# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_nimnt115
_database_code_depnum_ccdc_archive 'CCDC 1910384'
loop_
_audit_author_name
_audit_author_address
'Luciano Marchio'
;Universita degli studi di Parma
Italy
;
_audit_update_record             
;
2019-04-16 deposited with the CCDC.	2019-07-08 downloaded from the CCDC.
;
_audit_creation_date             2018-10-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H18 N4 Ni S4'
_chemical_formula_sum            'C22 H18 N4 Ni S4'
_chemical_formula_weight         525.35
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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                   9.040(3)
_cell_length_b                   11.556(3)
_cell_length_c                   12.136(4)
_cell_angle_alpha                73.582(4)
_cell_angle_beta                 70.444(5)
_cell_angle_gamma                83.313(5)
_cell_volume                     1145.6(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4328
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.404
_cell_measurement_theta_min      2.240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.8314.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12122
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.825
_diffrn_reflns_theta_max         24.825
_diffrn_reflns_theta_min         1.838
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart Breeze'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3258
_reflns_number_total             3935
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       Smart
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0418P)²+0.2650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0868
_refine_special_details          
'the ethylene bridge of one ligand was found disordered in two positions, which were refined with 0.6/0.4 site occupancy factors.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N11-C31A = N11-C31 = N21-C41A = N21-C41 = C31A-C41A = C31-C41
 1.5 with sigma of 0.02
3. Others
 Sof(C31)=Sof(H31C)=Sof(H31D)=Sof(C41)=Sof(H41C)=Sof(H41D)=1-FVAR(1)
 Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C121(H12A,H12B), C41A(H41A,H41B), C31A(H31A,H31B), C31(H31C,
 H31D), C41(H41C,H41D)
4.b Aromatic/amide H refined with riding coordinates:
 C71(H71), C81(H81), C91(H91), C101(H101), C111(H111), C181(H181), C171(H171),
 C161(H161), C151(H151), C141(H141)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.19681(4) 0.60441(3) 0.42554(3) 0.04229(12) Uani 1 1 d . . . . .
S11 S 0.37312(8) 0.46470(6) 0.38977(6) 0.05185(19) Uani 1 1 d . . . . .
S21 S 0.11394(9) 0.51432(6) 0.61549(6) 0.0579(2) Uani 1 1 d . . . . .
S12 S 0.25655(8) 0.71546(6) 0.23704(6) 0.04889(18) Uani 1 1 d . . . . .
S22 S 0.03912(9) 0.76157(6) 0.44695(6) 0.0557(2) Uani 1 1 d . . . . .
C11 C 0.3547(3) 0.3662(2) 0.5257(2) 0.0412(6) Uani 1 1 d . . . . .
N11 N 0.2125(2) 0.31285(19) 0.74048(18) 0.0500(5) Uani 1 1 d D . . . .
C12 C 0.1180(3) 0.8177(2) 0.2935(2) 0.0442(6) Uani 1 1 d . . . . .
N22 N -0.1277(3) 1.0638(2) 0.3376(3) 0.0817(8) Uani 1 1 d . . . . .
N12 N 0.1944(4) 0.9957(3) -0.0027(3) 0.1123(12) Uani 1 1 d . . . . .
N21 N 0.4464(2) 0.26966(18) 0.53750(19) 0.0475(5) Uani 1 1 d D . . . .
C51 C 0.5702(3) 0.2413(2) 0.4336(3) 0.0552(7) Uani 1 1 d . . . . .
H51A H 0.6401 0.1797 0.4634 0.066 Uiso 1 1 calc R . . . .
H51B H 0.6310 0.3130 0.3871 0.066 Uiso 1 1 calc R . . . .
C61 C 0.5094(3) 0.1980(2) 0.3512(2) 0.0497(6) Uani 1 1 d . . . . .
C71 C 0.5919(4) 0.2218(3) 0.2297(3) 0.0745(9) Uani 1 1 d . . . . .
H71 H 0.6818 0.2676 0.1987 0.089 Uiso 1 1 calc R . . . .
C81 C 0.5427(5) 0.1785(4) 0.1533(3) 0.0944(12) Uani 1 1 d . . . . .
H81 H 0.5992 0.1950 0.0711 0.113 Uiso 1 1 calc R . . . .
C91 C 0.4097(6) 0.1107(4) 0.1989(4) 0.0940(12) Uani 1 1 d . . . . .
H91 H 0.3766 0.0809 0.1477 0.113 Uiso 1 1 calc R . . . .
C101 C 0.3270(4) 0.0873(3) 0.3183(4) 0.0813(10) Uani 1 1 d . . . . .
H101 H 0.2367 0.0420 0.3489 0.098 Uiso 1 1 calc R . . . .
C111 C 0.3766(3) 0.1306(3) 0.3943(3) 0.0618(7) Uani 1 1 d . . . . .
H111 H 0.3193 0.1140 0.4762 0.074 Uiso 1 1 calc R . . . .
C121 C 0.0851(3) 0.3239(3) 0.8514(2) 0.0600(8) Uani 1 1 d . . . . .
H12A H 0.0313 0.2478 0.8892 0.072 Uiso 1 1 calc R . . . .
H12B H 0.0097 0.3851 0.8292 0.072 Uiso 1 1 calc R . . . .
C131 C 0.1413(3) 0.3563(2) 0.9416(2) 0.0514(6) Uani 1 1 d . . . . .
C181 C 0.2514(4) 0.4433(3) 0.9080(3) 0.0771(10) Uani 1 1 d . . . . .
H181 H 0.2966 0.4817 0.8266 0.092 Uiso 1 1 calc R . . . .
C171 C 0.2945(5) 0.4734(4) 0.9946(4) 0.0907(11) Uani 1 1 d . . . . .
H171 H 0.3696 0.5317 0.9714 0.109 Uiso 1 1 calc R . . . .
C161 C 0.2278(5) 0.4184(4) 1.1144(3) 0.0851(11) Uani 1 1 d . . . . .
H161 H 0.2570 0.4394 1.1727 0.102 Uiso 1 1 calc R . . . .
C151 C 0.1181(5) 0.3324(3) 1.1484(3) 0.0792(10) Uani 1 1 d . . . . .
H151 H 0.0725 0.2949 1.2301 0.095 Uiso 1 1 calc R . . . .
C141 C 0.0746(3) 0.3009(3) 1.0625(2) 0.0602(7) Uani 1 1 d . . . . .
H141 H 0.0001 0.2421 1.0862 0.072 Uiso 1 1 calc R . . . .
C21 C 0.2287(3) 0.3898(2) 0.6342(2) 0.0408(6) Uani 1 1 d . . . . .
C22 C 0.0748(3) 0.9262(2) 0.2272(2) 0.0502(6) Uani 1 1 d . . . . .
C42 C -0.0384(3) 1.0037(2) 0.2871(3) 0.0584(7) Uani 1 1 d . . . . .
C32 C 0.1410(4) 0.9647(3) 0.0996(3) 0.0689(8) Uani 1 1 d . . . . .
