# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_03685
_database_code_depnum_ccdc_archive 'CCDC 2476949'
loop_
_audit_author_name
_audit_author_address
'Josefina Perles'
;UNIVERSIDAD AUTONOMA DE MADRID
Spain
;
_audit_update_record             
;
2025-07-29 deposited with the CCDC.	2026-02-18 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            CV8_250K
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 N6 Ni O2 S2'
_chemical_formula_iupac          ?
_chemical_formula_weight         447.18

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.3593(3)
_cell_length_b                   16.3702(7)
_cell_length_c                   10.7142(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.787(2)
_cell_angle_gamma                90
_cell_volume                     916.67(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4711
_cell_measurement_theta_min      3.1616
_cell_measurement_theta_max      23.8461
_cell_measurement_temperature    250.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear intense yellow-green'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.081
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             460

_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.90

_exptl_special_details           
;
;

_diffrn_ambient_temperature      250.(2)

_diffrn_source                   'sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            26769
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_theta_min         3.90
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12

_refine_special_details          
;
;

_reflns_number_total             1679
_reflns_number_gt                1373
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0675
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.052
_refine_ls_number_reflns         1679
_refine_ls_number_parameters     128
_refine_ls_number_restraints     1
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0252P)²+0.7314P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
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'

_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4158(5) 0.38372(15) 0.5822(2) 0.0299(6) Uani d . . . 1 . .
C C2 0.1161(5) 0.42651(15) 0.2765(2) 0.0311(6) Uani d . . . 1 . .
H H2 -0.011377 0.463099 0.235853 0.037000 Uiso calc U . R 1 . .
C C3 0.2390(5) 0.38127(15) 0.1888(2) 0.0296(6) Uani d . . . 1 . .
C C4 0.1249(5) 0.38984(16) 0.0590(2) 0.0358(6) Uani d . . . 1 . .
H H4 -0.025169 0.421123 0.034962 0.043000 Uiso calc U . R 1 . .
C C5 0.2266(5) 0.35360(16) -0.0351(2) 0.0390(7) Uani d . . . 1 . .
H H5 0.145201 0.359581 -0.121765 0.047000 Uiso calc U . R 1 . .
C C6 0.4491(5) 0.30849(15) -0.0006(2) 0.0329(6) Uani d . . . 1 . .
C C7 0.5660(5) 0.29916(15) 0.1275(2) 0.0323(6) Uani d . . . 1 . .
H H7 0.717230 0.268345 0.150684 0.039000 Uiso calc U . R 1 . .
C C8 0.4627(5) 0.33466(15) 0.2212(2) 0.0311(6) Uani d . . . 1 . .
H H8 0.543326 0.327474 0.307768 0.037000 Uiso calc U . R 1 . .
N N1 0.1508(4) 0.42534(12) 0.39989(19) 0.0295(5) Uani d . . . 1 . .
N N2 0.3251(4) 0.36661(12) 0.4619(2) 0.0322(5) Uani d . . . 1 . .
N N3 0.5988(4) 0.33618(14) 0.6494(2) 0.0428(6) Uani d . . . 1 . .
H H3A 0.655287 0.294777 0.612809 0.051000 Uiso calc U . R 1 . .
H H3B 0.662009 0.346532 0.729815 0.051000 Uiso calc U . R 1 . .
Ni Ni1 0.000000 0.500000 0.500000 0.02628(14) Uani d . P S 1 . .
O O1 0.5462(4) 0.27527(12) -0.09674(18) 0.0451(5) Uani d . . D 1 . .
H H1O 0.652(5) 0.2373(16) -0.068(3) 0.062(11) Uiso d . . D 1 . .
S S1 0.30780(13) 0.46476(4) 0.65873(6) 0.03754(19) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N2 . 1.303(3) ?
C1 N3 . 1.332(3) ?
C1 S1 . 1.725(2) ?
C2 N1 . 1.293(3) ?
C2 C3 . 1.463(3) ?
C3 C4 . 1.397(3) ?
C3 C8 . 1.399(3) ?
C4 C5 . 1.381(3) ?
C5 C6 . 1.382(4) ?
C6 O1 . 1.366(3) ?
C6 C7 . 1.385(4) ?
C7 C8 . 1.378(3) ?
N1 N2 . 1.401(3) ?
N1 Ni1 . 1.9187(19) ?
Ni1 S1 . 2.1689(7) ?
Ni1 S1 3_566 2.1689(7) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 C1 N3 . . 118.5(2) ?
N2 C1 S1 . . 123.0(2) ?
N3 C1 S1 . . 118.5(2) ?
N1 C2 C3 . . 131.7(2) ?
C4 C3 C8 . . 117.6(2) ?
C4 C3 C2 . . 115.4(2) ?
C8 C3 C2 . . 126.9(2) ?
C5 C4 C3 . . 121.8(2) ?
C4 C5 C6 . . 119.4(2) ?
O1 C6 C5 . . 117.5(2) ?
O1 C6 C7 . . 122.6(2) ?
C5 C6 C7 . . 119.9(2) ?
C8 C7 C6 . . 120.6(2) ?
C7 C8 C3 . . 120.7(2) ?
C2 N1 N2 . . 115.2(2) ?
C2 N1 Ni1 . . 125.35(17) ?
N2 N1 Ni1 . . 119.40(15) ?
C1 N2 N1 . . 112.6(2) ?
N1 Ni1 N1 3_566 . 180.00(10) ?
N1 Ni1 S1 3_566 . 94.16(6) ?
N1 Ni1 S1 . . 85.84(7) ?
N1 Ni1 S1 3_566 3_566 85.84(7) ?
N1 Ni1 S1 . 3_566 94.16(6) ?
S1 Ni1 S1 . 3_566 180.000000 ?
C1 S1 Ni1 . . 96.25(9) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C2 C3 C4 . . . . 170.9(3) ?
N1 C2 C3 C8 . . . . -12.6(4) ?
C8 C3 C4 C5 . . . . 0.3(4) ?
C2 C3 C4 C5 . . . . 177.1(2) ?
C3 C4 C5 C6 . . . . -0.9(4) ?
C4 C5 C6 O1 . . . . -178.5(2) ?
C4 C5 C6 C7 . . . . 0.8(4) ?
O1 C6 C7 C8 . . . . 179.2(2) ?
C5 C6 C7 C8 . . . . -0.1(4) ?
C6 C7 C8 C3 . . . . -0.5(4) ?
C4 C3 C8 C7 . . . . 0.4(4) ?
C2 C3 C8 C7 . . . . -176.0(2) ?
C3 C2 N1 N2 . . . . -4.9(4) ?
C3 C2 N1 Ni1 . . . . 171.4(2) ?
N3 C1 N2 N1 . . . . -174.7(2) ?
S1 C1 N2 N1 . . . . 5.8(3) ?
C2 N1 N2 C1 . . . . 159.3(2) ?
Ni1 N1 N2 C1 . . . . -17.3(3) ?
N2 C1 S1 Ni1 . . . . 5.6(2) ?
N3 C1 S1 Ni1 . . . . -173.89(19) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2 H2 S1 3_566 0.940000 2.450000 3.083(2) 124.900000 ?
C7 H7 N3 4_665 0.940000 2.670000 3.581(3) 163.600000 ?
N3 H3B O1 1_556 0.870000 2.390000 2.969(3) 124.400000 ?
O1 H1O N1 4_665 0.853(18) 2.68(3) 3.333(3) 134.(3) ?
O1 H1O N2 4_665 0.853(18) 1.93(2) 2.758(3) 164.(3) ?



