# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1826889'
_audit_update_record             
;
2018-03-01 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;

_audit_creation_date             2017-07-12T09:16:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C8 H6 N2 Ni S8'
_chemical_formula_moiety         'C8 H6 N2 Ni S8'
_chemical_formula_weight         445.34

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.0234(9)
_cell_length_b                   21.360(4)
_cell_length_c                   7.1729(14)
_cell_angle_alpha                90
_cell_angle_beta                 106.652(5)
_cell_angle_gamma                90
_cell_volume                     737.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    620
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      21.93
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             448

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_T_max  0.907

#-------------------------------- Remark --------------------------------------#
# SADABS output:                                                               #
# Estimated minimum and maximum transmission:  0.6402  0.7455                  #
# The ratio of these values is more reliable than their absolute values!       #
#------------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_ub_11      -0.003217
_diffrn_orient_matrix_ub_12      0.046257
_diffrn_orient_matrix_ub_13      -0.022041
_diffrn_orient_matrix_ub_21      -0.116892
_diffrn_orient_matrix_ub_22      0.005537
_diffrn_orient_matrix_ub_23      0.090617
_diffrn_orient_matrix_ub_31      0.171754
_diffrn_orient_matrix_ub_32      0.004635
_diffrn_orient_matrix_ub_33      0.111703
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.1273
_diffrn_reflns_number            4945
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.114
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             1690
_reflns_number_gt                965
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     'direct - structure invariant direct methods'
_atom_sites_solution_secondary   'direct - structure invariant direct methods'
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1690
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1165
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_restrained_S_all      0.97
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.127

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 1 0.5 0.5 0.0280(3) Uani 1 2 d S . P . .
S3 S 1.4771(3) 0.41920(7) 0.0757(2) 0.0351(4) Uani 1 1 d . . . . .
S2 S 1.1768(3) 0.51451(7) 0.2644(2) 0.0322(4) Uani 1 1 d . . . . .
S1 S 1.1127(3) 0.40202(7) 0.5314(2) 0.0326(4) Uani 1 1 d . . . . .
S4 S 1.6548(4) 0.28204(8) 0.0902(3) 0.0481(5) Uani 1 1 d . . . . .
N1 N 1.3949(9) 0.3364(2) 0.3201(6) 0.0270(11) Uani 1 1 d . . . . .
C1 C 1.2788(10) 0.3921(3) 0.3577(8) 0.0284(14) Uani 1 1 d . . . . .
C3 C 1.5007(11) 0.3440(3) 0.1788(9) 0.0334(15) Uani 1 1 d . . . . .
C2 C 1.3044(10) 0.4431(3) 0.2397(8) 0.0267(14) Uani 1 1 d . . . . .
C4 C 1.7635(13) 0.3184(3) -0.0971(9) 0.0489(18) Uani 1 1 d . . . . .
H4A H 1.6035 0.3308 -0.2 0.073 Uiso 1 1 calc R U . . .
H4B H 1.8723 0.2894 -0.147 0.073 Uiso 1 1 calc R U . . .
H4C H 1.8736 0.3545 -0.0461 0.073 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   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 S2 2.1449(14) 3_766 ?
Ni1 S2 2.1449(14) . ?
Ni1 S1 2.1630(15) . ?
Ni1 S1 2.1630(15) 3_766 ?
S3 C2 1.727(5) . ?
S3 C3 1.758(6) . ?
S2 C2 1.684(5) . ?
S1 C1 1.700(5) . ?
S4 C3 1.743(6) . ?
S4 C4 1.768(6) . ?
N1 C3 1.283(6) . ?
N1 C1 1.385(7) . ?
C1 C2 1.408(7) . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
C4 H4C 0.96 . ?

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
S2 Ni1 S2 180.00(3) 3_766 . ?
S2 Ni1 S1 86.18(5) 3_766 . ?
S2 Ni1 S1 93.82(5) . . ?
S2 Ni1 S1 93.82(5) 3_766 3_766 ?
S2 Ni1 S1 86.18(5) . 3_766 ?
S1 Ni1 S1 180 . 3_766 ?
C2 S3 C3 88.3(3) . . ?
C2 S2 Ni1 102.00(19) . . ?
C1 S1 Ni1 102.3(2) . . ?
C3 S4 C4 102.1(3) . . ?
C3 N1 C1 109.7(5) . . ?
N1 C1 C2 115.6(5) . . ?
N1 C1 S1 124.9(4) . . ?
C2 C1 S1 119.5(4) . . ?
N1 C3 S4 121.3(4) . . ?
N1 C3 S3 117.1(4) . . ?
S4 C3 S3 121.6(3) . . ?
C1 C2 S2 122.3(4) . . ?
C1 C2 S3 109.4(4) . . ?
S2 C2 S3 128.3(3) . . ?
S4 C4 H4A 109.5 . . ?
S4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 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
C3 N1 C1 C2 -0.8(7) . . . . ?
C3 N1 C1 S1 179.0(4) . . . . ?
Ni1 S1 C1 N1 179.4(4) . . . . ?
Ni1 S1 C1 C2 -0.8(5) . . . . ?
C1 N1 C3 S4 -178.1(4) . . . . ?
C1 N1 C3 S3 0.7(6) . . . . ?
C4 S4 C3 N1 -179.7(5) . . . . ?
C4 S4 C3 S3 1.6(5) . . . . ?
C2 S3 C3 N1 -0.3(5) . . . . ?
C2 S3 C3 S4 178.5(4) . . . . ?
N1 C1 C2 S2 -179.9(4) . . . . ?
S1 C1 C2 S2 0.3(7) . . . . ?
N1 C1 C2 S3 0.6(6) . . . . ?
S1 C1 C2 S3 -179.2(3) . . . . ?
Ni1 S2 C2 C1 0.4(5) . . . . ?
Ni1 S2 C2 S3 179.8(3) . . . . ?
C3 S3 C2 C1 -0.2(4) . . . . ?
C3 S3 C2 S2 -179.7(4) . . . . ?


