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

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

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H11 Co N2 O6 S2'
_chemical_formula_sum            'C15 H11 Co N2 O6 S2'
_chemical_formula_weight         438.33

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'F d d d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   15.7239(19)
_cell_length_b                   16.158(2)
_cell_length_c                   40.866(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10383(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2348
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      19.30

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3552
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_process_details   multi-scan

_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_reflns_number            22754
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2990
_reflns_number_gt                2987
_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          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.090  0.411  0.000       850 362984544 ' '
   2 -0.033  0.783  0.250       850 367019232 ' '
   3  0.016  0.016  0.500       850 363027552 ' '
   4 -0.033  0.283  0.750       850 367019360 ' '
   5  0.125  0.125  0.125       110  35786196 ' '
   6  0.125  0.625  0.625       110  35786180 ' '
   7  0.375  0.875  0.375       110  35763584 ' '
   8  0.375  0.375  0.875       110  35763600 ' '
   9  0.625  0.625  0.125       110  35786100 ' '
  10  0.625  0.125  0.625       110  35786108 ' '
  11  0.875  0.375  0.375       110  35763588 ' '
  12  0.875  0.875  0.875       110  35763600 ' '
_platon_squeeze_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)+(0.0200P)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         2990
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0846
_refine_ls_wR_factor_ref         0.2475
_refine_ls_wR_factor_gt          0.2473
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_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 0.3750 0.3750 0.11128(2) 0.0240(3) Uani 1 2 d S . .
S1 S 0.11158(9) 0.18630(9) 0.00533(3) 0.0385(4) Uani 1 1 d . . .
O1 O 0.4608(2) 0.2812(2) 0.11179(8) 0.0241(7) Uani 1 1 d . . .
O2 O 0.4150(3) 0.1933(3) 0.14940(10) 0.0396(9) Uani 1 1 d . . .
N1 N 0.2963(2) 0.3130(2) 0.07631(8) 0.0206(7) Uani 1 1 d . . .
O3 O 0.3039(3) 0.3113(3) 0.14884(11) 0.0454(10) Uani 1 1 d . . .
H3 H 0.2528 0.3164 0.1453 0.068 Uiso 1 1 calc R . .
C8 C 0.6250 0.2137(4) 0.1250 0.0251(12) Uani 1 2 d S . .
H8 H 0.6250 0.2712 0.1250 0.030 Uiso 1 2 calc SR . .
C7 C 0.5471(3) 0.1682(2) 0.12531(10) 0.0185(8) Uani 1 1 d . . .
C1 C 0.2999(3) 0.2303(3) 0.07241(12) 0.0311(10) Uani 1 1 d . . .
H1 H 0.3406 0.2006 0.0840 0.037 Uiso 1 1 calc R . .
C5 C 0.2381(3) 0.3568(3) 0.05840(12) 0.0297(10) Uani 1 1 d . . .
H5 H 0.2351 0.4140 0.0607 0.036 Uiso 1 1 calc R . .
C3 C 0.1847(4) 0.2283(4) 0.03400(14) 0.0403(12) Uani 1 1 d . . .