####################################################################### 
# 
# 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_03719
_database_code_depnum_ccdc_archive 'CCDC 2476950'
loop_
_audit_author_name
_audit_author_address
'Josefina Perles'
;UNIVERSIDAD AUTONOMA DE MADRID
Spain
;
_audit_update_record             
;
2025-07-29 deposited with the CCDC.	2026-02-18 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            CV14.3_150K
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H50 N12 Ni O10 S2'
_chemical_formula_iupac          ?
_chemical_formula_weight         981.75

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1806(6)
_cell_length_b                   11.4484(9)
_cell_length_c                   13.8901(10)
_cell_angle_alpha                76.331(2)
_cell_angle_beta                 86.624(3)
_cell_angle_gamma                83.694(3)
_cell_volume                     1102.16(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6077
_cell_measurement_theta_min      2.8557
_cell_measurement_theta_max      26.1373
_cell_measurement_temperature    150.(2)

_exptl_crystal_description       ribbon
_exptl_crystal_colour            'clear intense orange-brown'
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.009
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             514

_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.99

_exptl_special_details           
;
;

_diffrn_ambient_temperature      150.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              ?
_diffrn_source_power             1.50
_diffrn_source_current           30.0
_diffrn_source_voltage           50

_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            7967
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16

_refine_special_details          
;
;

_reflns_number_total             4029
_reflns_number_gt                3215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0878
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_number_reflns         4029
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²+0.2149P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.409
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
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'

