Zn1 0.03569(18) 0.02028(16) 0.01601(14) 0.000 0.00422(11) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.477(3) . ?
C1 C2 1.501(3) . ?
C2 C3 1.508(3) . ?
C3 C3 1.518(4) 7_444 ?
O1 S1 1.5439(14) . ?
O1 Zn1 1.9623(13) . ?
O2 S1 1.4984(16) . ?
O3 S1 1.5187(15) . ?
O3 Zn1 1.9402(15) 5 ?
Zn1 O3 1.9401(15) 6_556 ?
Zn1 O3 1.9402(15) 5 ?
Zn1 O1 1.9623(13) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 112.29(18) . . ?
C1 C2 C3 112.9(2) . . ?
C2 C3 C3 113.8(3) . 7_444 ?
S1 O1 Zn1 126.49(9) . . ?
S1 O3 Zn1 125.66(9) . 5 ?
O2 S1 O3 104.64(9) . . ?
O2 S1 O1 103.28(9) . . ?
O3 S1 O1 105.25(9) . . ?
O3 Zn1 O3 121.07(10) 6_556 5 ?
O3 Zn1 O1 103.96(6) 6_556 2 ?
O3 Zn1 O1 110.99(6) 5 2 ?
O3 Zn1 O1 110.99(6) 6_556 . ?
O3 Zn1 O1 103.96(6) 5 . ?
O1 Zn1 O1 104.94(9) 2 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_complex5
_database_code_depnum_ccdc_archive 'CCDC 1417649'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Zn S2 O6 , C4 H12 N2, H2 O'
_chemical_formula_sum            'C4 H14 N2 O7 S2 Zn'
_chemical_formula_weight         331.66

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

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

_cell_length_a                   8.1135(2)
_cell_length_b                   8.4917(2)
_cell_length_c                   8.8022(3)
_cell_angle_alpha                87.946(2)
_cell_angle_beta                 88.256(3)
_cell_angle_gamma                63.296(2)
_cell_volume                     541.35(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3316
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      30.6