C2 C 0.2432(3) 0.1862(3) 0.05101(12) 0.0304(10) Uani 1 1 d . . .
H2 H 0.2471 0.1290 0.0490 0.037 Uiso 1 1 calc R . .
C4 C 0.1828(3) 0.3164(3) 0.03652(12) 0.0321(10) Uani 1 1 d . . .
H4 H 0.1452 0.3470 0.0238 0.038 Uiso 1 1 calc R . .
C6 C 0.4694(3) 0.2168(3) 0.12882(12) 0.0320(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.029(3) 14 ?
Co1 O1 2.029(3) . ?
Co1 N1 2.140(4) 14 ?
Co1 N1 2.140(4) . ?
Co1 O3 2.160(5) 14 ?
Co1 O3 2.160(5) . ?
S1 C3 1.776(6) . ?
S1 S1 2.026(3) 2 ?
O1 C6 1.260(6) . ?
O2 C6 1.258(7) . ?
N1 C1 1.346(6) . ?
N1 C5 1.369(6) . ?
O3 H3 0.8200 . ?
C8 C7 1.428(5) . ?
C8 C7 1.428(5) 4_655 ?
C8 H8 0.9300 . ?
C7 C7 1.397(8) 3 ?
C7 C6 1.458(6) . ?
C1 C2 1.438(7) . ?
C1 H1 0.9300 . ?
C5 C4 1.408(7) . ?
C5 H5 0.9300 . ?
C3 C2 1.339(8) . ?
C3 C4 1.428(8) . ?
C2 H2 0.9300 . ?
C4 H4 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
O1 Co1 O1 178.82(18) 14 . ?
O1 Co1 N1 92.39(13) 14 14 ?
O1 Co1 N1 88.40(13) . 14 ?
O1 Co1 N1 88.39(13) 14 . ?
O1 Co1 N1 92.39(13) . . ?
N1 Co1 N1 96.20(19) 14 . ?
O1 Co1 O3 88.91(15) 14 14 ?
O1 Co1 O3 90.25(15) . 14 ?
N1 Co1 O3 87.24(16) 14 14 ?
N1 Co1 O3 175.71(16) . 14 ?
O1 Co1 O3 90.26(15) 14 . ?
O1 Co1 O3 88.91(15) . . ?
N1 Co1 O3 175.71(16) 14 . ?
N1 Co1 O3 87.24(16) . . ?
O3 Co1 O3 89.4(3) 14 . ?
C3 S1 S1 103.8(2) . 2 ?
C6 O1 Co1 134.0(3) . . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Co1 121.3(3) . . ?
C5 N1 Co1 120.1(3) . . ?
Co1 O3 H3 109.5 . . ?
C7 C8 C7 118.1(6) . 4_655 ?
C7 C8 H8 120.9 . . ?
C7 C8 H8 120.9 4_655 . ?
C7 C7 C8 120.9(3) 3 . ?
C7 C7 C6 122.6(3) 3 . ?
C8 C7 C6 116.3(4) . . ?
N1 C1 C2 122.5(5) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
N1 C5 C4 120.8(5) . . ?
N1 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C2 C3 C4 118.9(6) . . ?
C2 C3 S1 126.3(5) . . ?
C4 C3 S1 114.5(4) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C5 C4 C3 119.7(5) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
O2 C6 O1 123.0(5) . . ?
O2 C6 C7 118.2(5) . . ?
O1 C6 C7 118.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 O1 C6 172.6(5) 14 . . . ?
N1 Co1 O1 C6 -91.2(5) . . . . ?
O3 Co1 O1 C6 85.4(5) 14 . . . ?
O3 Co1 O1 C6 -4.0(5) . . . . ?
O1 Co1 N1 C1 -156.7(4) 14 . . . ?
O1 Co1 N1 C1 22.4(4) . . . . ?
N1 Co1 N1 C1 111.0(4) 14 . . . ?
O3 Co1 N1 C1 -66.4(4) . . . . ?
O1 Co1 N1 C5 20.3(3) 14 . . . ?
O1 Co1 N1 C5 -160.6(3) . . . . ?
N1 Co1 N1 C5 -71.9(3) 14 . . . ?
O3 Co1 N1 C5 110.6(4) . . . . ?
C7 C8 C7 C7 -1.2(4) 4_655 . . 3 ?
C7 C8 C7 C6 174.3(4) 4_655 . . . ?
C5 N1 C1 C2 -2.1(7) . . . . ?
Co1 N1 C1 C2 175.0(4) . . . . ?
C1 N1 C5 C4 0.4(7) . . . . ?
Co1 N1 C5 C4 -176.7(4) . . . . ?
S1 S1 C3 C2 0.3(5) 2 . . . ?
S1 S1 C3 C4 175.3(4) 2 . . . ?
C4 C3 C2 C1 2.7(8) . . . . ?
S1 C3 C2 C1 177.6(4) . . . . ?
N1 C1 C2 C3 0.5(8) . . . . ?
N1 C5 C4 C3 2.8(8) . . . . ?
C2 C3 C4 C5 -4.4(8) . . . . ?
S1 C3 C4 C5 -179.8(4) . . . . ?
Co1 O1 C6 O2 6.8(8) . . . . ?
Co1 O1 C6 C7 -171.3(3) . . . . ?
C7 C7 C6 O2 42.8(8) 3 . . . ?
C8 C7 C6 O2 -132.6(4) . . . . ?
C7 C7 C6 O1 -139.0(6) 3 . . . ?
C8 C7 C6 O1 45.6(6) . . . . ?

