# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1039180'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 N5 Ni S4'
_chemical_formula_weight         565.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.2268(6)
_cell_length_b                   11.9210(9)
_cell_length_c                   13.1309(10)
_cell_angle_alpha                72.801(7)
_cell_angle_beta                 80.517(6)
_cell_angle_gamma                72.197(6)
_cell_volume                     1309.25(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582.0
_exptl_absorpt_coefficient_mu    4.228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8600
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         70.74
_reflns_number_total             4922
_reflns_number_gt                4063
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0994P)²+0.4027P] 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         4922
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1664
_refine_ls_wR_factor_gt          0.1539
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.004

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 0.60325(6) 0.04820(4) 0.60139(4) 0.04191(19) Uani 1 1 d . . .
S1 S 0.41905(9) 0.09137(7) 0.71850(6) 0.0474(2) Uani 1 1 d . . .
S2 S 0.72481(11) -0.10931(8) 0.71414(7) 0.0577(2) Uani 1 1 d . . .
S3 S 0.48287(9) 0.20293(7) 0.48550(6) 0.0494(2) Uani 1 1 d . . .
S4 S 0.78583(10) -0.00031(8) 0.48563(7) 0.0541(2) Uani 1 1 d . . .
N1 N 0.2927(5) -0.0186(3) 1.0028(3) 0.0749(9) Uani 1 1 d . . .
N2 N 0.6850(6) -0.2926(4) 0.9937(3) 0.1028(15) Uani 1 1 d . . .
N3 N 0.5109(5) 0.3635(3) 0.1972(3) 0.0742(9) Uani 1 1 d . . .
N4 N 0.9098(5) 0.0776(4) 0.2011(3) 0.0795(10) Uani 1 1 d . . .
N5 N 0.2271(4) 0.7413(3) 0.1490(2) 0.0525(7) Uani 1 1 d . . .
C1 C 0.3723(5) -0.0223(3) 0.9268(3) 0.0554(8) Uani 1 1 d . . .
C2 C 0.4720(4) -0.0246(3) 0.8316(2) 0.0474(7) Uani 1 1 d . . .
C3 C 0.6055(4) -0.1137(3) 0.8292(3) 0.0519(8) Uani 1 1 d . . .
C4 C 0.6500(5) -0.2134(4) 0.9214(3) 0.0677(10) Uani 1 1 d . . .
C5 C 0.5496(4) 0.2888(3) 0.2734(3) 0.0561(8) Uani 1 1 d . . .
C6 C 0.5973(4) 0.1979(3) 0.3691(2) 0.0459(7) Uani 1 1 d . . .
C7 C 0.7308(4) 0.1071(3) 0.3691(3) 0.0474(7) Uani 1 1 d . . .
C8 C 0.8292(4) 0.0931(3) 0.2747(3) 0.0569(8) Uani 1 1 d . . .
C9 C 0.3055(5) 0.6449(4) 0.1135(3) 0.0669(10) Uani 1 1 d . . .
H9 H 0.4021 0.6019 0.1364 0.080 Uiso 1 1 calc R . .
C10 C 0.2477(6) 0.6075(4) 0.0447(3) 0.0795(13) Uani 1 1 d . . .
H10 H 0.3033 0.5389 0.0213 0.095 Uiso 1 1 calc R . .
C11 C 0.1067(7) 0.6721(5) 0.0103(3) 0.0807(14) Uani 1 1 d . . .
H11 H 0.0653 0.6484 -0.0373 0.097 Uiso 1 1 calc R . .
C12 C 0.0272(5) 0.7714(4) 0.0463(3) 0.0704(10) Uani 1 1 d . . .
H12 H -0.0689 0.8162 0.0236 0.085 Uiso 1 1 calc R . .
C13 C 0.0896(5) 0.8049(3) 0.1159(3) 0.0591(8) Uani 1 1 d . . .
H13 H 0.0355 0.8728 0.1406 0.071 Uiso 1 1 calc R . .
C14 C 0.2916(6) 0.7778(4) 0.2273(3) 0.0768(13) Uani 1 1 d . . .
H14A H 0.2538 0.8655 0.2170 0.092 Uiso 1 1 calc R . .
H14B H 0.4020 0.7574 0.2146 0.092 Uiso 1 1 calc R . .
C15 C 0.2485(5) 0.7144(3) 0.3410(3) 0.0604(10) Uani 1 1 d . . .
C16 C 0.3322(5) 0.5986(4) 0.3890(3) 0.0697(11) Uani 1 1 d . . .
H16 H 0.4181 0.5596 0.3518 0.084 Uiso 1 1 calc R . .
C17 C 0.2892(5) 0.5394(4) 0.4930(3) 0.0646(9) Uani 1 1 d . . .
H17 H 0.3470 0.4611 0.5241 0.078 Uiso 1 1 calc R . .
C18 C 0.1623(4) 0.5945(3) 0.5507(2) 0.0455(7) Uani 1 1 d . A .
C19 C 0.0859(6) 0.7104(3) 0.5029(3) 0.0778(13) Uani 1 1 d . . .
H19 H 0.0024 0.7518 0.5403 0.093 Uiso 1 1 calc R . .
C20 C 0.1297(7) 0.7689(3) 0.3985(3) 0.0847(15) Uani 1 1 d . . .
H20 H 0.0743 0.8483 0.3682 0.102 Uiso 1 1 calc R . .
C21 C 0.1101(4) 0.5285(3) 0.6638(2) 0.0499(7) Uani 1 1 d . . .