C41A C 0.4077(17) 0.1765(12) 0.6578(9) 0.061(3) Uani 0.593(16) 1 d D . P A 1
H41A H 0.3325 0.1215 0.6605 0.074 Uiso 0.593(16) 1 calc R . P A 1
H41B H 0.5023 0.1301 0.6644 0.074 Uiso 0.593(16) 1 calc R . P A 1
C31A C 0.3415(9) 0.2293(8) 0.7639(6) 0.058(2) Uani 0.593(16) 1 d D . P A 1
H31A H 0.3022 0.1662 0.8379 0.070 Uiso 0.593(16) 1 calc R . P A 1
H31B H 0.4215 0.2724 0.7722 0.070 Uiso 0.593(16) 1 calc R . P A 1
C31 C 0.2985(15) 0.1922(10) 0.7385(11) 0.068(3) Uani 0.407(16) 1 d D . P A 2
H31C H 0.3049 0.1541 0.8190 0.082 Uiso 0.407(16) 1 calc R . P A 2
H31D H 0.2353 0.1413 0.7214 0.082 Uiso 0.407(16) 1 calc R . P A 2
C41 C 0.4584(18) 0.194(2) 0.6513(14) 0.067(5) Uani 0.407(16) 1 d D . P A 2
H41C H 0.5314 0.2273 0.6769 0.080 Uiso 0.407(16) 1 calc R . P A 2
H41D H 0.4944 0.1133 0.6444 0.080 Uiso 0.407(16) 1 calc R . P 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
Ni S11 2.1608(8) . ?
Ni S21 2.1512(10) . ?
Ni S12 2.2016(9) . ?
Ni S22 2.1941(8) . ?
S11 C11 1.686(2) . ?
S21 C21 1.680(3) . ?
S12 C12 1.724(3) . ?
S22 C12 1.712(3) . ?
C11 N21 1.314(3) . ?
C11 C21 1.495(4) . ?
N11 C121 1.476(3) . ?
N11 C21 1.316(3) . ?
N11 C31A 1.475(6) . ?
N11 C31 1.518(10) . ?
C12 C22 1.378(3) . ?
N22 C42 1.136(4) . ?
N12 C32 1.136(4) . ?
N21 C51 1.467(3) . ?
N21 C41A 1.507(10) . ?
N21 C41 1.442(15) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51 C61 1.506(4) . ?
C61 C71 1.374(4) . ?
C61 C111 1.375(4) . ?
C71 H71 0.9300 . ?
C71 C81 1.378(5) . ?
C81 H81 0.9300 . ?
C81 C91 1.377(5) . ?
C91 H91 0.9300 . ?
C91 C101 1.353(5) . ?
C101 H101 0.9300 . ?
C101 C111 1.376(4) . ?
C111 H111 0.9300 . ?
C121 H12A 0.9700 . ?
C121 H12B 0.9700 . ?
C121 C131 1.499(4) . ?
C131 C181 1.377(4) . ?
C131 C141 1.375(4) . ?
C181 H181 0.9300 . ?
C181 C171 1.375(4) . ?
C171 H171 0.9300 . ?
C171 C161 1.364(5) . ?
C161 H161 0.9300 . ?
C161 C151 1.366(5) . ?
C151 H151 0.9300 . ?
C151 C141 1.378(4) . ?
C141 H141 0.9300 . ?
C22 C42 1.426(4) . ?
C22 C32 1.416(4) . ?
C41A H41A 0.9700 . ?
C41A H41B 0.9700 . ?
C41A C31A 1.494(13) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C31 H31D 0.9700 . ?
C31 C41 1.476(16) . ?
C41 H41C 0.9700 . ?
C41 H41D 0.9700 . ?

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
S11 Ni S12 95.96(3) . . ?
S11 Ni S22 173.20(3) . . ?
S21 Ni S11 91.87(3) . . ?
S21 Ni S12 172.17(3) . . ?
S21 Ni S22 93.25(3) . . ?
S22 Ni S12 78.95(3) . . ?
C11 S11 Ni 105.40(9) . . ?
C21 S21 Ni 105.80(9) . . ?
C12 S12 Ni 85.87(9) . . ?
C12 S22 Ni 86.39(9) . . ?
N21 C11 S11 121.70(19) . . ?
N21 C11 C21 119.9(2) . . ?
C21 C11 S11 118.39(18) . . ?
C121 N11 C31A 113.8(3) . . ?
C121 N11 C31 118.8(4) . . ?
C21 N11 C121 122.8(2) . . ?
C21 N11 C31A 121.6(3) . . ?
C21 N11 C31 115.9(5) . . ?
S22 C12 S12 108.79(14) . . ?
C22 C12 S12 126.2(2) . . ?
C22 C12 S22 125.0(2) . . ?
C11 N21 C51 122.1(2) . . ?
C11 N21 C41A 118.6(6) . . ?
C11 N21 C41 124.8(9) . . ?
C51 N21 C41A 118.8(6) . . ?
C41 N21 C51 112.1(8) . . ?
N21 C51 H51A 108.8 . . ?
N21 C51 H51B 108.8 . . ?
N21 C51 C61 113.9(2) . . ?
H51A C51 H51B 107.7 . . ?
C61 C51 H51A 108.8 . . ?
C61 C51 H51B 108.8 . . ?
C71 C61 C51 119.5(3) . . ?
C71 C61 C111 118.4(3) . . ?
C111 C61 C51 122.0(3) . . ?
C61 C71 H71 119.7 . . ?
C61 C71 C81 120.6(3) . . ?
C81 C71 H71 119.7 . . ?
C71 C81 H81 120.1 . . ?
C91 C81 C71 119.8(4) . . ?
C91 C81 H81 120.1 . . ?
C81 C91 H91 119.9 . . ?
C101 C91 C81 120.1(3) . . ?
C101 C91 H91 119.9 . . ?
C91 C101 H101 120.0 . . ?
C91 C101 C111 119.9(4) . . ?
C111 C101 H101 120.0 . . ?
C61 C111 C101 121.2(3) . . ?
C61 C111 H111 119.4 . . ?
C101 C111 H111 119.4 . . ?
N11 C121 H12A 108.9 . . ?
N11 C121 H12B 108.9 . . ?
N11 C121 C131 113.5(2) . . ?
H12A C121 H12B 107.7 . . ?
C131 C121 H12A 108.9 . . ?
C131 C121 H12B 108.9 . . ?
C181 C131 C121 122.3(2) . . ?
C141 C131 C121 118.4(2) . . ?
C141 C131 C181 119.2(3) . . ?
C131 C181 H181 119.9 . . ?
C171 C181 C131 120.1(3) . . ?
C171 C181 H181 119.9 . . ?
C181 C171 H171 119.8 . . ?
C161 C171 C181 120.4(3) . . ?
C161 C171 H171 119.8 . . ?
C171 C161 H161 120.1 . . ?
C171 C161 C151 119.7(3) . . ?
C151 C161 H161 120.1 . . ?
C161 C151 H151 119.8 . . ?
C161 C151 C141 120.4(3) . . ?
C141 C151 H151 119.8 . . ?
C131 C141 C151 120.1(3) . . ?
C131 C141 H141 120.0 . . ?
C151 C141 H141 120.0 . . ?
C11 C21 S21 118.51(17) . . ?
N11 C21 S21 122.7(2) . . ?