# END of CIF
_chemical_name_common            '[Ni(MeS-tzdt)2]'
####################################################################### 
# 
# 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_ZJ29X1_2
_database_code_depnum_ccdc_archive 'CCDC 1826894'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H10 N2 Ni S8'
_chemical_formula_sum            'C10 H10 N2 Ni S8'
_chemical_formula_weight         473.39
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.6193(6)
_cell_length_b                   4.0075(4)
_cell_length_c                   15.4038(14)
_cell_angle_alpha                101.262(3)
_cell_angle_beta                 87.941(3)
_cell_angle_gamma                91.618(3)
_cell_volume                     400.39(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4642
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      27.46
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.015
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             240
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_T_max  0.967

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_av_r_equivalents  0.0316
_diffrn_reflns_av_uneti/neti     0.0157
_diffrn_reflns_number            4642
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         3.080
_diffrn_reflns_theta_max         27.462
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             1827
_reflns_number_gt                1700
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0442P)²+0.1038P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1827
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_restrained_S_all      1.288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.222

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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

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 1.0000 0.5000 0.5000 0.01105(12) Uani 1 2 d S . P . .
S2 S 0.72223(7) 0.75344(13) 0.49026(3) 0.01402(14) Uani 1 1 d . . . . .
S3 S 0.50884(7) 0.84181(13) 0.32306(3) 0.01363(14) Uani 1 1 d . . . . .
S1 S 1.04866(7) 0.36530(12) 0.35794(3) 0.01330(14) Uani 1 1 d . . . . .
S4 S 0.53561(8) 0.67303(13) 0.12198(3) 0.01701(14) Uani 1 1 d . . . . .
N1 N 0.8066(3) 0.5099(4) 0.23085(11) 0.0150(4) Uani 1 1 d . . . . .
C2 C 0.7000(3) 0.7051(5) 0.37966(13) 0.0118(4) Uani 1 1 d . . . . .
C1 C 0.8448(3) 0.5343(5) 0.31930(13) 0.0115(4) Uani 1 1 d . . . . .
C4 C 0.2920(3) 0.8635(6) 0.15624(14) 0.0185(4) Uani 1 1 d . . . . .
H4A H 0.2144 0.7224 0.1924 0.022 Uiso 1 1 calc R U . . .
H4B H 0.3127 1.0932 0.1929 0.022 Uiso 1 1 calc R U . . .
C3 C 0.6356(3) 0.6583(5) 0.22369(13) 0.0129(4) Uani 1 1 d . . . . .
C5 C 0.1743(4) 0.8887(6) 0.07497(15) 0.0254(5) Uani 1 1 d . . . . .
H5A H 0.2528 1.0246 0.0387 0.038 Uiso 1 1 calc R U . . .
H5B H 0.0450 0.9979 0.0936 0.038 Uiso 1 1 calc R U . . .
H5C H 0.1492 0.6600 0.0402 0.038 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              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 S2 2.1493(5) 2_766 ?
Ni1 S2 2.1493(5) . ?
Ni1 S1 2.1637(5) 2_766 ?
Ni1 S1 2.1637(5) . ?
S2 C2 1.688(2) . ?
S3 C2 1.722(2) . ?
S3 C3 1.758(2) . ?
S1 C1 1.703(2) . ?
S4 C3 1.734(2) . ?
S4 C4 1.820(2) . ?
N1 C3 1.312(3) . ?
N1 C1 1.379(3) . ?
C2 C1 1.406(3) . ?
C4 C5 1.519(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S2 180.0 2_766 . ?
S2 Ni1 S1 93.557(18) 2_766 2_766 ?
S2 Ni1 S1 86.443(18) . 2_766 ?
S2 Ni1 S1 86.443(18) 2_766 . ?
S2 Ni1 S1 93.557(18) . . ?
S1 Ni1 S1 180.0 2_766 . ?
C2 S2 Ni1 102.24(7) . . ?
C2 S3 C3 88.35(9) . . ?
C1 S1 Ni1 102.56(7) . . ?
C3 S4 C4 101.11(10) . . ?
C3 N1 C1 109.12(17) . . ?
C1 C2 S2 122.12(15) . . ?
C1 C2 S3 109.83(14) . . ?
S2 C2 S3 128.05(12) . . ?
N1 C1 C2 116.04(17) . . ?
N1 C1 S1 124.41(15) . . ?
C2 C1 S1 119.53(15) . . ?
C5 C4 S4 109.61(16) . . ?
C5 C4 H4A 109.7 . . ?
S4 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
S4 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N1 C3 S4 122.43(16) . . ?
N1 C3 S3 116.67(15) . . ?
S4 C3 S3 120.90(12) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 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
Ni1 S2 C2 C1 -0.35(17) . . . . ?
Ni1 S2 C2 S3 179.04(12) . . . . ?
C3 S3 C2 C1 0.41(15) . . . . ?
C3 S3 C2 S2 -179.04(15) . . . . ?
C3 N1 C1 C2 -0.2(2) . . . . ?
C3 N1 C1 S1 178.29(15) . . . . ?
S2 C2 C1 N1 179.26(14) . . . . ?
S3 C2 C1 N1 -0.2(2) . . . . ?
S2 C2 C1 S1 0.7(2) . . . . ?
S3 C2 C1 S1 -178.78(10) . . . . ?
Ni1 S1 C1 N1 -179.06(15) . . . . ?
Ni1 S1 C1 C2 -0.64(17) . . . . ?
C3 S4 C4 C5 -178.08(16) . . . . ?
C1 N1 C3 S4 -178.99(14) . . . . ?
C1 N1 C3 S3 0.5(2) . . . . ?
C4 S4 C3 N1 173.98(17) . . . . ?
C4 S4 C3 S3 -5.51(15) . . . . ?
C2 S3 C3 N1 -0.56(16) . . . . ?
C2 S3 C3 S4 178.96(13) . . . . ?

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR ZJ29X1_2                                               #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1826891'
_audit_update_record             
;
2018-03-01 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;

_audit_creation_date             2017-06-29T17:14:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            '	C32 H26 N2 Ni P S8'
_chemical_formula_moiety         'C24 H20 P, C8 H6 N2 Ni S8'

_chemical_formula_weight         784.69

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.777(3)
_cell_length_b                   7.5023(12)
_cell_length_c                   27.660(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.497(8)
_cell_angle_gamma                90
_cell_volume                     3354.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3979
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.25
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1612

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_T_max  0.977

#------------------------------- Remark -------------------------------------#
# SADABS output:                                                             #
# Estimated minimum and maximum transmission:  0.6229  0.7456                #
# The ratio of these values is more reliable than their absolute values!     #
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_ub_11      0.053412
_diffrn_orient_matrix_ub_12      -0.032786
_diffrn_orient_matrix_ub_13      -0.007264
_diffrn_orient_matrix_ub_21      -0.02708
_diffrn_orient_matrix_ub_22      -0.106504
_diffrn_orient_matrix_ub_23      -0.01929
_diffrn_orient_matrix_ub_31      -0.015492
_diffrn_orient_matrix_ub_32      0.073136
_diffrn_orient_matrix_ub_33      -0.031347
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_number            12617
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.996
_reflns_Friedel_coverage         0
_reflns_number_total             3860
_reflns_number_gt                2803
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0372P)²+2.5342P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3860
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0828
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.057