C22 C -0.0647(9) 0.5407(8) 0.6647(6) 0.079(2) Uani 0.653(11) 1 d P A 1
H22A H -0.0788 0.5020 0.6140 0.118 Uiso 0.653(11) 1 calc PR A 1
H22B H -0.1199 0.6255 0.6457 0.118 Uiso 0.653(11) 1 calc PR A 1
H22C H -0.1020 0.5022 0.7349 0.118 Uiso 0.653(11) 1 calc PR A 1
C23 C 0.1219(14) 0.5957(10) 0.7432(6) 0.099(5) Uani 0.653(11) 1 d P A 1
H23A H 0.0675 0.5671 0.8101 0.148 Uiso 0.653(11) 1 calc PR A 1
H23B H 0.0782 0.6817 0.7155 0.148 Uiso 0.653(11) 1 calc PR A 1
H23C H 0.2273 0.5805 0.7540 0.148 Uiso 0.653(11) 1 calc PR A 1
C24 C 0.1864(12) 0.3986(6) 0.6944(7) 0.097(4) Uani 0.653(11) 1 d P A 1
H24A H 0.1372 0.3607 0.7602 0.146 Uiso 0.653(11) 1 calc PR A 1
H24B H 0.2915 0.3868 0.7039 0.146 Uiso 0.653(11) 1 calc PR A 1
H24C H 0.1808 0.3624 0.6393 0.146 Uiso 0.653(11) 1 calc PR A 1
C22' C 0.264(2) 0.462(2) 0.7285(11) 0.123(10) Uani 0.347(11) 1 d P A 2
H22D H 0.2363 0.4228 0.8010 0.185 Uiso 0.347(11) 1 calc PR A 2
H22E H 0.3134 0.5226 0.7281 0.185 Uiso 0.347(11) 1 calc PR A 2
H22F H 0.3322 0.4029 0.6944 0.185 Uiso 0.347(11) 1 calc PR A 2
C23' C 0.070(2) 0.4151(15) 0.6527(10) 0.093(6) Uani 0.347(11) 1 d P A 2
H23D H 0.1536 0.3694 0.6146 0.140 Uiso 0.347(11) 1 calc PR A 2
H23E H -0.0198 0.4416 0.6142 0.140 Uiso 0.347(11) 1 calc PR A 2
H23F H 0.0505 0.3644 0.7226 0.140 Uiso 0.347(11) 1 calc PR A 2
C24' C -0.003(5) 0.592(2) 0.7231(16) 0.28(3) Uani 0.347(11) 1 d P A 2
H24D H -0.0704 0.5425 0.7599 0.413 Uiso 0.347(11) 1 calc PR A 2
H24E H -0.0596 0.6654 0.6767 0.413 Uiso 0.347(11) 1 calc PR A 2
H24F H 0.0413 0.6120 0.7742 0.413 Uiso 0.347(11) 1 calc PR A 2


_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 S4 2.1362(10) . ?
Ni1 S1 2.1425(9) . ?
Ni1 S2 2.1427(9) . ?
Ni1 S3 2.1438(9) . ?
S1 C2 1.723(3) . ?
S2 C3 1.714(4) . ?
S3 C6 1.714(3) . ?
S4 C7 1.714(3) . ?
N1 C1 1.141(5) . ?
N2 C4 1.132(5) . ?
N3 C5 1.148(5) . ?
N4 C8 1.144(5) . ?
N5 C9 1.326(5) . ?
N5 C13 1.331(5) . ?
N5 C14 1.493(4) . ?
C1 C2 1.426(5) . ?
C2 C3 1.361(5) . ?
C3 C4 1.437(5) . ?
C5 C6 1.426(5) . ?
C6 C7 1.368(5) . ?
C7 C8 1.431(5) . ?
C9 C10 1.358(6) . ?
C10 C11 1.366(7) . ?
C11 C12 1.360(7) . ?
C12 C13 1.361(5) . ?
C14 C15 1.510(5) . ?
C15 C20 1.332(6) . ?
C15 C16 1.375(6) . ?
C16 C17 1.394(5) . ?
C17 C18 1.382(5) . ?
C18 C19 1.355(5) . ?
C18 C21 1.536(4) . ?
C19 C20 1.397(6) . ?
C21 C24' 1.364(18) . ?
C21 C24 1.455(7) . ?
C21 C23 1.524(7) . ?
C21 C23' 1.559(12) . ?
C21 C22 1.573(8) . ?
C21 C22' 1.635(16) . ?

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
S4 Ni1 S1 178.23(4) . . ?
S4 Ni1 S2 86.49(4) . . ?
S1 Ni1 S2 92.53(4) . . ?
S4 Ni1 S3 92.39(4) . . ?
S1 Ni1 S3 88.56(3) . . ?
S2 Ni1 S3 178.45(4) . . ?
C2 S1 Ni1 103.21(13) . . ?
C3 S2 Ni1 103.57(12) . . ?
C6 S3 Ni1 103.62(12) . . ?
C7 S4 Ni1 103.70(12) . . ?
C9 N5 C13 120.1(3) . . ?
C9 N5 C14 120.1(4) . . ?
C13 N5 C14 119.8(3) . . ?
N1 C1 C2 178.9(4) . . ?
C3 C2 C1 122.0(3) . . ?
C3 C2 S1 120.4(3) . . ?
C1 C2 S1 117.6(3) . . ?
C2 C3 C4 121.5(4) . . ?
C2 C3 S2 120.2(2) . . ?
C4 C3 S2 118.3(3) . . ?
N2 C4 C3 179.5(4) . . ?
N3 C5 C6 178.9(4) . . ?
C7 C6 C5 121.3(3) . . ?
C7 C6 S3 120.0(2) . . ?
C5 C6 S3 118.7(3) . . ?
C6 C7 C8 123.5(3) . . ?
C6 C7 S4 120.2(2) . . ?
C8 C7 S4 116.2(3) . . ?
N4 C8 C7 177.5(4) . . ?
N5 C9 C10 121.4(4) . . ?
C9 C10 C11 119.0(4) . . ?
C12 C11 C10 119.4(4) . . ?
C11 C12 C13 119.5(4) . . ?
N5 C13 C12 120.7(4) . . ?
N5 C14 C15 111.3(3) . . ?
C20 C15 C16 117.9(3) . . ?
C20 C15 C14 121.3(4) . . ?
C16 C15 C14 120.9(4) . . ?
C15 C16 C17 120.5(4) . . ?
C18 C17 C16 121.3(4) . . ?
C19 C18 C17 116.7(3) . . ?
C19 C18 C21 121.4(3) . . ?
C17 C18 C21 121.9(3) . . ?
C18 C19 C20 121.4(4) . . ?
C15 C20 C19 122.0(4) . . ?
C24' C21 C24 126.5(9) . . ?
C24' C21 C23 51(2) . . ?
C24 C21 C23 113.3(6) . . ?
C24' C21 C18 119.7(8) . . ?
C24 C21 C18 113.8(4) . . ?
C23 C21 C18 109.3(4) . . ?
C24' C21 C23' 111(2) . . ?
C24 C21 C23' 47.8(7) . . ?
C23 C21 C23' 144.2(6) . . ?
C18 C21 C23' 106.4(5) . . ?
C24' C21 C22 56(2) . . ?
C24 C21 C22 106.6(6) . . ?
C23 C21 C22 106.1(6) . . ?
C18 C21 C22 107.1(4) . . ?
C23' C21 C22 63.9(8) . . ?
C24' C21 C22' 110.8(19) . . ?
C24 C21 C22' 53.0(9) . . ?
C23 C21 C22' 67.7(9) . . ?
C18 C21 C22' 106.4(6) . . ?
C23' C21 C22' 100.7(11) . . ?