_exptl_crystal_description       Plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             340
_exptl_absorpt_coefficient_mu    2.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9824
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         30.56
_reflns_number_total             3316
_reflns_number_gt                2416
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0288P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3316
_refine_ls_number_parameters     169
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.991
_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 -0.00525(4) 0.50367(4) 0.75152(3) 0.02161(10) Uani 1 1 d . . .
S1 S 0.12396(10) 0.68669(9) 0.99159(7) 0.02029(15) Uani 1 1 d . . .
S2 S 0.28344(9) 0.28539(9) 0.50164(7) 0.02059(15) Uani 1 1 d . . .
C1 C -0.4876(4) 1.0015(4) 0.8382(3) 0.0319(7) Uani 1 1 d . . .
H1C H -0.3582 0.9709 0.8215 0.038 Uiso 1 1 calc R . .
H1D H -0.5445 1.0178 0.7398 0.038 Uiso 1 1 calc R . .
C2 C -0.4948(4) 1.1455(4) 1.0745(3) 0.0310(7) Uani 1 1 d . . .
H2C H -0.5571 1.2542 1.1296 0.037 Uiso 1 1 calc R . .
H2D H -0.3656 1.1186 1.0629 0.037 Uiso 1 1 calc R . .
C3 C -0.0045(5) 0.0155(4) 0.6638(3) 0.0359(7) Uani 1 1 d . . .
H3A H -0.0884 -0.0321 0.6973 0.043 Uiso 1 1 calc R . .
H3B H 0.0362 0.0516 0.7527 0.043 Uiso 1 1 calc R . .
C4 C -0.1592(5) 0.1238(4) 0.4174(3) 0.0348(7) Uani 1 1 d . . .
H4A H -0.2160 0.2284 0.3523 0.042 Uiso 1 1 calc R . .
H4B H -0.2499 0.0809 0.4399 0.042 Uiso 1 1 calc R . .
N1 N -0.5780(4) 1.1675(3) 0.9228(3) 0.0290(6) Uani 1 1 d D . .
N2 N -0.1008(4) 0.1692(4) 0.5607(3) 0.0320(6) Uani 1 1 d . . .
O1 O 0.1652(3) 0.5593(3) 0.8620(2) 0.0319(5) Uani 1 1 d . . .
O2 O -0.0805(3) 0.7927(3) 0.9990(2) 0.0361(5) Uani 1 1 d . . .
O1W O -0.4330(3) 0.3503(3) 0.7281(2) 0.0301(5) Uani 1 1 d D . .
O3 O 0.1760(3) 0.5670(3) 1.13642(19) 0.0288(5) Uani 1 1 d . . .
O4 O 0.1648(3) 0.2888(2) 0.64348(19) 0.0276(5) Uani 1 1 d . . .
O5 O 0.1611(3) 0.2880(3) 0.3704(2) 0.0295(5) Uani 1 1 d . . .
O6 O 0.2896(3) 0.4576(3) 0.4957(2) 0.0349(5) Uani 1 1 d . . .
H1A H -0.695(3) 1.202(5) 0.940(4) 0.053(12) Uiso 1 1 d D . .
H1B H -0.558(5) 1.247(4) 0.877(3) 0.042(10) Uiso 1 1 d D . .
H1W H -0.512(4) 0.417(4) 0.670(3) 0.058(12) Uiso 1 1 d D . .
H2W H -0.382(6) 0.406(5) 0.765(5) 0.091(17) Uiso 1 1 d D . .
H2A H -0.193(6) 0.247(6) 0.612(4) 0.061(12) Uiso 1 1 d . . .
H2B H -0.047(5) 0.230(5) 0.542(4) 0.046(11) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.02287(19) 0.02200(17) 0.01887(15) 0.00002(11) -0.00113(11) -0.00909(14)
S1 0.0218(4) 0.0228(3) 0.0187(3) -0.0003(2) -0.0002(2) -0.0122(3)
S2 0.0195(4) 0.0209(3) 0.0181(3) 0.0004(2) -0.0011(2) -0.0062(3)
C1 0.0304(18) 0.0326(17) 0.0227(13) 0.0019(12) 0.0025(12) -0.0055(14)
C2 0.0290(17) 0.0288(16) 0.0347(15) -0.0050(12) 0.0018(12) -0.0124(13)
C3 0.043(2) 0.0332(17) 0.0295(15) -0.0072(12) 0.0063(13) -0.0150(15)
C4 0.0360(19) 0.0271(16) 0.0390(16) -0.0005(13) -0.0046(14) -0.0118(14)
N1 0.0283(16) 0.0230(13) 0.0299(13) 0.0060(10) 0.0021(11) -0.0071(12)
N2 0.0303(16) 0.0223(14) 0.0424(15) -0.0111(11) 0.0040(12) -0.0103(12)
O1 0.0271(12) 0.0436(13) 0.0248(10) -0.0138(9) 0.0021(8) -0.0150(10)
O2 0.0233(12) 0.0348(12) 0.0396(12) 0.0016(9) 0.0026(9) -0.0040(10)
O1W 0.0248(12) 0.0305(12) 0.0345(11) 0.0035(9) -0.0034(9) -0.0120(10)
O3 0.0261(12) 0.0426(13) 0.0223(9) 0.0086(8) -0.0057(8) -0.0199(10)
O4 0.0357(13) 0.0252(11) 0.0200(9) -0.0011(7) 0.0090(8) -0.0126(9)
O5 0.0380(13) 0.0251(11) 0.0230(9) 0.0000(8) -0.0108(8) -0.0116(9)
O6 0.0436(14) 0.0366(13) 0.0342(11) 0.0064(9) -0.0067(10) -0.0269(11)

_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 O1 1.945(2) . ?
Zn1 O5 1.9532(19) 2_566 ?
Zn1 O3 1.968(2) 2_567 ?
Zn1 O4 1.9798(19) . ?
S1 O2 1.491(2) . ?
S1 O1 1.5243(19) . ?
S1 O3 1.5463(19) . ?
S2 O6 1.485(2) . ?
S2 O5 1.5391(19) . ?
S2 O4 1.5462(19) . ?
C1 N1 1.481(4) . ?
C1 C2 1.501(4) 2_477 ?
C2 N1 1.482(4) . ?
C2 C1 1.501(4) 2_477 ?
C3 N2 1.476(4) . ?
C3 C4 1.505(4) 2_556 ?
C4 N2 1.483(4) . ?
C4 C3 1.505(4) 2_556 ?
O3 Zn1 1.968(2) 2_567 ?
O5 Zn1 1.9532(19) 2_566 ?