N11 C21 C11 118.8(2) . . ?
C12 C22 C42 119.9(2) . . ?
C12 C22 C32 121.8(3) . . ?
C32 C22 C42 118.2(2) . . ?
N22 C42 C22 178.2(3) . . ?
N12 C32 C22 179.9(5) . . ?
N21 C41A H41A 108.9 . . ?
N21 C41A H41B 108.9 . . ?
H41A C41A H41B 107.7 . . ?
C31A C41A N21 113.5(9) . . ?
C31A C41A H41A 108.9 . . ?
C31A C41A H41B 108.9 . . ?
N11 C31A C41A 106.5(8) . . ?
N11 C31A H31A 110.4 . . ?
N11 C31A H31B 110.4 . . ?
C41A C31A H31A 110.4 . . ?
C41A C31A H31B 110.4 . . ?
H31A C31A H31B 108.6 . . ?
N11 C31 H31C 108.1 . . ?
N11 C31 H31D 108.1 . . ?
H31C C31 H31D 107.3 . . ?
C41 C31 N11 116.9(13) . . ?
C41 C31 H31C 108.1 . . ?
C41 C31 H31D 108.1 . . ?
N21 C41 C31 105.6(12) . . ?
N21 C41 H41C 110.6 . . ?
N21 C41 H41D 110.6 . . ?
C31 C41 H41C 110.6 . . ?
C31 C41 H41D 110.6 . . ?
H41C C41 H41D 108.8 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_nimd115
_database_code_depnum_ccdc_archive 'CCDC 1910385'
loop_
_audit_author_name
_audit_author_address
'Luciano Marchio'
;Universita degli studi di Parma
Italy
;
_audit_update_record             
;
2019-05-28 deposited with the CCDC.	2019-07-08 downloaded from the CCDC.
;
_audit_creation_date             2019-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H24 N2 Ni O4 S4, C3 H7 N O'
_chemical_formula_sum            'C27 H31 N3 Ni O5 S4'
_chemical_formula_weight         664.50
_chemical_melting_point          ?
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 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3576 1.0944 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1212 0.1207 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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                   10.3749(3)
_cell_length_b                   12.0393(5)
_cell_length_c                   13.1825(5)
_cell_angle_alpha                64.188(4)
_cell_angle_beta                 89.513(3)
_cell_angle_gamma                81.625(3)
_cell_volume                     1463.70(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7387
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.2790
_cell_measurement_theta_min      1.8960
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.902
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22675
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.942
_diffrn_reflns_theta_min         1.693
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ      0.00 180.00   1.00    1.00   0.00   0.00   0.00    --   180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Huber 4-circles K goniometer, Pilatus 2M detector'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0279068000
_diffrn_orient_matrix_UB_12      0.0230898000
_diffrn_orient_matrix_UB_13      0.0369229000
_diffrn_orient_matrix_UB_21      0.0095335000
_diffrn_orient_matrix_UB_22      0.0603192000
_diffrn_orient_matrix_UB_23      -0.0377129000
_diffrn_orient_matrix_UB_31      -0.0616363000
_diffrn_orient_matrix_UB_32      0.0103082000
_diffrn_orient_matrix_UB_33      -0.0265898000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_source                   'Elettra synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5870
_reflns_number_total             5910
_reflns_odcompleteness_completeness 72.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.0328(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+0.6732P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0790
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C51(H51A,H51B), C121(H12A,H12B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C81(H81), C161(H161), C171(H171), C71(H71), C111(H111), C141(H141),
 C101(H101), C151(H151), C181(H181), C91(H91), C1S(H1S)
2.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C42(H42A,H42B,H42C), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,
 H2SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.18842(2) 0.43135(2) 0.07353(2) 0.01345(8) Uani 1 1 d . . . . .
S22 S 0.29064(3) 0.54161(3) 0.12646(3) 0.01508(9) Uani 1 1 d . . . . .
S11 S 0.08483(4) 0.32096(3) 0.01949(3) 0.01790(10) Uani 1 1 d . . . . .
S12 S 0.14769(3) 0.31304(3) 0.24332(3) 0.01695(10) Uani 1 1 d . . . . .
S21 S 0.24013(3) 0.54059(3) -0.09714(3) 0.01665(10) Uani 1 1 d . . . . .
O32 O 0.34657(10) 0.47830(10) 0.44369(8) 0.0210(2) Uani 1 1 d . . . . .
O12 O 0.11638(10) 0.32734(10) 0.49520(8) 0.0207(2) Uani 1 1 d . . . . .
O22 O 0.30163(10) 0.20393(9) 0.49713(8) 0.0221(2) Uani 1 1 d . . . . .
O42 O 0.36969(10) 0.63879(9) 0.27700(8) 0.0197(2) Uani 1 1 d . . . . .
C22 C 0.28294(13) 0.47156(12) 0.27337(11) 0.0144(3) Uani 1 1 d . . . . .
C61 C 0.02435(13) 0.12070(12) -0.15069(11) 0.0168(3) Uani 1 1 d . . . . .
C21 C 0.19196(13) 0.46820(12) -0.17173(11) 0.0143(3) Uani 1 1 d . . . . .
C11 C 0.10381(13) 0.37435(12) -0.12019(11) 0.0143(3) Uani 1 1 d . . . . .
N21 N 0.04611(12) 0.33476(11) -0.18464(10) 0.0157(2) Uani 1 1 d . . . . .
O1S O 0.39694(12) 0.20962(13) -0.10489(11) 0.0378(3) Uani 1 1 d . . . . .
C12 C 0.22291(13) 0.37024(13) 0.32334(11) 0.0147(3) Uani 1 1 d . . . . .
N11 N 0.23459(11) 0.48847(11) -0.27223(10) 0.0161(2) Uani 1 1 d . . . . .
C32 C 0.20739(13) 0.30185(12) 0.44757(11) 0.0156(3) Uani 1 1 d . . . . .
C52 C 0.33575(13) 0.52693(13) 0.34129(11) 0.0155(3) Uani 1 1 d . . . . .
C81 C 0.20390(15) -0.04713(14) -0.10671(14) 0.0266(3) Uani 1 1 d . . . . .
H81 H 0.2889 -0.0867 -0.0730 0.032 Uiso 1 1 calc R . . . .
C161 C 0.21856(19) 0.95133(15) -0.53672(14) 0.0318(4) Uani 1 1 d . . . . .
H161 H 0.1931 1.0372 -0.5865 0.038 Uiso 1 1 calc R . . . .
C131 C 0.29266(14) 0.69963(13) -0.39125(11) 0.0179(3) Uani 1 1 d . . . . .
C171 C 0.34838(17) 0.90417(15) -0.50118(14) 0.0298(3) Uani 1 1 d . . . . .
H171 H 0.4122 0.9579 -0.5268 0.036 Uiso 1 1 calc R . . . .
C31 C 0.19511(15) 0.41943(14) -0.33131(12) 0.0226(3) Uani 1 1 d . . . . .
H31A H 0.2561 0.3400 -0.3078 0.027 Uiso 1 1 calc R . . . .
H31B H 0.1996 0.4691 -0.4137 0.027 Uiso 1 1 calc R . . . .