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 1.17392(18) 0.0000(3) 0.98923(9) 0.0477(6) Uani 1 1 d . . . . .
C2 C 1.12972(17) -0.0576(3) 0.94309(9) 0.0459(6) Uani 1 1 d . . . . .
C3 C 1.25286(19) -0.0695(3) 0.92977(9) 0.0511(7) Uani 1 1 d . . . . .
C4 C 1.4208(2) -0.0691(5) 0.94478(12) 0.0720(9) Uani 1 1 d . . . . .
H4A H 1.4259 0.0537 0.955 0.108 Uiso 1 1 calc R U . . .
H4B H 1.4669 -0.1017 0.9322 0.108 Uiso 1 1 calc R U . . .
H4C H 1.4202 -0.1428 0.9731 0.108 Uiso 1 1 calc R U . . .
C5 C 0.92015(13) -0.0338(3) 0.76015(8) 0.0325(5) Uani 1 1 d . . . . .
C6 C 0.88650(15) -0.1608(3) 0.72365(9) 0.0449(6) Uani 1 1 d . . . . .
H6 H 0.9046 -0.1685 0.6947 0.054 Uiso 1 1 calc R U . . .
C7 C 0.82642(17) -0.2744(4) 0.73077(11) 0.0572(7) Uani 1 1 d . . . . .
H7 H 0.8025 -0.3571 0.7061 0.069 Uiso 1 1 calc R U . . .
C8 C 0.80135(17) -0.2666(4) 0.77425(12) 0.0616(8) Uani 1 1 d . . . . .
H8 H 0.7615 -0.3459 0.7791 0.074 Uiso 1 1 calc R U . . .
C9 C 0.83467(17) -0.1430(4) 0.81037(10) 0.0566(7) Uani 1 1 d . . . . .
H9 H 0.8174 -0.1387 0.8396 0.068 Uiso 1 1 calc R U . . .
C10 C 0.89396(15) -0.0244(3) 0.80353(9) 0.0432(6) Uani 1 1 d . . . . .
H10 H 0.916 0.0609 0.8278 0.052 Uiso 1 1 calc R U . . .
C11 C 1.03905(14) 0.2526(3) 0.80254(7) 0.0327(5) Uani 1 1 d . . . . .
C12 C 0.98925(16) 0.3950(3) 0.80876(9) 0.0474(6) Uani 1 1 d . . . . .
H12 H 0.9368 0.4095 0.787 0.057 Uiso 1 1 calc R U . . .
C13 C 1.0182(2) 0.5137(3) 0.84723(10) 0.0564(7) Uani 1 1 d . . . . .
H13 H 0.9854 0.6092 0.8515 0.068 Uiso 1 1 calc R U . . .
C14 C 1.0955(2) 0.4918(3) 0.87933(10) 0.0566(8) Uani 1 1 d . . . . .
H14 H 1.1148 0.573 0.9052 0.068 Uiso 1 1 calc R U . . .
C15 C 1.14450(17) 0.3517(4) 0.87369(9) 0.0535(7) Uani 1 1 d . . . . .
H15 H 1.1966 0.3377 0.8958 0.064 Uiso 1 1 calc R U . . .
C16 C 1.11647(15) 0.2310(3) 0.83509(8) 0.0400(5) Uani 1 1 d . . . . .
H16 H 1.1497 0.1358 0.8311 0.048 Uiso 1 1 calc R U . . .
N1 N 1.17480(15) -0.0972(3) 0.90942(7) 0.0522(6) Uani 1 1 d . . . . .
S1 S 1.02382(5) -0.07833(10) 0.92977(2) 0.0564(2) Uani 1 1 d . . . . .
S2 S 1.12872(5) 0.05431(10) 1.03602(2) 0.0551(2) Uani 1 1 d . . . . .
S3 S 1.27770(5) 0.00736(10) 0.99153(3) 0.0595(2) Uani 1 1 d . . . . .
S4 S 1.32644(6) -0.09976(12) 0.89648(3) 0.0711(2) Uani 1 1 d . . . . .
Ni1 Ni 1 0 1 0.04475(15) Uani 1 2 d S . P . .
P1 P 1 0.10824(10) 0.75 0.03029(19) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   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
C1 C2 1.364(3) . ?
C1 S2 1.715(3) . ?
C1 S3 1.726(3) . ?
C2 N1 1.380(3) . ?
C2 S1 1.722(3) . ?
C3 N1 1.297(3) . ?
C3 S4 1.741(3) . ?
C3 S3 1.745(3) . ?
C4 S4 1.793(3) . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
C4 H4C 0.96 . ?
C5 C10 1.386(3) . ?
C5 C6 1.393(3) . ?
C5 P1 1.792(2) . ?
C6 C7 1.374(3) . ?
C6 H6 0.93 . ?
C7 C8 1.377(4) . ?
C7 H7 0.93 . ?
C8 C9 1.368(4) . ?
C8 H8 0.93 . ?
C9 C10 1.385(4) . ?
C9 H9 0.93 . ?
C10 H10 0.93 . ?
C11 C16 1.378(3) . ?
C11 C12 1.395(3) . ?
C11 P1 1.790(2) . ?
C12 C13 1.373(3) . ?
C12 H12 0.93 . ?
C13 C14 1.371(4) . ?
C13 H13 0.93 . ?
C14 C15 1.369(4) . ?
C14 H14 0.93 . ?
C15 C16 1.383(3) . ?
C15 H15 0.93 . ?
C16 H16 0.93 . ?
S1 Ni1 2.1665(7) . ?
S2 Ni1 2.1615(8) . ?
Ni1 S2 2.1615(8) 5_757 ?
Ni1 S1 2.1664(7) 5_757 ?
P1 C11 1.790(2) 2_756 ?
P1 C5 1.791(2) 2_756 ?

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
C2 C1 S2 122.8(2) . . ?
C2 C1 S3 109.6(2) . . ?
S2 C1 S3 127.57(15) . . ?
C1 C2 N1 116.2(3) . . ?
C1 C2 S1 120.1(2) . . ?
N1 C2 S1 123.79(19) . . ?
N1 C3 S4 121.7(2) . . ?
N1 C3 S3 115.3(2) . . ?
S4 C3 S3 122.91(18) . . ?
S4 C4 H4A 109.5 . . ?
S4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C10 C5 C6 120.1(2) . . ?
C10 C5 P1 121.92(18) . . ?
C6 C5 P1 117.92(17) . . ?
C7 C6 C5 119.4(2) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 120.3(2) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C5 119.4(2) . . ?
C9 C10 H10 120.3 . . ?
C5 C10 H10 120.3 . . ?
C16 C11 C12 120.0(2) . . ?
C16 C11 P1 122.42(17) . . ?
C12 C11 P1 117.52(17) . . ?
C13 C12 C11 119.5(2) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.7(2) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15 120 . . ?
C16 C15 H15 120 . . ?
C11 C16 C15 119.6(2) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C3 N1 C2 110.2(2) . . ?
C2 S1 Ni1 102.15(9) . . ?
C1 S2 Ni1 101.31(9) . . ?
C1 S3 C3 88.78(13) . . ?
C3 S4 C4 101.47(15) . . ?
S2 Ni1 S2 180 5_757 . ?
S2 Ni1 S1 93.64(3) 5_757 5_757 ?
S2 Ni1 S1 86.36(3) . 5_757 ?
S2 Ni1 S1 86.36(3) 5_757 . ?
S2 Ni1 S1 93.64(3) . . ?
S1 Ni1 S1 180 5_757 . ?
C11 P1 C11 105.57(14) . 2_756 ?
C11 P1 C5 111.10(10) . 2_756 ?
C11 P1 C5 111.06(10) 2_756 2_756 ?
C11 P1 C5 111.06(10) . . ?
C11 P1 C5 111.10(10) 2_756 . ?
C5 P1 C5 107.02(14) 2_756 . ?

