# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_xcalibur
_database_code_depnum_ccdc_archive 'CCDC 1970593'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C30 H28 Cl2 N6 Ni O8 S2'
_chemical_formula_moiety         'C30 H28 Cl2 N6 Ni O8 S2'
_chemical_formula_weight         794.31
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
_space_group_IT_number           9
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 +X,-Y,1/2+Z
3 1/2+X,1/2+Y,+Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   21.948(2)
_cell_length_b                   8.33062(19)
_cell_length_c                   20.7006(8)
_cell_angle_alpha                90.0000
_cell_angle_beta                 115.404(5)
_cell_angle_gamma                90.0000
_cell_volume                     3419.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10689
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      31.25
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632.00
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_T_max  0.930

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            10487
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.178
_diffrn_reflns_theta_full        25.350
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5494
_reflns_number_gt                5345
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0932
_refine_ls_number_restraints     29
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5494
_refine_ls_number_parameters     453
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0703P)²+0.4539P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2435 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.014(10)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.817387(15) 0.20808(4) 0.421085(16) 0.02177(11) Uani 1 1 d . . .
Cl1 Cl 0.63196(4) 0.38757(10) 0.16940(5) 0.0387(2) Uani 1 1 d . . .
Cl2 Cl 0.96368(5) 0.61454(10) 0.23200(5) 0.0380(2) Uani 1 1 d . . .
S1 S 0.81068(4) 0.46352(9) 0.36446(4) 0.02563(17) Uani 1 1 d . . .
S2 S 0.87755(4) 0.10638(9) 0.35602(4) 0.02793(18) Uani 1 1 d . . .
O1 O 0.58438(19) 0.5061(4) 0.1298(2) 0.0853(14) Uani 1 1 d . . .
O2 O 0.68554(16) 0.3840(5) 0.14780(18) 0.0655(9) Uani 1 1 d . . .
O3 O 0.66045(18) 0.4235(4) 0.24421(18) 0.0628(8) Uani 1 1 d . . .
O4 O 0.60004(15) 0.2348(4) 0.15679(17) 0.0519(7) Uani 1 1 d . . .
O5 O 0.9840(3) 0.7719(5) 0.2268(3) 0.0979(15) Uani 1 1 d . . .
O6 O 1.0105(2) 0.5090(6) 0.2231(3) 0.0919(14) Uani 1 1 d . . .
O7 O 0.9646(3) 0.5983(7) 0.3000(2) 0.1023(17) Uani 1 1 d . . .
O8 O 0.89877(17) 0.5798(5) 0.1785(2) 0.0789(11) Uani 1 1 d . . .
N1 N 0.90102(13) 0.3035(3) 0.50085(14) 0.0217(5) Uani 1 1 d . . .
N2 N 0.84480(13) 0.0207(3) 0.49357(15) 0.0279(6) Uani 1 1 d . . .
N3 N 0.73594(13) 0.1090(3) 0.33980(14) 0.0261(5) Uani 1 1 d . . .
N4 N 0.74231(14) 0.2770(3) 0.44996(15) 0.0267(6) Uani 1 1 d . . .
N5A N 0.6591(7) 0.7858(15) 0.3809(8) 0.081(4) Uani 0.50 1 d PDU A 1
N6B N 0.6720(5) 0.7089(16) 0.3904(7) 0.077(3) Uani 0.50 1 d PDU A 2
N7 N 0.5343(2) 0.2928(6) -0.0391(3) 0.0693(12) Uani 1 1 d D . .
C1 C 0.88867(15) 0.5398(4) 0.43057(17) 0.0247(6) Uani 1 1 d . . .
C2 C 0.92484(15) 0.4568(3) 0.49398(16) 0.0240(6) Uani 1 1 d . . .
C3 C 0.98233(16) 0.5282(4) 0.54711(18) 0.0315(7) Uani 1 1 d . . .
H3 H 1.0071 0.4740 0.5897 0.038 Uiso 1 1 calc R . .
C4 C 1.00212(18) 0.6792(4) 0.5362(2) 0.0379(8) Uani 1 1 d . . .
H4 H 1.0401 0.7262 0.5718 0.045 Uiso 1 1 calc R . .
C5 C 0.96661(18) 0.7614(4) 0.4736(2) 0.0374(8) Uani 1 1 d . . .
H5 H 0.9806 0.8628 0.4669 0.045 Uiso 1 1 calc R . .
C6 C 0.90965(17) 0.6919(4) 0.4204(2) 0.0319(7) Uani 1 1 d . . .
H6 H 0.8855 0.7469 0.3779 0.038 Uiso 1 1 calc R . .
C7 C 0.93303(17) 0.2090(4) 0.55378(18) 0.0283(7) Uani 1 1 d . . .
H7 H 0.9743 0.2376 0.5905 0.034 Uiso 1 1 calc R . .
C8 C 0.90141(17) 0.0547(4) 0.55346(17) 0.0286(7) Uani 1 1 d . . .
C9 C 0.9274(2) -0.0525(4) 0.6103(2) 0.0401(8) Uani 1 1 d . . .
H9 H 0.9671 -0.0291 0.6504 0.048 Uiso 1 1 calc R . .
C10 C 0.8931(2) -0.1953(4) 0.6063(2) 0.0452(10) Uani 1 1 d . . .
H10 H 0.9090 -0.2683 0.6439 0.054 Uiso 1 1 calc R . .
C11 C 0.8356(2) -0.2264(4) 0.5461(2) 0.0439(9) Uani 1 1 d . . .
H11 H 0.8118 -0.3209 0.5423 0.053 Uiso 1 1 calc R . .
C12 C 0.81324(19) -0.1160(4) 0.4908(2) 0.0357(8) Uani 1 1 d . . .
H12 H 0.7742 -0.1390 0.4499 0.043 Uiso 1 1 calc R . .
C13 C 0.80717(17) 0.0100(4) 0.28724(17) 0.0311(7) Uani 1 1 d . . .
C14 C 0.74300(17) 0.0150(4) 0.28579(17) 0.0279(7) Uani 1 1 d . . .
C15 C 0.6909(2) -0.0775(4) 0.2355(2) 0.0389(8) Uani 1 1 d . . .
H15 H 0.6482 -0.0759 0.2345 0.047 Uiso 1 1 calc R . .
C16 C 0.7033(2) -0.1701(5) 0.1880(2) 0.0462(9) Uani 1 1 d . . .
H16 H 0.6687 -0.2314 0.1546 0.055 Uiso 1 1 calc R . .
C17 C 0.7664(2) -0.1739(5) 0.1890(2) 0.0518(11) Uani 1 1 d . . .
H17 H 0.7739 -0.2377 0.1563 0.062 Uiso 1 1 calc R . .
C18 C 0.8186(2) -0.0843(5) 0.2378(2) 0.0413(8) Uani 1 1 d . . .
H18 H 0.8610 -0.0867 0.2379 0.050 Uiso 1 1 calc R . .
C19 C 0.67890(17) 0.1443(4) 0.33909(19) 0.0327(7) Uani 1 1 d . . .
H19 H 0.6386 0.1127 0.3017 0.039 Uiso 1 1 calc R . .
C20 C 0.67989(17) 0.2364(4) 0.39972(19) 0.0299(7) Uani 1 1 d . . .
C21 C 0.62198(19) 0.2805(5) 0.4064(2) 0.0429(9) Uani 1 1 d . . .
H21 H 0.5795 0.2533 0.3714 0.051 Uiso 1 1 calc R . .
C22 C 0.6290(2) 0.3657(5) 0.4663(2) 0.0464(9) Uani 1 1 d . . .
H22 H 0.5909 0.3970 0.4718 0.056 Uiso 1 1 calc R . .
C23 C 0.6919(2) 0.4047(4) 0.5178(2) 0.0399(8) Uani 1 1 d . . .
H23 H 0.6968 0.4612 0.5585 0.048 Uiso 1 1 calc R . .
C24 C 0.74789(18) 0.3583(4) 0.50801(18) 0.0306(7) Uani 1 1 d . . .
H24 H 0.7906 0.3842 0.5428 0.037 Uiso 1 1 calc R . .
C25 C 0.83201(17) 0.4082(4) 0.29159(18) 0.0322(7) Uani 1 1 d . . .
H25A H 0.7922 0.3644 0.2527 0.039 Uiso 1 1 calc R . .
H25B H 0.8450 0.5041 0.2740 0.039 Uiso 1 1 calc R . .
C26 C 0.88823(18) 0.2873(4) 0.3124(2) 0.0326(7) Uani 1 1 d . . .
H26A H 0.9299 0.3391 0.3443 0.039 Uiso 1 1 calc R . .
H26B H 0.8931 0.2559 0.2697 0.039 Uiso 1 1 calc R . .
C27 C 0.5546(3) 0.6328(7) 0.2960(3) 0.0735(15) Uani 1 1 d U A .
H27A H 0.5624 0.5332 0.2774 0.088 Uiso 1 1 calc R . .
H27B H 0.5330 0.7071 0.2574 0.088 Uiso 1 1 calc R . .
H27C H 0.5261 0.6142 0.3197 0.088 Uiso 1 1 calc R . .
C28 C 0.6170(3) 0.6976(7) 0.3454(3) 0.0677(14) Uani 1 1 d DU . .
C29 C 0.6358(3) 0.1006(7) 0.0220(3) 0.0731(15) Uani 1 1 d . . .
H29A H 0.6595 0.0903 -0.0074 0.088 Uiso 1 1 calc R . .
H29B H 0.6200 -0.0029 0.0284 0.088 Uiso 1 1 calc R . .
H29C H 0.6657 0.1434 0.0678 0.088 Uiso 1 1 calc R . .
C30 C 0.5794(3) 0.2069(6) -0.0118(3) 0.0603(12) Uani 1 1 d D . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N3 2.032(3) . ?
Ni1 N1 2.032(3) . ?
Ni1 N4 2.061(3) . ?
Ni1 N2 2.068(3) . ?
Ni1 S1 2.4033(8) . ?
Ni1 S2 2.4086(8) . ?
Cl1 O1 1.415(3) . ?
Cl1 O4 1.422(3) . ?
Cl1 O2 1.427(3) . ?
Cl1 O3 1.431(3) . ?
Cl2 O5 1.403(4) . ?
Cl2 O7 1.406(4) . ?
Cl2 O8 1.409(4) . ?
Cl2 O6 1.424(4) . ?
S1 C1 1.788(3) . ?
S1 C25 1.820(3) . ?
S2 C13 1.781(3) . ?
S2 C26 1.823(3) . ?
N1 C7 1.286(4) . ?
N1 C2 1.410(4) . ?
N2 C12 1.321(4) . ?
N2 C8 1.356(4) . ?
N3 C19 1.280(4) . ?
N3 C14 1.427(4) . ?
N4 C24 1.338(4) . ?
N4 C20 1.360(4) . ?
N5A C28 1.161(8) . ?
N6B C28 1.170(8) . ?
N7 C30 1.153(6) . ?
C1 C2 1.392(4) . ?
C1 C6 1.394(4) . ?
C2 C3 1.402(4) . ?
C3 C4 1.381(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.460(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.390(5) . ?
C9 C10 1.392(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.364(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.395(5) . ?
C13 C14 1.397(5) . ?
C14 C15 1.401(5) . ?
C15 C16 1.365(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.377(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(6) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.463(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.386(5) . ?
C21 C22 1.378(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.383(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.505(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.419(7) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 C30 1.437(8) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 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
N3 Ni1 N1 177.91(11) . . ?
N3 Ni1 N4 79.89(11) . . ?
N1 Ni1 N4 102.20(10) . . ?
N3 Ni1 N2 99.97(10) . . ?
N1 Ni1 N2 79.95(10) . . ?
N4 Ni1 N2 91.14(10) . . ?
N3 Ni1 S1 96.18(7) . . ?
N1 Ni1 S1 83.96(7) . . ?
N4 Ni1 S1 90.31(7) . . ?
N2 Ni1 S1 163.79(8) . . ?
N3 Ni1 S2 83.84(8) . . ?
N1 Ni1 S2 94.08(7) . . ?
N4 Ni1 S2 163.44(8) . . ?
N2 Ni1 S2 94.68(8) . . ?
S1 Ni1 S2 88.41(3) . . ?
O1 Cl1 O4 109.6(2) . . ?
O1 Cl1 O2 109.6(3) . . ?
O4 Cl1 O2 109.3(2) . . ?
O1 Cl1 O3 110.6(3) . . ?
O4 Cl1 O3 109.8(2) . . ?
O2 Cl1 O3 107.9(2) . . ?
O5 Cl2 O7 107.3(3) . . ?
O5 Cl2 O8 112.3(3) . . ?
O7 Cl2 O8 110.1(3) . . ?
O5 Cl2 O6 107.2(3) . . ?
O7 Cl2 O6 111.7(4) . . ?
O8 Cl2 O6 108.3(2) . . ?
C1 S1 C25 102.84(15) . . ?
C1 S1 Ni1 95.93(10) . . ?
C25 S1 Ni1 101.31(11) . . ?
C13 S2 C26 103.21(16) . . ?
C13 S2 Ni1 96.32(11) . . ?
C26 S2 Ni1 101.76(11) . . ?
C7 N1 C2 123.4(3) . . ?
C7 N1 Ni1 115.2(2) . . ?
C2 N1 Ni1 121.16(19) . . ?
C12 N2 C8 118.5(3) . . ?
C12 N2 Ni1 129.4(2) . . ?
C8 N2 Ni1 111.9(2) . . ?
C19 N3 C14 123.5(3) . . ?
C19 N3 Ni1 115.2(2) . . ?
C14 N3 Ni1 121.3(2) . . ?
C24 N4 C20 119.1(3) . . ?
C24 N4 Ni1 128.7(2) . . ?
C20 N4 Ni1 112.2(2) . . ?
C2 C1 C6 120.2(3) . . ?
C2 C1 S1 121.1(2) . . ?
C6 C1 S1 118.5(2) . . ?
C1 C2 C3 119.1(3) . . ?
C1 C2 N1 117.3(3) . . ?
C3 C2 N1 123.6(3) . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 121.1(3) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
N1 C7 C8 116.8(3) . . ?
N1 C7 H7 121.6 . . ?
C8 C7 H7 121.6 . . ?
N2 C8 C9 121.5(3) . . ?
N2 C8 C7 115.8(3) . . ?
C9 C8 C7 122.7(3) . . ?
C8 C9 C10 118.8(4) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C11 C10 C9 118.8(3) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
N2 C12 C11 122.9(4) . . ?
N2 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C18 C13 C14 119.9(3) . . ?
C18 C13 S2 118.2(3) . . ?
C14 C13 S2 121.6(2) . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 N3 116.6(3) . . ?
C15 C14 N3 123.8(3) . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 120.8(4) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C16 C17 C18 120.9(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 119.3(4) . . ?
C17 C18 H18 120.4 . . ?
C13 C18 H18 120.4 . . ?
N3 C19 C20 117.1(3) . . ?
N3 C19 H19 121.4 . . ?
C20 C19 H19 121.4 . . ?
N4 C20 C21 121.6(3) . . ?
N4 C20 C19 115.2(3) . . ?
C21 C20 C19 123.2(3) . . ?
C22 C21 C20 118.2(4) . . ?
C22 C21 H21 120.9 . . ?
C20 C21 H21 120.9 . . ?
C23 C22 C21 120.5(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 118.7(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
N4 C24 C23 121.9(3) . . ?
N4 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C26 C25 S1 113.7(2) . . ?
C26 C25 H25A 108.8 . . ?
S1 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
S1 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 S2 115.5(2) . . ?
C25 C26 H26A 108.4 . . ?
S2 C26 H26A 108.4 . . ?
C25 C26 H26B 108.4 . . ?
S2 C26 H26B 108.4 . . ?
H26A C26 H26B 107.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N5A C28 N6B 34.6(8) . . ?
N5A C28 C27 163.0(10) . . ?
N6B C28 C27 162.2(9) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N7 C30 C29 179.6(6) . . ?

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
N3 Ni1 S1 C1 -172.56(13) . . . . ?
N1 Ni1 S1 C1 5.35(12) . . . . ?
N4 Ni1 S1 C1 107.58(13) . . . . ?
N2 Ni1 S1 C1 12.4(3) . . . . ?
S2 Ni1 S1 C1 -88.93(10) . . . . ?
N3 Ni1 S1 C25 -68.16(14) . . . . ?
N1 Ni1 S1 C25 109.75(13) . . . . ?
N4 Ni1 S1 C25 -148.02(14) . . . . ?
N2 Ni1 S1 C25 116.8(3) . . . . ?
S2 Ni1 S1 C25 15.47(12) . . . . ?
N3 Ni1 S2 C13 -2.97(12) . . . . ?
N1 Ni1 S2 C13 176.82(13) . . . . ?
N4 Ni1 S2 C13 -13.6(3) . . . . ?
N2 Ni1 S2 C13 96.58(13) . . . . ?
S1 Ni1 S2 C13 -99.36(11) . . . . ?
N3 Ni1 S2 C26 101.98(14) . . . . ?
N1 Ni1 S2 C26 -78.23(14) . . . . ?
N4 Ni1 S2 C26 91.3(3) . . . . ?
N2 Ni1 S2 C26 -158.47(14) . . . . ?
S1 Ni1 S2 C26 5.59(13) . . . . ?
N3 Ni1 N1 C7 -84(3) . . . . ?
N4 Ni1 N1 C7 93.0(2) . . . . ?
N2 Ni1 N1 C7 4.0(2) . . . . ?
S1 Ni1 N1 C7 -178.0(2) . . . . ?
S2 Ni1 N1 C7 -90.0(2) . . . . ?
N3 Ni1 N1 C2 90(3) . . . . ?
N4 Ni1 N1 C2 -93.1(2) . . . . ?
N2 Ni1 N1 C2 177.9(2) . . . . ?
S1 Ni1 N1 C2 -4.1(2) . . . . ?
S2 Ni1 N1 C2 83.9(2) . . . . ?
N3 Ni1 N2 C12 -7.2(3) . . . . ?
N1 Ni1 N2 C12 174.9(3) . . . . ?
N4 Ni1 N2 C12 72.7(3) . . . . ?
S1 Ni1 N2 C12 167.8(2) . . . . ?
S2 Ni1 N2 C12 -91.8(3) . . . . ?
N3 Ni1 N2 C8 177.5(2) . . . . ?
N1 Ni1 N2 C8 -0.4(2) . . . . ?
N4 Ni1 N2 C8 -102.6(2) . . . . ?
S1 Ni1 N2 C8 -7.6(4) . . . . ?
S2 Ni1 N2 C8 92.9(2) . . . . ?
N1 Ni1 N3 C19 -177(24) . . . . ?
N4 Ni1 N3 C19 6.2(2) . . . . ?
N2 Ni1 N3 C19 95.6(2) . . . . ?
S1 Ni1 N3 C19 -83.0(2) . . . . ?
S2 Ni1 N3 C19 -170.7(2) . . . . ?
N1 Ni1 N3 C14 0(3) . . . . ?
N4 Ni1 N3 C14 -177.3(2) . . . . ?
N2 Ni1 N3 C14 -87.9(2) . . . . ?
S1 Ni1 N3 C14 93.5(2) . . . . ?
S2 Ni1 N3 C14 5.8(2) . . . . ?
N3 Ni1 N4 C24 177.5(3) . . . . ?
N1 Ni1 N4 C24 -2.4(3) . . . . ?
N2 Ni1 N4 C24 77.5(3) . . . . ?
S1 Ni1 N4 C24 -86.3(3) . . . . ?
S2 Ni1 N4 C24 -171.77(19) . . . . ?
N3 Ni1 N4 C20 -5.3(2) . . . . ?
N1 Ni1 N4 C20 174.8(2) . . . . ?
N2 Ni1 N4 C20 -105.2(2) . . . . ?
S1 Ni1 N4 C20 90.9(2) . . . . ?
S2 Ni1 N4 C20 5.5(4) . . . . ?
C25 S1 C1 C2 -110.7(3) . . . . ?
Ni1 S1 C1 C2 -7.7(2) . . . . ?
C25 S1 C1 C6 75.1(3) . . . . ?
Ni1 S1 C1 C6 178.2(2) . . . . ?
C6 C1 C2 C3 0.0(4) . . . . ?
S1 C1 C2 C3 -174.0(2) . . . . ?
C6 C1 C2 N1 -179.9(3) . . . . ?
S1 C1 C2 N1 6.0(4) . . . . ?
C7 N1 C2 C1 173.6(3) . . . . ?
Ni1 N1 C2 C1 0.2(4) . . . . ?
C7 N1 C2 C3 -6.3(5) . . . . ?
Ni1 N1 C2 C3 -179.8(2) . . . . ?
C1 C2 C3 C4 0.3(5) . . . . ?
N1 C2 C3 C4 -179.8(3) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
C3 C4 C5 C6 0.3(6) . . . . ?
C4 C5 C6 C1 0.1(5) . . . . ?
C2 C1 C6 C5 -0.2(5) . . . . ?
S1 C1 C6 C5 174.0(3) . . . . ?
C2 N1 C7 C8 179.5(3) . . . . ?
Ni1 N1 C7 C8 -6.7(4) . . . . ?
C12 N2 C8 C9 1.8(5) . . . . ?
Ni1 N2 C8 C9 177.7(3) . . . . ?
C12 N2 C8 C7 -178.7(3) . . . . ?
Ni1 N2 C8 C7 -2.8(4) . . . . ?
N1 C7 C8 N2 6.5(5) . . . . ?
N1 C7 C8 C9 -174.1(3) . . . . ?
N2 C8 C9 C10 -2.1(6) . . . . ?
C7 C8 C9 C10 178.4(3) . . . . ?
C8 C9 C10 C11 1.1(6) . . . . ?
C9 C10 C11 C12 0.2(6) . . . . ?
C8 N2 C12 C11 -0.4(5) . . . . ?
Ni1 N2 C12 C11 -175.5(3) . . . . ?
C10 C11 C12 N2 -0.6(6) . . . . ?
C26 S2 C13 C18 82.8(3) . . . . ?
Ni1 S2 C13 C18 -173.5(3) . . . . ?
C26 S2 C13 C14 -103.1(3) . . . . ?
Ni1 S2 C13 C14 0.6(3) . . . . ?
C18 C13 C14 C15 1.3(5) . . . . ?
S2 C13 C14 C15 -172.7(3) . . . . ?
C18 C13 C14 N3 177.5(3) . . . . ?
S2 C13 C14 N3 3.6(4) . . . . ?
C19 N3 C14 C13 169.3(3) . . . . ?
Ni1 N3 C14 C13 -7.0(4) . . . . ?
C19 N3 C14 C15 -14.6(5) . . . . ?
Ni1 N3 C14 C15 169.1(3) . . . . ?
C13 C14 C15 C16 -0.7(5) . . . . ?
N3 C14 C15 C16 -176.7(3) . . . . ?
C14 C15 C16 C17 0.1(6) . . . . ?
C15 C16 C17 C18 -0.1(7) . . . . ?
C16 C17 C18 C13 0.6(6) . . . . ?
C14 C13 C18 C17 -1.2(6) . . . . ?
S2 C13 C18 C17 173.0(3) . . . . ?
C14 N3 C19 C20 177.7(3) . . . . ?
Ni1 N3 C19 C20 -5.9(4) . . . . ?
C24 N4 C20 C21 1.6(5) . . . . ?
Ni1 N4 C20 C21 -175.9(3) . . . . ?