C22 C21 C22' 145.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        70.74
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.142
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1039181'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 N5 Ni S4'
_chemical_formula_weight         565.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.2682(14)
_cell_length_b                   11.9800(14)
_cell_length_c                   13.0643(16)
_cell_angle_alpha                72.936(4)
_cell_angle_beta                 80.962(4)
_cell_angle_gamma                71.930(3)
_cell_volume                     1314.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23931
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4896
_reflns_number_gt                3354
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0686P)²+0.0486P] 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         4896
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1193
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.006
_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 0.60074(4) 0.04755(3) 0.60349(3) 0.05672(16) Uani 1 1 d . . .
S1 S 0.41713(8) 0.09066(6) 0.72015(6) 0.0646(2) Uani 1 1 d . . .
S2 S 0.72106(10) -0.11035(7) 0.71602(7) 0.0770(3) Uani 1 1 d . . .
S3 S 0.48152(9) 0.20292(7) 0.48780(6) 0.0664(2) Uani 1 1 d . . .
S4 S 0.78294(9) -0.00013(7) 0.48844(6) 0.0724(2) Uani 1 1 d . . .
N1 N 0.2910(4) -0.0196(3) 1.0035(2) 0.0986(10) Uani 1 1 d . . .
N2 N 0.6825(5) -0.2937(3) 0.9942(3) 0.1303(13) Uani 1 1 d . . .
N3 N 0.5098(4) 0.3652(3) 0.2008(2) 0.1006(10) Uani 1 1 d . . .
N4 N 0.9073(4) 0.0785(3) 0.2055(2) 0.1033(10) Uani 1 1 d . . .
N5 N 0.2243(3) 0.7432(2) 0.15054(17) 0.0675(6) Uani 1 1 d . . .
C1 C 0.3698(4) -0.0231(3) 0.9278(3) 0.0747(8) Uani 1 1 d . . .
C2 C 0.4707(4) -0.0260(3) 0.8330(2) 0.0621(8) Uani 1 1 d . . .
C3 C 0.6018(4) -0.1142(3) 0.8310(2) 0.0671(8) Uani 1 1 d . . .
C4 C 0.6471(4) -0.2141(3) 0.9219(3) 0.0897(11) Uani 1 1 d . . .
C5 C 0.5486(4) 0.2902(3) 0.2760(3) 0.0727(8) Uani 1 1 d . . .
C6 C 0.5966(3) 0.1976(3) 0.3715(2) 0.0610(7) Uani 1 1 d . . .
C7 C 0.7280(3) 0.1073(3) 0.3726(2) 0.0617(7) Uani 1 1 d . . .
C8 C 0.8269(4) 0.0948(3) 0.2780(3) 0.0754(9) Uani 1 1 d . . .
C9 C 0.3041(4) 0.6480(3) 0.1152(3) 0.0893(10) Uani 1 1 d . . .
H9A H 0.4004 0.6049 0.1389 0.107 Uiso 1 1 calc R . .
C10 C 0.2467(6) 0.6124(4) 0.0446(3) 0.1071(13) Uani 1 1 d . . .
H10A H 0.3026 0.5446 0.0204 0.129 Uiso 1 1 calc R . .
C11 C 0.1081(6) 0.6762(4) 0.0098(3) 0.1060(13) Uani 1 1 d . . .
H11A H 0.0680 0.6533 -0.0393 0.127 Uiso 1 1 calc R . .
C12 C 0.0280(4) 0.7731(4) 0.0462(3) 0.0925(11) Uani 1 1 d . . .
H12A H -0.0680 0.8175 0.0228 0.111 Uiso 1 1 calc R . .
C13 C 0.0883(4) 0.8055(3) 0.1172(3) 0.0779(9) Uani 1 1 d . . .
H13A H 0.0331 0.8724 0.1427 0.094 Uiso 1 1 calc R . .
C14 C 0.2856(5) 0.7792(4) 0.2304(2) 0.1038(14) Uani 1 1 d . . .
H14A H 0.2457 0.8663 0.2208 0.125 Uiso 1 1 calc R . .
H14B H 0.3955 0.7601 0.2184 0.125 Uiso 1 1 calc R . .
C15 C 0.2440(4) 0.7147(3) 0.3437(2) 0.0768(9) Uani 1 1 d . . .
C16 C 0.3274(4) 0.6006(4) 0.3910(3) 0.0875(10) Uani 1 1 d . . .
H16A H 0.4127 0.5616 0.3538 0.105 Uiso 1 1 calc R . .
C17 C 0.2855(4) 0.5423(3) 0.4946(3) 0.0815(10) Uani 1 1 d . . .
H17A H 0.3446 0.4645 0.5258 0.098 Uiso 1 1 calc R . .
C18 C 0.1605(3) 0.5950(2) 0.5525(2) 0.0573(7) Uani 1 1 d . A .
C19 C 0.0824(5) 0.7090(3) 0.5041(3) 0.0988(12) Uani 1 1 d . . .
H19A H -0.0021 0.7494 0.5412 0.119 Uiso 1 1 calc R . .
C20 C 0.1240(6) 0.7680(3) 0.4006(3) 0.1074(14) Uani 1 1 d . . .
H20A H 0.0669 0.8468 0.3701 0.129 Uiso 1 1 calc R . .
C21 C 0.1105(3) 0.5292(3) 0.6651(2) 0.0635(8) Uani 1 1 d . . .