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
S2 C1 C2 N1 -179.64(18) . . . . ?
S3 C1 C2 N1 0.4(3) . . . . ?
S2 C1 C2 S1 0.0(3) . . . . ?
S3 C1 C2 S1 180.00(13) . . . . ?
C10 C5 C6 C7 1.0(4) . . . . ?
P1 C5 C6 C7 178.6(2) . . . . ?
C5 C6 C7 C8 -1.9(4) . . . . ?
C6 C7 C8 C9 1.5(4) . . . . ?
C7 C8 C9 C10 0.0(4) . . . . ?
C8 C9 C10 C5 -1.0(4) . . . . ?
C6 C5 C10 C9 0.5(3) . . . . ?
P1 C5 C10 C9 -177.04(19) . . . . ?
C16 C11 C12 C13 0.5(4) . . . . ?
P1 C11 C12 C13 -177.1(2) . . . . ?
C11 C12 C13 C14 -0.2(4) . . . . ?
C12 C13 C14 C15 -0.3(4) . . . . ?
C13 C14 C15 C16 0.4(4) . . . . ?
C12 C11 C16 C15 -0.3(4) . . . . ?
P1 C11 C16 C15 177.15(19) . . . . ?
C14 C15 C16 C11 -0.1(4) . . . . ?
S4 C3 N1 C2 -177.83(17) . . . . ?
S3 C3 N1 C2 -0.1(3) . . . . ?
C1 C2 N1 C3 -0.2(3) . . . . ?
S1 C2 N1 C3 -179.81(19) . . . . ?
C1 C2 S1 Ni1 -1.0(2) . . . . ?
N1 C2 S1 Ni1 178.61(18) . . . . ?
C2 C1 S2 Ni1 1.0(2) . . . . ?
S3 C1 S2 Ni1 -179.00(15) . . . . ?
C2 C1 S3 C3 -0.31(19) . . . . ?
S2 C1 S3 C3 179.67(19) . . . . ?
N1 C3 S3 C1 0.2(2) . . . . ?
S4 C3 S3 C1 177.96(18) . . . . ?
N1 C3 S4 C4 -173.4(2) . . . . ?
S3 C3 S4 C4 9.0(2) . . . . ?
C16 C11 P1 C11 -131.1(2) . . . 2_756 ?
C12 C11 P1 C11 46.45(16) . . . 2_756 ?
C16 C11 P1 C5 -10.6(2) . . . 2_756 ?
C12 C11 P1 C5 166.94(18) . . . 2_756 ?
C16 C11 P1 C5 108.4(2) . . . . ?
C12 C11 P1 C5 -74.1(2) . . . . ?
C10 C5 P1 C11 1.0(2) . . . . ?
C6 C5 P1 C11 -176.63(17) . . . . ?
C10 C5 P1 C11 -116.23(19) . . . 2_756 ?
C6 C5 P1 C11 66.2(2) . . . 2_756 ?
C10 C5 P1 C5 122.4(2) . . . 2_756 ?
C6 C5 P1 C5 -55.21(16) . . . 2_756 ?


# END of CIF
_chemical_name_common            'PPh4+, [Ni(MeS-tzdt)2]-'
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1826892'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;

_audit_creation_date             2018-03-21T16:01:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C45 H46 N2 Ni P S8'
_chemical_formula_moiety         'C14 H18 N2 Ni S8, C24 H20 P, C7 H8'
_chemical_formula_weight         961

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.0877(11)
_cell_length_b                   7.5048(3)
_cell_length_c                   24.9380(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.474(2)
_cell_angle_gamma                90
_cell_volume                     4478.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3342
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      24.36
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.02

_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2004

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_T_max  0.983

#------------------------------- Remark -------------------------------------#
# SADABS output:                                                             #
# Estimated minimum and maximum transmission:  0.6692  0.7456             #
# The ratio of these values is more reliable than their absolute values!     #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_ub_11      0.012014
_diffrn_orient_matrix_ub_12      -0.121227
_diffrn_orient_matrix_ub_13      -0.007
_diffrn_orient_matrix_ub_21      -0.039828
_diffrn_orient_matrix_ub_22      -0.032064
_diffrn_orient_matrix_ub_23      -0.023971
_diffrn_orient_matrix_ub_31      0.003981
_diffrn_orient_matrix_ub_32      0.045066
_diffrn_orient_matrix_ub_33      -0.035884
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_number            13916
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.081
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_Friedel_coverage         0
_reflns_number_total             5122
_reflns_number_gt                3447
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0594P)²+7.3825P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5122
_refine_ls_number_parameters     282
_refine_ls_number_restraints     57
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1361
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.072