C24 N4 C20 C19 -178.5(3) . . . . ?
Ni1 N4 C20 C19 4.0(3) . . . . ?
N3 C19 C20 N4 1.1(4) . . . . ?
N3 C19 C20 C21 -178.9(3) . . . . ?
N4 C20 C21 C22 -0.9(5) . . . . ?
C19 C20 C21 C22 179.2(3) . . . . ?
C20 C21 C22 C23 -0.3(6) . . . . ?
C21 C22 C23 C24 0.7(6) . . . . ?
C20 N4 C24 C23 -1.2(5) . . . . ?
Ni1 N4 C24 C23 175.9(2) . . . . ?
C22 C23 C24 N4 0.1(5) . . . . ?
C1 S1 C25 C26 58.3(3) . . . . ?
Ni1 S1 C25 C26 -40.5(3) . . . . ?
S1 C25 C26 S2 52.1(3) . . . . ?
C13 S2 C26 C25 66.5(3) . . . . ?
Ni1 S2 C26 C25 -32.9(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_xcalibur_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1970596'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H16 Cl2 N4 Ni S2'
_chemical_formula_moiety         'C24 H16 Cl2 N4 Ni S2'
_chemical_formula_weight         554.14
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.9125(3)
_cell_length_b                   12.1348(5)
_cell_length_c                   12.2295(5)
_cell_angle_alpha                67.774(4)
_cell_angle_beta                 69.928(3)
_cell_angle_gamma                87.213(3)
_cell_volume                     1144.97(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5574
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      31.30
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             564.00
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_T_max  0.879

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            7986
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.523
_diffrn_reflns_theta_full        25.350
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4120
_reflns_number_gt                3530
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0859
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4120
_refine_ls_number_parameters     298
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0462P)²+0.4228P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.30
_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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.49839(4) 0.24657(3) 0.74775(3) 0.02477(12) Uani 1 1 d . . .
Cl1 Cl 0.43039(10) 0.17130(8) 1.35727(7) 0.0524(2) Uani 1 1 d . . .
Cl2 Cl 1.01275(9) 0.39019(7) 0.12602(7) 0.0484(2) Uani 1 1 d . . .
S1 S 0.59507(8) 0.41227(6) 0.77159(6) 0.03101(17) Uani 1 1 d . . .
S2 S 0.74161(8) 0.15280(6) 0.71699(6) 0.03353(18) Uani 1 1 d . . .
N1 N 0.4133(2) 0.17466(18) 0.93946(19) 0.0244(4) Uani 1 1 d . . .
N2 N 0.3547(3) 0.08871(18) 0.7875(2) 0.0298(5) Uani 1 1 d . . .
N3 N 0.5681(2) 0.30904(17) 0.55687(18) 0.0234(4) Uani 1 1 d . . .
N4 N 0.2926(2) 0.33041(18) 0.7175(2) 0.0280(5) Uani 1 1 d . . .
C1 C 0.5536(3) 0.3408(2) 0.9334(2) 0.0269(5) Uani 1 1 d . . .
C2 C 0.4624(3) 0.2296(2) 1.0058(2) 0.0268(5) Uani 1 1 d . . .
C3 C 0.4252(3) 0.1769(2) 1.1365(2) 0.0300(6) Uani 1 1 d . . .
H3 H 0.3644 0.1035 1.1839 0.036 Uiso 1 1 calc R . .
C4 C 0.4801(3) 0.2356(3) 1.1931(3) 0.0358(6) Uani 1 1 d . . .
C5 C 0.5733(3) 0.3429(3) 1.1254(3) 0.0370(7) Uani 1 1 d . . .
H5 H 0.6112 0.3801 1.1660 0.044 Uiso 1 1 calc R . .
C6 C 0.6099(3) 0.3945(3) 0.9973(3) 0.0360(6) Uani 1 1 d . . .
H6 H 0.6736 0.4668 0.9516 0.043 Uiso 1 1 calc R . .
C7 C 0.3180(3) 0.0788(2) 0.9922(2) 0.0303(6) Uani 1 1 d . . .
H7 H 0.2732 0.0421 1.0796 0.036 Uiso 1 1 calc R . .
C8 C 0.2812(3) 0.0284(2) 0.9126(2) 0.0290(6) Uani 1 1 d . . .
C9 C 0.1777(4) -0.0726(3) 0.9620(3) 0.0407(7) Uani 1 1 d . . .
H9 H 0.1304 -0.1131 1.0489 0.049 Uiso 1 1 calc R . .
C10 C 0.1451(4) -0.1129(3) 0.8801(3) 0.0472(8) Uani 1 1 d . . .
H10 H 0.0756 -0.1811 0.9110 0.057 Uiso 1 1 calc R . .
C11 C 0.2169(4) -0.0508(3) 0.7527(3) 0.0459(8) Uani 1 1 d . . .
H11 H 0.1946 -0.0752 0.6959 0.055 Uiso 1 1 calc R . .
C12 C 0.3228(4) 0.0485(2) 0.7099(3) 0.0374(7) Uani 1 1 d . . .
H12 H 0.3738 0.0888 0.6234 0.045 Uiso 1 1 calc R . .
C13 C 0.8124(3) 0.2173(2) 0.5534(2) 0.0297(6) Uani 1 1 d . . .
C14 C 0.7226(3) 0.2921(2) 0.4852(2) 0.0252(5) Uani 1 1 d . . .
C15 C 0.7851(3) 0.3453(2) 0.3539(2) 0.0302(6) Uani 1 1 d . . .
H15 H 0.7255 0.3961 0.3100 0.036 Uiso 1 1 calc R . .
C16 C 0.9345(3) 0.3228(2) 0.2898(2) 0.0355(6) Uani 1 1 d . . .
C17 C 1.0246(3) 0.2478(3) 0.3542(3) 0.0461(8) Uani 1 1 d . . .
H17 H 1.1256 0.2323 0.3100 0.055 Uiso 1 1 calc R . .
C18 C 0.9646(3) 0.1966(3) 0.4828(3) 0.0447(7) Uani 1 1 d . . .
H18 H 1.0263 0.1465 0.5251 0.054 Uiso 1 1 calc R . .
C19 C 0.4610(3) 0.3563(2) 0.5101(2) 0.0272(5) Uani 1 1 d . . .
H19 H 0.4828 0.3854 0.4236 0.033 Uiso 1 1 calc R . .
C20 C 0.3040(3) 0.3632(2) 0.5964(2) 0.0267(5) Uani 1 1 d . . .
C21 C 0.1735(3) 0.3953(2) 0.5582(3) 0.0360(6) Uani 1 1 d . . .
H21 H 0.1845 0.4183 0.4739 0.043 Uiso 1 1 calc R . .
C22 C 0.0272(3) 0.3923(3) 0.6475(3) 0.0420(7) Uani 1 1 d . . .
H22 H -0.0633 0.4101 0.6249 0.050 Uiso 1 1 calc R . .
C23 C 0.0157(3) 0.3631(2) 0.7701(3) 0.0393(7) Uani 1 1 d . . .
H23 H -0.0814 0.3636 0.8311 0.047 Uiso 1 1 calc R . .
C24 C 0.1521(3) 0.3329(2) 0.8012(3) 0.0341(6) Uani 1 1 d . . .
H24 H 0.1446 0.3135 0.8842 0.041 Uiso 1 1 calc R . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N3 2.030(2) . ?
Ni1 N1 2.032(2) . ?
Ni1 N4 2.129(2) . ?
Ni1 N2 2.157(2) . ?
Ni1 S1 2.3780(7) . ?
Ni1 S2 2.3789(7) . ?
Cl1 C4 1.754(3) . ?
Cl2 C16 1.740(3) . ?
S1 C1 1.742(3) . ?
S2 C13 1.735(3) . ?
N1 C7 1.282(3) . ?
N1 C2 1.405(3) . ?
N2 C12 1.330(3) . ?
N2 C8 1.349(3) . ?
N3 C19 1.281(3) . ?
N3 C14 1.410(3) . ?
N4 C24 1.325(3) . ?
N4 C20 1.348(3) . ?
C1 C2 1.405(4) . ?
C1 C6 1.405(4) . ?
C2 C3 1.400(3) . ?
C3 C4 1.365(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(4) . ?
C5 C6 1.371(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.454(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.373(4) . ?
C9 C10 1.383(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.371(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.383(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.405(4) . ?
C13 C14 1.406(3) . ?
C14 C15 1.393(3) . ?
C15 C16 1.369(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(4) . ?
C17 C18 1.365(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.456(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.384(3) . ?
C21 C22 1.376(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.371(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.388(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N1 174.96(8) . . ?
N3 Ni1 N4 78.73(8) . . ?
N1 Ni1 N4 99.02(8) . . ?
N3 Ni1 N2 96.90(8) . . ?
N1 Ni1 N2 78.27(8) . . ?
N4 Ni1 N2 82.01(8) . . ?
N3 Ni1 S1 100.13(6) . . ?
N1 Ni1 S1 84.43(6) . . ?
N4 Ni1 S1 92.72(6) . . ?
N2 Ni1 S1 160.83(6) . . ?
N3 Ni1 S2 84.21(6) . . ?
N1 Ni1 S2 97.44(6) . . ?
N4 Ni1 S2 161.69(6) . . ?
N2 Ni1 S2 93.57(6) . . ?
S1 Ni1 S2 96.82(3) . . ?
C1 S1 Ni1 95.52(9) . . ?
C13 S2 Ni1 96.36(9) . . ?
C7 N1 C2 124.1(2) . . ?
C7 N1 Ni1 116.29(17) . . ?
C2 N1 Ni1 119.56(16) . . ?
C12 N2 C8 117.9(2) . . ?
C12 N2 Ni1 130.48(19) . . ?
C8 N2 Ni1 111.48(17) . . ?
C19 N3 C14 124.1(2) . . ?
C19 N3 Ni1 115.80(17) . . ?
C14 N3 Ni1 119.98(16) . . ?
C24 N4 C20 118.3(2) . . ?
C24 N4 Ni1 129.32(18) . . ?
C20 N4 Ni1 111.01(16) . . ?
C2 C1 C6 117.2(2) . . ?
C2 C1 S1 122.54(19) . . ?
C6 C1 S1 120.3(2) . . ?
C3 C2 C1 121.1(2) . . ?
C3 C2 N1 122.5(2) . . ?
C1 C2 N1 116.4(2) . . ?
C4 C3 C2 118.6(2) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 122.1(3) . . ?
C3 C4 Cl1 118.7(2) . . ?
C5 C4 Cl1 119.2(2) . . ?
C6 C5 C4 119.3(2) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 121.6(3) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
N1 C7 C8 118.7(2) . . ?
N1 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N2 C8 C9 122.7(3) . . ?
N2 C8 C7 115.2(2) . . ?
C9 C8 C7 122.1(2) . . ?
C8 C9 C10 118.7(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 119.0(3) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 119.0(3) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N2 C12 C11 122.6(3) . . ?
N2 C12 H12 118.7 . . ?
C11 C12 H12 118.7 . . ?
C18 C13 C14 116.8(2) . . ?
C18 C13 S2 120.8(2) . . ?
C14 C13 S2 122.4(2) . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 N3 122.8(2) . . ?
C13 C14 N3 116.3(2) . . ?
C16 C15 C14 119.9(2) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 120.6(3) . . ?
C15 C16 Cl2 119.7(2) . . ?
C17 C16 Cl2 119.7(2) . . ?
C18 C17 C16 119.7(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C13 122.1(3) . . ?
C17 C18 H18 119.0 . . ?
C13 C18 H18 119.0 . . ?
N3 C19 C20 118.0(2) . . ?
N3 C19 H19 121.0 . . ?
C20 C19 H19 121.0 . . ?
N4 C20 C21 122.3(2) . . ?
N4 C20 C19 115.3(2) . . ?
C21 C20 C19 122.3(2) . . ?
C22 C21 C20 118.5(3) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C23 C22 C21 119.6(3) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 118.6(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
N4 C24 C23 122.7(3) . . ?
N4 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?

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
N3 Ni1 S1 C1 -172.38(10) . . . . ?
N1 Ni1 S1 C1 9.78(10) . . . . ?
N4 Ni1 S1 C1 108.58(10) . . . . ?
N2 Ni1 S1 C1 35.3(2) . . . . ?
S2 Ni1 S1 C1 -87.07(8) . . . . ?
N3 Ni1 S2 C13 5.59(10) . . . . ?
N1 Ni1 S2 C13 -179.20(10) . . . . ?
N4 Ni1 S2 C13 26.9(2) . . . . ?
N2 Ni1 S2 C13 102.17(10) . . . . ?
S1 Ni1 S2 C13 -93.96(9) . . . . ?
N3 Ni1 N1 C7 15.0(9) . . . . ?
N4 Ni1 N1 C7 78.06(19) . . . . ?
N2 Ni1 N1 C7 -1.76(18) . . . . ?
S1 Ni1 N1 C7 169.95(18) . . . . ?
S2 Ni1 N1 C7 -93.88(18) . . . . ?
N3 Ni1 N1 C2 -166.1(8) . . . . ?
N4 Ni1 N1 C2 -102.98(18) . . . . ?
N2 Ni1 N1 C2 177.19(18) . . . . ?
S1 Ni1 N1 C2 -11.10(16) . . . . ?
S2 Ni1 N1 C2 85.07(17) . . . . ?
N3 Ni1 N2 C12 -0.7(2) . . . . ?
N1 Ni1 N2 C12 177.8(3) . . . . ?
N4 Ni1 N2 C12 76.8(2) . . . . ?
S1 Ni1 N2 C12 151.89(19) . . . . ?
S2 Ni1 N2 C12 -85.3(2) . . . . ?
N3 Ni1 N2 C8 -176.49(17) . . . . ?
N1 Ni1 N2 C8 2.05(17) . . . . ?
N4 Ni1 N2 C8 -98.94(18) . . . . ?
S1 Ni1 N2 C8 -23.9(3) . . . . ?
S2 Ni1 N2 C8 98.92(17) . . . . ?
N1 Ni1 N3 C19 58.1(9) . . . . ?
N4 Ni1 N3 C19 -5.77(18) . . . . ?
N2 Ni1 N3 C19 74.62(18) . . . . ?
S1 Ni1 N3 C19 -96.55(18) . . . . ?
S2 Ni1 N3 C19 167.53(18) . . . . ?
N1 Ni1 N3 C14 -117.9(8) . . . . ?
N4 Ni1 N3 C14 178.23(18) . . . . ?
N2 Ni1 N3 C14 -101.38(17) . . . . ?
S1 Ni1 N3 C14 87.45(17) . . . . ?
S2 Ni1 N3 C14 -8.47(16) . . . . ?
N3 Ni1 N4 C24 175.2(2) . . . . ?
N1 Ni1 N4 C24 -0.2(2) . . . . ?
N2 Ni1 N4 C24 76.5(2) . . . . ?
S1 Ni1 N4 C24 -85.0(2) . . . . ?
S2 Ni1 N4 C24 153.54(18) . . . . ?
N3 Ni1 N4 C20 9.24(16) . . . . ?
N1 Ni1 N4 C20 -166.18(16) . . . . ?
N2 Ni1 N4 C20 -89.48(17) . . . . ?
S1 Ni1 N4 C20 109.03(16) . . . . ?
S2 Ni1 N4 C20 -12.4(3) . . . . ?
Ni1 S1 C1 C2 -10.2(2) . . . . ?
Ni1 S1 C1 C6 170.6(2) . . . . ?
C6 C1 C2 C3 2.0(4) . . . . ?
S1 C1 C2 C3 -177.17(19) . . . . ?
C6 C1 C2 N1 -177.2(2) . . . . ?
S1 C1 C2 N1 3.6(3) . . . . ?
C7 N1 C2 C3 7.3(4) . . . . ?
Ni1 N1 C2 C3 -171.60(18) . . . . ?
C7 N1 C2 C1 -173.5(2) . . . . ?
Ni1 N1 C2 C1 7.6(3) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
N1 C2 C3 C4 178.9(2) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C2 C3 C4 Cl1 178.75(19) . . . . ?
C3 C4 C5 C6 1.5(4) . . . . ?
Cl1 C4 C5 C6 -178.8(2) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
C2 C1 C6 C5 -2.1(4) . . . . ?
S1 C1 C6 C5 177.1(2) . . . . ?
C2 N1 C7 C8 -177.7(2) . . . . ?
Ni1 N1 C7 C8 1.2(3) . . . . ?
C12 N2 C8 C9 0.9(4) . . . . ?
Ni1 N2 C8 C9 177.3(2) . . . . ?
C12 N2 C8 C7 -178.4(2) . . . . ?
Ni1 N2 C8 C7 -2.1(3) . . . . ?
N1 C7 C8 N2 0.7(4) . . . . ?
N1 C7 C8 C9 -178.6(2) . . . . ?
N2 C8 C9 C10 -1.2(4) . . . . ?
C7 C8 C9 C10 178.0(3) . . . . ?
C8 C9 C10 C11 -0.1(5) . . . . ?
C9 C10 C11 C12 1.6(5) . . . . ?
C8 N2 C12 C11 0.8(4) . . . . ?
Ni1 N2 C12 C11 -174.8(2) . . . . ?
C10 C11 C12 N2 -2.0(5) . . . . ?
Ni1 S2 C13 C18 176.2(2) . . . . ?
Ni1 S2 C13 C14 -3.6(2) . . . . ?
C18 C13 C14 C15 -1.8(4) . . . . ?
S2 C13 C14 C15 178.02(19) . . . . ?
C18 C13 C14 N3 178.0(2) . . . . ?
S2 C13 C14 N3 -2.2(3) . . . . ?
C19 N3 C14 C15 12.6(4) . . . . ?
Ni1 N3 C14 C15 -171.73(18) . . . . ?
C19 N3 C14 C13 -167.2(2) . . . . ?
Ni1 N3 C14 C13 8.5(3) . . . . ?
C13 C14 C15 C16 1.5(4) . . . . ?
N3 C14 C15 C16 -178.4(2) . . . . ?
C14 C15 C16 C17 -0.2(4) . . . . ?
C14 C15 C16 Cl2 -179.58(19) . . . . ?
C15 C16 C17 C18 -0.6(5) . . . . ?
Cl2 C16 C17 C18 178.8(2) . . . . ?
C16 C17 C18 C13 0.2(5) . . . . ?
C14 C13 C18 C17 1.0(4) . . . . ?
S2 C13 C18 C17 -178.8(2) . . . . ?
C14 N3 C19 C20 177.3(2) . . . . ?
Ni1 N3 C19 C20 1.4(3) . . . . ?
C24 N4 C20 C21 -2.1(4) . . . . ?
Ni1 N4 C20 C21 165.7(2) . . . . ?
C24 N4 C20 C19 -179.0(2) . . . . ?
Ni1 N4 C20 C19 -11.3(3) . . . . ?
N3 C19 C20 N4 7.1(3) . . . . ?
N3 C19 C20 C21 -169.8(2) . . . . ?
N4 C20 C21 C22 -0.6(4) . . . . ?
C19 C20 C21 C22 176.0(2) . . . . ?
C20 C21 C22 C23 2.9(4) . . . . ?
C21 C22 C23 C24 -2.4(4) . . . . ?
C20 N4 C24 C23 2.6(4) . . . . ?
Ni1 N4 C24 C23 -162.5(2) . . . . ?
C22 C23 C24 N4 -0.4(4) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_xcalibur_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1970597'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C29 H22 F6 N4 Ni O S2'
_chemical_formula_moiety         'C29 H22 F6 N4 Ni O S2'
_chemical_formula_weight         679.33
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.3997(2)
_cell_length_b                   12.7078(2)
_cell_length_c                   13.3086(3)
_cell_angle_alpha                114.490(2)
_cell_angle_beta                 111.726(2)
_cell_angle_gamma                92.4482(17)
_cell_volume                     1446.31(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9009
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      31.35
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692.00
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_T_max  0.932

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            9650
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.167
_diffrn_reflns_theta_full        25.350
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5140
_reflns_number_gt                4833
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0861
_refine_ls_number_restraints     100
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5140
_refine_ls_number_parameters     487
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0468P)²+0.8451P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.34
_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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.23143(2) 1.00181(2) 0.76468(2) 0.02331(10) Uani 1 1 d . . .
S1 S 0.41951(5) 1.17591(5) 0.86626(5) 0.03018(13) Uani 1 1 d . . .
S2 S 0.28912(6) 0.90283(5) 0.59504(5) 0.03290(14) Uani 1 1 d . . .
F1A F -0.0660(18) 1.4509(15) 0.6503(12) 0.051(4) Uani 0.31 1 d PDU A 1
F2A F 0.1199(16) 1.5358(13) 0.6462(12) 0.049(3) Uani 0.37 1 d PDU A 1
F3A F 0.1099(15) 1.6071(11) 0.8156(15) 0.067(3) Uani 0.31 1 d PDU A 1
F1B F -0.071(3) 1.432(2) 0.614(3) 0.052(5) Uani 0.25 1 d PU A 2
F1C F -0.042(3) 1.438(3) 0.602(3) 0.074(8) Uani 0.25 1 d PU A 3
F1D F -0.060(2) 1.4728(19) 0.699(2) 0.065(5) Uani 0.19 1 d PU A 4
F2B F 0.156(2) 1.603(2) 0.765(3) 0.067(6) Uani 0.11 1 d PU A 5
F2C F 0.0698(17) 1.5071(15) 0.6204(16) 0.056(5) Uani 0.21 1 d PU A 6
F2D F 0.1441(17) 1.5618(14) 0.6879(12) 0.054(3) Uani 0.31 1 d PU A 7
F3B F 0.049(2) 1.5792(16) 0.7876(14) 0.053(3) Uani 0.32 1 d PU A 8
F3C F 0.059(4) 1.583(3) 0.825(2) 0.079(6) Uani 0.26 1 d PU B 9
F3D F -0.005(3) 1.534(3) 0.786(3) 0.064(6) Uani 0.11 1 d PU A 10
F4 F 0.64628(18) 0.60451(14) 0.87895(13) 0.0592(4) Uani 1 1 d . . .
F5 F 0.73548(16) 0.57958(15) 0.75224(18) 0.0636(5) Uani 1 1 d . . .
F6 F 0.53975(16) 0.46661(12) 0.69532(14) 0.0545(4) Uani 1 1 d . . .
O1 O -0.1561(3) 1.1592(2) 0.7966(2) 0.0836(7) Uani 1 1 d D C .
N1 N 0.10914(17) 1.10400(14) 0.70559(14) 0.0230(3) Uani 1 1 d . . .
N2 N 0.02630(17) 0.88288(15) 0.66040(15) 0.0272(4) Uani 1 1 d . . .
N3 N 0.33648(16) 0.89199(14) 0.82490(14) 0.0226(3) Uani 1 1 d . . .
N4 N 0.20068(17) 1.04488(14) 0.92615(14) 0.0253(3) Uani 1 1 d . . .
C1 C 0.3165(2) 1.26454(17) 0.81849(17) 0.0266(4) Uani 1 1 d . . .
C2 C 0.1684(2) 1.22376(17) 0.74295(17) 0.0249(4) Uani 1 1 d . . .
C3 C 0.0887(2) 1.29866(19) 0.7092(2) 0.0326(5) Uani 1 1 d . . .
H3 H -0.0085 1.2706 0.6600 0.039 Uiso 1 1 calc R . .
C4 C 0.1534(3) 1.4143(2) 0.7486(2) 0.0392(5) Uani 1 1 d . A .