_diffrn_measured_fraction_theta_max 1.00
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.00
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.098
_database_code_depnum_ccdc_archive 'CCDC 973648'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ss-954-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H18 Cu N4 O8 S4, 2(O)'
_chemical_formula_sum            'C30 H18 Cu N4 O10 S4'
_chemical_formula_weight         786.31

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 2/c'

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

_cell_length_a                   8.315(2)
_cell_length_b                   10.205(3)
_cell_length_c                   20.279(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.120(12)
_cell_angle_gamma                90.00
_cell_volume                     1582.6(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3019
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.82

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             798
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_process_details   multi-scan

_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_reflns_number            14034
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.45
_reflns_number_total             3617
_reflns_number_gt                3564
_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)+(0.1000P)²+4.0000P] 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         3617
_refine_ls_number_parameters     222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1713
_refine_ls_wR_factor_gt          0.1696
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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
Cu1 Cu 1.0000 1.16676(6) 0.2500 0.0436(3) Uani 1 2 d S . .
S1 S 0.55000(10) 0.72926(8) 0.01489(4) 0.0269(2) Uani 1 1 d . . .
S2 S 0.71484(12) 0.60608(8) -0.00648(4) 0.0271(2) Uani 1 1 d . . .
O1 O 0.2167(6) 0.6902(4) 0.11283(19) 0.0640(11) Uani 1 1 d . . .
O2 O 0.3790(6) 0.8254(4) 0.1944(3) 0.0890(17) Uani 1 1 d . . .
O3 O 0.3282(4) 0.1958(3) 0.12243(14) 0.0388(6) Uani 1 1 d . . .
O4 O 0.2672(4) 0.1603(3) 0.21850(15) 0.0364(6) Uani 1 1 d . . .
N1 N 0.9039(4) 0.3040(3) 0.17258(15) 0.0249(6) Uani 1 1 d . . .
N2 N 0.8729(4) 1.0301(3) 0.17741(15) 0.0246(6) Uani 1 1 d . . .
C1 C 0.9275(4) 0.2895(3) 0.11060(17) 0.0251(6) Uani 1 1 d . . .
H1 H 0.9850 0.2151 0.1046 0.030 Uiso 1 1 calc R . .
C2 C 0.8694(4) 0.3811(3) 0.05560(17) 0.0224(6) Uani 1 1 d . . .
H2 H 0.8884 0.3692 0.0137 0.027 Uiso 1 1 calc R . .
C3 C 0.7809(4) 0.4926(3) 0.06512(16) 0.0218(6) Uani 1 1 d . . .