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
O1 Zn1 O5 107.86(9) . 2_566 ?
O1 Zn1 O3 119.95(8) . 2_567 ?
O5 Zn1 O3 105.62(9) 2_566 2_567 ?
O1 Zn1 O4 101.97(8) . . ?
O5 Zn1 O4 118.02(8) 2_566 . ?
O3 Zn1 O4 104.16(8) 2_567 . ?
O2 S1 O1 106.45(12) . . ?
O2 S1 O3 105.84(12) . . ?
O1 S1 O3 104.26(12) . . ?
O6 S2 O5 107.01(11) . . ?
O6 S2 O4 106.06(11) . . ?
O5 S2 O4 102.44(12) . . ?
N1 C1 C2 110.5(2) . 2_477 ?
N1 C2 C1 109.5(2) . 2_477 ?
N2 C3 C4 109.8(2) . 2_556 ?
N2 C4 C3 110.2(3) . 2_556 ?
C1 N1 C2 110.6(2) . . ?
C3 N2 C4 113.3(2) . . ?
S1 O1 Zn1 128.70(13) . . ?
S1 O3 Zn1 123.87(12) . 2_567 ?
S2 O4 Zn1 125.16(11) . . ?
S2 O5 Zn1 125.27(12) . 2_566 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_complex6
_database_code_depnum_ccdc_archive 'CCDC 1417650'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H4 Mn O8 S2, C4 H12 N2, 2(H2 O)'
_chemical_formula_sum            'C4 H20 Mn N2 O10 S2'
_chemical_formula_weight         375.28