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.89285(13) 0.2030(4) 0.42550(13) 0.0333(7) Uani 1 1 d . . . . .
C2 C 0.93539(13) 0.3164(4) 0.43101(13) 0.0348(7) Uani 1 1 d . . . . .
C3 C 0.84203(14) 0.4268(5) 0.36330(14) 0.0433(8) Uani 1 1 d . . . . .
C4 C 0.78606(14) 0.1758(5) 0.38559(15) 0.0460(9) Uani 1 1 d . . . . .
C5 C 0.73217(17) 0.2764(7) 0.3493(2) 0.0883(17) Uani 1 1 d . . . . .
H5A H 0.7323 0.3902 0.3669 0.133 Uiso 1 1 calc R U . . .
H5B H 0.7005 0.2085 0.3481 0.133 Uiso 1 1 calc R U . . .
H5C H 0.73 0.2932 0.3103 0.133 Uiso 1 1 calc R U . . .
C6 C 0.78990(17) 0.1578(7) 0.44820(17) 0.0652(12) Uani 1 1 d . . . . .
H6A H 0.8199 0.0783 0.4697 0.098 Uiso 1 1 calc R U . . .
H6B H 0.7554 0.111 0.4475 0.098 Uiso 1 1 calc R U . . .
H6C H 0.7968 0.2727 0.4667 0.098 Uiso 1 1 calc R U . . .
C7 C 0.78201(17) -0.0055(6) 0.35615(18) 0.0591(11) Uani 1 1 d . . . . .
H7A H 0.7759 0.0117 0.3159 0.089 Uiso 1 1 calc R U . . .
H7B H 0.7514 -0.0717 0.3583 0.089 Uiso 1 1 calc R U . . .
H7C H 0.8162 -0.0702 0.3757 0.089 Uiso 1 1 calc R U . . .
C8 C 0.95317(13) 0.2736(5) 0.26677(14) 0.0354(7) Uani 1 1 d . . . . .
C9 C 0.89625(14) 0.2910(5) 0.23969(16) 0.0472(9) Uani 1 1 d . . . . .
H9 H 0.8805 0.3832 0.2133 0.057 Uiso 1 1 calc R U . . .
C10 C 0.86244(17) 0.1694(6) 0.25219(19) 0.0625(12) Uani 1 1 d . . . . .
H10 H 0.8238 0.1793 0.2336 0.075 Uiso 1 1 calc R U . . .
C11 C 0.88554(19) 0.0350(6) 0.29158(19) 0.0606(12) Uani 1 1 d . . . . .
H11 H 0.8625 -0.0464 0.2994 0.073 Uiso 1 1 calc R U . . .
C12 C 0.94191(19) 0.0202(5) 0.31924(18) 0.0541(10) Uani 1 1 d . . . . .
H12 H 0.9573 -0.0698 0.3466 0.065 Uiso 1 1 calc R U . . .
C13 C 0.97630(16) 0.1367(5) 0.30720(15) 0.0453(9) Uani 1 1 d . . . . .
H13 H 1.0149 0.1248 0.3259 0.054 Uiso 1 1 calc R U . . .
C14 C 1.03755(13) 0.5614(5) 0.30998(13) 0.0322(7) Uani 1 1 d . . . . .
C15 C 1.03537(15) 0.5427(5) 0.36400(14) 0.0431(9) Uani 1 1 d . . . . .
H15 H 1.0163 0.447 0.3711 0.052 Uiso 1 1 calc R U . . .
C16 C 1.06133(17) 0.6651(6) 0.40742(16) 0.0581(11) Uani 1 1 d . . . . .
H16 H 1.0593 0.6528 0.4437 0.07 Uiso 1 1 calc R U . . .
C17 C 1.09017(16) 0.8054(6) 0.39749(16) 0.0553(10) Uani 1 1 d . . . . .
H17 H 1.1073 0.8887 0.4268 0.066 Uiso 1 1 calc R U . . .
C18 C 1.09370(15) 0.8227(5) 0.34429(16) 0.0488(9) Uani 1 1 d . . . . .
H18 H 1.1141 0.916 0.338 0.059 Uiso 1 1 calc R U . . .
C19 C 1.06719(14) 0.7026(5) 0.30036(14) 0.0420(8) Uani 1 1 d . . . . .
H19 H 1.0691 0.716 0.2641 0.05 Uiso 1 1 calc R U . . .
C20 C 0.7530(5) 0.6868(15) 0.4622(6) 0.127(2) Uani 0.5 1 d G U P A -1
H20 H 0.7791 0.6375 0.4498 0.153 Uiso 0.5 1 calc R U P A -1
C21 C 0.6981(5) 0.7113(14) 0.4226(4) 0.125(2) Uani 0.5 1 d G U P A -1
H21 H 0.6875 0.6783 0.3837 0.151 Uiso 0.5 1 calc R U P A -1
C22 C 0.6591(4) 0.7850(17) 0.4412(5) 0.126(3) Uani 0.5 1 d G U P A -1
H22 H 0.6224 0.8014 0.4147 0.151 Uiso 0.5 1 calc R U P A -1
C23 C 0.6750(4) 0.8343(13) 0.4994(5) 0.120(2) Uani 0.5 1 d G U P A -1
H23 H 0.6489 0.8836 0.5118 0.144 Uiso 0.5 1 calc R U P A -1
C24 C 0.7298(5) 0.8098(14) 0.5389(4) 0.125(2) Uani 0.5 1 d G U P A -1
H24 H 0.7405 0.8428 0.5778 0.15 Uiso 0.5 1 calc R U P A -1
C25 C 0.7689(4) 0.7361(18) 0.5204(5) 0.130(2) Uani 0.5 1 d G U P A -1
C26 C 0.8302(7) 0.728(3) 0.5570(8) 0.148(4) Uani 0.5 1 d . U P A -1
H26A H 0.8488 0.6717 0.5352 0.223 Uiso 0.5 1 calc R U P A -1
H26B H 0.8444 0.8466 0.5675 0.223 Uiso 0.5 1 calc R U P A -1
H26C H 0.8366 0.6606 0.5918 0.223 Uiso 0.5 1 calc R U P A -1
N1 N 0.83907(10) 0.2693(4) 0.38914(11) 0.0367(6) Uani 1 1 d . . . . .
S1 S 0.90979(3) -0.00468(12) 0.45790(4) 0.0386(2) Uani 1 1 d . . . . .
S2 S 1.00432(3) 0.26758(12) 0.47095(4) 0.0386(2) Uani 1 1 d . . . . .
S3 S 0.90999(4) 0.50618(13) 0.38988(4) 0.0464(2) Uani 1 1 d . . . . .
S4 S 0.79524(5) 0.55212(18) 0.31119(5) 0.0720(4) Uani 1 1 d . . . . .
Ni Ni 1 0 0.5 0.02998(16) Uani 1 2 d S . P . .
P1 P 1 0.41658(17) 0.25 0.0308(3) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   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
C1 C2 1.361(5) . ?
C1 N1 1.423(4) . ?
C1 S1 1.730(3) . ?
C2 S2 1.713(3) . ?
C2 S3 1.726(3) . ?
C3 N1 1.363(5) . ?
C3 S4 1.673(4) . ?
C3 S3 1.733(4) . ?
C4 N1 1.521(4) . ?
C4 C7 1.529(5) . ?
C4 C6 1.530(5) . ?
C4 C5 1.533(5) . ?
C5 H5A 0.96 . ?
C5 H5B 0.96 . ?
C5 H5C 0.96 . ?
C6 H6A 0.96 . ?
C6 H6B 0.96 . ?
C6 H6C 0.96 . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
C8 C9 1.371(5) . ?
C8 C13 1.397(5) . ?
C8 P1 1.796(3) . ?
C9 C10 1.388(5) . ?
C9 H9 0.93 . ?
C10 C11 1.369(6) . ?
C10 H10 0.93 . ?
C11 C12 1.357(6) . ?
C11 H11 0.93 . ?
C12 C13 1.369(5) . ?
C12 H12 0.93 . ?
C13 H13 0.93 . ?
C14 C15 1.378(4) . ?
C14 C19 1.388(5) . ?
C14 P1 1.792(3) . ?
C15 C16 1.375(5) . ?
C15 H15 0.93 . ?
C16 C17 1.373(6) . ?
C16 H16 0.93 . ?
C17 C18 1.372(5) . ?
C17 H17 0.93 . ?
C18 C19 1.373(5) . ?
C18 H18 0.93 . ?
C19 H19 0.93 . ?
C20 C21 1.39 . ?
C20 C25 1.39 . ?
C20 H20 0.93 . ?
C21 C22 1.39 . ?
C21 H21 0.93 . ?
C22 C23 1.39 . ?
C22 H22 0.93 . ?
C23 C24 1.39 . ?
C23 H23 0.93 . ?
C24 C25 1.39 . ?
C24 H24 0.93 . ?
C25 C26 1.494(15) . ?
C26 H26A 0.96 . ?
C26 H26B 0.96 . ?
C26 H26C 0.96 . ?
S1 Ni 2.1619(8) . ?
S2 Ni 2.1530(8) . ?
Ni S2 2.1530(9) 5_756 ?
Ni S1 2.1619(8) 5_756 ?
P1 C14 1.792(3) 2_755 ?
P1 C8 1.796(3) 2_755 ?