_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1365)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.1383(3) 0.74749(18) 0.52018(15) 0.0135(5) Uani d . . . 1 . .
C C2 0.0177(3) 0.88824(19) 0.70594(15) 0.0137(5) Uani d . . . 1 . .
H H2 -0.018030 0.969677 0.709114 0.016000 Uiso calc U . R 1 . .
C C3 0.0517(3) 0.80772(19) 0.80214(15) 0.0144(5) Uani d . . . 1 . .
C C4 0.1263(3) 0.68608(19) 0.82225(16) 0.0170(5) Uani d . . . 1 . .
H H4 0.158178 0.647567 0.769141 0.020000 Uiso calc U . R 1 . .
C C5 0.1535(3) 0.6222(2) 0.91873(16) 0.0182(5) Uani d . . . 1 . .
H H5 0.205058 0.540224 0.931313 0.022000 Uiso calc U . R 1 . .
C C6 0.1067(3) 0.6762(2) 0.99757(16) 0.0172(5) Uani d . . . 1 . .
C C7 0.0336(3) 0.7965(2) 0.97926(16) 0.0180(5) Uani d . . . 1 . .
H H7 0.001022 0.834266 1.032725 0.022000 Uiso calc U . R 1 . .
C C8 0.0090(3) 0.86025(19) 0.88324(16) 0.0169(5) Uani d . . . 1 . .
H H8 -0.038676 0.942956 0.871314 0.020000 Uiso calc U . R 1 . .
C C9 0.1927(3) 0.52299(18) 0.55318(15) 0.0133(5) Uani d . . . 1 . .
C C10 0.2957(3) 0.43085(19) 0.51672(16) 0.0163(5) Uani d . . . 1 . .
H H10 0.361558 0.450108 0.454569 0.020000 Uiso calc U . R 1 . .
C C11 0.3029(3) 0.3136(2) 0.56918(16) 0.0180(5) Uani d . . . 1 . .
H H11 0.376011 0.251674 0.544820 0.022000 Uiso calc U . R 1 . .
C C12 0.2025(3) 0.28615(19) 0.65816(16) 0.0167(5) Uani d . . . 1 . .
C C13 0.0939(3) 0.3747(2) 0.69463(16) 0.0168(5) Uani d . . . 1 . .
H H13 0.023056 0.353923 0.755098 0.020000 Uiso calc U . R 1 . .
C C14 0.0894(3) 0.4929(2) 0.64262(15) 0.0158(5) Uani d . . . 1 . .
H H14 0.016119 0.554336 0.667417 0.019000 Uiso calc U . R 1 . .
N N1 0.1970(2) 0.63987(15) 0.49596(13) 0.0145(4) Uani d . . . 1 . .
H H1N 0.244217 0.645615 0.435298 0.017000 Uiso calc U . R 1 . .
N N2 0.0686(3) 0.75195(15) 0.60814(13) 0.0148(4) Uani d . . . 1 . .
N N3 0.0260(2) 0.87200(15) 0.61659(13) 0.0138(4) Uani d . . . 1 . .
N N4 0.2135(3) 0.16255(17) 0.71545(14) 0.0225(5) Uani d . . . 1 . .
Ni Ni1 0.000000 1.000000 0.500000 0.01296(12) Uani d . P S 1 . .
O O1 0.1283(2) 0.61625(14) 1.09286(11) 0.0244(4) Uani d . . . 1 . .
H H1O 0.171541 0.544488 1.095088 0.029000 Uiso calc U . R 1 . .
O O2 0.1188(3) 0.13896(15) 0.79369(12) 0.0325(4) Uani d . . . 1 . .
O O3 0.3160(3) 0.08565(15) 0.68517(13) 0.0329(4) Uani d . . . 1 . .
S S1 0.17063(8) 0.87572(5) 0.42734(4) 0.01867(15) Uani d . . . 1 . .
N N5 0.4704(3) 0.74830(16) 0.15714(13) 0.0206(4) Uani d . . . 1 . .
O O4 0.3609(2) 0.63152(15) 0.30118(11) 0.0259(4) Uani d . . . 1 . .
C C15 0.3675(3) 0.7284(2) 0.24096(17) 0.0228(5) Uani d . . . 1 . .