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   5.4228(3)
_cell_length_b                   6.6958(4)
_cell_length_c                   9.9304(5)
_cell_angle_alpha                104.871(3)
_cell_angle_beta                 95.917(3)
_cell_angle_gamma                99.602(3)
_cell_volume                     339.56(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2028
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      30.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             195
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5916
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         30.49
_reflns_number_total             2028
_reflns_number_gt                1719
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0432P)²+0.0624P] 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         2028
_refine_ls_number_parameters     112
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1715(4) 1.1354(3) 0.4442(2) 0.0307(4) Uani 1 1 d . . .
H1C H 0.2037 1.2105 0.3743 0.037 Uiso 1 1 calc R . .
H1D H 0.3271 1.1616 0.5094 0.037 Uiso 1 1 calc R . .
C2 C 0.0319(4) 0.7848(3) 0.4767(2) 0.0294(4) Uani 1 1 d . . .
H2A H 0.1831 0.8000 0.5428 0.035 Uiso 1 1 calc R . .
H2B H -0.0254 0.6363 0.4273 0.035 Uiso 1 1 calc R . .
N1 N 0.0916(3) 0.9061(3) 0.37380(16) 0.0262(3) Uani 1 1 d D . .
O1 O 0.3392(2) 0.97667(19) 0.13053(13) 0.0221(3) Uani 1 1 d . . .
O2 O 0.7620(2) 0.9014(2) 0.14737(13) 0.0242(3) Uani 1 1 d . . .
O1W O 0.0467(3) 1.3212(2) 0.13664(19) 0.0378(4) Uani 1 1 d . . .
O3 O 0.4268(2) 0.6990(2) 0.22898(15) 0.0281(3) Uani 1 1 d . . .
O2W O 0.6457(3) 0.3708(2) 0.27560(16) 0.0311(3) Uani 1 1 d D . .
S1 S 0.48123(7) 0.79458(6) 0.10743(4) 0.01863(11) Uani 1 1 d . . .
Mn1 Mn 0.0000 1.0000 0.0000 0.01825(11) Uani 1 2 d S . .
H1A H 0.216(4) 0.858(4) 0.332(3) 0.043(7) Uiso 1 1 d D . .
H1B H -0.044(4) 0.886(4) 0.308(2) 0.036(6) Uiso 1 1 d D . .
H1W1 H -0.078(6) 1.350(4) 0.178(3) 0.053(8) Uiso 1 1 d . . .
H1W2 H 0.145(6) 1.436(5) 0.151(3) 0.048(8) Uiso 1 1 d . . .
H2W1 H 0.570(5) 0.461(4) 0.264(3) 0.060(9) Uiso 1 1 d D . .
H2W2 H 0.555(5) 0.258(4) 0.236(3) 0.038(7) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0278(9) 0.0377(10) 0.0266(9) 0.0119(8) 0.0070(7) 0.0002(8)
C2 0.0354(10) 0.0317(10) 0.0234(9) 0.0106(7) 0.0030(8) 0.0094(8)
N1 0.0211(7) 0.0411(9) 0.0181(7) 0.0083(6) 0.0049(6) 0.0096(6)
O1 0.0171(5) 0.0282(6) 0.0242(6) 0.0106(5) 0.0015(5) 0.0089(5)
O2 0.0139(5) 0.0375(7) 0.0251(6) 0.0159(5) 0.0030(5) 0.0049(5)
O1W 0.0244(7) 0.0266(7) 0.0563(10) 0.0003(7) 0.0118(7) 0.0024(6)
O3 0.0271(6) 0.0326(7) 0.0344(7) 0.0205(6) 0.0129(6) 0.0111(5)
O2W 0.0282(7) 0.0286(7) 0.0353(8) 0.0079(6) -0.0018(6) 0.0080(6)
S1 0.01486(18) 0.0238(2) 0.0185(2) 0.00718(15) 0.00322(14) 0.00526(15)
Mn1 0.01358(16) 0.02453(19) 0.01920(18) 0.00947(14) 0.00292(13) 0.00532(13)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.483(3) . ?
C1 C2 1.509(3) 2_576 ?
C2 N1 1.488(2) . ?
C2 C1 1.509(3) 2_576 ?
O1 S1 1.5290(12) . ?
O1 Mn1 2.1902(11) . ?
O2 S1 1.5344(12) . ?
O2 Mn1 2.2008(12) 1_655 ?
O1W Mn1 2.1861(15) . ?
O3 S1 1.5365(13) . ?
Mn1 O1W 2.1861(15) 2_575 ?
Mn1 O1 2.1902(11) 2_575 ?
Mn1 O2 2.2008(12) 2_675 ?
Mn1 O2 2.2008(12) 1_455 ?

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 C1 C2 110.24(15) . 2_576 ?
N1 C2 C1 110.07(15) . 2_576 ?
C1 N1 C2 111.52(14) . . ?
S1 O1 Mn1 127.55(7) . . ?
S1 O2 Mn1 124.52(7) . 1_655 ?
O1 S1 O2 104.77(7) . . ?
O1 S1 O3 103.19(7) . . ?
O2 S1 O3 103.85(7) . . ?
O1W Mn1 O1W 180.00(5) . 2_575 ?
O1W Mn1 O1 93.39(5) . 2_575 ?
O1W Mn1 O1 86.61(5) 2_575 2_575 ?
O1W Mn1 O1 86.61(5) . . ?
O1W Mn1 O1 93.39(5) 2_575 . ?
O1 Mn1 O1 180.00(6) 2_575 . ?
O1W Mn1 O2 93.51(6) . 2_675 ?
O1W Mn1 O2 86.49(6) 2_575 2_675 ?
O1 Mn1 O2 90.38(4) 2_575 2_675 ?
O1 Mn1 O2 89.62(4) . 2_675 ?
O1W Mn1 O2 86.49(6) . 1_455 ?
O1W Mn1 O2 93.51(6) 2_575 1_455 ?
O1 Mn1 O2 89.62(4) 2_575 1_455 ?
O1 Mn1 O2 90.38(4) . 1_455 ?
O2 Mn1 O2 180.0 2_675 1_455 ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.082