C5 C 0.3000(3) 1.4558(2) 0.8214(2) 0.0420(5) Uani 1 1 d . . .
H5 H 0.3440 1.5335 0.8475 0.050 Uiso 1 1 calc R . .
C6 C 0.3793(2) 1.38250(19) 0.8545(2) 0.0366(5) Uani 1 1 d . . .
H6 H 0.4769 1.4112 0.9019 0.044 Uiso 1 1 calc R . .
C7 C -0.0220(2) 1.05245(18) 0.63275(18) 0.0272(4) Uani 1 1 d . . .
H7 H -0.0837 1.0923 0.5997 0.033 Uiso 1 1 calc R . .
C8 C -0.0717(2) 0.92957(17) 0.60313(17) 0.0262(4) Uani 1 1 d . . .
C9 C -0.2096(2) 0.8653(2) 0.5215(2) 0.0352(5) Uani 1 1 d . . .
H9 H -0.2748 0.8994 0.4828 0.042 Uiso 1 1 calc R . .
C10 C -0.2485(2) 0.7495(2) 0.4986(2) 0.0414(5) Uani 1 1 d . . .
H10 H -0.3405 0.7043 0.4442 0.050 Uiso 1 1 calc R . .
C11 C -0.1491(3) 0.7019(2) 0.5573(2) 0.0412(5) Uani 1 1 d . . .
H11 H -0.1730 0.6243 0.5437 0.049 Uiso 1 1 calc R . .
C12 C -0.0130(2) 0.77125(19) 0.6369(2) 0.0356(5) Uani 1 1 d . . .
H12 H 0.0540 0.7383 0.6757 0.043 Uiso 1 1 calc R . .
C13 C 0.0695(3) 1.4955(2) 0.7134(3) 0.0583(8) Uani 1 1 d . . .
C14 C 0.3802(2) 0.81062(18) 0.64589(18) 0.0278(4) Uani 1 1 d . . .
C15 C 0.39898(19) 0.81159(16) 0.75719(17) 0.0235(4) Uani 1 1 d . . .
C16 C 0.4759(2) 0.73805(17) 0.79638(18) 0.0256(4) Uani 1 1 d . . .
H16 H 0.4877 0.7403 0.8701 0.031 Uiso 1 1 calc R . .
C17 C 0.5344(2) 0.66197(17) 0.72605(19) 0.0290(4) Uani 1 1 d . . .
C18 C 0.5163(2) 0.6591(2) 0.6154(2) 0.0369(5) Uani 1 1 d . . .
H18 H 0.5554 0.6077 0.5677 0.044 Uiso 1 1 calc R . .
C19 C 0.4415(3) 0.7311(2) 0.5769(2) 0.0382(5) Uani 1 1 d . . .
H19 H 0.4306 0.7277 0.5030 0.046 Uiso 1 1 calc R . .
C20 C 0.3364(2) 0.89853(18) 0.92381(18) 0.0273(4) Uani 1 1 d . . .
H20 H 0.3802 0.8503 0.9561 0.033 Uiso 1 1 calc R . .
C21 C 0.2659(2) 0.98321(17) 0.98431(17) 0.0258(4) Uani 1 1 d . . .
C22 C 0.2658(2) 0.99888(19) 1.09380(19) 0.0329(5) Uani 1 1 d . . .
H22 H 0.3130 0.9563 1.1325 0.040 Uiso 1 1 calc R . .
C23 C 0.1940(2) 1.0793(2) 1.1444(2) 0.0367(5) Uani 1 1 d . . .
H23 H 0.1916 1.0913 1.2175 0.044 Uiso 1 1 calc R . .
C24 C 0.1264(2) 1.14091(19) 1.0848(2) 0.0348(5) Uani 1 1 d . . .
H24 H 0.0770 1.1949 1.1167 0.042 Uiso 1 1 calc R . .
C25 C 0.1326(2) 1.12182(18) 0.97642(19) 0.0306(4) Uani 1 1 d . . .
H25 H 0.0873 1.1646 0.9372 0.037 Uiso 1 1 calc R . .
C26 C 0.6137(2) 0.58039(18) 0.7641(2) 0.0340(5) Uani 1 1 d . . .
C27 C -0.2371(4) 1.2223(4) 0.7867(4) 0.0746(11) Uani 1 1 d D . .
C28A C -0.3672(11) 1.2024(9) 0.7020(9) 0.101(3) Uani 0.66 1 d PDU C 1
H28A H -0.4303 1.1418 0.6978 0.121 Uiso 0.66 1 calc PR C 1
H28B H -0.3645 1.1767 0.6242 0.121 Uiso 0.66 1 calc PR C 1
H28C H -0.4007 1.2743 0.7228 0.121 Uiso 0.66 1 calc PR C 1
C28B C -0.2034(17) 1.3428(13) 0.8476(13) 0.093(4) Uani 0.39 1 d PU C 2
H28F H -0.1098 1.3700 0.9132 0.111 Uiso 0.39 1 calc PR C 2
H28D H -0.2710 1.3697 0.8801 0.111 Uiso 0.39 1 calc PR C 2
H28E H -0.2056 1.3740 0.7926 0.111 Uiso 0.39 1 calc PR C 2
C29A C -0.193(2) 1.3522(16) 0.9021(12) 0.090(5) Uani 0.34 1 d PDU C 1
H29A H -0.1037 1.3951 0.9175 0.108 Uiso 0.34 1 calc PR C 1
H29B H -0.1833 1.3437 0.9728 0.108 Uiso 0.34 1 calc PR C 1
H29C H -0.2648 1.3950 0.8848 0.108 Uiso 0.34 1 calc PR C 1
C29B C -0.3910(11) 1.1431(10) 0.6675(10) 0.114(4) Uani 0.61 1 d PU C 2
H29D H -0.4297 1.0807 0.6783 0.136 Uiso 0.61 1 calc PR C 2
H29E H -0.3761 1.1091 0.5946 0.136 Uiso 0.61 1 calc PR C 2
H29F H -0.4562 1.1937 0.6606 0.136 Uiso 0.61 1 calc PR C 2


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N1 2.0421(15) . ?
Ni1 N3 2.0475(15) . ?
Ni1 N2 2.1342(17) . ?
Ni1 N4 2.1373(16) . ?
Ni1 S1 2.3962(6) . ?
Ni1 S2 2.3983(6) . ?
S1 C1 1.736(2) . ?
S2 C14 1.734(2) . ?
F1A C13 1.294(17) . ?
F2A C13 1.429(17) . ?
F3A C13 1.401(14) . ?
F1B C13 1.46(2) . ?
F1C C13 1.36(3) . ?
F1D C13 1.289(19) . ?
F2B C13 1.34(2) . ?
F2C C13 1.31(2) . ?
F2D C13 1.344(17) . ?
F3B C13 1.206(17) . ?
F3C C13 1.49(2) . ?
F3D C13 1.40(3) . ?
F4 C26 1.329(3) . ?
F5 C26 1.333(3) . ?
F6 C26 1.344(3) . ?
O1 C27 1.198(4) . ?
N1 C7 1.283(3) . ?
N1 C2 1.417(2) . ?
N2 C12 1.328(3) . ?
N2 C8 1.350(3) . ?
N3 C20 1.285(3) . ?
N3 C15 1.416(2) . ?
N4 C25 1.331(3) . ?
N4 C21 1.354(3) . ?
C1 C6 1.411(3) . ?
C1 C2 1.417(3) . ?
C2 C3 1.393(3) . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(3) . ?
C4 C13 1.489(3) . ?
C5 C6 1.370(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.460(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.384(3) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.376(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C14 C19 1.410(3) . ?
C14 C15 1.415(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.380(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.398(3) . ?
C17 C26 1.486(3) . ?
C18 C19 1.364(3) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.459(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.387(3) . ?
C22 C23 1.387(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.373(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.387(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C27 C28A 1.331(10) . ?
C27 C28B 1.356(14) . ?
C27 C29A 1.614(16) . ?
C27 C29B 1.658(11) . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C28B H28F 0.9600 . ?
C28B H28D 0.9600 . ?
C28B H28E 0.9600 . ?
C29A H29A 0.9600 . ?
C29A H29B 0.9600 . ?
C29A H29C 0.9600 . ?
C29B H29D 0.9600 . ?
C29B H29E 0.9600 . ?
C29B H29F 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
N1 Ni1 N3 174.16(6) . . ?
N1 Ni1 N2 78.65(6) . . ?
N3 Ni1 N2 96.53(6) . . ?
N1 Ni1 N4 97.70(6) . . ?
N3 Ni1 N4 78.78(6) . . ?
N2 Ni1 N4 88.80(6) . . ?
N1 Ni1 S1 83.74(5) . . ?
N3 Ni1 S1 100.97(5) . . ?
N2 Ni1 S1 162.33(5) . . ?
N4 Ni1 S1 92.22(5) . . ?
N1 Ni1 S2 99.46(4) . . ?
N3 Ni1 S2 83.66(5) . . ?
N2 Ni1 S2 89.26(5) . . ?
N4 Ni1 S2 161.99(5) . . ?
S1 Ni1 S2 95.02(2) . . ?
C1 S1 Ni1 96.81(7) . . ?
C14 S2 Ni1 96.80(7) . . ?
C7 N1 C2 123.15(16) . . ?
C7 N1 Ni1 115.81(13) . . ?
C2 N1 Ni1 121.04(12) . . ?
C12 N2 C8 118.01(18) . . ?
C12 N2 Ni1 130.07(15) . . ?
C8 N2 Ni1 111.63(13) . . ?
C20 N3 C15 123.45(16) . . ?
C20 N3 Ni1 115.58(13) . . ?
C15 N3 Ni1 120.92(12) . . ?
C25 N4 C21 117.86(17) . . ?
C25 N4 Ni1 130.53(14) . . ?
C21 N4 Ni1 111.59(12) . . ?
C6 C1 C2 117.00(18) . . ?
C6 C1 S1 120.32(16) . . ?
C2 C1 S1 122.69(15) . . ?
C3 C2 C1 120.94(18) . . ?
C3 C2 N1 123.38(18) . . ?
C1 C2 N1 115.69(16) . . ?
C4 C3 C2 120.3(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 C13 120.9(2) . . ?
C5 C4 C13 119.4(2) . . ?
C6 C5 C4 120.4(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C1 121.6(2) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
N1 C7 C8 118.22(17) . . ?
N1 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
N2 C8 C9 122.39(19) . . ?
N2 C8 C7 115.38(17) . . ?
C9 C8 C7 122.23(19) . . ?
C10 C9 C8 118.7(2) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C11 C10 C9 119.0(2) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 119.0(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N2 C12 C11 122.9(2) . . ?
N2 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
F3B C13 F1D 70.2(15) . . ?
F3B C13 F1A 90.9(13) . . ?
F1D C13 F1A 25.3(9) . . ?
F3B C13 F2C 115.4(12) . . ?
F1D C13 F2C 109.1(11) . . ?
F1A C13 F2C 87.3(10) . . ?
F3B C13 F2B 61.5(19) . . ?
F1D C13 F2B 127.5(15) . . ?
F1A C13 F2B 135.6(12) . . ?
F2C C13 F2B 76.3(16) . . ?
F3B C13 F2D 94.8(12) . . ?
F1D C13 F2D 136.3(12) . . ?
F1A C13 F2D 122.6(10) . . ?
F2C C13 F2D 39.7(9) . . ?
F2B C13 F2D 38.8(15) . . ?
F3B C13 F1C 115.0(16) . . ?
F1D C13 F1C 57.3(13) . . ?
F1A C13 F1C 32.0(12) . . ?
F2C C13 F1C 58.8(12) . . ?
F2B C13 F1C 128.4(17) . . ?
F2D C13 F1C 97.9(12) . . ?
F3B C13 F3D 33.5(15) . . ?
F1D C13 F3D 43.2(10) . . ?
F1A C13 F3D 68.0(13) . . ?
F2C C13 F3D 134.3(15) . . ?
F2B C13 F3D 94.7(17) . . ?
F2D C13 F3D 127.5(14) . . ?
F1C C13 F3D 99.2(17) . . ?
F3B C13 F3A 25.2(11) . . ?
F1D C13 F3A 95.3(11) . . ?
F1A C13 F3A 115.8(9) . . ?
F2C C13 F3A 110.4(10) . . ?
F2B C13 F3A 40.3(15) . . ?
F2D C13 F3A 78.2(9) . . ?
F1C C13 F3A 135.8(14) . . ?
F3D C13 F3A 55.5(13) . . ?
F3B C13 F2A 108.4(12) . . ?
F1D C13 F2A 127.4(11) . . ?
F1A C13 F2A 107.9(9) . . ?
F2C C13 F2A 21.3(7) . . ?
F2B C13 F2A 57.5(16) . . ?
F2D C13 F2A 19.1(7) . . ?
F1C C13 F2A 80.1(11) . . ?
F3D C13 F2A 137.5(14) . . ?
F3A C13 F2A 95.7(8) . . ?
F3B C13 F1B 104.9(17) . . ?
F1D C13 F1B 41.6(17) . . ?
F1A C13 F1B 16.3(16) . . ?
F2C C13 F1B 74.1(14) . . ?
F2B C13 F1B 136.6(15) . . ?
F2D C13 F1B 112.3(14) . . ?
F1C C13 F1B 16(2) . . ?
F3D C13 F1B 84.3(18) . . ?
F3A C13 F1B 128.9(14) . . ?
F2A C13 F1B 95.3(14) . . ?
F3B C13 C4 121.4(8) . . ?
F1D C13 C4 112.9(9) . . ?
F1A C13 C4 115.0(8) . . ?
F2C C13 C4 117.3(8) . . ?
F2B C13 C4 109.2(9) . . ?
F2D C13 C4 109.9(8) . . ?
F1C C13 C4 113.0(13) . . ?
F3D C13 C4 108.1(12) . . ?
F3A C13 C4 109.6(7) . . ?
F2A C13 C4 111.2(7) . . ?
F1B C13 C4 112.3(12) . . ?
C19 C14 C15 116.71(18) . . ?
C19 C14 S2 120.45(16) . . ?
C15 C14 S2 122.83(15) . . ?
C16 C15 C14 121.12(17) . . ?
C16 C15 N3 123.10(17) . . ?
C14 C15 N3 115.77(16) . . ?
C17 C16 C15 120.13(18) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.65(19) . . ?
C16 C17 C26 121.24(19) . . ?
C18 C17 C26 119.09(19) . . ?
C19 C18 C17 120.39(19) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C14 122.0(2) . . ?
C18 C19 H19 119.0 . . ?
C14 C19 H19 119.0 . . ?
N3 C20 C21 118.53(17) . . ?
N3 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
N4 C21 C22 122.51(18) . . ?
N4 C21 C20 115.45(17) . . ?
C22 C21 C20 122.04(18) . . ?
C21 C22 C23 118.6(2) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C24 C23 C22 118.9(2) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 119.3(2) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
N4 C25 C24 122.79(19) . . ?
N4 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
F4 C26 F5 106.43(19) . . ?
F4 C26 F6 105.89(18) . . ?
F5 C26 F6 104.57(17) . . ?
F4 C26 C17 113.98(17) . . ?
F5 C26 C17 113.08(18) . . ?
F6 C26 C17 112.14(18) . . ?
O1 C27 C28A 132.0(6) . . ?
O1 C27 C28B 125.9(8) . . ?
C28A C27 C28B 100.6(8) . . ?
O1 C27 C29A 116.3(7) . . ?
C28A C27 C29A 111.3(8) . . ?
C28B C27 C29A 23.2(9) . . ?
O1 C27 C29B 109.7(6) . . ?
C28A C27 C29B 22.8(6) . . ?
C28B C27 C29B 123.4(8) . . ?
C29A C27 C29B 132.2(8) . . ?
C27 C28A H28A 109.5 . . ?
C27 C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C27 C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C27 C28B H28F 109.5 . . ?
C27 C28B H28D 109.5 . . ?
H28F C28B H28D 109.5 . . ?
C27 C28B H28E 109.5 . . ?
H28F C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C27 C29A H29A 109.5 . . ?
C27 C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C27 C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C27 C29B H29D 109.5 . . ?
C27 C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C27 C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 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
N1 Ni1 S1 C1 0.77(8) . . . . ?
N3 Ni1 S1 C1 -175.74(8) . . . . ?
N2 Ni1 S1 C1 -3.73(17) . . . . ?
N4 Ni1 S1 C1 -96.74(8) . . . . ?
S2 Ni1 S1 C1 99.76(7) . . . . ?
N1 Ni1 S2 C14 -175.70(8) . . . . ?
N3 Ni1 S2 C14 -0.68(8) . . . . ?
N2 Ni1 S2 C14 -97.34(8) . . . . ?
N4 Ni1 S2 C14 -13.50(17) . . . . ?
S1 Ni1 S2 C14 99.83(7) . . . . ?
N3 Ni1 N1 C7 -38.6(7) . . . . ?
N2 Ni1 N1 C7 -3.94(14) . . . . ?
N4 Ni1 N1 C7 -91.15(14) . . . . ?
S1 Ni1 N1 C7 177.45(14) . . . . ?
S2 Ni1 N1 C7 83.38(14) . . . . ?
N3 Ni1 N1 C2 142.1(6) . . . . ?
N2 Ni1 N1 C2 176.75(14) . . . . ?
N4 Ni1 N1 C2 89.54(14) . . . . ?
S1 Ni1 N1 C2 -1.86(13) . . . . ?
S2 Ni1 N1 C2 -95.93(13) . . . . ?
N1 Ni1 N2 C12 178.67(19) . . . . ?
N3 Ni1 N2 C12 -4.67(19) . . . . ?
N4 Ni1 N2 C12 -83.23(19) . . . . ?
S1 Ni1 N2 C12 -176.78(14) . . . . ?
S2 Ni1 N2 C12 78.86(18) . . . . ?
N1 Ni1 N2 C8 5.10(13) . . . . ?
N3 Ni1 N2 C8 -178.24(13) . . . . ?
N4 Ni1 N2 C8 103.20(13) . . . . ?
S1 Ni1 N2 C8 9.7(3) . . . . ?
S2 Ni1 N2 C8 -94.71(13) . . . . ?
N1 Ni1 N3 C20 -53.5(6) . . . . ?
N2 Ni1 N3 C20 -87.58(14) . . . . ?
N4 Ni1 N3 C20 -0.12(14) . . . . ?
S1 Ni1 N3 C20 89.99(14) . . . . ?
S2 Ni1 N3 C20 -176.11(14) . . . . ?
N1 Ni1 N3 C15 124.0(6) . . . . ?
N2 Ni1 N3 C15 89.92(14) . . . . ?
N4 Ni1 N3 C15 177.39(14) . . . . ?
S1 Ni1 N3 C15 -92.51(13) . . . . ?
S2 Ni1 N3 C15 1.39(13) . . . . ?
N1 Ni1 N4 C25 -4.84(18) . . . . ?
N3 Ni1 N4 C25 179.88(18) . . . . ?
N2 Ni1 N4 C25 -83.22(18) . . . . ?
S1 Ni1 N4 C25 79.13(17) . . . . ?
S2 Ni1 N4 C25 -167.13(13) . . . . ?
N1 Ni1 N4 C21 176.80(13) . . . . ?
N3 Ni1 N4 C21 1.52(12) . . . . ?
N2 Ni1 N4 C21 98.43(13) . . . . ?
S1 Ni1 N4 C21 -99.22(12) . . . . ?
S2 Ni1 N4 C21 14.5(2) . . . . ?
Ni1 S1 C1 C6 -179.75(16) . . . . ?
Ni1 S1 C1 C2 0.21(17) . . . . ?
C6 C1 C2 C3 -1.8(3) . . . . ?
S1 C1 C2 C3 178.27(15) . . . . ?
C6 C1 C2 N1 178.34(17) . . . . ?
S1 C1 C2 N1 -1.6(2) . . . . ?
C7 N1 C2 C3 3.3(3) . . . . ?
Ni1 N1 C2 C3 -177.41(15) . . . . ?
C7 N1 C2 C1 -176.79(17) . . . . ?
Ni1 N1 C2 C1 2.5(2) . . . . ?
C1 C2 C3 C4 0.4(3) . . . . ?
N1 C2 C3 C4 -179.74(19) . . . . ?
C2 C3 C4 C5 0.8(3) . . . . ?
C2 C3 C4 C13 -179.9(2) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C13 C4 C5 C6 -179.8(2) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
C2 C1 C6 C5 2.1(3) . . . . ?
S1 C1 C6 C5 -177.93(18) . . . . ?
C2 N1 C7 C8 -178.51(16) . . . . ?
Ni1 N1 C7 C8 2.2(2) . . . . ?
C12 N2 C8 C9 -0.3(3) . . . . ?
Ni1 N2 C8 C9 174.13(16) . . . . ?
C12 N2 C8 C7 -179.96(18) . . . . ?
Ni1 N2 C8 C7 -5.5(2) . . . . ?
N1 C7 C8 N2 2.5(3) . . . . ?
N1 C7 C8 C9 -177.18(19) . . . . ?
N2 C8 C9 C10 0.5(3) . . . . ?
C7 C8 C9 C10 -179.85(19) . . . . ?
C8 C9 C10 C11 -0.1(3) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C8 N2 C12 C11 -0.3(3) . . . . ?
Ni1 N2 C12 C11 -173.53(16) . . . . ?
C10 C11 C12 N2 0.7(4) . . . . ?
C3 C4 C13 F3B 111.1(13) . . . . ?
C5 C4 C13 F3B -69.6(13) . . . . ?
C3 C4 C13 F1D 31.0(12) . . . . ?
C5 C4 C13 F1D -149.6(11) . . . . ?
C3 C4 C13 F1A 3.4(8) . . . . ?
C5 C4 C13 F1A -177.3(8) . . . . ?
C3 C4 C13 F2C -97.2(9) . . . . ?
C5 C4 C13 F2C 82.2(9) . . . . ?
C3 C4 C13 F2B 178.8(19) . . . . ?
C5 C4 C13 F2B -1.9(19) . . . . ?
C3 C4 C13 F2D -139.9(6) . . . . ?
C5 C4 C13 F2D 39.4(7) . . . . ?
C3 C4 C13 F1C -31.7(11) . . . . ?
C5 C4 C13 F1C 147.7(11) . . . . ?
C3 C4 C13 F3D 77.0(15) . . . . ?
C5 C4 C13 F3D -103.6(15) . . . . ?
C3 C4 C13 F3A 135.9(8) . . . . ?
C5 C4 C13 F3A -44.7(8) . . . . ?
C3 C4 C13 F2A -119.6(6) . . . . ?
C5 C4 C13 F2A 59.8(6) . . . . ?
C3 C4 C13 F1B -14.2(16) . . . . ?
C5 C4 C13 F1B 165.2(15) . . . . ?
Ni1 S2 C14 C19 -179.00(17) . . . . ?
Ni1 S2 C14 C15 0.08(17) . . . . ?
C19 C14 C15 C16 0.7(3) . . . . ?
S2 C14 C15 C16 -178.44(15) . . . . ?
C19 C14 C15 N3 -179.95(18) . . . . ?
S2 C14 C15 N3 0.9(3) . . . . ?
C20 N3 C15 C16 -5.0(3) . . . . ?
Ni1 N3 C15 C16 177.66(14) . . . . ?
C20 N3 C15 C14 175.59(17) . . . . ?