H H15 0.291668 0.795805 0.255631 0.027000 Uiso calc U . R 1 . .
C C16 0.4616(4) 0.8665(2) 0.09019(18) 0.0324(6) Uani d . . . 1 . .
H H16A 0.587676 0.893402 0.078756 0.049000 Uiso calc U . R 1 . .
H H16B 0.379218 0.923901 0.119466 0.049000 Uiso calc U . R 1 . .
H H16C 0.412104 0.862190 0.026998 0.049000 Uiso calc U . R 1 . .
C C17 0.5827(4) 0.6509(2) 0.12456(18) 0.0271(6) Uani d . . . 1 . .
H H17A 0.708656 0.674808 0.104262 0.041000 Uiso calc U . R 1 . .
H H17B 0.523978 0.633400 0.068286 0.041000 Uiso calc U . R 1 . .
H H17C 0.591411 0.578626 0.179082 0.041000 Uiso calc U . R 1 . .
N N6 0.4158(3) 0.24571(17) 1.24203(13) 0.0198(4) Uani d . . . 1 . .
O O5 0.3148(2) 0.40259(15) 1.11794(12) 0.0304(4) Uani d . . . 1 . .
C C18 0.3501(3) 0.3590(2) 1.20592(18) 0.0261(6) Uani d . . . 1 . .
H H18 0.328561 0.410705 1.250680 0.031000 Uiso calc U . R 1 . .
C C19 0.4583(4) 0.2005(2) 1.34606(18) 0.0327(6) Uani d . . . 1 . .
H H19A 0.587122 0.161763 1.351585 0.049000 Uiso calc U . R 1 . .
H H19B 0.371266 0.141346 1.377552 0.049000 Uiso calc U . R 1 . .
H H19C 0.445098 0.267749 1.379175 0.049000 Uiso calc U . R 1 . .
C C20 0.4515(4) 0.1624(2) 1.17796(19) 0.0315(6) Uani d . . . 1 . .
H H20A 0.404542 0.085095 1.210654 0.047000 Uiso calc U . R 1 . .
H H20B 0.586680 0.149677 1.164200 0.047000 Uiso calc U . R 1 . .
H H20C 0.387460 0.195882 1.115576 0.047000 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N2 . 1.303(3) ?
C1 N1 . 1.369(3) ?
C1 S1 . 1.737(2) ?
C2 N3 . 1.295(3) ?
C2 C3 . 1.450(3) ?
C3 C8 . 1.401(3) ?
C3 C4 . 1.405(3) ?
C4 C5 . 1.380(3) ?
C5 C6 . 1.387(3) ?
C6 O1 . 1.348(3) ?
C6 C7 . 1.389(3) ?
C7 C8 . 1.372(3) ?
C9 N1 . 1.388(3) ?
C9 C10 . 1.398(3) ?
C9 C14 . 1.399(3) ?
C10 C11 . 1.365(3) ?
C11 C12 . 1.381(3) ?
C12 C13 . 1.384(3) ?
C12 N4 . 1.447(3) ?
C13 C14 . 1.373(3) ?
N2 N3 . 1.406(2) ?
N3 Ni1 . 1.9128(17) ?
N4 O3 . 1.221(3) ?
N4 O2 . 1.237(2) ?
Ni1 S1 . 2.1666(6) ?
Ni1 S1 2_576 2.1666(6) ?
N5 C15 . 1.328(3) ?
N5 C16 . 1.447(3) ?
N5 C17 . 1.448(3) ?
O4 C15 . 1.225(3) ?
N6 C18 . 1.320(3) ?
N6 C20 . 1.445(3) ?
N6 C19 . 1.454(3) ?
O5 C18 . 1.236(3) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 C1 N1 . . 121.58(19) ?
N2 C1 S1 . . 123.02(16) ?
N1 C1 S1 . . 115.37(15) ?
N3 C2 C3 . . 133.2(2) ?
C8 C3 C4 . . 117.37(19) ?
C8 C3 C2 . . 115.03(19) ?
C4 C3 C2 . . 127.6(2) ?
C5 C4 C3 . . 120.4(2) ?
C4 C5 C6 . . 120.9(2) ?
O1 C6 C5 . . 122.7(2) ?
O1 C6 C7 . . 117.70(19) ?
C5 C6 C7 . . 119.6(2) ?
C8 C7 C6 . . 119.4(2) ?
C7 C8 C3 . . 122.3(2) ?
N1 C9 C10 . . 116.93(18) ?
N1 C9 C14 . . 124.04(19) ?
C10 C9 C14 . . 119.0(2) ?