C71 C 0.14871(14) 0.06257(14) -0.10179(12) 0.0221(3) Uani 1 1 d . . . . .
H71 H 0.1961 0.0978 -0.0649 0.027 Uiso 1 1 calc R . . . .
C111 C -0.04302(14) 0.06899(13) -0.20586(12) 0.0207(3) Uani 1 1 d . . . . .
H111 H -0.1276 0.1089 -0.2405 0.025 Uiso 1 1 calc R . . . .
C51 C -0.03790(14) 0.23728(13) -0.14163(12) 0.0181(3) Uani 1 1 d . . . . .
H51A H -0.1232 0.2693 -0.1853 0.022 Uiso 1 1 calc R . . . .
H51B H -0.0537 0.2166 -0.0617 0.022 Uiso 1 1 calc R . . . .
C141 C 0.16279(15) 0.74667(14) -0.42626(13) 0.0237(3) Uani 1 1 d . . . . .
H141 H 0.0988 0.6931 -0.4005 0.028 Uiso 1 1 calc R . . . .
C121 C 0.34003(14) 0.56180(13) -0.31881(12) 0.0182(3) Uani 1 1 d . . . . .
H12A H 0.3920 0.5272 -0.3648 0.022 Uiso 1 1 calc R . . . .
H12B H 0.3984 0.5526 -0.2557 0.022 Uiso 1 1 calc R . . . .
C41 C 0.06034(15) 0.39223(14) -0.30640(12) 0.0204(3) Uani 1 1 d . . . . .
H41A H -0.0025 0.4708 -0.3427 0.025 Uiso 1 1 calc R . . . .
H41B H 0.0405 0.3351 -0.3380 0.025 Uiso 1 1 calc R . . . .
C101 C 0.01263(16) -0.04083(14) -0.21070(13) 0.0244(3) Uani 1 1 d . . . . .
H101 H -0.0340 -0.0756 -0.2485 0.029 Uiso 1 1 calc R . . . .
C151 C 0.12592(17) 0.87252(15) -0.49919(15) 0.0312(4) Uani 1 1 d . . . . .
H151 H 0.0366 0.9046 -0.5234 0.037 Uiso 1 1 calc R . . . .
C181 C 0.38584(15) 0.77898(15) -0.42844(13) 0.0237(3) Uani 1 1 d . . . . .
H181 H 0.4751 0.7472 -0.4039 0.028 Uiso 1 1 calc R . . . .
N1S N 0.45236(13) 0.18277(13) 0.07212(13) 0.0286(3) Uani 1 1 d . . . . .
C62 C 0.41567(16) 0.70326(14) 0.33696(13) 0.0238(3) Uani 1 1 d . . . . .
H62A H 0.3427 0.7305 0.3728 0.036 Uiso 1 1 calc GR . . . .
H62B H 0.4518 0.7763 0.2837 0.036 Uiso 1 1 calc GR . . . .
H62C H 0.4836 0.6466 0.3949 0.036 Uiso 1 1 calc GR . . . .
C42 C 0.29044(17) 0.12722(15) 0.61614(12) 0.0274(3) Uani 1 1 d . . . . .
H42A H 0.3123 0.1714 0.6593 0.041 Uiso 1 1 calc GR . . . .
H42B H 0.3506 0.0483 0.6406 0.041 Uiso 1 1 calc GR . . . .
H42C H 0.2008 0.1100 0.6291 0.041 Uiso 1 1 calc GR . . . .
C91 C 0.13558(16) -0.09934(14) -0.16057(14) 0.0257(3) Uani 1 1 d . . . . .
H91 H 0.1732 -0.1749 -0.1629 0.031 Uiso 1 1 calc R . . . .
C1S C 0.44549(15) 0.24313(15) -0.04039(16) 0.0303(4) Uani 1 1 d . . . . .
H1S H 0.4813 0.3185 -0.0734 0.036 Uiso 1 1 calc R . . . .
C3S C 0.50380(17) 0.23345(18) 0.14197(17) 0.0357(4) Uani 1 1 d . . . . .
H3SA H 0.5304 0.3141 0.0937 0.054 Uiso 1 1 calc GR . . . .
H3SB H 0.5795 0.1754 0.1890 0.054 Uiso 1 1 calc GR . . . .
H3SC H 0.4363 0.2452 0.1904 0.054 Uiso 1 1 calc GR . . . .
C2S C 0.4007(2) 0.06668(18) 0.12946(17) 0.0437(5) Uani 1 1 d . . . . .
H2SA H 0.3223 0.0807 0.1671 0.066 Uiso 1 1 calc GR . . . .
H2SB H 0.4665 0.0037 0.1858 0.066 Uiso 1 1 calc GR . . . .
H2SC H 0.3782 0.0372 0.0743 0.066 Uiso 1 1 calc GR . . . .


_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
Ni S22 2.1455(4) . ?
Ni S11 2.1638(4) . ?
Ni S12 2.1448(4) . ?
Ni S21 2.1651(4) . ?
S22 C22 1.7501(13) . ?
S11 C11 1.6859(13) . ?
S12 C12 1.7319(14) . ?
S21 C21 1.6904(13) . ?
O32 C52 1.2136(17) . ?
O12 C32 1.2057(17) . ?
O22 C32 1.3330(17) . ?
O22 C42 1.4470(17) . ?
O42 C52 1.3398(17) . ?
O42 C62 1.4503(16) . ?
C22 C12 1.351(2) . ?
C22 C52 1.4767(19) . ?
C61 C71 1.389(2) . ?
C61 C111 1.391(2) . ?
C61 C51 1.5106(18) . ?
C21 C11 1.4821(19) . ?
C21 N11 1.3230(17) . ?
C11 N21 1.3237(18) . ?
N21 C51 1.4727(18) . ?
N21 C41 1.4613(17) . ?
O1S C1S 1.227(2) . ?
C12 C32 1.4985(18) . ?
N11 C31 1.4608(18) . ?
N11 C121 1.4665(18) . ?
C81 H81 0.9500 . ?
C81 C71 1.389(2) . ?
C81 C91 1.389(2) . ?
C161 H161 0.9500 . ?
C161 C171 1.383(3) . ?
C161 C151 1.385(2) . ?
C131 C141 1.382(2) . ?
C131 C121 1.5158(19) . ?
C131 C181 1.393(2) . ?
C171 H171 0.9500 . ?
C171 C181 1.385(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C41 1.484(2) . ?
C71 H71 0.9500 . ?
C111 H111 0.9500 . ?
C111 C101 1.391(2) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C141 H141 0.9500 . ?
C141 C151 1.391(2) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C101 H101 0.9500 . ?
C101 C91 1.381(2) . ?
C151 H151 0.9500 . ?
C181 H181 0.9500 . ?
N1S C1S 1.335(2) . ?
N1S C3S 1.448(2) . ?
N1S C2S 1.450(2) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C91 H91 0.9500 . ?
C1S H1S 0.9500 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?

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
S22 Ni S11 179.722(15) . . ?
S22 Ni S21 88.347(13) . . ?
S11 Ni S21 91.472(13) . . ?
S12 Ni S22 92.492(13) . . ?