Ni1 N3 C15 C14 -1.7(2) . . . . ?
C14 C15 C16 C17 -0.5(3) . . . . ?
N3 C15 C16 C17 -179.78(18) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C15 C16 C17 C26 -178.39(18) . . . . ?
C16 C17 C18 C19 0.2(3) . . . . ?
C26 C17 C18 C19 178.6(2) . . . . ?
C17 C18 C19 C14 0.1(4) . . . . ?
C15 C14 C19 C18 -0.5(3) . . . . ?
S2 C14 C19 C18 178.65(19) . . . . ?
C15 N3 C20 C21 -178.72(16) . . . . ?
Ni1 N3 C20 C21 -1.3(2) . . . . ?
C25 N4 C21 C22 -1.0(3) . . . . ?
Ni1 N4 C21 C22 177.59(16) . . . . ?
C25 N4 C21 C20 178.82(17) . . . . ?
Ni1 N4 C21 C20 -2.6(2) . . . . ?
N3 C20 C21 N4 2.7(3) . . . . ?
N3 C20 C21 C22 -177.48(18) . . . . ?
N4 C21 C22 C23 1.2(3) . . . . ?
C20 C21 C22 C23 -178.65(19) . . . . ?
C21 C22 C23 C24 -0.4(3) . . . . ?
C22 C23 C24 C25 -0.5(3) . . . . ?
C21 N4 C25 C24 0.1(3) . . . . ?
Ni1 N4 C25 C24 -178.18(14) . . . . ?
C23 C24 C25 N4 0.6(3) . . . . ?
C16 C17 C26 F4 -12.8(3) . . . . ?
C18 C17 C26 F4 168.8(2) . . . . ?
C16 C17 C26 F5 -134.5(2) . . . . ?
C18 C17 C26 F5 47.1(3) . . . . ?
C16 C17 C26 F6 107.5(2) . . . . ?
C18 C17 C26 F6 -70.9(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_xcalibur_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1970599'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H24 Cl2 N4 Ni O8 S2'
_chemical_formula_moiety         'C26 H24 Cl2 N4 Ni O8 S2'
_chemical_formula_weight         714.22
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_space_group_IT_number           19
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,-Y,1/2+Z
3 1/2+X,1/2-Y,-Z
4 -X,1/2+Y,1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.5516(3)
_cell_length_b                   10.2011(3)
_cell_length_c                   33.0145(8)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     2880.04(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13240
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      30.96
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464.00
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_T_max  0.958

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            19733
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.683
_diffrn_reflns_theta_full        25.350
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5256
_reflns_number_gt                4846
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1228
_refine_ls_number_restraints     18
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5256
_refine_ls_number_parameters     424
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0611P)²+7.1684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2241 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.99(2)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.05221(7) 0.02772(6) 0.117013(17) 0.02130(16) Uani 1 1 d . . .
Cl1 Cl -0.40942(15) 0.08889(13) 0.01108(4) 0.0330(3) Uani 1 1 d . . .
Cl2 Cl 0.14942(19) 0.07571(18) 0.29339(5) 0.0503(4) Uani 1 1 d . . .
S1 S -0.06125(17) -0.16651(12) 0.08444(4) 0.0293(3) Uani 1 1 d . . .
S2 S -0.20219(15) 0.12855(13) 0.10870(4) 0.0287(3) Uani 1 1 d . . .
O1 O -0.4416(9) 0.2177(5) 0.0259(2) 0.095(2) Uani 1 1 d . . .
O2 O -0.2478(6) 0.0758(9) 0.01126(16) 0.103(3) Uani 1 1 d . . .
O3 O -0.4726(7) 0.0784(7) -0.02759(15) 0.0824(19) Uani 1 1 d . . .
O4 O -0.4862(6) 0.0030(5) 0.03847(13) 0.0551(13) Uani 1 1 d . . .
O5A O 0.0277(15) 0.0002(15) 0.2988(4) 0.084(4) Uani 0.54 1 d PU A 1
O6A O 0.146(3) 0.1597(16) 0.2561(6) 0.103(7) Uani 0.53 1 d P A 1
O7A O 0.2917(16) 0.0034(14) 0.2900(5) 0.090(4) Uani 0.47 1 d PU A 1
O8A O 0.1773(15) 0.1694(13) 0.3243(3) 0.074(3) Uani 0.58 1 d P A 1
O5B O -0.0138(15) 0.1143(17) 0.3003(4) 0.084(4) Uani 0.46 1 d P A 2
O6B O 0.206(2) 0.117(2) 0.2595(7) 0.087(6) Uani 0.47 1 d PU A 2
O7B O 0.127(2) -0.0683(13) 0.2905(4) 0.109(5) Uani 0.53 1 d P A 2
O8B O 0.233(2) 0.0904(19) 0.3313(5) 0.086(5) Uani 0.42 1 d P A 2
N1 N 0.1335(5) 0.0626(4) 0.06029(11) 0.0214(8) Uani 1 1 d . . .
N2 N 0.1668(5) 0.2057(4) 0.12664(12) 0.0247(9) Uani 1 1 d . . .
N3 N -0.0335(5) -0.0152(4) 0.17330(11) 0.0227(8) Uani 1 1 d . . .
N4 N 0.2406(5) -0.0747(4) 0.14104(12) 0.0249(9) Uani 1 1 d . . .
C1 C 0.1022(5) -0.0211(5) 0.02747(13) 0.0218(9) Uani 1 1 d . . .
C2 C 0.0098(6) -0.1324(5) 0.03491(15) 0.0270(11) Uani 1 1 d . . .
C3 C -0.0253(7) -0.2187(6) 0.00374(16) 0.0371(13) Uani 1 1 d . . .
H3 H -0.0864 -0.2922 0.0088 0.045 Uiso 1 1 calc R . .
C4 C 0.0309(8) -0.1952(6) -0.03488(16) 0.0398(14) Uani 1 1 d . . .
H4 H 0.0079 -0.2533 -0.0558 0.048 Uiso 1 1 calc R . .
C5 C 0.1206(7) -0.0860(5) -0.04247(15) 0.0334(12) Uani 1 1 d . . .
H5 H 0.1563 -0.0702 -0.0686 0.040 Uiso 1 1 calc R . .
C6 C 0.1584(6) 0.0003(5) -0.01193(14) 0.0261(11) Uani 1 1 d . . .
H6 H 0.2211 0.0726 -0.0174 0.031 Uiso 1 1 calc R . .
C7 C 0.0507(8) -0.3124(5) 0.09581(17) 0.0417(14) Uani 1 1 d . . .
H7A H 0.0563 -0.3240 0.1246 0.050 Uiso 1 1 calc R . .
H7B H 0.1545 -0.3034 0.0850 0.050 Uiso 1 1 calc R . .
H7C H 0.0009 -0.3873 0.0838 0.050 Uiso 1 1 calc R . .
C8 C 0.2143(6) 0.1682(5) 0.05680(15) 0.0254(10) Uani 1 1 d . . .
H8 H 0.2577 0.1921 0.0320 0.030 Uiso 1 1 calc R . .
C9 C 0.2360(6) 0.2492(5) 0.09248(14) 0.0250(11) Uani 1 1 d . . .
C10 C 0.3211(6) 0.3655(5) 0.09112(16) 0.0292(11) Uani 1 1 d . . .
H10 H 0.3687 0.3930 0.0673 0.035 Uiso 1 1 calc R . .
C11 C 0.3330(7) 0.4392(5) 0.12626(17) 0.0356(13) Uani 1 1 d . . .
H11 H 0.3895 0.5171 0.1264 0.043 Uiso 1 1 calc R . .
C12 C 0.2603(7) 0.3959(6) 0.16098(17) 0.0364(13) Uani 1 1 d . . .
H12 H 0.2652 0.4452 0.1846 0.044 Uiso 1 1 calc R . .
C13 C 0.1795(6) 0.2780(5) 0.16028(15) 0.0302(11) Uani 1 1 d . . .
H13 H 0.1327 0.2482 0.1840 0.036 Uiso 1 1 calc R . .
C14 C -0.1835(5) 0.0248(5) 0.18567(13) 0.0222(9) Uani 1 1 d . . .
C15 C -0.2701(6) 0.1020(5) 0.15898(15) 0.0256(10) Uani 1 1 d . . .
C16 C -0.4175(6) 0.1492(5) 0.17013(16) 0.0312(12) Uani 1 1 d . . .
H16 H -0.4741 0.2013 0.1523 0.037 Uiso 1 1 calc R . .
C17 C -0.4786(6) 0.1189(6) 0.20738(17) 0.0353(13) Uani 1 1 d . . .
H17 H -0.5750 0.1528 0.2151 0.042 Uiso 1 1 calc R . .
C18 C -0.3962(6) 0.0376(6) 0.23356(15) 0.0341(12) Uani 1 1 d . . .
H18 H -0.4403 0.0134 0.2582 0.041 Uiso 1 1 calc R . .
C19 C -0.2491(6) -0.0077(6) 0.22325(15) 0.0322(12) Uani 1 1 d . . .
H19 H -0.1935 -0.0598 0.2413 0.039 Uiso 1 1 calc R . .
C20 C -0.1901(8) 0.3054(6) 0.1059(2) 0.0431(15) Uani 1 1 d . . .
H20A H -0.2937 0.3418 0.1057 0.052 Uiso 1 1 calc R . .
H20B H -0.1361 0.3304 0.0816 0.052 Uiso 1 1 calc R . .
H20C H -0.1342 0.3380 0.1291 0.052 Uiso 1 1 calc R . .
C21 C 0.0570(6) -0.0872(5) 0.19484(14) 0.0261(10) Uani 1 1 d . . .
H21 H 0.0256 -0.1168 0.2202 0.031 Uiso 1 1 calc R . .
C22 C 0.2100(6) -0.1216(5) 0.17865(15) 0.0287(11) Uani 1 1 d . . .
C23 C 0.3148(7) -0.1968(6) 0.20022(16) 0.0357(13) Uani 1 1 d . . .
H23 H 0.2905 -0.2277 0.2260 0.043 Uiso 1 1 calc R . .
C24 C 0.4589(7) -0.2252(6) 0.18221(16) 0.0376(13) Uani 1 1 d . . .
H24 H 0.5322 -0.2766 0.1957 0.045 Uiso 1 1 calc R . .
C25 C 0.4907(6) -0.1761(6) 0.14418(17) 0.0334(12) Uani 1 1 d . . .
H25 H 0.5864 -0.1932 0.1319 0.040 Uiso 1 1 calc R . .
C26 C 0.3802(6) -0.1017(5) 0.12464(15) 0.0277(11) Uani 1 1 d . . .
H26 H 0.4032 -0.0689 0.0990 0.033 Uiso 1 1 calc R . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N1 2.029(4) . ?
Ni1 N3 2.045(4) . ?
Ni1 N4 2.077(4) . ?
Ni1 N2 2.088(4) . ?
Ni1 S2 2.4220(14) . ?
Ni1 S1 2.4543(14) . ?
Cl1 O2 1.388(5) . ?
Cl1 O3 1.391(5) . ?
Cl1 O4 1.420(4) . ?
Cl1 O1 1.429(6) . ?
Cl2 O5A 1.308(10) . ?
Cl2 O6B 1.291(19) . ?
Cl2 O6A 1.500(16) . ?
Cl2 O8A 1.417(10) . ?
Cl2 O7A 1.427(13) . ?
Cl2 O8B 1.450(16) . ?
Cl2 O5B 1.468(13) . ?
Cl2 O7B 1.484(13) . ?
S1 C2 1.779(5) . ?
S1 C7 1.809(6) . ?
S2 C15 1.779(5) . ?
S2 C20 1.810(6) . ?
N1 C8 1.285(6) . ?
N1 C1 1.405(6) . ?
N2 C13 1.337(6) . ?
N2 C9 1.349(6) . ?
N3 C21 1.282(6) . ?
N3 C14 1.407(6) . ?
N4 C26 1.340(6) . ?
N4 C22 1.356(6) . ?
C1 C6 1.404(6) . ?
C1 C2 1.405(7) . ?
C2 C3 1.387(7) . ?
C3 C4 1.383(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.450(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.393(7) . ?
C10 C11 1.386(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(8) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.394(7) . ?
C14 C19 1.402(7) . ?
C15 C16 1.399(7) . ?
C16 C17 1.372(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.390(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.382(7) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.457(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.378(7) . ?
C23 C24 1.399(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.379(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.373(7) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 177.47(16) . . ?
N1 Ni1 N4 100.07(16) . . ?
N3 Ni1 N4 79.83(16) . . ?
N1 Ni1 N2 80.04(15) . . ?
N3 Ni1 N2 102.48(15) . . ?
N4 Ni1 N2 90.88(16) . . ?
N1 Ni1 S2 97.40(11) . . ?
N3 Ni1 S2 82.64(12) . . ?
N4 Ni1 S2 162.43(12) . . ?
N2 Ni1 S2 93.97(12) . . ?
N1 Ni1 S1 82.69(11) . . ?
N3 Ni1 S1 94.79(12) . . ?
N4 Ni1 S1 93.90(12) . . ?
N2 Ni1 S1 162.64(11) . . ?
S2 Ni1 S1 86.45(5) . . ?
O2 Cl1 O3 112.5(4) . . ?
O2 Cl1 O4 113.5(4) . . ?
O3 Cl1 O4 110.9(3) . . ?
O2 Cl1 O1 106.2(5) . . ?
O3 Cl1 O1 108.1(5) . . ?
O4 Cl1 O1 105.1(3) . . ?
O5A Cl2 O6B 127.6(12) . . ?
O5A Cl2 O6A 115.7(11) . . ?
O6B Cl2 O6A 27.2(11) . . ?
O5A Cl2 O8A 115.6(8) . . ?
O6B Cl2 O8A 110.0(11) . . ?
O6A Cl2 O8A 102.0(9) . . ?
O5A Cl2 O7A 112.6(9) . . ?
O6B Cl2 O7A 77.2(11) . . ?
O6A Cl2 O7A 104.4(10) . . ?
O8A Cl2 O7A 105.1(8) . . ?
O5A Cl2 O8B 109.6(9) . . ?
O6B Cl2 O8B 122.0(12) . . ?
O6A Cl2 O8B 131.3(11) . . ?
O8A Cl2 O8B 39.3(7) . . ?
O7A Cl2 O8B 72.5(10) . . ?
O5A Cl2 O5B 51.7(8) . . ?
O6B Cl2 O5B 113.9(11) . . ?
O6A Cl2 O5B 87.4(10) . . ?
O8A Cl2 O5B 82.4(8) . . ?
O7A Cl2 O5B 164.0(9) . . ?
O8B Cl2 O5B 107.9(10) . . ?
O5A Cl2 O7B 47.4(9) . . ?
O6B Cl2 O7B 108.2(11) . . ?
O6A Cl2 O7B 120.6(9) . . ?
O8A Cl2 O7B 137.3(8) . . ?
O7A Cl2 O7B 66.0(9) . . ?
O8B Cl2 O7B 102.8(9) . . ?
O5B Cl2 O7B 98.9(10) . . ?
C2 S1 C7 99.8(3) . . ?
C2 S1 Ni1 96.30(18) . . ?
C7 S1 Ni1 111.3(2) . . ?
C15 S2 C20 102.6(3) . . ?
C15 S2 Ni1 97.04(17) . . ?
C20 S2 Ni1 112.2(2) . . ?
C8 N1 C1 122.9(4) . . ?
C8 N1 Ni1 114.5(3) . . ?
C1 N1 Ni1 122.7(3) . . ?
C13 N2 C9 118.5(4) . . ?
C13 N2 Ni1 130.1(4) . . ?
C9 N2 Ni1 111.4(3) . . ?
C21 N3 C14 123.8(4) . . ?
C21 N3 Ni1 114.2(3) . . ?
C14 N3 Ni1 121.9(3) . . ?
C26 N4 C22 118.0(4) . . ?
C26 N4 Ni1 129.8(3) . . ?
C22 N4 Ni1 112.2(3) . . ?
C6 C1 C2 118.7(4) . . ?
C6 C1 N1 123.7(4) . . ?
C2 C1 N1 117.6(4) . . ?
C3 C2 C1 120.3(5) . . ?
C3 C2 S1 119.0(4) . . ?
C1 C2 S1 120.7(4) . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 121.0(5) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 119.9(5) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
S1 C7 H7A 109.5 . . ?
S1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 118.2(4) . . ?
N1 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
N2 C9 C10 122.4(4) . . ?
N2 C9 C8 115.8(4) . . ?
C10 C9 C8 121.7(4) . . ?
C11 C10 C9 118.3(5) . . ?
C11 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
C12 C11 C10 119.3(5) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 119.3(5) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
N2 C13 C12 122.2(5) . . ?
N2 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C15 C14 C19 118.7(4) . . ?
C15 C14 N3 117.7(4) . . ?
C19 C14 N3 123.6(4) . . ?
C14 C15 C16 120.4(5) . . ?
C14 C15 S2 120.2(4) . . ?
C16 C15 S2 119.1(4) . . ?
C17 C16 C15 120.1(5) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.9(5) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C14 120.2(5) . . ?
C18 C19 H19 119.9 . . ?
C14 C19 H19 119.9 . . ?
S2 C20 H20A 109.5 . . ?
S2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 C22 118.5(4) . . ?
N3 C21 H21 120.8 . . ?
C22 C21 H21 120.8 . . ?
N4 C22 C23 123.0(5) . . ?
N4 C22 C21 115.1(4) . . ?
C23 C22 C21 121.9(5) . . ?
C22 C23 C24 117.9(5) . . ?
C22 C23 H23 121.0 . . ?
C24 C23 H23 121.0 . . ?
C25 C24 C23 119.0(5) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C26 C25 C24 119.5(5) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
N4 C26 C25 122.5(5) . . ?
N4 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 S1 C2 -0.6(2) . . . . ?
N3 Ni1 S1 C2 179.6(2) . . . . ?
N4 Ni1 S1 C2 -100.3(2) . . . . ?
N2 Ni1 S1 C2 5.4(4) . . . . ?
S2 Ni1 S1 C2 97.32(17) . . . . ?
N1 Ni1 S1 C7 102.5(2) . . . . ?
N3 Ni1 S1 C7 -77.2(2) . . . . ?
N4 Ni1 S1 C7 2.9(2) . . . . ?
N2 Ni1 S1 C7 108.5(4) . . . . ?
S2 Ni1 S1 C7 -159.5(2) . . . . ?
N1 Ni1 S2 C15 -178.3(2) . . . . ?
N3 Ni1 S2 C15 4.3(2) . . . . ?
N4 Ni1 S2 C15 7.9(4) . . . . ?
N2 Ni1 S2 C15 -97.8(2) . . . . ?
S1 Ni1 S2 C15 99.55(17) . . . . ?
N1 Ni1 S2 C20 -71.6(3) . . . . ?
N3 Ni1 S2 C20 110.9(3) . . . . ?
N4 Ni1 S2 C20 114.5(5) . . . . ?
N2 Ni1 S2 C20 8.8(3) . . . . ?
S1 Ni1 S2 C20 -153.8(2) . . . . ?
N3 Ni1 N1 C8 -175(4) . . . . ?
N4 Ni1 N1 C8 -87.9(4) . . . . ?
N2 Ni1 N1 C8 1.3(3) . . . . ?
S2 Ni1 N1 C8 94.0(3) . . . . ?
S1 Ni1 N1 C8 179.5(4) . . . . ?
N3 Ni1 N1 C1 6(4) . . . . ?
N4 Ni1 N1 C1 92.9(4) . . . . ?
N2 Ni1 N1 C1 -178.0(4) . . . . ?
S2 Ni1 N1 C1 -85.2(3) . . . . ?
S1 Ni1 N1 C1 0.2(3) . . . . ?
N1 Ni1 N2 C13 178.4(5) . . . . ?
N3 Ni1 N2 C13 -1.7(5) . . . . ?
N4 Ni1 N2 C13 -81.5(5) . . . . ?
S2 Ni1 N2 C13 81.6(4) . . . . ?
S1 Ni1 N2 C13 172.4(3) . . . . ?
N1 Ni1 N2 C9 -1.5(3) . . . . ?
N3 Ni1 N2 C9 178.3(3) . . . . ?
N4 Ni1 N2 C9 98.5(3) . . . . ?
S2 Ni1 N2 C9 -98.4(3) . . . . ?
S1 Ni1 N2 C9 -7.5(6) . . . . ?
N1 Ni1 N3 C21 84(4) . . . . ?
N4 Ni1 N3 C21 -4.1(4) . . . . ?
N2 Ni1 N3 C21 -92.7(4) . . . . ?
S2 Ni1 N3 C21 174.8(4) . . . . ?
S1 Ni1 N3 C21 89.0(4) . . . . ?
N1 Ni1 N3 C14 -92(4) . . . . ?
N4 Ni1 N3 C14 179.8(4) . . . . ?
N2 Ni1 N3 C14 91.2(4) . . . . ?
S2 Ni1 N3 C14 -1.3(3) . . . . ?
S1 Ni1 N3 C14 -87.1(3) . . . . ?
N1 Ni1 N4 C26 4.2(5) . . . . ?
N3 Ni1 N4 C26 -178.4(5) . . . . ?
N2 Ni1 N4 C26 -75.9(4) . . . . ?
S2 Ni1 N4 C26 178.0(3) . . . . ?
S1 Ni1 N4 C26 87.4(4) . . . . ?
N1 Ni1 N4 C22 -174.1(3) . . . . ?
N3 Ni1 N4 C22 3.3(3) . . . . ?
N2 Ni1 N4 C22 105.8(3) . . . . ?
S2 Ni1 N4 C22 -0.3(6) . . . . ?
S1 Ni1 N4 C22 -90.9(3) . . . . ?
C8 N1 C1 C6 1.5(7) . . . . ?
Ni1 N1 C1 C6 -179.4(3) . . . . ?
C8 N1 C1 C2 -178.8(5) . . . . ?
Ni1 N1 C1 C2 0.4(6) . . . . ?
C6 C1 C2 C3 -0.3(7) . . . . ?
N1 C1 C2 C3 179.9(5) . . . . ?
C6 C1 C2 S1 178.7(4) . . . . ?
N1 C1 C2 S1 -1.1(6) . . . . ?
C7 S1 C2 C3 67.0(5) . . . . ?
Ni1 S1 C2 C3 -180.0(4) . . . . ?
C7 S1 C2 C1 -111.9(5) . . . . ?
Ni1 S1 C2 C1 1.1(4) . . . . ?
C1 C2 C3 C4 0.0(9) . . . . ?
S1 C2 C3 C4 -179.0(5) . . . . ?
C2 C3 C4 C5 -0.4(10) . . . . ?
C3 C4 C5 C6 1.1(10) . . . . ?
C4 C5 C6 C1 -1.4(8) . . . . ?
C2 C1 C6 C5 1.0(7) . . . . ?
N1 C1 C6 C5 -179.3(5) . . . . ?
C1 N1 C8 C9 178.4(4) . . . . ?
Ni1 N1 C8 C9 -0.8(6) . . . . ?
C13 N2 C9 C10 0.6(7) . . . . ?
Ni1 N2 C9 C10 -179.5(4) . . . . ?
C13 N2 C9 C8 -178.4(4) . . . . ?
Ni1 N2 C9 C8 1.6(5) . . . . ?
N1 C8 C9 N2 -0.6(7) . . . . ?
N1 C8 C9 C10 -179.6(5) . . . . ?