C22 C 0.1937(11) 0.4011(6) 0.6981(6) 0.130(4) Uani 0.644(10) 1 d P A 1
H22A H 0.1417 0.3534 0.6783 0.195 Uiso 0.644(10) 1 calc PR A 1
H22B H 0.1999 0.3767 0.7745 0.195 Uiso 0.644(10) 1 calc PR A 1
H22C H 0.2945 0.3887 0.6633 0.195 Uiso 0.644(10) 1 calc PR A 1
C23 C 0.1215(13) 0.5966(10) 0.7422(6) 0.127(5) Uani 0.644(10) 1 d P A 1
H23A H 0.0337 0.6656 0.7395 0.190 Uiso 0.644(10) 1 calc PR A 1
H23B H 0.2117 0.6236 0.7230 0.190 Uiso 0.644(10) 1 calc PR A 1
H23C H 0.1261 0.5437 0.8135 0.190 Uiso 0.644(10) 1 calc PR A 1
C24 C -0.0638(7) 0.5421(7) 0.6679(5) 0.100(3) Uani 0.644(10) 1 d P A 1
H24A H -0.1051 0.6012 0.6045 0.149 Uiso 0.644(10) 1 calc PR A 1
H24B H -0.1153 0.5680 0.7302 0.149 Uiso 0.644(10) 1 calc PR A 1
H24C H -0.0776 0.4650 0.6708 0.149 Uiso 0.644(10) 1 calc PR A 1
C22' C 0.014(4) 0.5938(15) 0.7319(17) 0.25(2) Uani 0.356(10) 1 d P A 2
H22D H -0.0807 0.6375 0.6993 0.368 Uiso 0.356(10) 1 calc PR A 2
H22E H 0.0592 0.6503 0.7439 0.368 Uiso 0.356(10) 1 calc PR A 2
H22F H -0.0054 0.5388 0.7992 0.368 Uiso 0.356(10) 1 calc PR A 2
C23' C 0.077(2) 0.4183(14) 0.6546(10) 0.127(6) Uani 0.356(10) 1 d P A 2
H23D H -0.0153 0.4426 0.6187 0.190 Uiso 0.356(10) 1 calc PR A 2
H23E H 0.0640 0.3659 0.7247 0.190 Uiso 0.356(10) 1 calc PR A 2
H23F H 0.1593 0.3758 0.6137 0.190 Uiso 0.356(10) 1 calc PR A 2
C24' C 0.2715(18) 0.463(2) 0.7300(9) 0.151(9) Uani 0.356(10) 1 d P A 2
H24D H 0.3530 0.4921 0.6874 0.226 Uiso 0.356(10) 1 calc PR A 2
H24E H 0.2968 0.3762 0.7416 0.226 Uiso 0.356(10) 1 calc PR A 2
H24F H 0.2564 0.4822 0.7978 0.226 Uiso 0.356(10) 1 calc PR A 2


_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 S4 2.1319(8) . ?
Ni1 S2 2.1349(8) . ?
Ni1 S3 2.1372(8) . ?
Ni1 S1 2.1418(8) . ?
S1 C2 1.721(3) . ?
S2 C3 1.717(3) . ?
S3 C6 1.719(3) . ?
S4 C7 1.702(3) . ?
N1 C1 1.136(4) . ?
N2 C4 1.133(4) . ?
N3 C5 1.138(4) . ?
N4 C8 1.134(4) . ?
N5 C13 1.317(4) . ?
N5 C9 1.318(4) . ?
N5 C14 1.483(4) . ?
C1 C2 1.432(5) . ?
C2 C3 1.343(4) . ?
C3 C4 1.425(5) . ?
C5 C6 1.428(4) . ?
C6 C7 1.354(4) . ?
C7 C8 1.435(5) . ?
C9 C10 1.358(5) . ?
C10 C11 1.346(5) . ?
C11 C12 1.343(5) . ?
C12 C13 1.353(5) . ?
C14 C15 1.507(4) . ?
C15 C20 1.332(5) . ?
C15 C16 1.358(5) . ?
C16 C17 1.385(4) . ?
C17 C18 1.365(4) . ?
C18 C19 1.347(4) . ?
C18 C21 1.526(4) . ?
C19 C20 1.386(5) . ?
C21 C22' 1.374(14) . ?
C21 C22 1.455(6) . ?
C21 C23 1.495(7) . ?
C21 C23' 1.504(12) . ?
C21 C24 1.570(6) . ?
C21 C24' 1.686(13) . ?

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
S4 Ni1 S2 86.47(3) . . ?
S4 Ni1 S3 92.45(3) . . ?
S2 Ni1 S3 178.50(3) . . ?
S4 Ni1 S1 178.49(3) . . ?
S2 Ni1 S1 92.58(3) . . ?
S3 Ni1 S1 88.48(3) . . ?
C2 S1 Ni1 102.85(11) . . ?
C3 S2 Ni1 103.41(11) . . ?
C6 S3 Ni1 103.31(11) . . ?
C7 S4 Ni1 103.52(11) . . ?
C13 N5 C9 120.5(3) . . ?
C13 N5 C14 119.4(3) . . ?
C9 N5 C14 120.1(3) . . ?
N1 C1 C2 178.9(4) . . ?
C3 C2 C1 122.4(3) . . ?
C3 C2 S1 120.8(2) . . ?
C1 C2 S1 116.8(3) . . ?
C2 C3 C4 122.2(3) . . ?
C2 C3 S2 120.3(2) . . ?
C4 C3 S2 117.5(3) . . ?
N2 C4 C3 179.6(4) . . ?
N3 C5 C6 179.0(4) . . ?
C7 C6 C5 122.2(3) . . ?
C7 C6 S3 119.8(2) . . ?
C5 C6 S3 118.0(2) . . ?
C6 C7 C8 122.9(3) . . ?
C6 C7 S4 120.9(2) . . ?
C8 C7 S4 116.3(2) . . ?
N4 C8 C7 176.4(4) . . ?
N5 C9 C10 120.4(4) . . ?
C11 C10 C9 119.3(4) . . ?
C12 C11 C10 119.7(4) . . ?
C11 C12 C13 119.4(4) . . ?
N5 C13 C12 120.7(3) . . ?
N5 C14 C15 111.6(2) . . ?
C20 C15 C16 117.9(3) . . ?
C20 C15 C14 120.9(4) . . ?
C16 C15 C14 121.2(4) . . ?
C15 C16 C17 120.2(3) . . ?
C18 C17 C16 122.3(3) . . ?
C19 C18 C17 115.9(3) . . ?
C19 C18 C21 121.6(3) . . ?
C17 C18 C21 122.5(3) . . ?
C18 C19 C20 122.0(3) . . ?
C15 C20 C19 121.6(3) . . ?
C22' C21 C22 124.8(9) . . ?
C22' C21 C23 42.3(15) . . ?
C22 C21 C23 111.6(6) . . ?
C22' C21 C23' 117.9(14) . . ?
C22 C21 C23' 49.4(6) . . ?
C23 C21 C23' 144.9(6) . . ?
C22' C21 C18 120.3(8) . . ?
C22 C21 C18 114.0(3) . . ?
C23 C21 C18 108.4(4) . . ?
C23' C21 C18 106.6(5) . . ?
C22' C21 C24 62.6(15) . . ?
C22 C21 C24 109.5(5) . . ?
C23 C21 C24 104.9(5) . . ?
C23' C21 C24 66.0(7) . . ?
C18 C21 C24 107.9(3) . . ?
C22' C21 C24' 104.0(14) . . ?
C22 C21 C24' 50.6(7) . . ?
C23 C21 C24' 68.4(7) . . ?
C23' C21 C24' 99.9(10) . . ?
C18 C21 C24' 105.2(5) . . ?