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
C2 C1 N1 113.8(3) . . ?
C2 C1 S1 118.0(2) . . ?
N1 C1 S1 128.0(3) . . ?
C1 C2 S2 123.4(2) . . ?
C1 C2 S3 110.6(2) . . ?
S2 C2 S3 126.0(2) . . ?
N1 C3 S4 133.9(3) . . ?
N1 C3 S3 111.1(2) . . ?
S4 C3 S3 115.0(2) . . ?
N1 C4 C7 109.0(3) . . ?
N1 C4 C6 107.0(3) . . ?
C7 C4 C6 112.0(4) . . ?
N1 C4 C5 114.0(3) . . ?
C7 C4 C5 106.4(3) . . ?
C6 C4 C5 108.5(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 119.9(3) . . ?
C9 C8 P1 122.1(3) . . ?
C13 C8 P1 118.0(3) . . ?
C8 C9 C10 119.1(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 120.5(4) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.5(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 119.7(4) . . ?
C12 C13 H13 120.2 . . ?
C8 C13 H13 120.2 . . ?
C15 C14 C19 119.3(3) . . ?
C15 C14 P1 122.2(3) . . ?
C19 C14 P1 118.4(2) . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17 120 . . ?
C16 C17 H17 120 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 120.1(3) . . ?
C18 C19 H19 120 . . ?
C14 C19 H19 120 . . ?
C21 C20 C25 120 . . ?
C21 C20 H20 120 . . ?
C25 C20 H20 120 . . ?
C20 C21 C22 120 . . ?
C20 C21 H21 120 . . ?
C22 C21 H21 120 . . ?
C23 C22 C21 120 . . ?
C23 C22 H22 120 . . ?
C21 C22 H22 120 . . ?
C24 C23 C22 120 . . ?
C24 C23 H23 120 . . ?
C22 C23 H23 120 . . ?
C25 C24 C23 120 . . ?
C25 C24 H24 120 . . ?
C23 C24 H24 120 . . ?
C24 C25 C20 120 . . ?
C24 C25 C26 124.1(10) . . ?
C20 C25 C26 115.4(10) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 N1 C1 112.2(3) . . ?
C3 N1 C4 126.4(3) . . ?
C1 N1 C4 121.2(3) . . ?
C1 S1 Ni 103.78(11) . . ?
C2 S2 Ni 102.22(12) . . ?
C2 S3 C3 92.03(17) . . ?
S2 Ni S2 180 . 5_756 ?
S2 Ni S1 87.45(3) . 5_756 ?
S2 Ni S1 92.56(3) 5_756 5_756 ?
S2 Ni S1 92.55(3) . . ?
S2 Ni S1 87.45(3) 5_756 . ?
S1 Ni S1 180 5_756 . ?
C14 P1 C14 105.3(2) 2_755 . ?
C14 P1 C8 111.11(14) 2_755 . ?
C14 P1 C8 111.37(14) . . ?
C14 P1 C8 111.37(14) 2_755 2_755 ?
C14 P1 C8 111.11(14) . 2_755 ?
C8 P1 C8 106.6(2) . 2_755 ?

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 C1 C2 S2 -178.6(2) . . . . ?
S1 C1 C2 S2 -3.0(4) . . . . ?
N1 C1 C2 S3 -1.4(4) . . . . ?
S1 C1 C2 S3 174.18(16) . . . . ?
C13 C8 C9 C10 -1.3(5) . . . . ?
P1 C8 C9 C10 176.2(3) . . . . ?
C8 C9 C10 C11 0.8(6) . . . . ?
C9 C10 C11 C12 0.5(6) . . . . ?
C10 C11 C12 C13 -1.4(6) . . . . ?
C11 C12 C13 C8 1.0(6) . . . . ?
C9 C8 C13 C12 0.4(5) . . . . ?
P1 C8 C13 C12 -177.2(3) . . . . ?
C19 C14 C15 C16 1.4(5) . . . . ?
P1 C14 C15 C16 -174.9(3) . . . . ?
C14 C15 C16 C17 -0.8(6) . . . . ?
C15 C16 C17 C18 -0.7(7) . . . . ?
C16 C17 C18 C19 1.7(6) . . . . ?
C17 C18 C19 C14 -1.2(6) . . . . ?
C15 C14 C19 C18 -0.4(5) . . . . ?
P1 C14 C19 C18 176.1(3) . . . . ?
C25 C20 C21 C22 0 . . . . ?
C20 C21 C22 C23 0 . . . . ?
C21 C22 C23 C24 0 . . . . ?
C22 C23 C24 C25 0 . . . . ?
C23 C24 C25 C20 0 . . . . ?
C23 C24 C25 C26 171.0(18) . . . . ?
C21 C20 C25 C24 0 . . . . ?
C21 C20 C25 C26 -171.7(17) . . . . ?
S4 C3 N1 C1 170.9(3) . . . . ?
S3 C3 N1 C1 -6.8(3) . . . . ?
S4 C3 N1 C4 -14.0(5) . . . . ?
S3 C3 N1 C4 168.3(2) . . . . ?
C2 C1 N1 C3 5.4(4) . . . . ?
S1 C1 N1 C3 -169.7(2) . . . . ?
C2 C1 N1 C4 -170.0(3) . . . . ?
S1 C1 N1 C4 15.0(4) . . . . ?
C7 C4 N1 C3 118.0(4) . . . . ?
C6 C4 N1 C3 -120.6(4) . . . . ?
C5 C4 N1 C3 -0.7(5) . . . . ?
C7 C4 N1 C1 -67.3(4) . . . . ?
C6 C4 N1 C1 54.0(4) . . . . ?
C5 C4 N1 C1 174.0(3) . . . . ?
C2 C1 S1 Ni 1.4(3) . . . . ?
N1 C1 S1 Ni 176.3(2) . . . . ?
C1 C2 S2 Ni 2.8(3) . . . . ?
S3 C2 S2 Ni -173.91(19) . . . . ?
C1 C2 S3 C3 -2.1(3) . . . . ?
S2 C2 S3 C3 175.0(2) . . . . ?
N1 C3 S3 C2 5.1(3) . . . . ?
S4 C3 S3 C2 -173.0(2) . . . . ?
C15 C14 P1 C14 129.1(3) . . . 2_755 ?
C19 C14 P1 C14 -47.2(2) . . . 2_755 ?
C15 C14 P1 C8 8.6(3) . . . . ?
C19 C14 P1 C8 -167.8(3) . . . . ?
C15 C14 P1 C8 -110.1(3) . . . 2_755 ?
C19 C14 P1 C8 73.5(3) . . . 2_755 ?
C9 C8 P1 C14 -6.0(3) . . . 2_755 ?
C13 C8 P1 C14 171.6(3) . . . 2_755 ?
C9 C8 P1 C14 111.1(3) . . . . ?
C13 C8 P1 C14 -71.4(3) . . . . ?
C9 C8 P1 C8 -127.5(3) . . . 2_755 ?
C13 C8 P1 C8 50.0(2) . . . 2_755 ?