C4 C 0.7532(4) 0.5066(3) 0.12803(17) 0.0249(6) Uani 1 1 d . . .
H4 H 0.6948 0.5793 0.1353 0.030 Uiso 1 1 calc R . .
C5 C 0.8148(4) 0.4093(3) 0.17975(17) 0.0245(6) Uani 1 1 d . . .
H5 H 0.7936 0.4173 0.2213 0.029 Uiso 1 1 calc R . .
C6 C 0.8674(4) 0.8332(3) 0.11145(17) 0.0234(6) Uani 1 1 d . . .
H6 H 0.9271 0.7639 0.1015 0.028 Uiso 1 1 calc R . .
C7 C 0.6873(4) 0.8444(3) 0.07708(17) 0.0216(6) Uani 1 1 d . . .
C8 C 0.5985(4) 0.9493(3) 0.09203(17) 0.0245(6) Uani 1 1 d . . .
H8 H 0.4777 0.9576 0.0690 0.029 Uiso 1 1 calc R . .
C9 C 0.6970(4) 1.0406(3) 0.14248(18) 0.0279(7) Uani 1 1 d . . .
H9 H 0.6404 1.1115 0.1527 0.034 Uiso 1 1 calc R . .
C10 C 0.9569(4) 0.9300(3) 0.16178(18) 0.0272(7) Uani 1 1 d . . .
H10 H 1.0779 0.9246 0.1850 0.033 Uiso 1 1 calc R . .
C11 C 0.3384(5) 0.2249(4) 0.18487(19) 0.0321(7) Uani 1 1 d . . .
C12 C 0.4288(5) 0.3506(4) 0.21808(19) 0.0296(7) Uani 1 1 d . . .
C13 C 0.3603(5) 0.4696(4) 0.18538(19) 0.0317(7) Uani 1 1 d . . .
H13 H 0.2642 0.4682 0.1418 0.038 Uiso 1 1 calc R . .
C14 C 0.4301(5) 0.5920(4) 0.2153(2) 0.0332(8) Uani 1 1 d . . .
C15 C 0.3294(6) 0.7007(5) 0.1713(2) 0.0456(11) Uani 1 1 d . . .
O5 O 0.1658(4) 0.9832(4) 0.0499(2) 0.0531(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
Cu1 N2 2.002(3) . ?
Cu1 N2 2.002(3) 2_755 ?
Cu1 N1 2.020(3) 2_765 ?
Cu1 N1 2.020(3) 1_565 ?
S1 C7 1.773(3) . ?
S1 S2 2.0281(12) . ?
S2 C3 1.768(3) . ?
O1 C15 1.193(6) . ?
O2 C15 1.363(7) . ?
O3 C11 1.271(5) . ?
O4 C11 1.251(5) . ?
N1 C5 1.344(4) . ?
N1 C1 1.354(4) . ?
N1 Cu1 2.020(3) 1_545 ?
N2 C10 1.343(4) . ?
N2 C9 1.356(4) . ?
C1 C2 1.389(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.409(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(4) . ?
C4 C5 1.388(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.386(4) . ?
C6 C10 1.405(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.400(4) . ?
C8 C9 1.388(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.506(5) . ?
C12 C12 1.369(7) 2_655 ?
C12 C13 1.393(5) . ?
C13 C14 1.410(5) . ?
C13 H13 0.9300 . ?
C14 C14 1.432(8) 2_655 ?
C14 C15 1.462(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N2 91.65(15) . 2_755 ?
N2 Cu1 N1 171.18(12) . 2_765 ?
N2 Cu1 N1 88.75(11) 2_755 2_765 ?
N2 Cu1 N1 88.75(11) . 1_565 ?
N2 Cu1 N1 171.18(12) 2_755 1_565 ?
N1 Cu1 N1 92.20(15) 2_765 1_565 ?
C7 S1 S2 105.20(11) . . ?
C3 S2 S1 104.39(11) . . ?
C5 N1 C1 118.3(3) . . ?
C5 N1 Cu1 122.4(2) . 1_545 ?
C1 N1 Cu1 119.2(2) . 1_545 ?
C10 N2 C9 119.4(3) . . ?
C10 N2 Cu1 122.0(2) . . ?
C9 N2 Cu1 118.6(2) . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C1 C2 C3 118.0(3) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 S2 125.3(2) . . ?