C24 C21 C24' 146.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.065
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1039182'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 N5 Ni S4'
_chemical_formula_weight         565.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.3162(9)
_cell_length_b                   12.0910(11)
_cell_length_c                   13.0809(13)
_cell_angle_alpha                73.081(8)
_cell_angle_beta                 81.247(8)
_cell_angle_gamma                71.461(8)
_cell_volume                     1333.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582.0
_exptl_absorpt_coefficient_mu    4.151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8783
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         70.71
_reflns_number_total             5013
_reflns_number_gt                3446
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1167P)²+0.0770P] 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         5013
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0669
_refine_ls_wR_factor_ref         0.2009
_refine_ls_wR_factor_gt          0.1753
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Ni1 Ni 0.59818(7) 0.04706(5) 0.60560(5) 0.0669(2) Uani 1 1 d . . .
S1 S 0.41537(12) 0.09005(9) 0.72180(8) 0.0762(3) Uani 1 1 d . . .
S2 S 0.71813(14) -0.11126(10) 0.71779(10) 0.0899(4) Uani 1 1 d . . .
S3 S 0.47944(13) 0.20310(9) 0.48971(9) 0.0780(3) Uani 1 1 d . . .
S4 S 0.78059(13) -0.00009(10) 0.49125(9) 0.0843(3) Uani 1 1 d . . .
N1 N 0.2903(7) -0.0206(5) 1.0038(4) 0.1183(16) Uani 1 1 d . . .
N2 N 0.6818(9) -0.2941(5) 0.9948(4) 0.161(3) Uani 1 1 d . . .
N3 N 0.5108(6) 0.3655(5) 0.2041(4) 0.1206(16) Uani 1 1 d . . .
N4 N 0.9052(6) 0.0822(5) 0.2090(4) 0.1224(16) Uani 1 1 d . . .
N5 N 0.2222(5) 0.7441(3) 0.1524(3) 0.0813(10) Uani 1 1 d . . .
C1 C 0.3679(6) -0.0239(4) 0.9283(4) 0.0879(12) Uani 1 1 d . . .
C2 C 0.4678(6) -0.0261(4) 0.8344(3) 0.0778(11) Uani 1 1 d . . .
C3 C 0.6002(6) -0.1157(4) 0.8317(3) 0.0808(11) Uani 1 1 d . . .
C4 C 0.6449(7) -0.2158(5) 0.9240(4) 0.1077(17) Uani 1 1 d . . .
C5 C 0.5472(6) 0.2911(4) 0.2798(4) 0.0879(12) Uani 1 1 d . . .
C6 C 0.5947(5) 0.1988(4) 0.3750(3) 0.0737(10) Uani 1 1 d . . .
C7 C 0.7267(5) 0.1091(4) 0.3750(3) 0.0763(10) Uani 1 1 d . . .
C8 C 0.8252(6) 0.0962(5) 0.2819(4) 0.0914(13) Uani 1 1 d . . .
C9 C 0.3024(7) 0.6494(5) 0.1163(4) 0.1055(16) Uani 1 1 d . . .
H9 H 0.3981 0.6061 0.1410 0.127 Uiso 1 1 calc R . .
C10 C 0.2489(10) 0.6142(6) 0.0450(5) 0.130(2) Uani 1 1 d . . .
H10 H 0.3065 0.5475 0.0204 0.155 Uiso 1 1 calc R . .
C11 C 0.1080(11) 0.6784(7) 0.0092(4) 0.129(2) Uani 1 1 d . . .
H11 H 0.0684 0.6552 -0.0397 0.155 Uiso 1 1 calc R . .
C12 C 0.0277(7) 0.7746(6) 0.0448(5) 0.1147(18) Uani 1 1 d . . .
H12 H -0.0676 0.8195 0.0202 0.138 Uiso 1 1 calc R . .
C13 C 0.0859(6) 0.8062(5) 0.1171(4) 0.0947(13) Uani 1 1 d . . .
H13 H 0.0294 0.8727 0.1424 0.114 Uiso 1 1 calc R . .
C14 C 0.2817(8) 0.7813(6) 0.2327(4) 0.120(2) Uani 1 1 d . . .
H14A H 0.2404 0.8678 0.2229 0.144 Uiso 1 1 calc R . .
H14B H 0.3913 0.7625 0.2217 0.144 Uiso 1 1 calc R . .
C15 C 0.2393(7) 0.7166(5) 0.3457(3) 0.0896(14) Uani 1 1 d . . .
C16 C 0.3256(6) 0.6012(6) 0.3931(4) 0.1089(18) Uani 1 1 d . . .
H16 H 0.4114 0.5634 0.3558 0.131 Uiso 1 1 calc R . .
C17 C 0.2849(6) 0.5412(5) 0.4962(4) 0.0947(14) Uani 1 1 d . . .
H17 H 0.3436 0.4634 0.5268 0.114 Uiso 1 1 calc R . .
C18 C 0.1582(5) 0.5956(3) 0.5538(3) 0.0707(10) Uani 1 1 d . A .
C19 C 0.0812(8) 0.7085(4) 0.5061(4) 0.116(2) Uani 1 1 d . . .
H19 H -0.0026 0.7488 0.5434 0.139 Uiso 1 1 calc R . .
C20 C 0.1214(9) 0.7679(5) 0.4030(4) 0.130(2) Uani 1 1 d . . .
H20 H 0.0633 0.8463 0.3734 0.156 Uiso 1 1 calc R . .
C21 C 0.1098(5) 0.5289(4) 0.6663(3) 0.0764(11) Uani 1 1 d . . .