C11 C10 C9 . . 120.9(2) ?
C10 C11 C12 . . 119.1(2) ?
C11 C12 C13 . . 121.4(2) ?
C11 C12 N4 . . 119.4(2) ?
C13 C12 N4 . . 119.17(19) ?
C14 C13 C12 . . 119.4(2) ?
C13 C14 C9 . . 120.1(2) ?
C1 N1 C9 . . 129.39(18) ?
C1 N2 N3 . . 111.19(17) ?
C2 N3 N2 . . 115.72(17) ?
C2 N3 Ni1 . . 124.11(14) ?
N2 N3 Ni1 . . 120.05(13) ?
O3 N4 O2 . . 122.49(19) ?
O3 N4 C12 . . 118.94(19) ?
O2 N4 C12 . . 118.57(19) ?
N3 Ni1 N3 2_576 . 180.00(13) ?
N3 Ni1 S1 2_576 . 95.04(5) ?
N3 Ni1 S1 . . 84.96(5) ?
N3 Ni1 S1 2_576 2_576 84.96(5) ?
N3 Ni1 S1 . 2_576 95.04(5) ?
S1 Ni1 S1 . 2_576 180.000000 ?
C1 S1 Ni1 . . 95.57(7) ?
C15 N5 C16 . . 121.2(2) ?
C15 N5 C17 . . 121.5(2) ?
C16 N5 C17 . . 117.07(19) ?
O4 C15 N5 . . 126.3(2) ?
C18 N6 C20 . . 120.5(2) ?
C18 N6 C19 . . 121.9(2) ?
C20 N6 C19 . . 117.5(2) ?
O5 C18 N6 . . 124.5(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N3 C2 C3 C8 . . . . -174.1(2) ?
N3 C2 C3 C4 . . . . 7.9(4) ?
C8 C3 C4 C5 . . . . 0.6(3) ?
C2 C3 C4 C5 . . . . 178.7(2) ?
C3 C4 C5 C6 . . . . 0.5(3) ?
C4 C5 C6 O1 . . . . 178.9(2) ?
C4 C5 C6 C7 . . . . -0.8(3) ?
O1 C6 C7 C8 . . . . -179.8(2) ?
C5 C6 C7 C8 . . . . 0.0(3) ?
C6 C7 C8 C3 . . . . 1.3(3) ?
C4 C3 C8 C7 . . . . -1.5(3) ?
C2 C3 C8 C7 . . . . -179.8(2) ?
N1 C9 C10 C11 . . . . 178.5(2) ?
C14 C9 C10 C11 . . . . -2.8(3) ?
C9 C10 C11 C12 . . . . 1.7(3) ?
C10 C11 C12 C13 . . . . 0.6(3) ?
C10 C11 C12 N4 . . . . -178.4(2) ?
C11 C12 C13 C14 . . . . -1.7(3) ?
N4 C12 C13 C14 . . . . 177.22(19) ?
C12 C13 C14 C9 . . . . 0.6(3) ?
N1 C9 C14 C13 . . . . -179.77(19) ?
C10 C9 C14 C13 . . . . 1.7(3) ?
N2 C1 N1 C9 . . . . 1.2(4) ?
S1 C1 N1 C9 . . . . 179.23(17) ?
C10 C9 N1 C1 . . . . -167.5(2) ?
C14 C9 N1 C1 . . . . 13.9(4) ?
N1 C1 N2 N3 . . . . 177.50(18) ?
S1 C1 N2 N3 . . . . -0.4(3) ?
C3 C2 N3 N2 . . . . 3.2(3) ?
C3 C2 N3 Ni1 . . . . -172.70(18) ?
C1 N2 N3 C2 . . . . -157.38(19) ?
C1 N2 N3 Ni1 . . . . 18.7(2) ?
C11 C12 N4 O3 . . . . 2.2(3) ?
C13 C12 N4 O3 . . . . -176.8(2) ?
C11 C12 N4 O2 . . . . -178.1(2) ?
C13 C12 N4 O2 . . . . 3.0(3) ?
N2 C1 S1 Ni1 . . . . -13.75(19) ?
N1 C1 S1 Ni1 . . . . 168.23(15) ?
C16 N5 C15 O4 . . . . 178.0(2) ?
C17 N5 C15 O4 . . . . 3.6(4) ?
C20 N6 C18 O5 . . . . -0.1(4) ?
C19 N6 C18 O5 . . . . 178.7(2) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2 H2 S1 2_576 0.95 2.48 3.112(2) 123.8 ?
C7 H7 O2 2_567 0.95 2.59 3.494(3) 159.7 ?
C10 H10 O4 . 0.95 2.60 3.359(3) 137.1 ?
C13 H13 O1 2_567 0.95 2.40 3.290(3) 156.4 ?
C14 H14 N2 . 0.95 2.28 2.879(3) 120.1 ?
N1 H1N O4 . 0.88 2.03 2.904(2) 171.4 ?
O1 H1O O5 . 0.84 1.80 2.614(2) 164.0 ?
C15 H15 S1 . 0.95 2.81 3.557(2) 136.3 ?