C2 C3 S2 115.3(2) . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N1 C5 C4 123.0(3) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C7 C6 C10 117.8(3) . . ?
C7 C6 H6 121.1 . . ?
C10 C6 H6 121.1 . . ?
C6 C7 C8 120.8(3) . . ?
C6 C7 S1 124.7(2) . . ?
C8 C7 S1 114.4(2) . . ?
C9 C8 C7 117.6(3) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
N2 C9 C8 122.4(3) . . ?
N2 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
N2 C10 C6 122.0(3) . . ?
N2 C10 H10 119.0 . . ?
C6 C10 H10 119.0 . . ?
O4 C11 O3 124.0(4) . . ?
O4 C11 C12 117.7(3) . . ?
O3 C11 C12 118.1(3) . . ?
C12 C12 C13 119.4(2) 2_655 . ?
C12 C12 C11 121.2(2) 2_655 . ?
C13 C12 C11 119.4(3) . . ?
C12 C13 C14 123.0(3) . . ?
C12 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C13 C14 C14 117.4(2) . 2_655 ?
C13 C14 C15 111.7(4) . . ?
C14 C14 C15 130.5(3) 2_655 . ?
O1 C15 O2 116.0(5) . . ?
O1 C15 C14 125.2(5) . . ?
O2 C15 C14 118.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 S1 S2 C3 82.57(15) . . . . ?
N2 Cu1 N2 C10 -50.0(2) 2_755 . . . ?
N1 Cu1 N2 C10 121.2(3) 1_565 . . . ?
N2 Cu1 N2 C9 130.9(3) 2_755 . . . ?
N1 Cu1 N2 C9 -57.9(3) 1_565 . . . ?
C5 N1 C1 C2 2.5(5) . . . . ?
Cu1 N1 C1 C2 -178.3(2) 1_545 . . . ?
N1 C1 C2 C3 -0.7(5) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C1 C2 C3 S2 178.8(2) . . . . ?
S1 S2 C3 C4 -12.5(3) . . . . ?
S1 S2 C3 C2 168.1(2) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
S2 C3 C4 C5 -179.3(2) . . . . ?
C1 N1 C5 C4 -3.1(5) . . . . ?
Cu1 N1 C5 C4 177.8(2) 1_545 . . . ?
C3 C4 C5 N1 1.8(5) . . . . ?
C10 C6 C7 C8 0.3(5) . . . . ?
C10 C6 C7 S1 -177.2(2) . . . . ?
S2 S1 C7 C6 -10.3(3) . . . . ?
S2 S1 C7 C8 172.1(2) . . . . ?
C6 C7 C8 C9 -0.3(5) . . . . ?
S1 C7 C8 C9 177.4(3) . . . . ?
C10 N2 C9 C8 1.7(5) . . . . ?
Cu1 N2 C9 C8 -179.2(3) . . . . ?
C7 C8 C9 N2 -0.7(5) . . . . ?
C9 N2 C10 C6 -1.7(5) . . . . ?
Cu1 N2 C10 C6 179.2(2) . . . . ?
C7 C6 C10 N2 0.7(5) . . . . ?
O4 C11 C12 C12 63.5(6) . . . 2_655 ?
O3 C11 C12 C12 -121.4(5) . . . 2_655 ?
O4 C11 C12 C13 -112.7(4) . . . . ?
O3 C11 C12 C13 62.4(5) . . . . ?
C12 C12 C13 C14 -0.5(6) 2_655 . . . ?
C11 C12 C13 C14 175.8(3) . . . . ?
C12 C13 C14 C14 -4.4(6) . . . 2_655 ?
C12 C13 C14 C15 -177.8(3) . . . . ?
C13 C14 C15 O1 -9.3(6) . . . . ?
C14 C14 C15 O1 178.3(5) 2_655 . . . ?
C13 C14 C15 O2 178.5(4) . . . . ?
C14 C14 C15 O2 6.2(8) 2_655 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.094
_database_code_depnum_ccdc_archive 'CCDC 973649'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_platon