C22 C -0.0652(12) 0.5439(12) 0.6682(8) 0.094(4) Uani 0.520(14) 1 d P A 1
H22A H -0.0826 0.5111 0.6143 0.141 Uiso 0.520(14) 1 calc PR A 1
H22B H -0.1207 0.6281 0.6543 0.141 Uiso 0.520(14) 1 calc PR A 1
H22C H -0.0988 0.5017 0.7373 0.141 Uiso 0.520(14) 1 calc PR A 1
C23 C 0.034(6) 0.600(3) 0.736(2) 0.42(4) Uani 0.520(14) 1 d P A 1
H23A H -0.0683 0.5943 0.7518 0.626 Uiso 0.520(14) 1 calc PR A 1
H23B H 0.0317 0.6821 0.7030 0.626 Uiso 0.520(14) 1 calc PR A 1
H23C H 0.0852 0.5712 0.8010 0.626 Uiso 0.520(14) 1 calc PR A 1
C24 C 0.1827(18) 0.3999(9) 0.6957(10) 0.113(5) Uani 0.520(14) 1 d P A 1
H24A H 0.2083 0.3708 0.6324 0.170 Uiso 0.520(14) 1 calc PR A 1
H24B H 0.1148 0.3600 0.7433 0.170 Uiso 0.520(14) 1 calc PR A 1
H24C H 0.2734 0.3835 0.7307 0.170 Uiso 0.520(14) 1 calc PR A 1
C22' C 0.262(2) 0.458(3) 0.7279(13) 0.188(11) Uani 0.480(14) 1 d P A 2
H22D H 0.3304 0.4057 0.6873 0.281 Uiso 0.480(14) 1 calc PR A 2
H22E H 0.2370 0.4097 0.7971 0.281 Uiso 0.480(14) 1 calc PR A 2
H22F H 0.3083 0.5143 0.7364 0.281 Uiso 0.480(14) 1 calc PR A 2
C23' C 0.067(4) 0.422(2) 0.6554(13) 0.212(16) Uani 0.480(14) 1 d P A 2
H23D H 0.1396 0.3837 0.6064 0.319 Uiso 0.480(14) 1 calc PR A 2
H23E H -0.0320 0.4492 0.6288 0.319 Uiso 0.480(14) 1 calc PR A 2
H23F H 0.0670 0.3650 0.7241 0.319 Uiso 0.480(14) 1 calc PR A 2
C24' C 0.122(2) 0.5920(15) 0.7468(10) 0.112(6) Uani 0.480(14) 1 d P A 2
H24D H 0.0769 0.5583 0.8149 0.168 Uiso 0.480(14) 1 calc PR A 2
H24E H 0.0705 0.6766 0.7232 0.168 Uiso 0.480(14) 1 calc PR A 2
H24F H 0.2273 0.5814 0.7537 0.168 Uiso 0.480(14) 1 calc PR A 2


_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 S4 2.1347(13) . ?
Ni1 S2 2.1379(12) . ?
Ni1 S1 2.1424(12) . ?
Ni1 S3 2.1447(12) . ?
S1 C2 1.720(4) . ?
S2 C3 1.709(5) . ?
S3 C6 1.711(4) . ?
S4 C7 1.717(4) . ?
N1 C1 1.134(7) . ?
N2 C4 1.119(6) . ?
N3 C5 1.137(6) . ?
N4 C8 1.136(6) . ?
N5 C9 1.326(7) . ?
N5 C13 1.326(6) . ?
N5 C14 1.491(6) . ?
C1 C2 1.425(7) . ?
C2 C3 1.363(7) . ?
C3 C4 1.441(6) . ?
C5 C6 1.427(6) . ?
C6 C7 1.357(6) . ?
C7 C8 1.425(7) . ?
C9 C10 1.345(8) . ?
C10 C11 1.368(10) . ?
C11 C12 1.337(9) . ?
C12 C13 1.353(7) . ?
C14 C15 1.516(6) . ?
C15 C20 1.318(8) . ?
C15 C16 1.384(8) . ?
C16 C17 1.392(7) . ?
C17 C18 1.385(7) . ?
C18 C19 1.336(6) . ?
C18 C21 1.535(6) . ?
C19 C20 1.389(8) . ?
C21 C24 1.449(10) . ?
C21 C23 1.39(2) . ?
C21 C24' 1.506(10) . ?
C21 C23' 1.518(17) . ?
C21 C22 1.580(11) . ?
C21 C22' 1.600(16) . ?

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
S4 Ni1 S2 86.57(5) . . ?
S4 Ni1 S1 178.67(5) . . ?
S2 Ni1 S1 92.41(5) . . ?
S4 Ni1 S3 92.23(5) . . ?
S2 Ni1 S3 178.39(5) . . ?
S1 Ni1 S3 88.78(5) . . ?
C2 S1 Ni1 103.35(18) . . ?
C3 S2 Ni1 103.72(16) . . ?
C6 S3 Ni1 103.48(15) . . ?
C7 S4 Ni1 103.76(17) . . ?
C9 N5 C13 119.3(4) . . ?
C9 N5 C14 121.2(5) . . ?
C13 N5 C14 119.5(5) . . ?
N1 C1 C2 178.3(5) . . ?
C3 C2 C1 122.4(4) . . ?
C3 C2 S1 120.1(4) . . ?
C1 C2 S1 117.4(4) . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 S2 120.3(3) . . ?
C4 C3 S2 118.4(4) . . ?
N2 C4 C3 178.9(9) . . ?
N3 C5 C6 178.9(6) . . ?
C7 C6 C5 121.3(4) . . ?
C7 C6 S3 120.5(3) . . ?
C5 C6 S3 118.2(4) . . ?
C6 C7 C8 123.8(4) . . ?
C6 C7 S4 120.0(3) . . ?
C8 C7 S4 116.2(4) . . ?
N4 C8 C7 177.9(6) . . ?
N5 C9 C10 121.6(6) . . ?
C9 C10 C11 118.8(6) . . ?
C12 C11 C10 119.6(6) . . ?
C11 C12 C13 119.5(6) . . ?
N5 C13 C12 121.2(5) . . ?
N5 C14 C15 110.8(4) . . ?
C20 C15 C16 117.5(5) . . ?
C20 C15 C14 121.9(6) . . ?
C16 C15 C14 120.6(6) . . ?
C15 C16 C17 120.5(5) . . ?
C18 C17 C16 121.0(5) . . ?
C19 C18 C17 116.4(4) . . ?
C19 C18 C21 122.2(4) . . ?
C17 C18 C21 121.4(4) . . ?
C18 C19 C20 122.5(5) . . ?
C15 C20 C19 122.1(5) . . ?
C24 C21 C23 126.3(11) . . ?
C24 C21 C24' 113.7(10) . . ?
C23 C21 C24' 33(3) . . ?
C24 C21 C23' 47.2(10) . . ?
C23 C21 C23' 124(3) . . ?
C24' C21 C23' 142.9(9) . . ?
C24 C21 C18 114.8(6) . . ?
C23 C21 C18 116.7(14) . . ?
C24' C21 C18 109.6(6) . . ?
C23' C21 C18 107.5(7) . . ?
C24 C21 C22 105.6(8) . . ?
C23 C21 C22 72(3) . . ?
C24' C21 C22 104.9(9) . . ?
C23' C21 C22 63.4(12) . . ?
C18 C21 C22 107.4(5) . . ?
C24 C21 C22' 51.8(10) . . ?
C23 C21 C22' 99(2) . . ?
C24' C21 C22' 70.1(13) . . ?
C23' C21 C22' 99.0(14) . . ?
C18 C21 C22' 106.8(7) . . ?