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1826890'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;

_audit_creation_date             2018-03-21T14:20:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C38 H38 N2 Ni P S8'
_chemical_formula_moiety         'C14 H18 N2 Ni S8, C24 H20 P'
_chemical_formula_weight         868.86

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.7636(17)
_cell_length_b                   7.3314(5)
_cell_length_c                   23.4795(14)
_cell_angle_alpha                90
_cell_angle_beta                 124.372(4)
_cell_angle_gamma                90
_cell_volume                     4086.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3256
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      26.03
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1804

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_T_max  0.972

#------------------------------- Remark -------------------------------------#
# SADABS output:                                                             #
# Estimated minimum and maximum transmission:  0.6047  0.7461                #
# The ratio of these values is more reliable than their absolute values!     #
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_ub_11      0.028436
_diffrn_orient_matrix_ub_12      0.100056
_diffrn_orient_matrix_ub_13      0.023005
_diffrn_orient_matrix_ub_21      0.014776
_diffrn_orient_matrix_ub_22      -0.030788
_diffrn_orient_matrix_ub_23      -0.028489
_diffrn_orient_matrix_ub_31      -0.027336
_diffrn_orient_matrix_ub_32      0.08744
_diffrn_orient_matrix_ub_33      -0.036355
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_number            17557
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.837
_diffrn_reflns_theta_max         30.511
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_reflns_Friedel_coverage         0
_reflns_number_total             6172
_reflns_number_gt                3812
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     'direct - structure invariant direct methods'
_atom_sites_solution_secondary   'direct - structure invariant direct methods'
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1035P)²+9.1133P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6172
_refine_ls_number_parameters     251
_refine_ls_number_restraints     40
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.066
_refine_ls_wR_factor_ref         0.2128
_refine_ls_wR_factor_gt          0.1804
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.096