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C15 H9 N2 Ni O6 S2), 2(C2 O), 11(O)'
_chemical_formula_sum            'C34 H18 N4 Ni2 O25 S4'
_chemical_formula_weight         1128.18

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'
N N 0.0061 0.0033 '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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/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                   15.8979(12)
_cell_length_b                   15.7892(12)
_cell_length_c                   20.3288(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.324(8)
_cell_angle_gamma                90.00
_cell_volume                     4897.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2557
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      19.03

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2280
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_process_details   multi-scan

_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_reflns_number            12718
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.68
_reflns_number_total             2187
_reflns_number_gt                1878
_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)+(0.1000P)²+0.0579P] 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         2187
_refine_ls_number_parameters     308
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2606
_refine_ls_wR_factor_gt          0.2556
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.156
_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 0.21744(11) 0.05982(10) 0.22301(9) 0.0203(7) Uani 1 1 d . . .
S1 S -0.1106(2) -0.2183(2) 0.13621(19) 0.0310(11) Uani 1 1 d . . .
S2 S -0.2250(2) -0.1577(2) 0.0932(2) 0.0311(11) Uani 1 1 d . . .
O1 O 0.2159(6) 0.2736(6) 0.2311(5) 0.028(2) Uani 1 1 d . . .
O2 O 0.1335(5) 0.1568(6) 0.2223(5) 0.027(3) Uani 1 1 d . . .
O3 O 0.3043(5) -0.0392(5) 0.2259(5) 0.021(2) Uani 1 1 d . . .
O4 O 0.3640(6) -0.0545(6) 0.3387(5) 0.034(3) Uani 1 1 d . . .
O6 O 0.3251(6) 0.1445(6) 0.2567(5) 0.030(3) Uani 1 1 d . . .
O5 O 0.2240(6) 0.0431(6) 0.3266(5) 0.028(2) Uani 1 1 d . . .
N1 N 0.1110(7) -0.0229(7) 0.1944(6) 0.024(3) Uani 1 1 d . . .
N2 N -0.2196(8) -0.0860(7) -0.1229(6) 0.022(3) Uani 1 1 d . . .
C1 C 0.0259(9) 0.0024(9) 0.1728(7) 0.020(3) Uani 1 1 d U . .
H1 H 0.0149 0.0603 0.1708 0.025 Uiso 1 1 calc R . .
C2 C -0.0446(9) -0.0508(9) 0.1538(7) 0.026(3) Uani 1 1 d U . .
H2 H -0.1014 -0.0296 0.1391 0.031 Uiso 1 1 calc R . .
C3 C -0.0292(9) -0.1374(9) 0.1569(7) 0.026(3) Uani 1 1 d U . .
C4 C 0.0586(10) -0.1650(9) 0.1803(8) 0.033(4) Uani 1 1 d U . .
H4 H 0.0717 -0.2225 0.1833 0.039 Uiso 1 1 calc R . .
C6 C -0.2184(9) -0.1327(9) 0.0095(7) 0.026(3) Uani 1 1 d U . .
C15 C 0.0000 0.4178(12) 0.2500 0.026(5) Uani 1 2 d SU . .
H15 H 0.0000 0.4767 0.2500 0.031 Uiso 1 2 calc SR . .
C14 C 0.0703(8) 0.3750(8) 0.2367(6) 0.017(3) Uani 1 1 d U . .
C12 C 0.0706(8) 0.2875(8) 0.2382(6) 0.017(3) Uani 1 1 d U . .
C13 C 0.0000 0.2456(12) 0.2500 0.017(4) Uani 1 2 d SU . .
H13 H 0.0000 0.1867 0.2500 0.020 Uiso 1 2 calc SR . .
C11 C 0.1464(9) 0.2346(10) 0.2295(7) 0.019(3) Uani 1 1 d U . .