C22 C21 C22' 145.0(8) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        70.71
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.128
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1039183'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 N5 Ni S4'
_chemical_formula_weight         565.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.3555(11)
_cell_length_b                   12.1960(12)
_cell_length_c                   13.0415(14)
_cell_angle_alpha                73.212(9)
_cell_angle_beta                 81.693(9)
_cell_angle_gamma                71.004(10)
_cell_volume                     1344.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582.0
_exptl_absorpt_coefficient_mu    4.116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_T_max  0.539
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8818
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         70.85
_reflns_number_total             5054
_reflns_number_gt                2830
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1267P)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         5054
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0745
_refine_ls_wR_factor_ref         0.2462
_refine_ls_wR_factor_gt          0.1887
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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 0.59502(9) 0.04653(6) 0.60814(6) 0.0848(3) Uani 1 1 d . . .
S1 S 0.41315(16) 0.08896(11) 0.72375(11) 0.0960(4) Uani 1 1 d . . .
S2 S 0.71426(18) -0.11274(13) 0.71999(13) 0.1116(5) Uani 1 1 d . . .
S3 S 0.47699(16) 0.20296(12) 0.49256(11) 0.0976(4) Uani 1 1 d . . .
S4 S 0.77783(17) 0.00005(13) 0.49471(12) 0.1051(5) Uani 1 1 d . . .
N1 N 0.2896(8) -0.0224(6) 1.0048(5) 0.148(2) Uani 1 1 d . . .
N2 N 0.6786(10) -0.2950(7) 0.9953(5) 0.196(3) Uani 1 1 d . . .
N3 N 0.5070(8) 0.3678(6) 0.2076(5) 0.149(2) Uani 1 1 d . . .
N4 N 0.9017(8) 0.0837(6) 0.2139(5) 0.147(2) Uani 1 1 d . . .
N5 N 0.2202(6) 0.7455(5) 0.1550(3) 0.1014(13) Uani 1 1 d . . .
C1 C 0.3660(8) -0.0255(6) 0.9299(6) 0.1130(18) Uani 1 1 d . . .
C2 C 0.4664(7) -0.0278(5) 0.8357(4) 0.0975(15) Uani 1 1 d . . .
C3 C 0.5965(8) -0.1167(5) 0.8337(4) 0.1017(16) Uani 1 1 d . . .
C4 C 0.6423(9) -0.2172(6) 0.9254(6) 0.132(2) Uani 1 1 d . . .
C5 C 0.5469(7) 0.2918(6) 0.2823(5) 0.1100(17) Uani 1 1 d . . .
C6 C 0.5912(7) 0.1998(5) 0.3781(4) 0.0943(14) Uani 1 1 d . . .
C7 C 0.7230(7) 0.1101(5) 0.3784(4) 0.0938(14) Uani 1 1 d . . .
C8 C 0.8223(8) 0.0972(6) 0.2860(6) 0.1168(19) Uani 1 1 d . . .
C9 C 0.3020(9) 0.6541(7) 0.1188(6) 0.134(2) Uani 1 1 d . . .
H9 H 0.3979 0.6125 0.1442 0.161 Uiso 1 1 calc R . .
C10 C 0.2529(13) 0.6174(8) 0.0458(7) 0.166(4) Uani 1 1 d . . .
H10 H 0.3124 0.5514 0.0214 0.199 Uiso 1 1 calc R . .
C11 C 0.1138(14) 0.6806(10) 0.0097(6) 0.157(3) Uani 1 1 d . . .
H11 H 0.0760 0.6575 -0.0402 0.189 Uiso 1 1 calc R . .
C12 C 0.0303(9) 0.7754(8) 0.0445(6) 0.142(2) Uani 1 1 d . . .
H12 H -0.0644 0.8197 0.0182 0.171 Uiso 1 1 calc R . .
C13 C 0.0861(8) 0.8069(6) 0.1202(5) 0.1197(19) Uani 1 1 d . . .
H13 H 0.0283 0.8721 0.1464 0.144 Uiso 1 1 calc R . .
C14 C 0.2776(10) 0.7816(7) 0.2365(4) 0.142(3) Uani 1 1 d . . .
H14A H 0.2364 0.8678 0.2261 0.170 Uiso 1 1 calc R . .
H14B H 0.3870 0.7619 0.2272 0.170 Uiso 1 1 calc R . .
C15 C 0.2336(9) 0.7188(6) 0.3491(5) 0.1125(19) Uani 1 1 d . . .
C16 C 0.3215(7) 0.6050(7) 0.3947(5) 0.129(2) Uani 1 1 d . . .
H16 H 0.4073 0.5682 0.3572 0.154 Uiso 1 1 calc R . .
C17 C 0.2812(7) 0.5440(6) 0.4987(5) 0.1163(19) Uani 1 1 d . . .
H17 H 0.3412 0.4668 0.5291 0.140 Uiso 1 1 calc R . .
C18 C 0.1558(6) 0.5961(4) 0.5557(4) 0.0868(13) Uani 1 1 d . A .
C19 C 0.0759(9) 0.7084(5) 0.5081(5) 0.135(3) Uani 1 1 d . . .
H19 H -0.0077 0.7476 0.5459 0.162 Uiso 1 1 calc R . .
C20 C 0.1120(10) 0.7684(6) 0.4056(5) 0.148(3) Uani 1 1 d . . .
H20 H 0.0501 0.8450 0.3753 0.178 Uiso 1 1 calc R . .
C21 C 0.1089(7) 0.5292(5) 0.6676(4) 0.0941(14) Uani 1 1 d . . .