S12 Ni S11 87.703(14) . . ?
S12 Ni S21 176.051(14) . . ?
C22 S22 Ni 103.58(5) . . ?
C11 S11 Ni 105.73(5) . . ?
C12 S12 Ni 103.61(5) . . ?
C21 S21 Ni 104.72(5) . . ?
C32 O22 C42 115.59(11) . . ?
C52 O42 C62 116.04(11) . . ?
C12 C22 S22 119.50(11) . . ?
C12 C22 C52 120.36(12) . . ?
C52 C22 S22 120.07(10) . . ?
C71 C61 C111 119.31(13) . . ?
C71 C61 C51 120.15(13) . . ?
C111 C61 C51 120.52(13) . . ?
C11 C21 S21 118.69(10) . . ?
N11 C21 S21 122.31(11) . . ?
N11 C21 C11 118.94(12) . . ?
C21 C11 S11 117.76(10) . . ?
N21 C11 S11 123.23(11) . . ?
N21 C11 C21 119.00(12) . . ?
C11 N21 C51 123.72(11) . . ?
C11 N21 C41 119.73(12) . . ?
C41 N21 C51 116.50(11) . . ?
C22 C12 S12 120.75(10) . . ?
C22 C12 C32 125.36(12) . . ?
C32 C12 S12 113.80(10) . . ?
C21 N11 C31 120.41(12) . . ?
C21 N11 C121 121.69(12) . . ?
C31 N11 C121 116.95(11) . . ?
O12 C32 O22 124.22(12) . . ?
O12 C32 C12 124.12(12) . . ?
O22 C32 C12 111.49(11) . . ?
O32 C52 O42 123.18(13) . . ?
O32 C52 C22 124.49(13) . . ?
O42 C52 C22 112.32(11) . . ?
C71 C81 H81 119.8 . . ?
C91 C81 H81 119.8 . . ?
C91 C81 C71 120.44(14) . . ?
C171 C161 H161 120.2 . . ?
C171 C161 C151 119.56(15) . . ?
C151 C161 H161 120.2 . . ?
C141 C131 C121 122.33(13) . . ?
C141 C131 C181 119.71(14) . . ?
C181 C131 C121 117.85(13) . . ?
C161 C171 H171 119.8 . . ?
C161 C171 C181 120.37(15) . . ?
C181 C171 H171 119.8 . . ?
N11 C31 H31A 109.4 . . ?
N11 C31 H31B 109.4 . . ?
N11 C31 C41 111.04(11) . . ?
H31A C31 H31B 108.0 . . ?
C41 C31 H31A 109.4 . . ?
C41 C31 H31B 109.4 . . ?
C61 C71 C81 120.05(14) . . ?
C61 C71 H71 120.0 . . ?
C81 C71 H71 120.0 . . ?
C61 C111 H111 119.8 . . ?
C61 C111 C101 120.46(14) . . ?
C101 C111 H111 119.8 . . ?
C61 C51 H51A 109.4 . . ?
C61 C51 H51B 109.4 . . ?
N21 C51 C61 111.15(11) . . ?
N21 C51 H51A 109.4 . . ?
N21 C51 H51B 109.4 . . ?
H51A C51 H51B 108.0 . . ?
C131 C141 H141 120.0 . . ?
C131 C141 C151 119.93(14) . . ?
C151 C141 H141 120.0 . . ?
N11 C121 C131 113.83(11) . . ?
N11 C121 H12A 108.8 . . ?
N11 C121 H12B 108.8 . . ?
C131 C121 H12A 108.8 . . ?
C131 C121 H12B 108.8 . . ?
H12A C121 H12B 107.7 . . ?
N21 C41 C31 110.54(12) . . ?
N21 C41 H41A 109.5 . . ?
N21 C41 H41B 109.5 . . ?
C31 C41 H41A 109.5 . . ?
C31 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
C111 C101 H101 120.0 . . ?
C91 C101 C111 120.06(14) . . ?
C91 C101 H101 120.0 . . ?
C161 C151 C141 120.41(16) . . ?
C161 C151 H151 119.8 . . ?
C141 C151 H151 119.8 . . ?
C131 C181 H181 120.0 . . ?
C171 C181 C131 120.02(14) . . ?
C171 C181 H181 120.0 . . ?
C1S N1S C3S 121.86(15) . . ?
C1S N1S C2S 120.85(15) . . ?
C3S N1S C2S 117.18(16) . . ?
O42 C62 H62A 109.5 . . ?
O42 C62 H62B 109.5 . . ?
O42 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O22 C42 H42A 109.5 . . ?
O22 C42 H42B 109.5 . . ?
O22 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C81 C91 H91 120.2 . . ?
C101 C91 C81 119.67(14) . . ?
C101 C91 H91 120.2 . . ?
O1S C1S N1S 125.61(16) . . ?
O1S C1S H1S 117.2 . . ?
N1S C1S H1S 117.2 . . ?
N1S C3S H3SA 109.5 . . ?
N1S C3S H3SB 109.5 . . ?
N1S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
N1S C2S H2SA 109.5 . . ?
N1S C2S H2SB 109.5 . . ?
N1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?

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
Ni S22 C22 C12 1.03(12) . . . . ?
Ni S22 C22 C52 -175.84(9) . . . . ?
Ni S11 C11 C21 6.14(11) . . . . ?
Ni S11 C11 N21 -175.23(10) . . . . ?
Ni S12 C12 C22 2.90(12) . . . . ?
Ni S12 C12 C32 179.71(9) . . . . ?
Ni S21 C21 C11 13.84(11) . . . . ?
Ni S21 C21 N11 -163.19(10) . . . . ?
S22 C22 C12 S12 -2.74(16) . . . . ?
S22 C22 C12 C32 -179.16(10) . . . . ?
S22 C22 C52 O32 -172.21(11) . . . . ?
S22 C22 C52 O42 8.45(15) . . . . ?
S11 C11 N21 C51 -1.86(19) . . . . ?
S11 C11 N21 C41 175.67(10) . . . . ?
S12 C12 C32 O12 -87.45(15) . . . . ?
S12 C12 C32 O22 87.99(12) . . . . ?
S21 C21 C11 S11 -13.95(15) . . . . ?
S21 C21 C11 N21 167.36(10) . . . . ?
S21 C21 N11 C31 177.10(10) . . . . ?
S21 C21 N11 C121 8.57(18) . . . . ?
C22 C12 C32 O12 89.19(19) . . . . ?
C22 C12 C32 O22 -95.38(16) . . . . ?
C61 C111 C101 C91 0.0(2) . . . . ?
C21 C11 N21 C51 176.75(11) . . . . ?
C21 C11 N21 C41 -5.71(18) . . . . ?
C21 N11 C31 C41 33.34(18) . . . . ?
C21 N11 C121 C131 -92.20(15) . . . . ?
C11 C21 N11 C31 0.08(19) . . . . ?
C11 C21 N11 C121 -168.46(12) . . . . ?
C11 N21 C51 C61 -112.80(14) . . . . ?
C11 N21 C41 C31 38.91(17) . . . . ?
C12 C22 C52 O32 11.0(2) . . . . ?