C5 C 0.1224(10) -0.1078(10) 0.1981(8) 0.035(4) Uani 1 1 d U . .
H5A H 0.1795 -0.1278 0.2145 0.042 Uiso 1 1 calc R . .
C7 C -0.1457(10) -0.1445(10) -0.0132(8) 0.036(4) Uani 1 1 d U . .
H7 H -0.0951 -0.1686 0.0153 0.044 Uiso 1 1 calc R . .
C9 C -0.2896(10) -0.0760(9) -0.1002(8) 0.028(4) Uani 1 1 d U . .
H9 H -0.3401 -0.0536 -0.1300 0.033 Uiso 1 1 calc R . .
C8 C -0.1488(10) -0.1201(10) -0.0793(8) 0.033(4) Uani 1 1 d U . .
H8 H -0.0990 -0.1278 -0.0941 0.039 Uiso 1 1 calc R . .
C10 C -0.2915(10) -0.0971(10) -0.0350(8) 0.036(4) Uani 1 1 d U . .
H10 H -0.3416 -0.0873 -0.0211 0.043 Uiso 1 1 calc R . .
O8 O 0.0000 0.6363(10) 0.2500 0.069(6) Uani 1 2 d S . .
O11 O 0.2832(12) 0.8644(8) 0.1045(6) 0.090(5) Uani 1 1 d . . .
O9 O 0.0393(13) 0.6217(14) 0.1165(12) 0.148(8) Uani 1 1 d . . .
O10 O 0.2428(16) 0.6927(9) 0.0999(7) 0.150(10) Uani 1 1 d . . .
O12 O 0.139(2) 0.878(2) 0.9921(14) 0.27(2) Uani 1 1 d . . .
C18 C 0.5374(14) 0.9163(16) 0.4324(11) 0.083(7) Uani 1 1 d U . .
O7 O 0.4799(18) 0.9621(17) 0.4584(11) 0.170(9) Uani 1 1 d . . .
C16 C 0.3601(9) -0.0702(8) 0.2772(7) 0.017(3) Uiso 1 1 d . . .
O13 O 0.5703(18) 0.772(2) 0.5148(15) 0.214(13) Uani 1 1 d . . .
C17 C 0.6205(16) 0.8500(18) 0.4754(12) 0.099(8) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.029(9) . ?
Ni1 O3 2.076(8) . ?
Ni1 N1 2.086(11) . ?
Ni1 N2 2.087(11) 5 ?
Ni1 O5 2.095(9) . ?
Ni1 O6 2.128(9) . ?
S1 C3 1.781(14) . ?
S1 S2 2.023(5) . ?
S2 C6 1.778(15) . ?
O1 C11 1.257(16) . ?
O2 C11 1.248(16) . ?
O3 C16 1.261(16) . ?
O4 C16 1.259(16) . ?
N1 C5 1.353(18) . ?
N1 C1 1.359(17) . ?
N2 C9 1.329(17) . ?
N2 C8 1.334(18) . ?
N2 Ni1 2.087(11) 5 ?
C1 C2 1.368(19) . ?
C1 H1 0.9300 . ?
C2 C3 1.39(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.41(2) . ?
C4 C5 1.33(2) . ?
C4 H4 0.9300 . ?
C6 C7 1.37(2) . ?
C6 C10 1.38(2) . ?
C15 C14 1.395(16) . ?
C15 C14 1.395(16) 2 ?
C15 H15 0.9300 . ?
C14 C12 1.382(19) . ?
C14 C16 1.494(19) 4 ?
C12 C13 1.381(15) . ?
C12 C11 1.516(19) . ?
C13 C12 1.381(15) 2 ?
C13 H13 0.9300 . ?
C5 H5A 0.9300 . ?
C7 C8 1.39(2) . ?
C7 H7 0.9300 . ?
C9 C10 1.37(2) . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C10 H10 0.9300 . ?
C18 O7 1.38(3) . ?
C18 C17 1.72(3) . ?
C16 C14 1.494(19) 4_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O3 178.8(4) . . ?
O2 Ni1 N1 89.4(4) . . ?
O3 Ni1 N1 91.0(4) . . ?
O2 Ni1 N2 92.0(4) . 5 ?
O3 Ni1 N2 89.1(4) . 5 ?
N1 Ni1 N2 95.0(4) . 5 ?
O2 Ni1 O5 87.1(4) . . ?
O3 Ni1 O5 91.8(4) . . ?
N1 Ni1 O5 90.5(4) . . ?
N2 Ni1 O5 174.5(4) 5 . ?
O2 Ni1 O6 89.7(4) . . ?
O3 Ni1 O6 89.8(3) . . ?
N1 Ni1 O6 177.4(4) . . ?
N2 Ni1 O6 87.6(4) 5 . ?
O5 Ni1 O6 87.0(4) . . ?
C3 S1 S2 105.5(5) . . ?
C6 S2 S1 103.3(5) . . ?
C11 O2 Ni1 131.0(9) . . ?
C16 O3 Ni1 128.6(9) . . ?
C5 N1 C1 114.5(12) . . ?
C5 N1 Ni1 121.3(9) . . ?
C1 N1 Ni1 124.2(9) . . ?
C9 N2 C8 116.8(12) . . ?
C9 N2 Ni1 124.1(10) . 5 ?
C8 N2 Ni1 119.0(9) . 5 ?
N1 C1 C2 125.0(13) . . ?
N1 C1 H1 117.5 . . ?
C2 C1 H1 117.5 . . ?
C1 C2 C3 118.2(13) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C2 C3 C4 117.7(13) . . ?
C2 C3 S1 126.1(11) . . ?
C4 C3 S1 116.2(11) . . ?