N2 C9 C10 C11 -0.6(8) . . . . ?
C8 C9 C10 C11 178.3(5) . . . . ?
C9 C10 C11 C12 -0.4(8) . . . . ?
C10 C11 C12 C13 1.4(8) . . . . ?
C9 N2 C13 C12 0.5(8) . . . . ?
Ni1 N2 C13 C12 -179.5(4) . . . . ?
C11 C12 C13 N2 -1.5(8) . . . . ?
C21 N3 C14 C15 -179.3(5) . . . . ?
Ni1 N3 C14 C15 -3.6(6) . . . . ?
C21 N3 C14 C19 1.3(8) . . . . ?
Ni1 N3 C14 C19 177.0(4) . . . . ?
C19 C14 C15 C16 2.0(8) . . . . ?
N3 C14 C15 C16 -177.5(4) . . . . ?
C19 C14 C15 S2 -172.2(4) . . . . ?
N3 C14 C15 S2 8.4(6) . . . . ?
C20 S2 C15 C14 -122.6(5) . . . . ?
Ni1 S2 C15 C14 -8.0(4) . . . . ?
C20 S2 C15 C16 63.2(5) . . . . ?
Ni1 S2 C15 C16 177.8(4) . . . . ?
C14 C15 C16 C17 -0.6(8) . . . . ?
S2 C15 C16 C17 173.6(4) . . . . ?
C15 C16 C17 C18 -2.1(9) . . . . ?
C16 C17 C18 C19 3.4(9) . . . . ?
C17 C18 C19 C14 -2.0(9) . . . . ?
C15 C14 C19 C18 -0.7(8) . . . . ?
N3 C14 C19 C18 178.7(5) . . . . ?
C14 N3 C21 C22 -179.8(4) . . . . ?
Ni1 N3 C21 C22 4.2(6) . . . . ?
C26 N4 C22 C23 -0.9(8) . . . . ?
Ni1 N4 C22 C23 177.6(5) . . . . ?
C26 N4 C22 C21 179.3(4) . . . . ?
Ni1 N4 C22 C21 -2.2(5) . . . . ?
N3 C21 C22 N4 -1.3(7) . . . . ?
N3 C21 C22 C23 178.9(5) . . . . ?
N4 C22 C23 C24 0.0(9) . . . . ?
C21 C22 C23 C24 179.8(5) . . . . ?
C22 C23 C24 C25 0.8(9) . . . . ?
C23 C24 C25 C26 -0.7(9) . . . . ?
C22 N4 C26 C25 1.0(7) . . . . ?
Ni1 N4 C26 C25 -177.2(4) . . . . ?
C24 C25 C26 N4 -0.2(8) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_xcalibur_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1970598'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C27 H25 N5 Ni O S2'
_chemical_formula_moiety         'C27 H25 N5 Ni O S2'
_chemical_formula_weight         558.35
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   11.3962(4)
_cell_length_b                   18.9231(4)
_cell_length_c                   12.9723(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.313(4)
_cell_angle_gamma                90.0000
_cell_volume                     2549.38(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8781
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      29.65
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160.00
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.962

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            17291
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.757
_diffrn_reflns_theta_full        25.350
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4657
_reflns_number_gt                3801
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1220
_refine_ls_wR_factor_gt          0.1132
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4657
_refine_ls_number_parameters     325
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0630P)²+1.5308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.42
_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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.92036(4) 0.102925(19) 0.76303(3) 0.03200(14) Uani 1 1 d . . .
S1 S 0.82916(8) 0.14858(4) 0.88677(7) 0.0409(2) Uani 1 1 d . . .
S2 S 0.72592(8) 0.05770(4) 0.62081(7) 0.0403(2) Uani 1 1 d . . .
O1 O 1.4358(3) 0.00230(17) 0.7660(3) 0.0915(11) Uani 1 1 d . . .
N1 N 0.8931(2) 0.20341(12) 0.70123(19) 0.0316(5) Uani 1 1 d . . .
N2 N 1.0180(2) 0.09920(13) 0.6530(2) 0.0349(6) Uani 1 1 d . . .
N3 N 0.9502(2) 0.00097(12) 0.81808(19) 0.0319(5) Uani 1 1 d . . .
N4 N 1.1094(2) 0.10951(13) 0.8937(2) 0.0356(6) Uani 1 1 d . . .
N5 N 1.4517(3) 0.11728(16) 0.7298(3) 0.0571(8) Uani 1 1 d . . .
C1 C 0.7905(3) 0.23204(15) 0.8242(2) 0.0351(7) Uani 1 1 d . . .
C2 C 0.8234(3) 0.25310(15) 0.7359(2) 0.0349(7) Uani 1 1 d . . .
C3 C 0.7883(3) 0.31969(16) 0.6864(3) 0.0433(8) Uani 1 1 d . . .
H3 H 0.8090 0.3325 0.6267 0.052 Uiso 1 1 calc R . .
C4 C 0.7236(3) 0.36635(17) 0.7248(3) 0.0509(9) Uani 1 1 d . . .
H4 H 0.7009 0.4107 0.6916 0.061 Uiso 1 1 calc R . .
C5 C 0.6922(3) 0.34725(17) 0.8133(3) 0.0498(9) Uani 1 1 d . . .
H5 H 0.6503 0.3794 0.8408 0.060 Uiso 1 1 calc R . .
C6 C 0.7225(3) 0.28103(17) 0.8608(3) 0.0431(7) Uani 1 1 d . . .
H6 H 0.6977 0.2684 0.9181 0.052 Uiso 1 1 calc R . .
C7 C 0.9343(3) 0.21602(16) 0.6249(2) 0.0366(7) Uani 1 1 d . . .
H7 H 0.9199 0.2596 0.5886 0.044 Uiso 1 1 calc R . .
C8 C 1.0044(3) 0.16034(16) 0.5963(2) 0.0354(7) Uani 1 1 d . . .
C9 C 1.0538(3) 0.17038(18) 0.5162(3) 0.0453(8) Uani 1 1 d . . .
H9 H 1.0423 0.2131 0.4778 0.054 Uiso 1 1 calc R . .
C10 C 1.1207(3) 0.1157(2) 0.4943(3) 0.0512(9) Uani 1 1 d . . .
H10 H 1.1542 0.1208 0.4404 0.061 Uiso 1 1 calc R . .
C11 C 1.1367(3) 0.05400(19) 0.5532(3) 0.0490(9) Uani 1 1 d . . .
H11 H 1.1826 0.0168 0.5408 0.059 Uiso 1 1 calc R . .
C12 C 1.0840(3) 0.04764(17) 0.6313(3) 0.0431(8) Uani 1 1 d . . .
H12 H 1.0951 0.0053 0.6707 0.052 Uiso 1 1 calc R . .
C13 C 0.7421(3) -0.02734(16) 0.6755(2) 0.0363(7) Uani 1 1 d . . .
C14 C 0.8539(3) -0.05039(15) 0.7674(2) 0.0341(7) Uani 1 1 d . . .
C15 C 0.8660(3) -0.12031(16) 0.8047(3) 0.0429(8) Uani 1 1 d . . .
H15 H 0.9407 -0.1347 0.8651 0.052 Uiso 1 1 calc R . .
C16 C 0.7688(4) -0.16796(18) 0.7531(3) 0.0507(9) Uani 1 1 d . . .
H16 H 0.7784 -0.2148 0.7769 0.061 Uiso 1 1 calc R . .
C17 C 0.6565(4) -0.14594(18) 0.6655(3) 0.0494(8) Uani 1 1 d . . .
H17 H 0.5897 -0.1779 0.6317 0.059 Uiso 1 1 calc R . .
C18 C 0.6423(3) -0.07694(18) 0.6276(3) 0.0437(8) Uani 1 1 d . . .
H18 H 0.5653 -0.0630 0.5693 0.052 Uiso 1 1 calc R . .
C19 C 1.0596(3) -0.01161(16) 0.9002(2) 0.0379(7) Uani 1 1 d . . .
H19 H 1.0802 -0.0568 0.9306 0.045 Uiso 1 1 calc R . .
C20 C 1.1503(3) 0.04635(16) 0.9444(2) 0.0366(7) Uani 1 1 d . . .
C21 C 1.2716(3) 0.03749(19) 1.0319(3) 0.0475(8) Uani 1 1 d . . .
H21 H 1.2977 -0.0065 1.0656 0.057 Uiso 1 1 calc R . .
C22 C 1.3525(3) 0.0950(2) 1.0676(3) 0.0550(10) Uani 1 1 d . . .
H22 H 1.4338 0.0906 1.1263 0.066 Uiso 1 1 calc R . .
C23 C 1.3112(3) 0.1588(2) 1.0154(3) 0.0544(9) Uani 1 1 d . . .
H23 H 1.3650 0.1980 1.0379 0.065 Uiso 1 1 calc R . .
C24 C 1.1892(3) 0.16479(17) 0.9289(3) 0.0427(8) Uani 1 1 d . . .
H24 H 1.1621 0.2085 0.8943 0.051 Uiso 1 1 calc R . .
C25 C 1.4527(4) 0.0487(2) 0.7089(4) 0.0620(10) Uani 1 1 d . . .
H25 H 1.4674 0.0352 0.6463 0.074 Uiso 1 1 calc R . .
C26 C 1.4665(4) 0.1688(2) 0.6555(4) 0.0691(12) Uani 1 1 d . . .
H26A H 1.5242 0.2052 0.6993 0.083 Uiso 1 1 calc R . .
H26B H 1.3842 0.1891 0.6098 0.083 Uiso 1 1 calc R . .
H26C H 1.5012 0.1466 0.6075 0.083 Uiso 1 1 calc R . .
C27 C 1.4387(9) 0.1407(3) 0.8266(7) 0.168(4) Uani 1 1 d . . .
H27A H 1.5088 0.1230 0.8926 0.202 Uiso 1 1 calc R . .
H27B H 1.3587 0.1239 0.8256 0.202 Uiso 1 1 calc R . .
H27C H 1.4396 0.1915 0.8283 0.202 Uiso 1 1 calc R . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N3 2.037(2) . ?
Ni1 N1 2.037(2) . ?
Ni1 N4 2.127(3) . ?
Ni1 N2 2.142(3) . ?
Ni1 S2 2.3832(9) . ?
Ni1 S1 2.4036(8) . ?
S1 C1 1.747(3) . ?
S2 C13 1.737(3) . ?
O1 C25 1.214(5) . ?
N1 C7 1.281(4) . ?
N1 C2 1.418(4) . ?
N2 C12 1.331(4) . ?
N2 C8 1.345(4) . ?
N3 C19 1.285(4) . ?
N3 C14 1.409(4) . ?
N4 C24 1.337(4) . ?
N4 C20 1.351(4) . ?
N5 C25 1.327(5) . ?
N5 C27 1.397(6) . ?
N5 C26 1.428(5) . ?
C1 C2 1.402(4) . ?
C1 C6 1.409(4) . ?
C2 C3 1.396(4) . ?
C3 C4 1.369(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.459(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.384(4) . ?
C9 C10 1.382(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.366(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.407(4) . ?
C13 C14 1.409(4) . ?
C14 C15 1.396(4) . ?
C15 C16 1.370(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.453(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.391(4) . ?
C21 C22 1.377(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.369(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.386(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 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
N3 Ni1 N1 176.99(9) . . ?
N3 Ni1 N4 78.93(9) . . ?
N1 Ni1 N4 101.50(9) . . ?
N3 Ni1 N2 98.34(9) . . ?
N1 Ni1 N2 78.77(9) . . ?
N4 Ni1 N2 84.24(9) . . ?
N3 Ni1 S2 84.21(7) . . ?
N1 Ni1 S2 95.05(7) . . ?
N4 Ni1 S2 162.16(7) . . ?
N2 Ni1 S2 92.56(7) . . ?
N3 Ni1 S1 99.32(7) . . ?
N1 Ni1 S1 83.66(7) . . ?
N4 Ni1 S1 91.21(7) . . ?
N2 Ni1 S1 160.56(7) . . ?
S2 Ni1 S1 97.25(3) . . ?
C1 S1 Ni1 96.33(10) . . ?
C13 S2 Ni1 96.20(11) . . ?
C7 N1 C2 123.6(2) . . ?
C7 N1 Ni1 115.66(19) . . ?
C2 N1 Ni1 120.58(18) . . ?
C12 N2 C8 117.6(3) . . ?
C12 N2 Ni1 131.2(2) . . ?
C8 N2 Ni1 111.21(19) . . ?
C19 N3 C14 124.2(3) . . ?
C19 N3 Ni1 115.5(2) . . ?
C14 N3 Ni1 120.29(19) . . ?
C24 N4 C20 118.4(3) . . ?
C24 N4 Ni1 129.9(2) . . ?
C20 N4 Ni1 111.68(19) . . ?
C25 N5 C27 120.5(4) . . ?
C25 N5 C26 121.1(4) . . ?
C27 N5 C26 118.4(4) . . ?
C2 C1 C6 117.2(3) . . ?
C2 C1 S1 122.4(2) . . ?
C6 C1 S1 120.4(2) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 N1 123.0(3) . . ?
C1 C2 N1 116.4(2) . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C1 121.3(3) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
N1 C7 C8 118.4(3) . . ?
N1 C7 H7 120.8 . . ?
C8 C7 H7 120.8 . . ?
N2 C8 C9 122.5(3) . . ?
N2 C8 C7 115.7(3) . . ?
C9 C8 C7 121.8(3) . . ?
C10 C9 C8 118.7(3) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C11 C10 C9 118.9(3) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 119.1(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
N2 C12 C11 123.1(3) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C18 C13 C14 116.9(3) . . ?
C18 C13 S2 120.5(3) . . ?
C14 C13 S2 122.6(2) . . ?
C15 C14 C13 120.8(3) . . ?
C15 C14 N3 123.1(3) . . ?
C13 C14 N3 116.1(3) . . ?
C16 C15 C14 120.7(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 119.5(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 120.8(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 121.2(3) . . ?
C17 C18 H18 119.4 . . ?
C13 C18 H18 119.4 . . ?
N3 C19 C20 118.5(3) . . ?
N3 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N4 C20 C21 122.1(3) . . ?
N4 C20 C19 115.4(3) . . ?
C21 C20 C19 122.5(3) . . ?
C22 C21 C20 118.8(3) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C23 C22 C21 119.0(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 119.9(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
N4 C24 C23 121.8(3) . . ?
N4 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
O1 C25 N5 124.5(4) . . ?
O1 C25 H25 117.8 . . ?
N5 C25 H25 117.8 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 H27A 109.5 . . ?
N5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
N3 Ni1 S1 C1 -173.80(12) . . . . ?
N1 Ni1 S1 C1 5.79(12) . . . . ?
N4 Ni1 S1 C1 107.22(12) . . . . ?
N2 Ni1 S1 C1 31.2(2) . . . . ?
S2 Ni1 S1 C1 -88.52(10) . . . . ?
N3 Ni1 S2 C13 5.84(12) . . . . ?
N1 Ni1 S2 C13 -177.09(12) . . . . ?
N4 Ni1 S2 C13 24.8(3) . . . . ?
N2 Ni1 S2 C13 103.96(12) . . . . ?
S1 Ni1 S2 C13 -92.86(10) . . . . ?
N3 Ni1 N1 C7 -11(2) . . . . ?
N4 Ni1 N1 C7 86.5(2) . . . . ?
N2 Ni1 N1 C7 4.8(2) . . . . ?
S2 Ni1 N1 C7 -86.8(2) . . . . ?
S1 Ni1 N1 C7 176.4(2) . . . . ?
N3 Ni1 N1 C2 163.9(18) . . . . ?
N4 Ni1 N1 C2 -98.3(2) . . . . ?
N2 Ni1 N1 C2 180.0(2) . . . . ?
S2 Ni1 N1 C2 88.4(2) . . . . ?
S1 Ni1 N1 C2 -8.4(2) . . . . ?
N3 Ni1 N2 C12 -3.2(3) . . . . ?
N1 Ni1 N2 C12 177.6(3) . . . . ?
N4 Ni1 N2 C12 74.7(3) . . . . ?
S2 Ni1 N2 C12 -87.7(3) . . . . ?
S1 Ni1 N2 C12 151.9(2) . . . . ?
N3 Ni1 N2 C8 175.04(19) . . . . ?
N1 Ni1 N2 C8 -4.11(19) . . . . ?
N4 Ni1 N2 C8 -107.1(2) . . . . ?
S2 Ni1 N2 C8 90.53(19) . . . . ?
S1 Ni1 N2 C8 -29.9(4) . . . . ?
N1 Ni1 N3 C19 98.9(18) . . . . ?
N4 Ni1 N3 C19 0.6(2) . . . . ?
N2 Ni1 N3 C19 83.0(2) . . . . ?
S2 Ni1 N3 C19 174.7(2) . . . . ?
S1 Ni1 N3 C19 -88.8(2) . . . . ?
N1 Ni1 N3 C14 -81.5(19) . . . . ?
N4 Ni1 N3 C14 -179.9(2) . . . . ?
N2 Ni1 N3 C14 -97.5(2) . . . . ?
S2 Ni1 N3 C14 -5.77(19) . . . . ?
S1 Ni1 N3 C14 90.7(2) . . . . ?
N3 Ni1 N4 C24 178.4(3) . . . . ?
N1 Ni1 N4 C24 1.4(3) . . . . ?
N2 Ni1 N4 C24 78.7(3) . . . . ?
S2 Ni1 N4 C24 159.1(2) . . . . ?
S1 Ni1 N4 C24 -82.4(3) . . . . ?
N3 Ni1 N4 C20 -0.43(19) . . . . ?
N1 Ni1 N4 C20 -177.40(19) . . . . ?
N2 Ni1 N4 C20 -100.1(2) . . . . ?
S2 Ni1 N4 C20 -19.7(4) . . . . ?
S1 Ni1 N4 C20 98.83(19) . . . . ?
Ni1 S1 C1 C2 -4.1(3) . . . . ?
Ni1 S1 C1 C6 175.2(2) . . . . ?
C6 C1 C2 C3 -0.8(4) . . . . ?
S1 C1 C2 C3 178.6(2) . . . . ?
C6 C1 C2 N1 179.3(3) . . . . ?
S1 C1 C2 N1 -1.4(4) . . . . ?
C7 N1 C2 C3 2.9(5) . . . . ?
Ni1 N1 C2 C3 -171.9(2) . . . . ?
C7 N1 C2 C1 -177.2(3) . . . . ?
Ni1 N1 C2 C1 8.0(3) . . . . ?
C1 C2 C3 C4 1.6(5) . . . . ?
N1 C2 C3 C4 -178.5(3) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C3 C4 C5 C6 -1.7(5) . . . . ?
C4 C5 C6 C1 2.5(5) . . . . ?
C2 C1 C6 C5 -1.3(5) . . . . ?
S1 C1 C6 C5 179.4(3) . . . . ?
C2 N1 C7 C8 -179.7(3) . . . . ?
Ni1 N1 C7 C8 -4.7(3) . . . . ?
C12 N2 C8 C9 1.4(4) . . . . ?
Ni1 N2 C8 C9 -177.2(2) . . . . ?
C12 N2 C8 C7 -178.4(3) . . . . ?
Ni1 N2 C8 C7 3.1(3) . . . . ?
N1 C7 C8 N2 0.9(4) . . . . ?
N1 C7 C8 C9 -178.9(3) . . . . ?
N2 C8 C9 C10 -0.6(5) . . . . ?
C7 C8 C9 C10 179.2(3) . . . . ?
C8 C9 C10 C11 -0.6(5) . . . . ?
C9 C10 C11 C12 1.1(5) . . . . ?
C8 N2 C12 C11 -0.9(5) . . . . ?
Ni1 N2 C12 C11 177.3(2) . . . . ?
C10 C11 C12 N2 -0.3(5) . . . . ?
Ni1 S2 C13 C18 173.7(2) . . . . ?
Ni1 S2 C13 C14 -7.0(2) . . . . ?
C18 C13 C14 C15 3.0(4) . . . . ?
S2 C13 C14 C15 -176.3(2) . . . . ?
C18 C13 C14 N3 -176.8(3) . . . . ?
S2 C13 C14 N3 3.8(4) . . . . ?
C19 N3 C14 C15 2.6(4) . . . . ?
Ni1 N3 C14 C15 -176.9(2) . . . . ?
C19 N3 C14 C13 -177.6(3) . . . . ?
Ni1 N3 C14 C13 2.9(3) . . . . ?
C13 C14 C15 C16 -0.5(5) . . . . ?
N3 C14 C15 C16 179.3(3) . . . . ?
C14 C15 C16 C17 -1.8(5) . . . . ?
C15 C16 C17 C18 1.6(5) . . . . ?
C16 C17 C18 C13 1.1(5) . . . . ?
C14 C13 C18 C17 -3.3(5) . . . . ?
S2 C13 C18 C17 176.1(2) . . . . ?
C14 N3 C19 C20 179.9(3) . . . . ?
Ni1 N3 C19 C20 -0.6(3) . . . . ?
C24 N4 C20 C21 0.5(4) . . . . ?
Ni1 N4 C20 C21 179.4(2) . . . . ?
C24 N4 C20 C19 -178.7(3) . . . . ?
Ni1 N4 C20 C19 0.3(3) . . . . ?
N3 C19 C20 N4 0.2(4) . . . . ?
N3 C19 C20 C21 -179.0(3) . . . . ?
N4 C20 C21 C22 -0.1(5) . . . . ?
C19 C20 C21 C22 179.0(3) . . . . ?
C20 C21 C22 C23 -0.5(5) . . . . ?
C21 C22 C23 C24 0.7(5) . . . . ?
C20 N4 C24 C23 -0.3(5) . . . . ?
Ni1 N4 C24 C23 -179.0(2) . . . . ?
C22 C23 C24 N4 -0.3(5) . . . . ?
C27 N5 C25 O1 4.3(8) . . . . ?
C26 N5 C25 O1 -177.1(4) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_xcalibur_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1970595'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C46 H50 Cl6 Co N4 Ni S2'
_chemical_formula_moiety         'C46 H50 Cl6 Co N4 Ni S2'
_chemical_formula_weight         1053.40
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.1761(3)
_cell_length_b                   12.4123(4)
_cell_length_c                   19.1814(5)
_cell_angle_alpha                96.674(2)
_cell_angle_beta                 91.868(2)
_cell_angle_gamma                96.713(3)
_cell_volume                     2387.24(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12143
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      31.18
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1086.00
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_T_max  0.930

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            14717
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_theta_max         24.749
_diffrn_reflns_theta_min         1.867
_diffrn_reflns_theta_full        24.749
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7838
_reflns_number_gt                7072
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1300
_refine_ls_wR_factor_gt          0.1256
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7838
_refine_ls_number_parameters     541
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0700P)²+2.5032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.79
_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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Co Co 0.3494 0.9721
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Ni1 Ni 0.64850(3) 0.42889(3) 0.25738(2) 0.03645(13) Uani 1 1 d . . . . .
Co1 Co 1.10897(4) 0.96660(3) 0.24769(2) 0.03857(14) Uani 1 1 d . . . . .
Cl1 Cl 0.22357(11) 0.14376(9) 0.00396(5) 0.0768(3) Uani 1 1 d . . . . .
Cl2 Cl 0.63143(12) 0.92506(8) 0.44574(6) 0.0771(3) Uani 1 1 d . . . . .
Cl3 Cl 0.11942(11) 0.71580(13) 0.54005(8) 0.0951(4) Uani 1 1 d . . . . .