C22 C -0.0645(18) 0.5388(19) 0.6691(12) 0.158(8) Uani 0.66(3) 1 d P A 1
H22A H -0.0743 0.4815 0.6353 0.238 Uiso 0.66(3) 1 calc PR A 1
H22B H -0.1192 0.6183 0.6310 0.238 Uiso 0.66(3) 1 calc PR A 1
H22C H -0.1049 0.5224 0.7420 0.238 Uiso 0.66(3) 1 calc PR A 1
C23 C 0.106(2) 0.6001(15) 0.7478(9) 0.134(6) Uani 0.66(3) 1 d P A 1
H23A H 0.0607 0.5666 0.8153 0.201 Uiso 0.66(3) 1 calc PR A 1
H23B H 0.0483 0.6824 0.7208 0.201 Uiso 0.66(3) 1 calc PR A 1
H23C H 0.2078 0.5959 0.7574 0.201 Uiso 0.66(3) 1 calc PR A 1
C24 C 0.197(3) 0.4053(12) 0.7015(14) 0.226(17) Uani 0.66(3) 1 d P A 1
H24A H 0.1394 0.3625 0.7559 0.339 Uiso 0.66(3) 1 calc PR A 1
H24B H 0.2887 0.3998 0.7298 0.339 Uiso 0.66(3) 1 calc PR A 1
H24C H 0.2205 0.3709 0.6412 0.339 Uiso 0.66(3) 1 calc PR A 1
C22' C 0.249(5) 0.489(5) 0.735(2) 0.22(3) Uani 0.34(3) 1 d P A 2
H22D H 0.2449 0.4214 0.7934 0.328 Uiso 0.34(3) 1 calc PR A 2
H22E H 0.2504 0.5542 0.7618 0.328 Uiso 0.34(3) 1 calc PR A 2
H22F H 0.3395 0.4677 0.6901 0.328 Uiso 0.34(3) 1 calc PR A 2
C23' C 0.076(5) 0.421(3) 0.652(2) 0.165(17) Uani 0.34(3) 1 d P A 2
H23D H 0.1690 0.3668 0.6316 0.248 Uiso 0.34(3) 1 calc PR A 2
H23E H 0.0060 0.4470 0.5971 0.248 Uiso 0.34(3) 1 calc PR A 2
H23F H 0.0340 0.3810 0.7182 0.248 Uiso 0.34(3) 1 calc PR A 2
C24' C -0.019(5) 0.591(3) 0.729(3) 0.21(3) Uani 0.34(3) 1 d P A 2
H24D H -0.0840 0.5414 0.7582 0.308 Uiso 0.34(3) 1 calc PR A 2
H24E H -0.0742 0.6655 0.6837 0.308 Uiso 0.34(3) 1 calc PR A 2
H24F H 0.0182 0.6065 0.7872 0.308 Uiso 0.34(3) 1 calc PR A 2


_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 S4 2.1346(16) . ?
Ni1 S2 2.1374(16) . ?
Ni1 S1 2.1383(15) . ?
Ni1 S3 2.1400(15) . ?
S1 C2 1.719(5) . ?
S2 C3 1.714(6) . ?
S3 C6 1.708(6) . ?
S4 C7 1.722(5) . ?
N1 C1 1.126(8) . ?
N2 C4 1.108(8) . ?
N3 C5 1.143(7) . ?
N4 C8 1.127(8) . ?
N5 C9 1.301(8) . ?
N5 C13 1.303(8) . ?
N5 C14 1.483(7) . ?
C1 C2 1.436(9) . ?
C2 C3 1.344(8) . ?
C3 C4 1.440(8) . ?
C5 C6 1.424(8) . ?
C6 C7 1.356(8) . ?
C7 C8 1.425(8) . ?
C9 C10 1.351(11) . ?
C10 C11 1.350(12) . ?
C11 C12 1.329(11) . ?
C12 C13 1.376(9) . ?
C14 C15 1.515(7) . ?
C15 C20 1.330(10) . ?
C15 C16 1.370(9) . ?
C16 C17 1.409(8) . ?
C17 C18 1.367(8) . ?
C18 C19 1.340(7) . ?
C18 C21 1.533(7) . ?
C19 C20 1.380(9) . ?
C21 C24 1.436(12) . ?
C21 C24' 1.46(3) . ?
C21 C23' 1.52(2) . ?
C21 C23 1.530(12) . ?
C21 C22' 1.55(3) . ?
C21 C22 1.585(14) . ?

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
S4 Ni1 S2 86.52(6) . . ?
S4 Ni1 S1 178.71(6) . . ?
S2 Ni1 S1 92.30(6) . . ?
S4 Ni1 S3 92.25(6) . . ?
S2 Ni1 S3 178.26(6) . . ?
S1 Ni1 S3 88.92(6) . . ?
C2 S1 Ni1 103.2(2) . . ?
C3 S2 Ni1 103.6(2) . . ?
C6 S3 Ni1 103.8(2) . . ?
C7 S4 Ni1 103.5(2) . . ?
C9 N5 C13 120.5(6) . . ?
C9 N5 C14 120.8(7) . . ?
C13 N5 C14 118.7(6) . . ?
N1 C1 C2 178.2(7) . . ?
C3 C2 C1 122.2(5) . . ?
C3 C2 S1 120.7(5) . . ?
C1 C2 S1 117.1(5) . . ?
C2 C3 C4 122.0(6) . . ?
C2 C3 S2 120.2(4) . . ?
C4 C3 S2 117.8(6) . . ?
N2 C4 C3 179.4(11) . . ?
N3 C5 C6 177.5(8) . . ?
C7 C6 C5 120.2(5) . . ?
C7 C6 S3 120.2(4) . . ?
C5 C6 S3 119.6(5) . . ?
C6 C7 C8 124.2(5) . . ?
C6 C7 S4 120.2(4) . . ?
C8 C7 S4 115.6(5) . . ?
N4 C8 C7 178.2(7) . . ?
N5 C9 C10 122.5(8) . . ?
C11 C10 C9 117.2(8) . . ?
C12 C11 C10 120.9(8) . . ?
C11 C12 C13 119.0(8) . . ?
N5 C13 C12 119.9(7) . . ?
N5 C14 C15 111.2(4) . . ?
C20 C15 C16 118.2(6) . . ?
C20 C15 C14 123.0(7) . . ?
C16 C15 C14 118.8(7) . . ?
C15 C16 C17 119.8(7) . . ?
C18 C17 C16 121.4(6) . . ?
C19 C18 C17 116.3(6) . . ?
C19 C18 C21 122.0(5) . . ?
C17 C18 C21 121.7(5) . . ?
C18 C19 C20 123.0(6) . . ?
C15 C20 C19 121.3(7) . . ?
C24 C21 C24' 125.3(13) . . ?
C24 C21 C23' 52.5(13) . . ?
C24' C21 C23' 109(2) . . ?
C24 C21 C23 112.7(11) . . ?
C24' C21 C23 50(2) . . ?
C23' C21 C23 145.4(12) . . ?
C24 C21 C18 114.7(7) . . ?
C24' C21 C18 120.0(11) . . ?
C23' C21 C18 105.6(11) . . ?
C23 C21 C18 108.9(6) . . ?
C24 C21 C22' 58.4(16) . . ?
C24' C21 C22' 106(2) . . ?
C23' C21 C22' 111(2) . . ?
C23 C21 C22' 62.3(19) . . ?
C18 C21 C22' 105.3(13) . . ?
C24 C21 C22 109.7(12) . . ?
C24' C21 C22 52(2) . . ?
C23' C21 C22 64.1(16) . . ?
C23 C21 C22 101.9(9) . . ?
C18 C21 C22 108.2(6) . . ?
C22' C21 C22 146.2(14) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        70.85
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.127
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       'Magnetic properties'