C5 C4 C3 119.3(14) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C7 C6 C10 118.0(14) . . ?
C7 C6 S2 125.1(12) . . ?
C10 C6 S2 117.0(11) . . ?
C14 C15 C14 122.1(17) . 2 ?
C14 C15 H15 119.0 . . ?
C14 C15 H15 119.0 2 . ?
C12 C14 C15 118.6(12) . . ?
C12 C14 C16 125.8(12) . 4 ?
C15 C14 C16 115.6(12) . 4 ?
C13 C12 C14 118.9(12) . . ?
C13 C12 C11 117.9(13) . . ?
C14 C12 C11 123.1(12) . . ?
C12 C13 C12 122.8(17) . 2 ?
C12 C13 H13 118.6 . . ?
C12 C13 H13 118.6 2 . ?
O2 C11 O1 126.8(12) . . ?
O2 C11 C12 116.4(12) . . ?
O1 C11 C12 116.7(13) . . ?
C4 C5 N1 125.3(14) . . ?
C4 C5 H5A 117.3 . . ?
N1 C5 H5A 117.3 . . ?
C6 C7 C8 119.1(14) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
N2 C9 C10 123.6(14) . . ?
N2 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
N2 C8 C7 123.3(13) . . ?
N2 C8 H8 118.4 . . ?
C7 C8 H8 118.4 . . ?
C9 C10 C6 119.3(14) . . ?
C9 C10 H10 120.4 . . ?
C6 C10 H10 120.4 . . ?
O7 C18 C17 128(2) . . ?
O4 C16 O3 124.8(12) . . ?
O4 C16 C14 118.0(12) . 4_545 ?
O3 C16 C14 117.1(12) . 4_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 S1 S2 C6 75.8(7) . . . . ?
N1 Ni1 O2 C11 -173.4(12) . . . . ?
N2 Ni1 O2 C11 -78.4(12) 5 . . . ?
O5 Ni1 O2 C11 96.1(12) . . . . ?
O6 Ni1 O2 C11 9.1(12) . . . . ?
N1 Ni1 O3 C16 -112.8(11) . . . . ?
N2 Ni1 O3 C16 152.2(11) 5 . . . ?
O5 Ni1 O3 C16 -22.3(10) . . . . ?
O6 Ni1 O3 C16 64.7(10) . . . . ?
O2 Ni1 N1 C5 -166.7(12) . . . . ?
O3 Ni1 N1 C5 12.2(11) . . . . ?
N2 Ni1 N1 C5 101.3(12) 5 . . . ?
O5 Ni1 N1 C5 -79.6(11) . . . . ?
O2 Ni1 N1 C1 11.3(11) . . . . ?
O3 Ni1 N1 C1 -169.8(11) . . . . ?
N2 Ni1 N1 C1 -80.6(11) 5 . . . ?
O5 Ni1 N1 C1 98.4(11) . . . . ?
C5 N1 C1 C2 -2(2) . . . . ?
Ni1 N1 C1 C2 179.9(10) . . . . ?
N1 C1 C2 C3 0(2) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
C1 C2 C3 S1 178.8(10) . . . . ?
S2 S1 C3 C2 9.1(14) . . . . ?
S2 S1 C3 C4 -172.7(10) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
S1 C3 C4 C5 -178.5(12) . . . . ?
S1 S2 C6 C7 -7.1(14) . . . . ?
S1 S2 C6 C10 174.4(10) . . . . ?
C14 C15 C14 C12 -1.3(8) 2 . . . ?
C14 C15 C14 C16 179.4(12) 2 . . 4 ?
C15 C14 C12 C13 2.6(17) . . . . ?
C16 C14 C12 C13 -178.2(11) 4 . . . ?
C15 C14 C12 C11 -175.6(10) . . . . ?
C16 C14 C12 C11 4(2) 4 . . . ?
C14 C12 C13 C12 -1.3(9) . . . 2 ?
C11 C12 C13 C12 177.0(12) . . . 2 ?
Ni1 O2 C11 O1 9(2) . . . . ?
Ni1 O2 C11 C12 -169.8(8) . . . . ?
C13 C12 C11 O2 11.4(17) . . . . ?
C14 C12 C11 O2 -170.3(12) . . . . ?
C13 C12 C11 O1 -167.7(10) . . . . ?
C14 C12 C11 O1 10.5(19) . . . . ?
C3 C4 C5 N1 -2(2) . . . . ?
C1 N1 C5 C4 3(2) . . . . ?
Ni1 N1 C5 C4 -179.2(12) . . . . ?
C10 C6 C7 C8 0(2) . . . . ?
S2 C6 C7 C8 -178.3(11) . . . . ?
C8 N2 C9 C10 1(2) . . . . ?
Ni1 N2 C9 C10 177.0(11) 5 . . . ?
C9 N2 C8 C7 0(2) . . . . ?
Ni1 N2 C8 C7 -175.9(11) 5 . . . ?
C6 C7 C8 N2 -1(2) . . . . ?
N2 C9 C10 C6 -2(2) . . . . ?
C7 C6 C10 C9 1(2) . . . . ?
S2 C6 C10 C9 179.6(11) . . . . ?
Ni1 O3 C16 O4 11.6(19) . . . . ?
Ni1 O3 C16 C14 -164.2(8) . . . 4_545 ?

_diffrn_measured_fraction_theta_max 1.00
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 1.00
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.155
_database_code_depnum_ccdc_archive 'CCDC 973650'