Cl4 Cl 0.40114(12) 0.77547(12) 0.53421(8) 0.0979(4) Uani 1 1 d . . . . .
Cl5 Cl -0.11014(13) 0.54368(10) 0.08591(7) 0.0898(4) Uani 1 1 d . . . . .
Cl6 Cl -0.00546(16) 0.33589(9) 0.07277(7) 0.0918(4) Uani 1 1 d . . . . .
S1 S 0.71203(8) 0.27716(7) 0.21405(5) 0.0519(2) Uani 1 1 d . . . . .
S2 S 0.83137(7) 0.49351(8) 0.31254(5) 0.0508(2) Uani 1 1 d . . . . .
N1 N 0.4907(2) 0.38978(18) 0.20797(12) 0.0347(5) Uani 1 1 d . . . . .
N2 N 0.2945(2) 0.5555(2) 0.11916(13) 0.0410(6) Uani 1 1 d . . . . .
N3 N 0.5786(2) 0.55249(19) 0.29155(12) 0.0357(5) Uani 1 1 d . . . . .
N4 N 0.2333(3) 0.5177(3) 0.34058(15) 0.0513(7) Uani 1 1 d . . . . .
C1 C 0.5739(3) 0.2312(3) 0.15776(18) 0.0471(7) Uani 1 1 d . . . . .
C2 C 0.4708(3) 0.3001(2) 0.15923(15) 0.0385(6) Uani 1 1 d . . . . .
C3 C 0.3619(3) 0.2722(2) 0.11137(15) 0.0418(7) Uani 1 1 d . . . . .
H3 H 0.295233 0.317225 0.109925 0.050 Uiso 1 1 calc R U . . .
C4 C 0.3559(4) 0.1768(3) 0.06663(18) 0.0553(9) Uani 1 1 d . . . . .
C5 C 0.4498(4) 0.1068(3) 0.0665(2) 0.0702(12) Uani 1 1 d . . . . .
H5 H 0.440024 0.041716 0.036391 0.084 Uiso 1 1 calc R U . . .
C6 C 0.5598(4) 0.1345(3) 0.1120(2) 0.0663(11) Uani 1 1 d . . . . .
H6 H 0.625125 0.088027 0.112098 0.080 Uiso 1 1 calc R U . . .
C7 C 0.3999(3) 0.4733(2) 0.21052(14) 0.0318(6) Uani 1 1 d . . . . .
H7 H 0.308958 0.437613 0.211839 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4095(3) 0.5370(2) 0.14739(14) 0.0339(6) Uani 1 1 d . . . . .
C9 C 0.5293(3) 0.5735(3) 0.12087(19) 0.0572(9) Uani 1 1 d . . . . .
H9 H 0.608499 0.560118 0.141858 0.069 Uiso 1 1 calc R U . . .
C10 C 0.5302(4) 0.6300(4) 0.0630(2) 0.0692(11) Uani 1 1 d . . . . .
H10 H 0.609804 0.655096 0.044554 0.083 Uiso 1 1 calc R U . . .
C11 C 0.4122(4) 0.6486(3) 0.03328(18) 0.0581(9) Uani 1 1 d . . . . .
H11 H 0.409584 0.686245 -0.005850 0.070 Uiso 1 1 calc R U . . .
C12 C 0.2981(4) 0.6102(3) 0.06287(17) 0.0498(8) Uani 1 1 d . . . . .
H12 H 0.217882 0.622809 0.042587 0.060 Uiso 1 1 calc R U . . .
C13 C 0.7833(3) 0.6170(3) 0.34969(15) 0.0453(7) Uani 1 1 d . . . . .
C14 C 0.6490(3) 0.6334(2) 0.33573(14) 0.0381(6) Uani 1 1 d . . . . .
C15 C 0.6025(3) 0.7279(3) 0.36716(16) 0.0462(7) Uani 1 1 d . . . . .
H15 H 0.514270 0.738732 0.360501 0.055 Uiso 1 1 calc R U . . .
C16 C 0.6897(4) 0.8052(3) 0.40833(17) 0.0548(9) Uani 1 1 d . . . . .
C17 C 0.8213(4) 0.7908(3) 0.42027(18) 0.0603(10) Uani 1 1 d . . . . .
H17 H 0.878025 0.844357 0.447933 0.072 Uiso 1 1 calc R U . . .
C18 C 0.8665(3) 0.6981(4) 0.39133(17) 0.0578(10) Uani 1 1 d . . . . .
H18 H 0.954737 0.688537 0.399426 0.069 Uiso 1 1 calc R U . . .
C19 C 0.4361(3) 0.5475(2) 0.28050(14) 0.0315(6) Uani 1 1 d . . . . .
H19 H 0.413702 0.620984 0.275516 0.038 Uiso 1 1 calc R U . . .
C20 C 0.3614(3) 0.5041(2) 0.34073(14) 0.0322(6) Uani 1 1 d . . . . .
C21 C 0.4196(3) 0.4540(3) 0.39210(18) 0.0532(9) Uani 1 1 d . . . . .
H21 H 0.509137 0.445535 0.391251 0.064 Uiso 1 1 calc R U . . .
C22 C 0.3440(4) 0.4163(3) 0.44495(19) 0.0603(10) Uani 1 1 d . . . . .
H22 H 0.381966 0.382080 0.479814 0.072 Uiso 1 1 calc R U . . .
C23 C 0.2138(3) 0.4302(3) 0.44513(18) 0.0553(9) Uani 1 1 d . . . . .
H23 H 0.160736 0.406831 0.480380 0.066 Uiso 1 1 calc R U . . .
C24 C 0.1631(3) 0.4791(4) 0.3922(2) 0.0624(10) Uani 1 1 d . . . . .
H24 H 0.073201 0.486404 0.391818 0.075 Uiso 1 1 calc R U . . .
C25 C 1.2815(3) 0.9777(3) 0.19571(19) 0.0538(8) Uani 1 1 d . . . . .
C26 C 1.2740(4) 1.0761(3) 0.24167(18) 0.0560(9) Uani 1 1 d . . . . .
C27 C 1.1574(3) 1.1211(3) 0.22174(16) 0.0465(7) Uani 1 1 d . . . . .
C28 C 1.0934(3) 1.0511(2) 0.16323(15) 0.0417(7) Uani 1 1 d . . . . .
C29 C 1.1703(3) 0.9634(3) 0.14733(16) 0.0463(7) Uani 1 1 d . . . . .
C30 C 1.3894(4) 0.9043(4) 0.1956(3) 0.0838(14) Uani 1 1 d . . . . .
H30A H 1.453161 0.931239 0.233410 0.101 Uiso 1 1 calc R U . . .
H30B H 1.351545 0.831554 0.201552 0.101 Uiso 1 1 calc R U . . .
H30C H 1.432260 0.903169 0.151692 0.101 Uiso 1 1 calc R U . . .
C31 C 1.3730(5) 1.1260(4) 0.2996(2) 0.0843(15) Uani 1 1 d . . . . .
H31A H 1.442285 1.080244 0.302573 0.101 Uiso 1 1 calc R U . . .
H31B H 1.410184 1.197080 0.289821 0.101 Uiso 1 1 calc R U . . .
H31C H 1.329812 1.132556 0.343356 0.101 Uiso 1 1 calc R U . . .
C32 C 1.1134(5) 1.2265(3) 0.2538(2) 0.0660(11) Uani 1 1 d . . . . .
H32A H 1.031845 1.237595 0.230747 0.079 Uiso 1 1 calc R U . . .
H32B H 1.100315 1.223232 0.302926 0.079 Uiso 1 1 calc R U . . .
H32C H 1.180048 1.286015 0.248373 0.079 Uiso 1 1 calc R U . . .
C33 C 0.9683(4) 1.0667(3) 0.12489(18) 0.0526(8) Uani 1 1 d . . . . .
H33A H 0.935884 1.131960 0.145891 0.063 Uiso 1 1 calc R U . . .
H33B H 0.985409 1.073312 0.076546 0.063 Uiso 1 1 calc R U . . .
H33C H 0.903139 1.005030 0.127575 0.063 Uiso 1 1 calc R U . . .
C34 C 1.1407(5) 0.8741(3) 0.08752(19) 0.0632(10) Uani 1 1 d . . . . .
H34A H 1.059728 0.883187 0.063023 0.076 Uiso 1 1 calc R U . . .
H34B H 1.211805 0.877226 0.055850 0.076 Uiso 1 1 calc R U . . .
H34C H 1.131593 0.804577 0.105331 0.076 Uiso 1 1 calc R U . . .
C35 C 1.1225(4) 0.8787(3) 0.33098(17) 0.0530(8) Uani 1 1 d . . . . .
C36 C 1.0558(3) 0.8116(2) 0.27274(17) 0.0457(7) Uani 1 1 d . . . . .
C37 C 0.9411(3) 0.8587(2) 0.25416(16) 0.0438(7) Uani 1 1 d . . . . .
C38 C 0.9372(4) 0.9573(3) 0.30050(17) 0.0499(8) Uani 1 1 d . . . . .
C39 C 1.0497(4) 0.9689(3) 0.34797(16) 0.0544(9) Uani 1 1 d . . . . .
C40 C 1.2444(5) 0.8543(4) 0.3694(2) 0.0809(13) Uani 1 1 d . . . . .
H40A H 1.270814 0.911892 0.406861 0.097 Uiso 1 1 calc R U . . .
H40B H 1.225797 0.786328 0.388550 0.097 Uiso 1 1 calc R U . . .
H40C H 1.314704 0.849145 0.337453 0.097 Uiso 1 1 calc R U . . .
C41 C 1.0955(4) 0.7061(3) 0.2385(2) 0.0628(10) Uani 1 1 d . . . . .
H41A H 1.033749 0.676982 0.200131 0.075 Uiso 1 1 calc R U . . .
H41B H 1.182683 0.719052 0.221081 0.075 Uiso 1 1 calc R U . . .
H41C H 1.095619 0.654776 0.272235 0.075 Uiso 1 1 calc R U . . .
C42 C 0.8371(4) 0.8098(3) 0.1987(2) 0.0625(10) Uani 1 1 d . . . . .
H42A H 0.769962 0.857691 0.196388 0.075 Uiso 1 1 calc R U . . .
H42B H 0.876870 0.800139 0.154057 0.075 Uiso 1 1 calc R U . . .
H42C H 0.798001 0.740263 0.210166 0.075 Uiso 1 1 calc R U . . .
C43 C 0.8318(4) 1.0310(3) 0.3012(2) 0.0710(11) Uani 1 1 d . . . . .
H43A H 0.767444 1.004733 0.263535 0.085 Uiso 1 1 calc R U . . .
H43B H 0.789494 1.032353 0.345229 0.085 Uiso 1 1 calc R U . . .
H43C H 0.870524 1.103507 0.295237 0.085 Uiso 1 1 calc R U . . .
C44 C 1.0833(6) 1.0575(4) 0.4078(2) 0.0846(15) Uani 1 1 d . . . . .
H44A H 1.164219 1.046565 0.431625 0.102 Uiso 1 1 calc R U . . .
H44B H 1.093977 1.127185 0.390231 0.102 Uiso 1 1 calc R U . . .
H44C H 1.013084 1.055721 0.440108 0.102 Uiso 1 1 calc R U . . .
C45 C 0.2781(4) 0.6970(5) 0.5696(3) 0.0872(15) Uani 1 1 d . . . . .
H45A H 0.285504 0.713902 0.620310 0.105 Uiso 1 1 calc R U . . .
H45B H 0.290341 0.620743 0.558250 0.105 Uiso 1 1 calc R U . . .
C46 C -0.0245(4) 0.4533(3) 0.1279(2) 0.0621(9) Uani 1 1 d . . . . .
H46A H 0.062161 0.489786 0.144655 0.075 Uiso 1 1 calc R U . . .
H46B H -0.072261 0.433308 0.168329 0.075 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N1 1.823(2) . ?
Ni1 N3 1.828(2) . ?
Ni1 S2 2.1333(9) . ?
Ni1 S1 2.1474(9) . ?
Co1 C39 2.032(3) . ?
Co1 C28 2.041(3) . ?
Co1 C29 2.041(3) . ?
Co1 C25 2.046(3) . ?
Co1 C38 2.047(3) . ?
Co1 C27 2.046(3) . ?
Co1 C26 2.049(3) . ?
Co1 C35 2.047(3) . ?
Co1 C36 2.053(3) . ?
Co1 C37 2.060(3) . ?
Cl1 C4 1.755(4) . ?
Cl2 C16 1.750(4) . ?
Cl3 C45 1.744(4) . ?
Cl4 C45 1.703(5) . ?
Cl5 C46 1.749(4) . ?
Cl6 C46 1.732(4) . ?
S1 C1 1.743(4) . ?
S2 C13 1.744(4) . ?
N1 C2 1.359(4) . ?
N1 C7 1.465(3) . ?
N2 C8 1.329(4) . ?
N2 C12 1.340(4) . ?
N3 C14 1.355(4) . ?
N3 C19 1.451(3) . ?
N4 C20 1.334(4) . ?
N4 C24 1.341(4) . ?
C1 C6 1.392(5) . ?
C1 C2 1.428(4) . ?
C2 C3 1.400(4) . ?
C3 C4 1.373(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(6) . ?
C5 C6 1.382(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.521(4) . ?
C7 C19 1.545(4) . ?
C7 H7 0.9800 . ?
C8 C9 1.384(4) . ?
C9 C10 1.379(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.369(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.392(5) . ?
C13 C14 1.426(4) . ?
C14 C15 1.396(5) . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.387(6) . ?
C17 C18 1.355(6) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.519(4) . ?
C19 H19 0.9800 . ?
C20 C21 1.378(4) . ?
C21 C22 1.384(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.356(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.359(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C29 1.421(5) . ?
C25 C26 1.432(5) . ?
C25 C30 1.507(5) . ?
C26 C27 1.428(5) . ?
C26 C31 1.501(5) . ?
C27 C28 1.426(4) . ?
C27 C32 1.503(5) . ?
C28 C29 1.424(5) . ?
C28 C33 1.493(5) . ?
C29 C34 1.496(5) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.415(5) . ?
C35 C39 1.426(5) . ?
C35 C40 1.502(5) . ?
C36 C37 1.419(5) . ?
C36 C41 1.501(5) . ?
C37 C38 1.432(5) . ?
C37 C42 1.498(5) . ?
C38 C39 1.422(5) . ?
C38 C43 1.488(5) . ?
C39 C44 1.496(5) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 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
N1 Ni1 N3 85.82(10) . . ?
N1 Ni1 S2 173.34(8) . . ?
N3 Ni1 S2 89.01(7) . . ?
N1 Ni1 S1 88.98(8) . . ?
N3 Ni1 S1 174.61(8) . . ?
S2 Ni1 S1 96.28(4) . . ?
C39 Co1 C28 139.75(14) . . ?
C39 Co1 C29 179.32(15) . . ?
C28 Co1 C29 40.85(13) . . ?
C39 Co1 C25 138.74(15) . . ?
C28 Co1 C25 68.89(13) . . ?
C29 Co1 C25 40.70(14) . . ?
C39 Co1 C38 40.81(15) . . ?
C28 Co1 C38 111.11(13) . . ?
C29 Co1 C38 139.76(14) . . ?
C25 Co1 C38 179.25(15) . . ?
C39 Co1 C27 111.63(13) . . ?
C28 Co1 C27 40.84(12) . . ?
C29 Co1 C27 68.66(13) . . ?
C25 Co1 C27 69.00(14) . . ?
C38 Co1 C27 110.48(14) . . ?
C39 Co1 C26 111.35(14) . . ?
C28 Co1 C26 68.63(13) . . ?
C29 Co1 C26 68.43(14) . . ?
C25 Co1 C26 40.94(16) . . ?
C38 Co1 C26 138.32(15) . . ?
C27 Co1 C26 40.83(15) . . ?
C39 Co1 C35 40.93(15) . . ?
C28 Co1 C35 178.65(13) . . ?
C29 Co1 C35 138.47(14) . . ?
C25 Co1 C35 111.28(15) . . ?
C38 Co1 C35 68.74(14) . . ?
C27 Co1 C35 140.50(14) . . ?
C26 Co1 C35 112.42(14) . . ?
C39 Co1 C36 68.45(14) . . ?
C28 Co1 C36 138.26(12) . . ?
C29 Co1 C36 111.27(13) . . ?
C25 Co1 C36 111.90(14) . . ?
C38 Co1 C36 68.63(13) . . ?
C27 Co1 C36 178.63(13) . . ?
C26 Co1 C36 140.51(15) . . ?
C35 Co1 C36 40.40(13) . . ?
C39 Co1 C37 68.28(13) . . ?
C28 Co1 C37 110.98(12) . . ?
C29 Co1 C37 111.95(13) . . ?
C25 Co1 C37 139.94(14) . . ?
C38 Co1 C37 40.80(13) . . ?
C27 Co1 C37 138.29(13) . . ?
C26 Co1 C37 178.98(15) . . ?
C35 Co1 C37 67.98(13) . . ?
C36 Co1 C37 40.38(13) . . ?
C1 S1 Ni1 97.54(11) . . ?
C13 S2 Ni1 97.80(10) . . ?
C2 N1 C7 120.7(2) . . ?
C2 N1 Ni1 121.6(2) . . ?
C7 N1 Ni1 115.94(17) . . ?
C8 N2 C12 117.5(3) . . ?
C14 N3 C19 121.6(2) . . ?
C14 N3 Ni1 122.1(2) . . ?
C19 N3 Ni1 115.00(17) . . ?
C20 N4 C24 117.0(3) . . ?
C6 C1 C2 119.3(3) . . ?
C6 C1 S1 124.5(3) . . ?
C2 C1 S1 116.2(2) . . ?
N1 C2 C3 126.0(3) . . ?
N1 C2 C1 114.9(3) . . ?
C3 C2 C1 119.1(3) . . ?
C4 C3 C2 118.4(3) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C5 C4 C3 123.7(4) . . ?
C5 C4 Cl1 117.4(3) . . ?
C3 C4 Cl1 118.9(3) . . ?
C4 C5 C6 118.7(3) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
N1 C7 C8 112.4(2) . . ?
N1 C7 C19 105.6(2) . . ?
C8 C7 C19 112.2(2) . . ?
N1 C7 H7 108.9 . . ?
C8 C7 H7 108.9 . . ?
C19 C7 H7 108.9 . . ?
N2 C8 C9 121.9(3) . . ?
N2 C8 C7 115.4(2) . . ?
C9 C8 C7 122.7(3) . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C12 C11 C10 117.9(3) . . ?
C12 C11 H11 121.0 . . ?
C10 C11 H11 121.0 . . ?
N2 C12 C11 124.2(3) . . ?
N2 C12 H12 117.9 . . ?
C11 C12 H12 117.9 . . ?
C18 C13 C14 119.2(3) . . ?
C18 C13 S2 124.4(3) . . ?
C14 C13 S2 116.3(2) . . ?
N3 C14 C15 126.3(3) . . ?
N3 C14 C13 114.6(3) . . ?
C15 C14 C13 119.1(3) . . ?
C16 C15 C14 118.9(3) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 122.0(4) . . ?
C15 C16 Cl2 118.6(3) . . ?
C17 C16 Cl2 119.4(3) . . ?
C18 C17 C16 119.5(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C13 121.2(3) . . ?
C17 C18 H18 119.4 . . ?
C13 C18 H18 119.4 . . ?
N3 C19 C20 112.3(2) . . ?
N3 C19 C7 106.0(2) . . ?
C20 C19 C7 111.5(2) . . ?
N3 C19 H19 109.0 . . ?
C20 C19 H19 109.0 . . ?
C7 C19 H19 109.0 . . ?
N4 C20 C21 121.6(3) . . ?
N4 C20 C19 115.0(2) . . ?
C21 C20 C19 123.4(3) . . ?
C20 C21 C22 119.7(3) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C23 C22 C21 119.0(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 118.0(3) . . ?
C22 C23 H23 121.0 . . ?
C24 C23 H23 121.0 . . ?
N4 C24 C23 124.8(3) . . ?
N4 C24 H24 117.6 . . ?
C23 C24 H24 117.6 . . ?
C29 C25 C26 107.4(3) . . ?
C29 C25 C30 125.4(4) . . ?
C26 C25 C30 127.1(4) . . ?
C29 C25 Co1 69.44(19) . . ?
C26 C25 Co1 69.6(2) . . ?
C30 C25 Co1 128.1(3) . . ?
C27 C26 C25 108.2(3) . . ?
C27 C26 C31 125.4(4) . . ?
C25 C26 C31 126.3(4) . . ?
C27 C26 Co1 69.48(18) . . ?
C25 C26 Co1 69.42(19) . . ?
C31 C26 Co1 128.1(3) . . ?
C26 C27 C28 107.8(3) . . ?
C26 C27 C32 126.4(3) . . ?
C28 C27 C32 125.8(3) . . ?
C26 C27 Co1 69.69(18) . . ?
C28 C27 Co1 69.39(16) . . ?
C32 C27 Co1 128.8(2) . . ?
C29 C28 C27 107.9(3) . . ?
C29 C28 C33 125.8(3) . . ?
C27 C28 C33 126.3(3) . . ?
C29 C28 Co1 69.55(17) . . ?
C27 C28 Co1 69.77(17) . . ?
C33 C28 Co1 126.5(2) . . ?
C25 C29 C28 108.7(3) . . ?
C25 C29 C34 126.2(3) . . ?
C28 C29 C34 125.1(3) . . ?
C25 C29 Co1 69.86(19) . . ?
C28 C29 Co1 69.60(17) . . ?
C34 C29 Co1 128.4(2) . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C32 H32A 109.5 . . ?
C27 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C27 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C34 H34A 109.5 . . ?
C29 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C29 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C39 107.9(3) . . ?
C36 C35 C40 125.1(4) . . ?
C39 C35 C40 126.9(4) . . ?
C36 C35 Co1 70.03(17) . . ?
C39 C35 Co1 69.00(18) . . ?
C40 C35 Co1 128.7(3) . . ?
C35 C36 C37 108.2(3) . . ?
C35 C36 C41 126.2(3) . . ?
C37 C36 C41 125.6(3) . . ?
C35 C36 Co1 69.58(18) . . ?
C37 C36 Co1 70.10(17) . . ?
C41 C36 Co1 128.1(2) . . ?
C36 C37 C38 108.3(3) . . ?
C36 C37 C42 125.8(3) . . ?
C38 C37 C42 125.8(3) . . ?
C36 C37 Co1 69.52(18) . . ?
C38 C37 Co1 69.09(18) . . ?
C42 C37 Co1 130.1(2) . . ?
C39 C38 C37 107.2(3) . . ?
C39 C38 C43 126.3(4) . . ?
C37 C38 C43 126.4(3) . . ?
C39 C38 Co1 69.1(2) . . ?
C37 C38 Co1 70.10(19) . . ?
C43 C38 Co1 128.2(2) . . ?
C38 C39 C35 108.4(3) . . ?
C38 C39 C44 126.1(4) . . ?
C35 C39 C44 125.4(4) . . ?
C38 C39 Co1 70.14(18) . . ?
C35 C39 Co1 70.07(19) . . ?
C44 C39 Co1 127.8(3) . . ?
C35 C40 H40A 109.5 . . ?
C35 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C35 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C36 C41 H41A 109.5 . . ?
C36 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C36 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Cl4 C45 Cl3 113.7(3) . . ?