C12 C22 C52 O42 -168.38(12) . . . . ?
N11 C21 C11 S11 163.19(10) . . . . ?
N11 C21 C11 N21 -15.50(19) . . . . ?
N11 C31 C41 N21 -50.96(16) . . . . ?
C52 C22 C12 S12 174.12(9) . . . . ?
C52 C22 C12 C32 -2.3(2) . . . . ?
C161 C171 C181 C131 0.4(2) . . . . ?
C131 C141 C151 C161 -0.3(3) . . . . ?
C171 C161 C151 C141 0.0(3) . . . . ?
C31 N11 C121 C131 98.88(14) . . . . ?
C71 C61 C111 C101 0.9(2) . . . . ?
C71 C61 C51 N21 55.21(17) . . . . ?
C71 C81 C91 C101 0.8(2) . . . . ?
C111 C61 C71 C81 -1.0(2) . . . . ?
C111 C61 C51 N21 -126.14(14) . . . . ?
C111 C101 C91 C81 -0.9(2) . . . . ?
C51 C61 C71 C81 177.68(13) . . . . ?
C51 C61 C111 C101 -177.73(13) . . . . ?
C51 N21 C41 C31 -143.38(12) . . . . ?
C141 C131 C121 N11 -11.05(19) . . . . ?
C141 C131 C181 C171 -0.7(2) . . . . ?
C121 N11 C31 C41 -157.60(12) . . . . ?
C121 C131 C141 C151 -175.46(14) . . . . ?
C121 C131 C181 C171 175.55(13) . . . . ?
C41 N21 C51 C61 69.60(15) . . . . ?
C151 C161 C171 C181 -0.1(3) . . . . ?
C181 C131 C141 C151 0.6(2) . . . . ?
C181 C131 C121 N11 172.79(12) . . . . ?
C62 O42 C52 O32 -2.72(19) . . . . ?
C62 O42 C52 C22 176.63(11) . . . . ?
C42 O22 C32 O12 -0.9(2) . . . . ?
C42 O22 C32 C12 -176.29(12) . . . . ?
C91 C81 C71 C61 0.1(2) . . . . ?
C3S N1S C1S O1S -175.85(16) . . . . ?
C2S N1S C1S O1S 0.3(3) . . . . ?

_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.740
####################################################################### 
# 
# 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_4_niddd115_1_
_database_code_depnum_ccdc_archive 'CCDC 1910386'
loop_
_audit_author_name
_audit_author_address
'Luciano Marchio'
;Universita degli studi di Parma
Italy
;
_audit_update_record             
;
2019-04-16 deposited with the CCDC.	2019-07-08 downloaded from the CCDC.
;
_audit_creation_date             2018-10-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H24 N2 Ni O4 S6, C3 H7 N O'
_chemical_formula_sum            'C29 H31 N3 Ni O5 S6'
_chemical_formula_weight         752.64
_chemical_melting_point          ?
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 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3576 1.0944 '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 0.1212 0.1207 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_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                   17.6638(2)
_cell_length_b                   8.31590(10)
_cell_length_c                   23.1526(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.2360(10)
_cell_angle_gamma                90
_cell_volume                     3230.09(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8780
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.8220
_cell_measurement_theta_min      1.7070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16441
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        24.623
_diffrn_reflns_theta_max         24.623
_diffrn_reflns_theta_min         1.716
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ      0.00 180.00   1.00    3.00   0.00   0.00   0.00    --   180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Huber 4-circles K goniometer, Pilatus 2M detector'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0411321000
_diffrn_orient_matrix_UB_12      -0.0088880000
_diffrn_orient_matrix_UB_13      0.0058650000
_diffrn_orient_matrix_UB_21      -0.0058153000
_diffrn_orient_matrix_UB_22      -0.0071930000
_diffrn_orient_matrix_UB_23      -0.0312105000
_diffrn_orient_matrix_UB_31      0.0038710000
_diffrn_orient_matrix_UB_32      0.0834071000
_diffrn_orient_matrix_UB_33      -0.0020780000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_source                   'Elettra synchrotron XRD1 BL'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4912
_reflns_number_total             5438
_reflns_odcompleteness_completeness 76.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.00
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 data collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    ?
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.436
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1238
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C41(H41A,H41B), C51(H51A,H51B), C121(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C111(H111), C71(H71), C81(H81), C101(H101), C91(H91), C181(H181), C141(H141),
 C171(H171), C151(H151), C161(H161), C1S(H1S)
2.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C82(H82A,H82B,H82C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,
 H3SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.08293(2) 0.16923(3) 0.99487(2) 0.01834(13) Uani 1 1 d . . . . .
S22 S 0.19713(3) 0.17968(7) 1.06529(2) 0.01948(16) Uani 1 1 d . . . . .
S11 S -0.03126(3) 0.17286(7) 0.92443(3) 0.02136(16) Uani 1 1 d . . . . .
S12 S 0.13414(3) 0.06502(7) 0.93024(2) 0.01968(16) Uani 1 1 d . . . . .
S42 S 0.36613(3) 0.15528(7) 1.06482(3) 0.02151(16) Uani 1 1 d . . . . .
S32 S 0.30233(3) 0.03958(7) 0.92610(2) 0.02184(16) Uani 1 1 d . . . . .
S21 S 0.03237(3) 0.27888(7) 1.05864(2) 0.02158(16) Uani 1 1 d . . . . .
O22 O 0.37313(10) -0.3507(2) 0.97561(7) 0.0252(4) Uani 1 1 d . . . . .
O12 O 0.43895(11) -0.2139(2) 0.92159(8) 0.0315(4) Uani 1 1 d . . . . .
O42 O 0.48808(9) -0.04584(19) 1.14032(7) 0.0234(4) Uani 1 1 d . . . . .
N11 N -0.11480(10) 0.3728(2) 1.04707(8) 0.0188(4) Uani 1 1 d . . . . .
N21 N -0.17338(11) 0.2639(2) 0.92703(8) 0.0185(4) Uani 1 1 d . . . . .
O32 O 0.50940(10) -0.2091(2) 1.06988(8) 0.0294(4) Uani 1 1 d . . . . .
C12 C 0.23610(12) 0.0890(3) 0.96687(10) 0.0194(5) Uani 1 1 d . . . . .
C31 C -0.19407(13) 0.4260(3) 1.00900(10) 0.0232(5) Uani 1 1 d . . . . .
H31A H -0.1896 0.5285 0.9903 0.028 Uiso 1 1 calc R . . . .
H31B H -0.2286 0.4402 1.0340 0.028 Uiso 1 1 calc R . . . .
C22 C 0.26328(13) 0.1380(3) 1.02508(10) 0.0198(5) Uani 1 1 d . . . . .
C41 C -0.22946(13) 0.3031(3) 0.96047(10) 0.0229(5) Uani 1 1 d . . . . .
H41A H -0.2421 0.2063 0.9789 0.027 Uiso 1 1 calc R . . . .
H41B H -0.2785 0.3447 0.9324 0.027 Uiso 1 1 calc R . . . .
C42 C 0.37542(13) -0.0708(3) 0.98226(10) 0.0212(5) Uani 1 1 d . . . . .