Cl4 C45 H45A 108.8 . . ?
Cl3 C45 H45A 108.8 . . ?
Cl4 C45 H45B 108.8 . . ?
Cl3 C45 H45B 108.8 . . ?
H45A C45 H45B 107.7 . . ?
Cl6 C46 Cl5 112.3(2) . . ?
Cl6 C46 H46A 109.1 . . ?
Cl5 C46 H46A 109.1 . . ?
Cl6 C46 H46B 109.1 . . ?
Cl5 C46 H46B 109.1 . . ?
H46A C46 H46B 107.9 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ni1 N1 C2 173.0(2) . . . . ?
S1 Ni1 N1 C2 -8.4(2) . . . . ?
N3 Ni1 N1 C7 7.78(19) . . . . ?
S1 Ni1 N1 C7 -173.67(18) . . . . ?
N1 Ni1 N3 C14 -177.5(2) . . . . ?
S2 Ni1 N3 C14 -1.7(2) . . . . ?
N1 Ni1 N3 C19 15.13(19) . . . . ?
S2 Ni1 N3 C19 -169.07(18) . . . . ?
Ni1 S1 C1 C6 177.6(3) . . . . ?
Ni1 S1 C1 C2 -1.5(2) . . . . ?
C7 N1 C2 C3 -5.2(4) . . . . ?
Ni1 N1 C2 C3 -169.8(2) . . . . ?
C7 N1 C2 C1 173.7(2) . . . . ?
Ni1 N1 C2 C1 9.2(3) . . . . ?
C6 C1 C2 N1 176.9(3) . . . . ?
S1 C1 C2 N1 -4.0(3) . . . . ?
C6 C1 C2 C3 -4.1(4) . . . . ?
S1 C1 C2 C3 175.0(2) . . . . ?
N1 C2 C3 C4 -178.5(3) . . . . ?
C1 C2 C3 C4 2.7(4) . . . . ?
C2 C3 C4 C5 0.6(5) . . . . ?
C2 C3 C4 Cl1 -177.4(2) . . . . ?
C3 C4 C5 C6 -2.4(6) . . . . ?
Cl1 C4 C5 C6 175.6(3) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C2 C1 C6 C5 2.4(5) . . . . ?
S1 C1 C6 C5 -176.7(3) . . . . ?
C2 N1 C7 C8 -69.0(3) . . . . ?
Ni1 N1 C7 C8 96.4(2) . . . . ?
C2 N1 C7 C19 168.4(2) . . . . ?
Ni1 N1 C7 C19 -26.2(3) . . . . ?
C12 N2 C8 C9 0.9(4) . . . . ?
C12 N2 C8 C7 -179.2(3) . . . . ?
N1 C7 C8 N2 137.2(2) . . . . ?
C19 C7 C8 N2 -104.1(3) . . . . ?
N1 C7 C8 C9 -42.9(4) . . . . ?
C19 C7 C8 C9 75.9(4) . . . . ?
N2 C8 C9 C10 -0.6(6) . . . . ?
C7 C8 C9 C10 179.4(3) . . . . ?
C8 C9 C10 C11 0.0(7) . . . . ?
C9 C10 C11 C12 0.2(6) . . . . ?
C8 N2 C12 C11 -0.6(5) . . . . ?
C10 C11 C12 N2 0.0(6) . . . . ?
Ni1 S2 C13 C18 -178.0(3) . . . . ?
Ni1 S2 C13 C14 2.3(2) . . . . ?
C19 N3 C14 C15 -10.1(4) . . . . ?
Ni1 N3 C14 C15 -176.7(2) . . . . ?
C19 N3 C14 C13 170.1(2) . . . . ?
Ni1 N3 C14 C13 3.6(3) . . . . ?
C18 C13 C14 N3 176.5(3) . . . . ?
S2 C13 C14 N3 -3.8(3) . . . . ?
C18 C13 C14 C15 -3.3(4) . . . . ?
S2 C13 C14 C15 176.5(2) . . . . ?
N3 C14 C15 C16 -176.8(3) . . . . ?
C13 C14 C15 C16 2.9(4) . . . . ?
C14 C15 C16 C17 -1.1(5) . . . . ?
C14 C15 C16 Cl2 178.4(2) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
Cl2 C16 C17 C18 -180.0(3) . . . . ?
C16 C17 C18 C13 0.1(5) . . . . ?
C14 C13 C18 C17 1.8(5) . . . . ?
S2 C13 C18 C17 -177.9(3) . . . . ?
C14 N3 C19 C20 -77.6(3) . . . . ?
Ni1 N3 C19 C20 89.9(2) . . . . ?
C14 N3 C19 C7 160.5(2) . . . . ?
Ni1 N3 C19 C7 -32.1(3) . . . . ?
N1 C7 C19 N3 34.9(3) . . . . ?
C8 C7 C19 N3 -87.8(3) . . . . ?
N1 C7 C19 C20 -87.6(3) . . . . ?
C8 C7 C19 C20 149.7(2) . . . . ?
C24 N4 C20 C21 -0.8(5) . . . . ?
C24 N4 C20 C19 179.0(3) . . . . ?
N3 C19 C20 N4 167.3(2) . . . . ?
C7 C19 C20 N4 -73.9(3) . . . . ?
N3 C19 C20 C21 -12.8(4) . . . . ?
C7 C19 C20 C21 106.0(3) . . . . ?
N4 C20 C21 C22 0.2(5) . . . . ?
C19 C20 C21 C22 -179.7(3) . . . . ?
C20 C21 C22 C23 -0.3(6) . . . . ?
C21 C22 C23 C24 1.1(6) . . . . ?
C20 N4 C24 C23 1.8(6) . . . . ?
C22 C23 C24 N4 -1.9(7) . . . . ?
C29 C25 C26 C27 0.6(4) . . . . ?
C30 C25 C26 C27 178.2(4) . . . . ?
Co1 C25 C26 C27 -58.8(2) . . . . ?
C29 C25 C26 C31 -177.7(3) . . . . ?
C30 C25 C26 C31 -0.2(6) . . . . ?
Co1 C25 C26 C31 122.9(4) . . . . ?
C29 C25 C26 Co1 59.4(2) . . . . ?
C30 C25 C26 Co1 -123.0(4) . . . . ?
C25 C26 C27 C28 -0.4(4) . . . . ?
C31 C26 C27 C28 178.0(3) . . . . ?
Co1 C26 C27 C28 -59.2(2) . . . . ?
C25 C26 C27 C32 -177.3(3) . . . . ?
C31 C26 C27 C32 1.0(5) . . . . ?
Co1 C26 C27 C32 123.9(3) . . . . ?
C25 C26 C27 Co1 58.8(2) . . . . ?
C31 C26 C27 Co1 -122.9(4) . . . . ?
C26 C27 C28 C29 0.0(3) . . . . ?
C32 C27 C28 C29 177.0(3) . . . . ?
Co1 C27 C28 C29 -59.3(2) . . . . ?
C26 C27 C28 C33 -179.6(3) . . . . ?
C32 C27 C28 C33 -2.6(5) . . . . ?
Co1 C27 C28 C33 121.0(3) . . . . ?
C26 C27 C28 Co1 59.3(2) . . . . ?
C32 C27 C28 Co1 -123.7(3) . . . . ?
C26 C25 C29 C28 -0.6(4) . . . . ?
C30 C25 C29 C28 -178.2(3) . . . . ?
Co1 C25 C29 C28 58.9(2) . . . . ?
C26 C25 C29 C34 177.1(3) . . . . ?
C30 C25 C29 C34 -0.6(6) . . . . ?
Co1 C25 C29 C34 -123.4(3) . . . . ?
C26 C25 C29 Co1 -59.5(2) . . . . ?
C30 C25 C29 Co1 122.9(4) . . . . ?
C27 C28 C29 C25 0.3(3) . . . . ?
C33 C28 C29 C25 180.0(3) . . . . ?
Co1 C28 C29 C25 -59.1(2) . . . . ?
C27 C28 C29 C34 -177.3(3) . . . . ?
C33 C28 C29 C34 2.3(5) . . . . ?
Co1 C28 C29 C34 123.2(3) . . . . ?
C27 C28 C29 Co1 59.5(2) . . . . ?
C33 C28 C29 Co1 -120.9(3) . . . . ?
C39 C35 C36 C37 -0.9(4) . . . . ?
C40 C35 C36 C37 176.4(3) . . . . ?
Co1 C35 C36 C37 -59.7(2) . . . . ?
C39 C35 C36 C41 -178.3(3) . . . . ?
C40 C35 C36 C41 -1.0(6) . . . . ?
Co1 C35 C36 C41 122.9(3) . . . . ?
C39 C35 C36 Co1 58.8(2) . . . . ?
C40 C35 C36 Co1 -123.9(4) . . . . ?
C35 C36 C37 C38 1.0(4) . . . . ?
C41 C36 C37 C38 178.4(3) . . . . ?
Co1 C36 C37 C38 -58.3(2) . . . . ?
C35 C36 C37 C42 -175.3(3) . . . . ?
C41 C36 C37 C42 2.1(5) . . . . ?
Co1 C36 C37 C42 125.4(3) . . . . ?
C35 C36 C37 Co1 59.4(2) . . . . ?
C41 C36 C37 Co1 -123.2(3) . . . . ?
C36 C37 C38 C39 -0.7(4) . . . . ?
C42 C37 C38 C39 175.5(3) . . . . ?
Co1 C37 C38 C39 -59.3(2) . . . . ?
C36 C37 C38 C43 -178.0(3) . . . . ?
C42 C37 C38 C43 -1.7(5) . . . . ?
Co1 C37 C38 C43 123.4(3) . . . . ?
C36 C37 C38 Co1 58.6(2) . . . . ?
C42 C37 C38 Co1 -125.1(3) . . . . ?
C37 C38 C39 C35 0.2(4) . . . . ?
C43 C38 C39 C35 177.4(3) . . . . ?
Co1 C38 C39 C35 -59.8(2) . . . . ?
C37 C38 C39 C44 -177.1(3) . . . . ?
C43 C38 C39 C44 0.2(6) . . . . ?
Co1 C38 C39 C44 122.9(4) . . . . ?
C37 C38 C39 Co1 60.0(2) . . . . ?
C43 C38 C39 Co1 -122.7(3) . . . . ?
C36 C35 C39 C38 0.5(4) . . . . ?
C40 C35 C39 C38 -176.7(3) . . . . ?
Co1 C35 C39 C38 59.9(2) . . . . ?
C36 C35 C39 C44 177.7(3) . . . . ?
C40 C35 C39 C44 0.5(6) . . . . ?
Co1 C35 C39 C44 -122.8(4) . . . . ?
C36 C35 C39 Co1 -59.4(2) . . . . ?
C40 C35 C39 Co1 123.4(4) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_xcalibur_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1970594'
loop_
_audit_author_name
_audit_author_address
'Satoshi Inoue'
;Kanagawa University
Japan
;
_audit_update_record             
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C46 H52 Cl4 Co N4 Ni S2'
_chemical_formula_moiety         'C46 H52 Cl4 Co N4 Ni S2'
_chemical_formula_weight         984.51
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   12.3345(4)
_cell_length_b                   22.2711(6)
_cell_length_c                   18.1248(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.540(4)
_cell_angle_gamma                90.0000
_cell_volume                     4692.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17730
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      31.23
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2044.00
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.081
_exptl_absorpt_correction_T_max  0.925

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            27808
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.982
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7942
_reflns_number_gt                6803
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2248
_refine_ls_wR_factor_gt          0.2118
_refine_ls_number_restraints     144
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7942
_refine_ls_number_parameters     541
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1558P)²+6.1038P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         2.01
_refine_diff_density_min         -0.64
_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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Co Co 0.3494 0.9721
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Ni1 Ni 0.39306(5) 0.75907(3) 0.51920(3) 0.0410(2) Uani 1 1 d . . . . .
Co1 Co 0.60168(4) 0.64706(2) 0.26482(3) 0.0295(2) Uani 1 1 d . . . . .
Cl1 Cl 0.64109(15) 0.96556(8) 0.57064(10) 0.0788(5) Uani 1 1 d . . . . .
Cl2 Cl 0.70723(17) 0.93286(9) 0.43734(12) 0.0884(5) Uani 1 1 d . . . . .
Cl3A Cl 0.1973(4) 0.9328(3) 0.2859(5) 0.135(2) Uani 0.6 1 d D U P A 1
Cl4A Cl 0.4220(3) 0.90246(19) 0.2801(4) 0.1158(13) Uani 0.75 1 d D U P A 1
Cl3B Cl 0.1593(6) 0.9082(5) 0.2764(10) 0.157(4) Uani 0.4 1 d D U P A 2
Cl4B Cl 0.3926(9) 0.9276(5) 0.2788(12) 0.124(4) Uani 0.25 1 d D U P A 2
S1 S 0.57564(11) 0.76450(6) 0.54428(7) 0.0496(3) Uani 1 1 d . . . . .
S2 S 0.36290(11) 0.85445(5) 0.51380(8) 0.0512(3) Uani 1 1 d . . . . .
N1 N 0.4057(4) 0.67701(18) 0.5236(2) 0.0463(9) Uani 1 1 d . . . . .
N2 N 0.2030(4) 0.6066(2) 0.6089(3) 0.0759(9) Uani 1 1 d D U . . .
N3 N 0.2385(4) 0.74742(17) 0.4966(2) 0.0427(8) Uani 1 1 d . . . . .
N4 N 0.1310(4) 0.6157(2) 0.3703(3) 0.0669(11) Uani 1 1 d . U . . .
C1 C 0.6032(4) 0.6872(2) 0.5485(2) 0.0480(11) Uani 1 1 d . . . . .
C2 C 0.5082(5) 0.6490(2) 0.5393(3) 0.0464(11) Uani 1 1 d . . . . .
C3 C 0.5293(6) 0.5862(2) 0.5477(3) 0.0581(13) Uani 1 1 d . . . . .
H3 H 0.468958 0.559942 0.543597 0.070 Uiso 1 1 calc R U . . .
C4 C 0.6381(6) 0.5641(3) 0.5619(3) 0.0640(15) Uani 1 1 d . . . . .
H4 H 0.650408 0.522876 0.566851 0.077 Uiso 1 1 calc R U . . .
C5 C 0.7310(6) 0.6023(3) 0.5689(3) 0.0683(16) Uani 1 1 d . . . . .
H5 H 0.803847 0.586277 0.577577 0.082 Uiso 1 1 calc R U . . .
C6 C 0.7151(5) 0.6633(3) 0.5631(3) 0.0578(13) Uani 1 1 d . . . . .
H6 H 0.777106 0.688804 0.568801 0.069 Uiso 1 1 calc R U . . .
C7 C 0.3014(5) 0.6459(2) 0.5240(3) 0.0502(12) Uani 1 1 d . . . . .
H7 H 0.295635 0.607574 0.496358 0.060 Uiso 1 1 calc R U . . .
C8 C 0.3012(4) 0.6336(3) 0.6075(3) 0.0726(10) Uani 1 1 d D U . . .
C9 C 0.3893(6) 0.6476(3) 0.6737(3) 0.0795(11) Uani 1 1 d D U . . .
H9 H 0.455003 0.665843 0.669755 0.095 Uiso 1 1 calc R U . . .
C10 C 0.3829(6) 0.6355(3) 0.7456(3) 0.0863(11) Uani 1 1 d D U . . .
H10 H 0.441765 0.645227 0.791680 0.104 Uiso 1 1 calc R U . . .
C11 C 0.2843(5) 0.6082(3) 0.7455(4) 0.0859(11) Uani 1 1 d D U . . .
H11 H 0.277752 0.598308 0.793682 0.103 Uiso 1 1 calc R U . . .
C12 C 0.1947(6) 0.5941(3) 0.6802(3) 0.0823(10) Uani 1 1 d D U . . .
H12 H 0.128762 0.576235 0.684206 0.099 Uiso 1 1 calc R U . . .
C13 C 0.2152(4) 0.8525(2) 0.4950(3) 0.0433(10) Uani 1 1 d . . . . .
C14 C 0.1641(4) 0.7946(2) 0.4864(2) 0.0399(9) Uani 1 1 d . . . . .
C15 C 0.0434(4) 0.7908(2) 0.4679(3) 0.0478(11) Uani 1 1 d . . . . .
H15 H 0.007394 0.753544 0.459834 0.057 Uiso 1 1 calc R U . . .
C16 C -0.0208(4) 0.8422(2) 0.4617(3) 0.0511(11) Uani 1 1 d . . . . .
H16 H -0.099741 0.838994 0.450899 0.061 Uiso 1 1 calc R U . . .
C17 C 0.0295(4) 0.8992(2) 0.4713(3) 0.0481(11) Uani 1 1 d . . . . .
H17 H -0.015448 0.933379 0.467089 0.058 Uiso 1 1 calc R U . . .
C18 C 0.1450(5) 0.9041(2) 0.4868(3) 0.0505(11) Uani 1 1 d . . . . .
H18 H 0.178474 0.941998 0.492176 0.061 Uiso 1 1 calc R U . . .
C19 C 0.1994(4) 0.6859(2) 0.4782(3) 0.0466(11) Uani 1 1 d . . . . .
H19 H 0.135319 0.678595 0.497643 0.056 Uiso 1 1 calc R U . . .
C20 C 0.1588(4) 0.6725(3) 0.3895(3) 0.0578(10) Uani 1 1 d . U . . .
C21 C 0.1525(5) 0.7166(3) 0.3345(3) 0.0624(11) Uani 1 1 d . U . . .
H21 H 0.172020 0.756091 0.349664 0.075 Uiso 1 1 calc R U . . .
C22 C 0.1160(5) 0.7002(4) 0.2552(4) 0.0716(12) Uani 1 1 d . U . . .
H22 H 0.110719 0.729060 0.217099 0.086 Uiso 1 1 calc R U . . .
C23 C 0.0893(5) 0.6443(3) 0.2350(4) 0.0764(13) Uani 1 1 d . U . . .
H23 H 0.065948 0.633205 0.182540 0.092 Uiso 1 1 calc R U . . .
C24 C 0.0959(5) 0.6027(3) 0.2907(4) 0.0759(13) Uani 1 1 d . U . . .
H24 H 0.075825 0.563280 0.275010 0.091 Uiso 1 1 calc R U . . .
C25 C 0.6554(4) 0.69762(19) 0.3647(2) 0.0367(9) Uani 1 1 d . . . . .
C26 C 0.7163(4) 0.64221(19) 0.3769(2) 0.0384(9) Uani 1 1 d . . . . .
C27 C 0.6337(4) 0.5948(2) 0.3626(2) 0.0422(10) Uani 1 1 d . . . . .
C28 C 0.5219(4) 0.6210(2) 0.3431(2) 0.0408(9) Uani 1 1 d . . . . .
C29 C 0.5353(4) 0.6844(2) 0.3436(2) 0.0378(9) Uani 1 1 d . . . . .
C30 C 0.7073(5) 0.7591(2) 0.3764(3) 0.0556(13) Uani 1 1 d . . . . .
H30A H 0.647223 0.788625 0.364077 0.067 Uiso 1 1 calc R U . . .
H30B H 0.755860 0.763707 0.429903 0.067 Uiso 1 1 calc R U . . .
H30C H 0.752233 0.764374 0.342620 0.067 Uiso 1 1 calc R U . . .
C31 C 0.8442(4) 0.6354(3) 0.4024(3) 0.0594(13) Uani 1 1 d . . . . .
H31A H 0.863681 0.593501 0.406273 0.071 Uiso 1 1 calc R U . . .
H31B H 0.872518 0.654125 0.364697 0.071 Uiso 1 1 calc R U . . .
H31C H 0.878518 0.654168 0.452470 0.071 Uiso 1 1 calc R U . . .
C32 C 0.6635(6) 0.5293(2) 0.3717(3) 0.0623(14) Uani 1 1 d . . . . .
H32A H 0.594108 0.505996 0.358929 0.075 Uiso 1 1 calc R U . . .
H32B H 0.704803 0.518582 0.337199 0.075 Uiso 1 1 calc R U . . .
H32C H 0.710500 0.521322 0.424847 0.075 Uiso 1 1 calc R U . . .
C33 C 0.4096(5) 0.5897(3) 0.3272(3) 0.0628(14) Uani 1 1 d . . . . .
H33A H 0.421911 0.547072 0.330051 0.075 Uiso 1 1 calc R U . . .
H33B H 0.375644 0.601583 0.365498 0.075 Uiso 1 1 calc R U . . .
H33C H 0.359070 0.600247 0.275904 0.075 Uiso 1 1 calc R U . . .
C34 C 0.4414(5) 0.7308(3) 0.3288(3) 0.0552(13) Uani 1 1 d . . . . .
H34A H 0.474310 0.770264 0.332695 0.066 Uiso 1 1 calc R U . . .
H34B H 0.386574 0.725256 0.277279 0.066 Uiso 1 1 calc R U . . .
H34C H 0.403476 0.726573 0.366922 0.066 Uiso 1 1 calc R U . . .
C35 C 0.5726(4) 0.70020(18) 0.1676(2) 0.0370(9) Uani 1 1 d . . . . .
C36 C 0.4879(4) 0.6538(2) 0.1534(2) 0.0381(9) Uani 1 1 d . . . . .
C37 C 0.5449(4) 0.59746(19) 0.1642(2) 0.0400(9) Uani 1 1 d . . . . .
C38 C 0.6650(4) 0.6083(2) 0.1847(2) 0.0398(9) Uani 1 1 d . . . . .
C39 C 0.6829(4) 0.6725(2) 0.1867(2) 0.0403(9) Uani 1 1 d . . . . .
C40 C 0.5492(5) 0.7659(2) 0.1595(3) 0.0552(12) Uani 1 1 d . . . . .
H40A H 0.468130 0.772838 0.146357 0.066 Uiso 1 1 calc R U . . .
H40B H 0.589700 0.785589 0.208039 0.066 Uiso 1 1 calc R U . . .
H40C H 0.574760 0.781727 0.118809 0.066 Uiso 1 1 calc R U . . .
C41 C 0.3598(4) 0.6636(3) 0.1284(3) 0.0557(12) Uani 1 1 d . . . . .
H41A H 0.343824 0.705850 0.125505 0.067 Uiso 1 1 calc R U . . .
H41B H 0.323648 0.645720 0.077848 0.067 Uiso 1 1 calc R U . . .
H41C H 0.330295 0.645337 0.165748 0.067 Uiso 1 1 calc R U . . .
C42 C 0.4871(5) 0.5369(2) 0.1530(3) 0.0565(13) Uani 1 1 d . . . . .
H42A H 0.544347 0.505851 0.163906 0.068 Uiso 1 1 calc R U . . .
H42B H 0.443840 0.533020 0.188057 0.068 Uiso 1 1 calc R U . . .
H42C H 0.436193 0.533126 0.099962 0.068 Uiso 1 1 calc R U . . .
C43 C 0.7574(5) 0.5621(3) 0.1973(3) 0.0605(14) Uani 1 1 d . . . . .
H43A H 0.830810 0.581656 0.210622 0.073 Uiso 1 1 calc R U . . .
H43B H 0.756867 0.535852 0.239229 0.073 Uiso 1 1 calc R U . . .
H43C H 0.743903 0.539139 0.150280 0.073 Uiso 1 1 calc R U . . .
C44 C 0.7941(5) 0.7034(3) 0.2036(3) 0.0566(13) Uani 1 1 d . . . . .
H44A H 0.854776 0.674257 0.214684 0.068 Uiso 1 1 calc R U . . .
H44B H 0.793336 0.726994 0.159116 0.068 Uiso 1 1 calc R U . . .
H44C H 0.806781 0.729208 0.248196 0.068 Uiso 1 1 calc R U . . .
C45 C 0.6036(5) 0.9246(4) 0.4830(4) 0.0762(18) Uani 1 1 d . . . . .
H45A H 0.596111 0.882485 0.493988 0.091 Uiso 1 1 calc R U . . .
H45B H 0.529704 0.938495 0.448056 0.091 Uiso 1 1 calc R U . . .
C46 C 0.2907(4) 0.87372(18) 0.2834(6) 0.129(4) Uani 1 1 d D . . . .
H46A H 0.255231 0.848946 0.237630 0.155 Uiso 0.5 1 calc R U P A 1
H46B H 0.304843 0.848785 0.329533 0.155 Uiso 0.5 1 calc R U P A 1
H46C H 0.278507 0.845166 0.240956 0.155 Uiso 0.5 1 calc R U P A 2
H46D H 0.319784 0.851924 0.332421 0.155 Uiso 0.5 1 calc R U P A 2


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N3 1.829(4) . ?
Ni1 N1 1.834(4) . ?
Ni1 S1 2.1466(14) . ?
Ni1 S2 2.1533(13) . ?
Co1 C36 2.044(4) . ?
Co1 C29 2.045(4) . ?
Co1 C37 2.045(4) . ?
Co1 C25 2.045(4) . ?
Co1 C27 2.046(4) . ?
Co1 C35 2.052(4) . ?
Co1 C26 2.053(4) . ?
Co1 C38 2.055(4) . ?
Co1 C28 2.062(4) . ?
Co1 C39 2.069(4) . ?
Cl1 C45 1.753(7) . ?
Cl2 C45 1.750(6) . ?
Cl3A C46 1.760(2) . ?
Cl4A C46 1.760(2) . ?
Cl3B C46 1.759(2) . ?
Cl4B C46 1.760(2) . ?
S1 C1 1.751(5) . ?
S2 C13 1.738(5) . ?
N1 C2 1.352(7) . ?
N1 C7 1.464(6) . ?
N2 C8 1.359(2) . ?
N2 C12 1.359(2) . ?
N3 C14 1.366(6) . ?
N3 C19 1.453(5) . ?
N4 C20 1.326(8) . ?
N4 C24 1.390(8) . ?
C1 C2 1.413(7) . ?
C1 C6 1.419(8) . ?
C2 C3 1.421(7) . ?
C3 C4 1.371(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(9) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C19 1.539(8) . ?
C7 C8 1.540(7) . ?
C7 H7 0.9800 . ?
C8 C9 1.359(2) . ?
C9 C10 1.359(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.359(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.359(2) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.416(7) . ?
C13 C14 1.422(6) . ?
C14 C15 1.415(7) . ?
C15 C16 1.375(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.397(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.361(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.545(7) . ?
C19 H19 0.9800 . ?
C20 C21 1.383(9) . ?
C21 C22 1.402(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.309(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.353(11) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.423(6) . ?
C25 C29 1.431(6) . ?
C25 C30 1.496(6) . ?
C26 C27 1.429(6) . ?
C26 C31 1.497(7) . ?
C27 C28 1.430(7) . ?
C27 C32 1.500(7) . ?
C28 C29 1.419(6) . ?
C28 C33 1.490(7) . ?
C29 C34 1.510(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C39 1.427(6) . ?
C35 C36 1.431(6) . ?
C35 C40 1.490(6) . ?
C36 C37 1.420(6) . ?
C36 C41 1.506(7) . ?
C37 C38 1.421(7) . ?
C37 C42 1.509(6) . ?
C38 C39 1.446(6) . ?
C38 C43 1.495(7) . ?
C39 C44 1.473(6) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 H46C 0.9700 . ?
C46 H46D 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
N3 Ni1 N1 86.31(18) . . ?
N3 Ni1 S1 175.01(13) . . ?
N1 Ni1 S1 88.79(14) . . ?
N3 Ni1 S2 88.77(13) . . ?
N1 Ni1 S2 174.98(14) . . ?
S1 Ni1 S2 96.15(5) . . ?
C36 Co1 C29 110.95(17) . . ?
C36 Co1 C37 40.64(18) . . ?
C29 Co1 C37 138.14(18) . . ?
C36 Co1 C25 138.30(18) . . ?
C29 Co1 C25 40.96(17) . . ?
C37 Co1 C25 178.85(18) . . ?
C36 Co1 C27 140.17(18) . . ?
C29 Co1 C27 68.44(18) . . ?
C37 Co1 C27 111.99(18) . . ?
C25 Co1 C27 68.58(18) . . ?
C36 Co1 C35 40.89(17) . . ?
C29 Co1 C35 111.71(17) . . ?
C37 Co1 C35 68.67(17) . . ?
C25 Co1 C35 110.77(17) . . ?
C27 Co1 C35 178.91(19) . . ?
C36 Co1 C26 178.80(17) . . ?
C29 Co1 C26 68.54(17) . . ?
C37 Co1 C26 140.44(18) . . ?
C25 Co1 C26 40.63(17) . . ?
C27 Co1 C26 40.82(18) . . ?
C35 Co1 C26 138.13(17) . . ?
C36 Co1 C38 68.29(18) . . ?
C29 Co1 C38 178.63(18) . . ?
C37 Co1 C38 40.56(18) . . ?
C25 Co1 C38 140.35(18) . . ?
C27 Co1 C38 111.34(18) . . ?
C35 Co1 C38 68.54(17) . . ?
C26 Co1 C38 112.25(18) . . ?
C36 Co1 C28 111.88(18) . . ?
C29 Co1 C28 40.43(18) . . ?
C37 Co1 C28 111.23(17) . . ?
C25 Co1 C28 68.49(17) . . ?
C27 Co1 C28 40.73(19) . . ?
C35 Co1 C28 140.04(18) . . ?
C26 Co1 C28 68.50(18) . . ?
C38 Co1 C28 138.56(18) . . ?
C36 Co1 C39 68.48(17) . . ?
C29 Co1 C39 139.96(18) . . ?
C37 Co1 C39 68.72(17) . . ?
C25 Co1 C39 111.57(17) . . ?
C27 Co1 C39 138.72(19) . . ?
C35 Co1 C39 40.51(18) . . ?
C26 Co1 C39 111.16(17) . . ?
C38 Co1 C39 41.05(18) . . ?
C28 Co1 C39 179.43(19) . . ?
C1 S1 Ni1 97.39(18) . . ?
C13 S2 Ni1 97.94(16) . . ?
C2 N1 C7 122.8(4) . . ?
C2 N1 Ni1 122.0(3) . . ?
C7 N1 Ni1 114.2(3) . . ?
C8 N2 C12 117.3(5) . . ?
C14 N3 C19 122.4(4) . . ?
C14 N3 Ni1 121.6(3) . . ?
C19 N3 Ni1 115.3(3) . . ?
C20 N4 C24 115.8(6) . . ?
C2 C1 C6 120.8(5) . . ?
C2 C1 S1 116.5(4) . . ?
C6 C1 S1 122.7(4) . . ?
N1 C2 C1 115.2(4) . . ?
N1 C2 C3 127.0(5) . . ?
C1 C2 C3 117.7(5) . . ?
C4 C3 C2 120.4(6) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.3(5) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 120.3(6) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 119.4(6) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
N1 C7 C19 106.6(4) . . ?
N1 C7 C8 112.3(4) . . ?
C19 C7 C8 111.3(4) . . ?
N1 C7 H7 108.9 . . ?
C19 C7 H7 108.9 . . ?
C8 C7 H7 108.9 . . ?
N2 C8 C9 122.7(6) . . ?
N2 C8 C7 113.0(4) . . ?
C9 C8 C7 124.3(4) . . ?
C8 C9 C10 121.0(6) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 115.2(7) . . ?
C11 C10 H10 122.4 . . ?
C9 C10 H10 122.4 . . ?
C12 C11 C10 124.9(7) . . ?
C12 C11 H11 117.6 . . ?
C10 C11 H11 117.6 . . ?
C11 C12 N2 118.9(6) . . ?
C11 C12 H12 120.6 . . ?
N2 C12 H12 120.6 . . ?
C18 C13 C14 119.5(4) . . ?
C18 C13 S2 124.3(4) . . ?
C14 C13 S2 116.2(4) . . ?
N3 C14 C15 126.4(4) . . ?
N3 C14 C13 115.4(4) . . ?
C15 C14 C13 118.2(4) . . ?
C16 C15 C14 120.1(4) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 121.8(5) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C18 C17 C16 119.3(5) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C13 121.1(4) . . ?
C17 C18 H18 119.4 . . ?
C13 C18 H18 119.4 . . ?
N3 C19 C7 105.9(4) . . ?
N3 C19 C20 112.8(4) . . ?
C7 C19 C20 111.7(4) . . ?
N3 C19 H19 108.8 . . ?
C7 C19 H19 108.8 . . ?
C20 C19 H19 108.8 . . ?
N4 C20 C21 122.7(5) . . ?
N4 C20 C19 115.1(5) . . ?
C21 C20 C19 122.3(5) . . ?
C20 C21 C22 118.4(6) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 H21 120.8 . . ?
C23 C22 C21 119.9(7) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 119.7(6) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 N4 123.4(6) . . ?
C23 C24 H24 118.3 . . ?
N4 C24 H24 118.3 . . ?
C26 C25 C29 107.9(4) . . ?
C26 C25 C30 126.4(4) . . ?
C29 C25 C30 125.6(4) . . ?
C26 C25 Co1 70.0(2) . . ?
C29 C25 Co1 69.5(2) . . ?
C30 C25 Co1 128.7(3) . . ?
C25 C26 C27 107.8(4) . . ?
C25 C26 C31 125.7(4) . . ?
C27 C26 C31 126.5(4) . . ?
C25 C26 Co1 69.4(2) . . ?
C27 C26 Co1 69.3(2) . . ?
C31 C26 Co1 128.1(3) . . ?
C26 C27 C28 108.2(4) . . ?
C26 C27 C32 124.5(5) . . ?
C28 C27 C32 127.3(5) . . ?
C26 C27 Co1 69.9(2) . . ?
C28 C27 Co1 70.3(2) . . ?
C32 C27 Co1 128.2(3) . . ?
C29 C28 C27 107.7(4) . . ?
C29 C28 C33 124.5(5) . . ?
C27 C28 C33 127.8(5) . . ?
C29 C28 Co1 69.1(2) . . ?
C27 C28 Co1 69.0(2) . . ?
C33 C28 Co1 128.7(3) . . ?
C28 C29 C25 108.4(4) . . ?
C28 C29 C34 126.8(4) . . ?
C25 C29 C34 124.8(4) . . ?
C28 C29 Co1 70.5(2) . . ?
C25 C29 Co1 69.5(2) . . ?
C34 C29 Co1 128.1(3) . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C32 H32A 109.5 . . ?
C27 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C27 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C34 H34A 109.5 . . ?
C29 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C29 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C39 C35 C36 108.1(4) . . ?
C39 C35 C40 125.9(4) . . ?
C36 C35 C40 125.9(4) . . ?
C39 C35 Co1 70.4(2) . . ?
C36 C35 Co1 69.2(2) . . ?
C40 C35 Co1 128.6(3) . . ?
C37 C36 C35 108.3(4) . . ?
C37 C36 C41 126.2(4) . . ?
C35 C36 C41 125.4(4) . . ?
C37 C36 Co1 69.7(2) . . ?
C35 C36 Co1 69.9(2) . . ?
C41 C36 Co1 127.8(3) . . ?
C36 C37 C38 108.1(4) . . ?
C36 C37 C42 125.6(4) . . ?
C38 C37 C42 126.3(4) . . ?
C36 C37 Co1 69.6(2) . . ?
C38 C37 Co1 70.1(2) . . ?
C42 C37 Co1 127.5(3) . . ?
C37 C38 C39 108.1(4) . . ?
C37 C38 C43 126.7(4) . . ?
C39 C38 C43 125.0(4) . . ?
C37 C38 Co1 69.3(2) . . ?
C39 C38 Co1 70.0(2) . . ?
C43 C38 Co1 129.1(3) . . ?
C35 C39 C38 107.2(4) . . ?
C35 C39 C44 126.5(4) . . ?
C38 C39 C44 126.3(4) . . ?
C35 C39 Co1 69.1(2) . . ?
C38 C39 Co1 69.0(2) . . ?
C44 C39 Co1 128.0(3) . . ?
C35 C40 H40A 109.5 . . ?
C35 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C35 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C36 C41 H41A 109.5 . . ?
C36 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C36 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Cl2 C45 Cl1 111.1(4) . . ?
Cl2 C45 H45A 109.4 . . ?
Cl1 C45 H45A 109.4 . . ?
Cl2 C45 H45B 109.4 . . ?
Cl1 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
Cl3B C46 Cl4B 110.7(3) . . ?
Cl3A C46 Cl4A 110.3(2) . . ?
Cl3A C46 H46A 109.6 . . ?
Cl4A C46 H46A 109.6 . . ?
Cl3A C46 H46B 109.6 . . ?
Cl4A C46 H46B 109.6 . . ?
H46A C46 H46B 108.1 . . ?
Cl3B C46 H46C 109.5 . . ?
Cl4B C46 H46C 109.5 . . ?
Cl3B C46 H46D 109.5 . . ?
Cl4B C46 H46D 109.5 . . ?
H46C C46 H46D 108.1 . . ?

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
N3 Ni1 N1 C2 179.6(3) . . . . ?
S1 Ni1 N1 C2 0.5(3) . . . . ?
N3 Ni1 N1 C7 -11.6(3) . . . . ?
S1 Ni1 N1 C7 169.3(3) . . . . ?
N1 Ni1 N3 C14 177.9(3) . . . . ?
S2 Ni1 N3 C14 -1.1(3) . . . . ?
N1 Ni1 N3 C19 -11.4(3) . . . . ?
S2 Ni1 N3 C19 169.6(3) . . . . ?
Ni1 S1 C1 C2 -3.0(3) . . . . ?
Ni1 S1 C1 C6 179.3(4) . . . . ?
C7 N1 C2 C1 -170.5(4) . . . . ?
Ni1 N1 C2 C1 -2.7(5) . . . . ?
C7 N1 C2 C3 9.1(7) . . . . ?
Ni1 N1 C2 C3 176.9(4) . . . . ?
C6 C1 C2 N1 -178.4(4) . . . . ?
S1 C1 C2 N1 3.8(5) . . . . ?
C6 C1 C2 C3 1.9(7) . . . . ?
S1 C1 C2 C3 -175.8(3) . . . . ?
N1 C2 C3 C4 178.5(5) . . . . ?
C1 C2 C3 C4 -1.9(7) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C3 C4 C5 C6 1.2(8) . . . . ?
C4 C5 C6 C1 -1.2(8) . . . . ?
C2 C1 C6 C5 -0.4(7) . . . . ?
S1 C1 C6 C5 177.2(4) . . . . ?
C2 N1 C7 C19 -161.7(4) . . . . ?
Ni1 N1 C7 C19 29.6(4) . . . . ?
C2 N1 C7 C8 76.2(5) . . . . ?
Ni1 N1 C7 C8 -92.5(4) . . . . ?
C12 N2 C8 C9 0.4(9) . . . . ?
C12 N2 C8 C7 -179.8(5) . . . . ?
N1 C7 C8 N2 177.8(5) . . . . ?
C19 C7 C8 N2 58.4(6) . . . . ?
N1 C7 C8 C9 -2.4(8) . . . . ?
C19 C7 C8 C9 -121.8(6) . . . . ?
N2 C8 C9 C10 -0.4(10) . . . . ?
C7 C8 C9 C10 179.8(6) . . . . ?
C8 C9 C10 C11 0.9(10) . . . . ?
C9 C10 C11 C12 -1.5(11) . . . . ?
C10 C11 C12 N2 1.6(11) . . . . ?
C8 N2 C12 C11 -0.9(9) . . . . ?
Ni1 S2 C13 C18 178.5(4) . . . . ?
Ni1 S2 C13 C14 -2.4(3) . . . . ?
C19 N3 C14 C15 9.1(7) . . . . ?
Ni1 N3 C14 C15 179.2(3) . . . . ?
C19 N3 C14 C13 -170.3(4) . . . . ?
Ni1 N3 C14 C13 -0.3(5) . . . . ?
C18 C13 C14 N3 -178.9(4) . . . . ?
S2 C13 C14 N3 2.0(5) . . . . ?
C18 C13 C14 C15 1.6(6) . . . . ?
S2 C13 C14 C15 -177.5(3) . . . . ?
N3 C14 C15 C16 178.0(4) . . . . ?
C13 C14 C15 C16 -2.6(6) . . . . ?
C14 C15 C16 C17 1.7(7) . . . . ?
C15 C16 C17 C18 0.3(7) . . . . ?
C16 C17 C18 C13 -1.3(7) . . . . ?
C14 C13 C18 C17 0.3(7) . . . . ?
S2 C13 C18 C17 179.3(4) . . . . ?
C14 N3 C19 C7 -160.0(4) . . . . ?
Ni1 N3 C19 C7 29.3(4) . . . . ?
C14 N3 C19 C20 77.5(5) . . . . ?
Ni1 N3 C19 C20 -93.2(4) . . . . ?
N1 C7 C19 N3 -35.7(4) . . . . ?
C8 C7 C19 N3 87.0(4) . . . . ?
N1 C7 C19 C20 87.5(4) . . . . ?
C8 C7 C19 C20 -149.8(4) . . . . ?
C24 N4 C20 C21 0.6(8) . . . . ?
C24 N4 C20 C19 -179.1(5) . . . . ?
N3 C19 C20 N4 174.8(4) . . . . ?
C7 C19 C20 N4 55.6(5) . . . . ?
N3 C19 C20 C21 -5.0(7) . . . . ?
C7 C19 C20 C21 -124.1(5) . . . . ?
N4 C20 C21 C22 -0.5(8) . . . . ?
C19 C20 C21 C22 179.3(5) . . . . ?
C20 C21 C22 C23 -0.3(8) . . . . ?
C21 C22 C23 C24 0.8(9) . . . . ?
C22 C23 C24 N4 -0.6(10) . . . . ?
C20 N4 C24 C23 -0.1(9) . . . . ?
C29 C25 C26 C27 0.5(5) . . . . ?
C30 C25 C26 C27 177.2(4) . . . . ?
Co1 C25 C26 C27 -58.9(3) . . . . ?
C29 C25 C26 C31 -177.9(4) . . . . ?
C30 C25 C26 C31 -1.2(7) . . . . ?
Co1 C25 C26 C31 122.8(4) . . . . ?
C29 C25 C26 Co1 59.4(3) . . . . ?
C30 C25 C26 Co1 -123.9(4) . . . . ?
C25 C26 C27 C28 -1.1(5) . . . . ?
C31 C26 C27 C28 177.2(4) . . . . ?
Co1 C26 C27 C28 -60.0(3) . . . . ?
C25 C26 C27 C32 -177.9(4) . . . . ?
C31 C26 C27 C32 0.4(7) . . . . ?
Co1 C26 C27 C32 123.2(4) . . . . ?
C25 C26 C27 Co1 58.9(3) . . . . ?
C31 C26 C27 Co1 -122.7(5) . . . . ?
C26 C27 C28 C29 1.3(5) . . . . ?
C32 C27 C28 C29 178.0(4) . . . . ?
Co1 C27 C28 C29 -58.5(3) . . . . ?
C26 C27 C28 C33 -176.9(4) . . . . ?
C32 C27 C28 C33 -0.2(7) . . . . ?
Co1 C27 C28 C33 123.4(5) . . . . ?
C26 C27 C28 Co1 59.8(3) . . . . ?
C32 C27 C28 Co1 -123.5(5) . . . . ?
C27 C28 C29 C25 -1.0(4) . . . . ?
C33 C28 C29 C25 177.2(4) . . . . ?
Co1 C28 C29 C25 -59.4(3) . . . . ?
C27 C28 C29 C34 -178.1(4) . . . . ?
C33 C28 C29 C34 0.1(7) . . . . ?
Co1 C28 C29 C34 123.5(4) . . . . ?
C27 C28 C29 Co1 58.4(3) . . . . ?
C33 C28 C29 Co1 -123.3(4) . . . . ?
C26 C25 C29 C28 0.3(4) . . . . ?
C30 C25 C29 C28 -176.4(4) . . . . ?
Co1 C25 C29 C28 60.0(3) . . . . ?
C26 C25 C29 C34 177.5(4) . . . . ?
C30 C25 C29 C34 0.7(7) . . . . ?
Co1 C25 C29 C34 -122.8(4) . . . . ?
C26 C25 C29 Co1 -59.7(3) . . . . ?
C30 C25 C29 Co1 123.6(4) . . . . ?
C39 C35 C36 C37 0.5(5) . . . . ?
C40 C35 C36 C37 177.4(4) . . . . ?
Co1 C35 C36 C37 -59.3(3) . . . . ?
C39 C35 C36 C41 -177.5(4) . . . . ?
C40 C35 C36 C41 -0.6(7) . . . . ?
Co1 C35 C36 C41 122.7(4) . . . . ?
C39 C35 C36 Co1 59.8(3) . . . . ?
C40 C35 C36 Co1 -123.3(4) . . . . ?
C35 C36 C37 C38 -0.3(5) . . . . ?
C41 C36 C37 C38 177.6(4) . . . . ?
Co1 C36 C37 C38 -59.7(3) . . . . ?
C35 C36 C37 C42 -178.4(4) . . . . ?
C41 C36 C37 C42 -0.5(7) . . . . ?
Co1 C36 C37 C42 122.2(4) . . . . ?
C35 C36 C37 Co1 59.4(3) . . . . ?
C41 C36 C37 Co1 -122.6(5) . . . . ?
C36 C37 C38 C39 0.0(5) . . . . ?
C42 C37 C38 C39 178.1(4) . . . . ?
Co1 C37 C38 C39 -59.4(3) . . . . ?
C36 C37 C38 C43 -176.5(4) . . . . ?
C42 C37 C38 C43 1.6(7) . . . . ?
Co1 C37 C38 C43 124.1(5) . . . . ?
C36 C37 C38 Co1 59.4(3) . . . . ?
C42 C37 C38 Co1 -122.5(4) . . . . ?
C36 C35 C39 C38 -0.5(4) . . . . ?
C40 C35 C39 C38 -177.3(4) . . . . ?
Co1 C35 C39 C38 58.6(3) . . . . ?
C36 C35 C39 C44 178.4(4) . . . . ?
C40 C35 C39 C44 1.5(7) . . . . ?
Co1 C35 C39 C44 -122.5(4) . . . . ?
C36 C35 C39 Co1 -59.1(3) . . . . ?
C40 C35 C39 Co1 124.0(4) . . . . ?
C37 C38 C39 C35 0.3(4) . . . . ?
C43 C38 C39 C35 176.9(4) . . . . ?
Co1 C38 C39 C35 -58.7(3) . . . . ?
C37 C38 C39 C44 -178.5(4) . . . . ?
C43 C38 C39 C44 -2.0(7) . . . . ?
Co1 C38 C39 C44 122.4(4) . . . . ?
C37 C38 C39 Co1 59.0(3) . . . . ?
C43 C38 C39 Co1 -124.4(4) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