C52 C 0.40170(13) -0.2182(3) 0.95734(10) 0.0228(5) Uani 1 1 d . . . . .
C32 C 0.40360(12) -0.0192(3) 1.03997(10) 0.0214(5) Uani 1 1 d . . . . .
C11 C -0.09645(13) 0.2518(3) 0.95717(10) 0.0189(4) Uani 1 1 d . . . . .
C111 C -0.16929(14) 0.4788(3) 0.82881(10) 0.0262(5) Uani 1 1 d . . . . .
H111 H -0.1780 0.5265 0.8625 0.031 Uiso 1 1 calc R . . . .
C51 C -0.20607(13) 0.2096(3) 0.86337(10) 0.0223(5) Uani 1 1 d . . . . .
H51A H -0.2638 0.2091 0.8517 0.027 Uiso 1 1 calc R . . . .
H51B H -0.1886 0.1003 0.8602 0.027 Uiso 1 1 calc R . . . .
C21 C -0.06554(13) 0.3039(3) 1.02129(10) 0.0195(5) Uani 1 1 d . . . . .
C71 C -0.16921(15) 0.2461(3) 0.76832(11) 0.0304(6) Uani 1 1 d . . . . .
H71 H -0.1772 0.1363 0.7615 0.036 Uiso 1 1 calc R . . . .
C72 C 0.47192(13) -0.1043(3) 1.08431(10) 0.0219(5) Uani 1 1 d . . . . .
C61 C -0.18019(13) 0.3157(3) 0.81994(10) 0.0209(5) Uani 1 1 d . . . . .
C81 C -0.14656(16) 0.3394(4) 0.72740(12) 0.0381(7) Uani 1 1 d . . . . .
H81 H -0.1402 0.2922 0.6928 0.046 Uiso 1 1 calc R . . . .
C101 C -0.14535(15) 0.5734(3) 0.78797(12) 0.0341(6) Uani 1 1 d . . . . .
H101 H -0.1376 0.6833 0.7947 0.041 Uiso 1 1 calc R . . . .
C62 C 0.39379(16) -0.5027(3) 0.95325(12) 0.0335(6) Uani 1 1 d . . . . .
H62A H 0.3583 -0.5224 0.9130 0.050 Uiso 1 1 calc GR . . . .
H62B H 0.3890 -0.5881 0.9798 0.050 Uiso 1 1 calc GR . . . .
H62C H 0.4476 -0.4979 0.9522 0.050 Uiso 1 1 calc GR . . . .
C82 C 0.55869(14) -0.1109(3) 1.18411(11) 0.0303(5) Uani 1 1 d . . . . .
H82A H 0.5548 -0.2260 1.1847 0.045 Uiso 1 1 calc GR . . . .
H82B H 0.5635 -0.0690 1.2237 0.045 Uiso 1 1 calc GR . . . .
H82C H 0.6048 -0.0809 1.1730 0.045 Uiso 1 1 calc GR . . . .
C91 C -0.13311(15) 0.5033(4) 0.73723(12) 0.0374(6) Uani 1 1 d . . . . .
H91 H -0.1161 0.5652 0.7102 0.045 Uiso 1 1 calc R . . . .
N1S N -0.01515(12) 0.0263(2) 0.71280(9) 0.0280(4) Uani 1 1 d . . . . .
C121 C -0.08257(14) 0.4351(3) 1.10995(10) 0.0274(5) Uani 1 1 d . . . . .
H12A H -0.0595 0.5405 1.1089 0.033 Uiso 1 1 calc R . . . .
H12B H -0.0404 0.3644 1.1333 0.033 Uiso 1 1 calc R . . . .
C181 C -0.18420(15) 0.3127(3) 1.15262(10) 0.0254(5) Uani 1 1 d . . . . .
H181 H -0.1722 0.2121 1.1402 0.030 Uiso 1 1 calc R . . . .
C131 C -0.14525(13) 0.4478(3) 1.14134(9) 0.0216(5) Uani 1 1 d . . . . .
C141 C -0.16415(14) 0.5978(3) 1.16022(10) 0.0243(5) Uani 1 1 d . . . . .
H141 H -0.1387 0.6897 1.1527 0.029 Uiso 1 1 calc R . . . .
O1S O -0.10936(12) -0.1432(2) 0.65558(9) 0.0413(5) Uani 1 1 d . . . . .
C171 C -0.24097(16) 0.3265(3) 1.18230(11) 0.0301(6) Uani 1 1 d . . . . .
H171 H -0.2675 0.2354 1.1891 0.036 Uiso 1 1 calc R . . . .
C151 C -0.22053(14) 0.6104(3) 1.19012(11) 0.0291(5) Uani 1 1 d . . . . .
H151 H -0.2331 0.7106 1.2024 0.035 Uiso 1 1 calc R . . . .
C161 C -0.25825(15) 0.4743(3) 1.20169(11) 0.0327(6) Uani 1 1 d . . . . .
H161 H -0.2953 0.4827 1.2226 0.039 Uiso 1 1 calc R . . . .
C1S C -0.06395(15) -0.0282(3) 0.66054(12) 0.0304(6) Uani 1 1 d . . . . .
H1S H -0.0638 0.0244 0.6251 0.036 Uiso 1 1 calc R . . . .
C2S C 0.03336(17) 0.1690(3) 0.71425(16) 0.0410(7) Uani 1 1 d . . . . .
H2SA H 0.0267 0.2040 0.6734 0.061 Uiso 1 1 calc GR . . . .
H2SB H 0.0884 0.1438 0.7342 0.061 Uiso 1 1 calc GR . . . .
H2SC H 0.0170 0.2531 0.7361 0.061 Uiso 1 1 calc GR . . . .
C3S C -0.01261(17) -0.0433(4) 0.76999(12) 0.0405(7) Uani 1 1 d . . . . .
H3SA H -0.0501 -0.1303 0.7632 0.061 Uiso 1 1 calc GR . . . .
H3SB H -0.0261 0.0369 0.7949 0.061 Uiso 1 1 calc GR . . . .
H3SC H 0.0401 -0.0833 0.7901 0.061 Uiso 1 1 calc GR . . . .


_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
Ni S22 2.1624(6) . ?
Ni S11 2.1611(6) . ?
Ni S12 2.1574(6) . ?
Ni S21 2.1528(6) . ?
S22 C22 1.741(2) . ?
S11 C11 1.696(2) . ?
S12 C12 1.746(2) . ?
S42 C22 1.767(2) . ?
S42 C32 1.764(2) . ?
S32 C12 1.766(2) . ?
S32 C42 1.775(2) . ?
S21 C21 1.687(2) . ?
O22 C52 1.334(3) . ?
O22 C62 1.455(3) . ?
O12 C52 1.208(3) . ?
O42 C72 1.330(3) . ?
O42 C82 1.444(3) . ?
N11 C31 1.470(3) . ?
N11 C21 1.330(3) . ?
N11 C121 1.481(3) . ?
N21 C41 1.472(3) . ?
N21 C11 1.323(3) . ?
N21 C51 1.475(3) . ?
O32 C72 1.203(3) . ?
C12 C22 1.345(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C41 1.503(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C52 1.489(3) . ?
C42 C32 1.342(3) . ?
C32 C72 1.495(3) . ?
C11 C21 1.477(3) . ?
C111 H111 0.9300 . ?
C111 C61 1.376(3) . ?
C111 C101 1.394(4) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51 C61 1.512(3) . ?
C71 H71 0.9300 . ?
C71 C61 1.395(3) . ?
C71 C81 1.377(4) . ?
C81 H81 0.9300 . ?
C81 C91 1.390(4) . ?
C101 H101 0.9300 . ?
C101 C91 1.388(4) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
C91 H91 0.9300 . ?
N1S C1S 1.326(3) . ?
N1S C2S 1.458(3) . ?
N1S C3S 1.433(3) . ?
C121 H12A 0.9700 . ?
C121 H12B 0.9700 . ?
C121 C131 1.506(3) . ?
C181 H181 0.9300 . ?
C181 C131 1.384(3) . ?
C181 C171 1.386(4) . ?
C131 C141 1.397(3) . ?
C141 H141 0.9300 . ?
C141 C151 1.383(3) . ?
O1S C1S 1.231(3) . ?
C171 H171 0.9300 . ?
C171 C161 1.376(4) . ?
C151 H151 0.9300 . ?
C151 C161 1.381(4) . ?
C161 H161 0.9300 . ?
C1S H1S 0.9300 . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9600 . ?
C2S H2SC 0.9600 . ?
C3S H3SA 0.9600 . ?
C3S H3SB 0.9600 . ?
C3S H3SC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S11 Ni S22 176.89(2) . . ?
S12 Ni S22 92.55(2) . . ?
S12 Ni S11 88.69(2) . . ?
S21 Ni S22 87.43(2) . . ?
S21 Ni S11 91.26(2) . . ?
S21 Ni S12 178.62(3) . . ?
C22 S22 Ni 102.28(7) . . ?
C11 S11 Ni 105.79(8) . . ?
C12 S12 Ni 102.11(8) . . ?
C32 S42 C22 101.13(11) . . ?
C12 S32 C42 100.40(10) . . ?
C21 S21 Ni 106.23(8) . . ?
C52 O22 C62 116.28(19) . . ?
C72 O42 C82 114.99(18) . . ?
C31 N11 C121 119.03(18) . . ?
C21 N11 C31 119.67(18) . . ?
C21 N11 C121 119.20(18) . . ?
C41 N21 C51 118.41(17) . . ?
C11 N21 C41 119.25(18) . . ?
C11 N21 C51 121.33(18) . . ?
S12 C12 S32 117.96(12) . . ?
C22 C12 S12 120.80(17) . . ?
C22 C12 S32 121.19(17) . . ?
N11 C31 H31A 109.7 . . ?
N11 C31 H31B 109.7 . . ?
N11 C31 C41 109.82(18) . . ?
H31A C31 H31B 108.2 . . ?
C41 C31 H31A 109.7 . . ?
C41 C31 H31B 109.7 . . ?
S22 C22 S42 117.27(12) . . ?
C12 C22 S22 120.48(17) . . ?
C12 C22 S42 122.21(18) . . ?
N21 C41 C31 110.66(18) . . ?
N21 C41 H41A 109.5 . . ?
N21 C41 H41B 109.5 . . ?
C31 C41 H41A 109.5 . . ?
C31 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
C52 C42 S32 112.66(16) . . ?
C32 C42 S32 121.48(18) . . ?
C32 C42 C52 125.8(2) . . ?
O22 C52 C42 111.22(19) . . ?
O12 C52 O22 125.6(2) . . ?
O12 C52 C42 122.9(2) . . ?
C42 C32 S42 121.84(18) . . ?
C42 C32 C72 120.0(2) . . ?
C72 C32 S42 118.04(16) . . ?
N21 C11 S11 121.51(17) . . ?
N21 C11 C21 120.23(19) . . ?
C21 C11 S11 118.25(16) . . ?
C61 C111 H111 119.6 . . ?
C61 C111 C101 120.9(2) . . ?
C101 C111 H111 119.6 . . ?
N21 C51 H51A 109.1 . . ?
N21 C51 H51B 109.1 . . ?
N21 C51 C61 112.36(18) . . ?
H51A C51 H51B 107.9 . . ?
C61 C51 H51A 109.1 . . ?
C61 C51 H51B 109.1 . . ?
N11 C21 S21 122.21(17) . . ?
N11 C21 C11 119.32(19) . . ?
C11 C21 S21 118.44(17) . . ?
C61 C71 H71 119.9 . . ?
C81 C71 H71 119.9 . . ?
C81 C71 C61 120.3(3) . . ?
O42 C72 C32 112.15(19) . . ?
O32 C72 O42 124.5(2) . . ?
O32 C72 C32 123.3(2) . . ?
C111 C61 C51 122.2(2) . . ?
C111 C61 C71 119.1(2) . . ?
C71 C61 C51 118.7(2) . . ?
C71 C81 H81 119.6 . . ?
C71 C81 C91 120.8(3) . . ?
C91 C81 H81 119.6 . . ?
C111 C101 H101 120.1 . . ?
C91 C101 C111 119.9(3) . . ?
C91 C101 H101 120.1 . . ?
O22 C62 H62A 109.5 . . ?
O22 C62 H62B 109.5 . . ?
O22 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O42 C82 H82A 109.5 . . ?
O42 C82 H82B 109.5 . . ?
O42 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C91 H91 120.4 . . ?
C101 C91 C81 119.1(3) . . ?
C101 C91 H91 120.4 . . ?
C1S N1S C2S 120.6(2) . . ?
C1S N1S C3S 121.9(2) . . ?
C3S N1S C2S 117.3(2) . . ?
N11 C121 H12A 109.1 . . ?
N11 C121 H12B 109.1 . . ?
N11 C121 C131 112.59(18) . . ?
H12A C121 H12B 107.8 . . ?
C131 C121 H12A 109.1 . . ?
C131 C121 H12B 109.1 . . ?
C131 C181 H181 119.8 . . ?
C131 C181 C171 120.4(2) . . ?
C171 C181 H181 119.8 . . ?
C181 C131 C121 121.2(2) . . ?
C181 C131 C141 119.0(2) . . ?
C141 C131 C121 119.8(2) . . ?
C131 C141 H141 119.9 . . ?
C151 C141 C131 120.3(2) . . ?
C151 C141 H141 119.9 . . ?
C181 C171 H171 119.9 . . ?
C161 C171 C181 120.3(2) . . ?
C161 C171 H171 119.9 . . ?
C141 C151 H151 119.9 . . ?
C161 C151 C141 120.1(2) . . ?
C161 C151 H151 119.9 . . ?
C171 C161 C151 119.9(2) . . ?
C171 C161 H161 120.0 . . ?
C151 C161 H161 120.0 . . ?
N1S C1S H1S 117.7 . . ?
O1S C1S N1S 124.7(2) . . ?
O1S C1S H1S 117.7 . . ?
N1S C2S H2SA 109.5 . . ?
N1S C2S H2SB 109.5 . . ?
N1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N1S C3S H3SA 109.5 . . ?
N1S C3S H3SB 109.5 . . ?
N1S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.705

#END