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.81092(15) 0.0699(5) 0.4900(2) 0.0430(8) Uani 1 1 d . . . . .
C2 C 0.81039(15) -0.0471(6) 0.4446(2) 0.0427(8) Uani 1 1 d . . . . .
C4 C 0.8426(3) -0.0694(12) 0.3597(3) 0.0968(14) Uani 1 1 d . U . . .
C5 C 0.7960(4) -0.1888(15) 0.3176(4) 0.1269(19) Uani 1 1 d . U . . .
H5A H 0.7876 -0.1925 0.2719 0.19 Uiso 1 1 calc R U . . .
H5B H 0.7636 -0.145 0.3157 0.19 Uiso 1 1 calc R U . . .
H5C H 0.8053 -0.3092 0.3371 0.19 Uiso 1 1 calc R U . . .
C6 C 0.8446(4) 0.0826(14) 0.3157(4) 0.127(2) Uani 1 1 d . U . . .
H6A H 0.8376 0.031 0.2739 0.191 Uiso 1 1 calc R U . . .
H6B H 0.8811 0.1389 0.3413 0.191 Uiso 1 1 calc R U . . .
H6C H 0.8164 0.1724 0.3046 0.191 Uiso 1 1 calc R U . . .
C7 C 0.8993(4) -0.1655(13) 0.3915(4) 0.1116(17) Uani 1 1 d . U . . .
H7A H 0.929 -0.0873 0.4253 0.167 Uiso 1 1 calc R U . . .
H7B H 0.9052 -0.193 0.356 0.167 Uiso 1 1 calc R U . . .
H7C H 0.8994 -0.2766 0.4132 0.167 Uiso 1 1 calc R U . . .
C8 C 0.97106(15) -0.0208(5) 0.67618(18) 0.0380(7) Uani 1 1 d . . . . .
C9 C 0.93384(18) -0.1576(6) 0.6673(2) 0.0479(9) Uani 1 1 d . . . . .
H9 H 0.9232 -0.167 0.698 0.057 Uiso 1 1 calc R U . . .
C10 C 0.9126(2) -0.2800(6) 0.6127(2) 0.0544(11) Uani 1 1 d . . . . .
H10 H 0.8871 -0.3694 0.6063 0.065 Uiso 1 1 calc R U . . .
C11 C 0.9292(2) -0.2684(6) 0.5686(2) 0.0568(11) Uani 1 1 d . . . . .
H11 H 0.9155 -0.3516 0.5327 0.068 Uiso 1 1 calc R U . . .
C12 C 0.9668(2) -0.1324(8) 0.5773(2) 0.0633(13) Uani 1 1 d . . . . .
H12 H 0.9778 -0.1246 0.547 0.076 Uiso 1 1 calc R U . . .
C13 C 0.98747(18) -0.0091(6) 0.6313(2) 0.0513(10) Uani 1 1 d . . . . .
H13 H 1.0124 0.0816 0.6372 0.062 Uiso 1 1 calc R U . . .
C14 C 1.05352(15) 0.2726(5) 0.75764(19) 0.0372(7) Uani 1 1 d . . . . .
C15 C 1.03754(18) 0.4096(6) 0.7088(2) 0.0484(9) Uani 1 1 d . . . . .
H15 H 0.9999 0.4225 0.6725 0.058 Uiso 1 1 calc R U . . .
C16 C 1.0781(2) 0.5272(6) 0.7147(3) 0.0568(11) Uani 1 1 d . . . . .
H16 H 1.0678 0.6166 0.6815 0.068 Uiso 1 1 calc R U . . .
C17 C 1.1328(2) 0.5113(7) 0.7689(3) 0.0604(12) Uani 1 1 d . . . . .
H17 H 1.1594 0.5923 0.7731 0.073 Uiso 1 1 calc R U . . .
C18 C 1.14924(18) 0.3777(7) 0.8176(3) 0.0612(12) Uani 1 1 d . . . . .
H18 H 1.1868 0.3685 0.8543 0.073 Uiso 1 1 calc R U . . .
C19 C 1.10963(17) 0.2553(6) 0.8122(2) 0.0478(9) Uani 1 1 d . . . . .
H19 H 1.1208 0.1635 0.8448 0.057 Uiso 1 1 calc R U . . .
N1 N 0.84187(14) 0.0196(5) 0.41825(19) 0.0496(8) Uani 1 1 d D . . . .
P1 P 1 0.12661(18) 0.75 0.0345(3) Uani 1 2 d S T P . .
S1 S 0.77890(4) 0.02509(13) 0.53189(6) 0.0441(3) Uani 1 1 d . . . . .
S2 S 0.77802(5) -0.25691(14) 0.43133(6) 0.0467(3) Uani 1 1 d . . . . .
S3 S 0.85224(6) 0.25992(15) 0.50473(9) 0.0646(4) Uani 1 1 d D . . . .
Ni1 Ni 0.75 -0.25 0.5 0.03501(19) Uani 1 2 d S . P . .
C3 C 0.8729(4) 0.1757(10) 0.4534(5) 0.054(2) Uani 0.750(18) 1 d D U P A 1
S4 S 0.9242(2) 0.2935(4) 0.4555(3) 0.0781(14) Uani 0.750(18) 1 d D U P A 1
C3B C 0.8626(8) 0.1902(16) 0.4437(8) 0.082(12) Uani 0.250(18) 1 d D U P A 2
S4B S 0.8948(16) 0.3014(18) 0.414(2) 0.133(7) Uani 0.250(18) 1 d D U P A 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
C1 C2 1.362(6) . ?
C1 S1 1.717(4) . ?
C1 S3 1.734(4) . ?
C2 N1 1.440(5) . ?
C2 S2 1.733(4) . ?
C4 C5 1.431(10) . ?
C4 C7 1.529(11) . ?
C4 N1 1.533(7) . ?
C4 C6 1.542(10) . ?
C5 H5A 0.96 . ?
C5 H5B 0.96 . ?
C5 H5C 0.96 . ?
C6 H6A 0.96 . ?
C6 H6B 0.96 . ?
C6 H6C 0.96 . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
C8 C13 1.380(5) . ?
C8 C9 1.394(5) . ?
C8 P1 1.799(4) . ?
C9 C10 1.392(6) . ?
C9 H9 0.93 . ?
C10 C11 1.368(7) . ?
C10 H10 0.93 . ?
C11 C12 1.398(7) . ?
C11 H11 0.93 . ?
C12 C13 1.388(6) . ?
C12 H12 0.93 . ?
C13 H13 0.93 . ?
C14 C19 1.388(5) . ?
C14 C15 1.392(5) . ?
C14 P1 1.799(4) . ?
C15 C16 1.394(6) . ?
C15 H15 0.93 . ?
C16 C17 1.359(7) . ?
C16 H16 0.93 . ?
C17 C18 1.370(7) . ?
C17 H17 0.93 . ?
C18 C19 1.399(6) . ?
C18 H18 0.93 . ?
C19 H19 0.93 . ?
N1 C3B 1.369(10) . ?
N1 C3 1.398(7) . ?
P1 C8 1.799(4) 2_756 ?
P1 C14 1.799(4) 2_756 ?
S1 Ni1 2.1486(9) . ?
S2 Ni1 2.1724(10) . ?
S3 C3B 1.699(9) . ?
S3 C3 1.730(6) . ?
Ni1 S1 2.1486(9) 7_646 ?
Ni1 S2 2.1724(10) 7_646 ?
C3 S4 1.687(6) . ?
C3B S4B 1.657(9) . ?

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
C2 C1 S1 123.7(3) . . ?
C2 C1 S3 111.5(3) . . ?
S1 C1 S3 124.6(2) . . ?
C1 C2 N1 113.0(4) . . ?
C1 C2 S2 117.9(3) . . ?
N1 C2 S2 129.0(3) . . ?
C5 C4 C7 112.4(8) . . ?
C5 C4 N1 113.4(5) . . ?
C7 C4 N1 108.0(5) . . ?
C5 C4 C6 110.8(7) . . ?
C7 C4 C6 103.2(6) . . ?
N1 C4 C6 108.5(6) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C8 C9 119.7(4) . . ?
C13 C8 P1 121.8(3) . . ?
C9 C8 P1 118.3(3) . . ?
C10 C9 C8 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 119.8(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.5(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C8 C13 C12 120.2(4) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C19 C14 C15 119.8(4) . . ?
C19 C14 P1 121.4(3) . . ?
C15 C14 P1 118.7(3) . . ?
C14 C15 C16 119.7(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 120.1(4) . . ?
C17 C16 H16 120 . . ?
C15 C16 H16 120 . . ?
C16 C17 C18 121.0(4) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 119.2(4) . . ?
C14 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C3B N1 C2 110.3(5) . . ?
C3 N1 C2 111.7(4) . . ?
C3B N1 C4 123.8(5) . . ?
C3 N1 C4 123.4(4) . . ?
C2 N1 C4 124.8(4) . . ?
C8 P1 C8 106.2(2) . 2_756 ?
C8 P1 C14 110.97(16) . . ?
C8 P1 C14 110.91(16) 2_756 . ?
C8 P1 C14 110.91(16) . 2_756 ?
C8 P1 C14 110.96(16) 2_756 2_756 ?
C14 P1 C14 107.0(2) . 2_756 ?
C1 S1 Ni1 101.96(14) . . ?
C2 S2 Ni1 103.48(13) . . ?
C3B S3 C1 90.9(4) . . ?
C3 S3 C1 92.3(2) . . ?
S1 Ni1 S1 180 7_646 . ?
S1 Ni1 S2 92.74(4) 7_646 7_646 ?
S1 Ni1 S2 87.26(4) . 7_646 ?
S1 Ni1 S2 87.26(4) 7_646 . ?
S1 Ni1 S2 92.74(4) . . ?
S2 Ni1 S2 180.00(5) 7_646 . ?
N1 C3 S4 133.8(5) . . ?
N1 C3 S3 110.4(4) . . ?
S4 C3 S3 115.8(4) . . ?
N1 C3B S4B 118.4(10) . . ?
N1 C3B S3 113.7(6) . . ?
S4B C3B S3 127.9(10) . . ?

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
S1 C1 C2 N1 -178.0(3) . . . . ?
S3 C1 C2 N1 -2.6(5) . . . . ?
S1 C1 C2 S2 -2.8(5) . . . . ?
S3 C1 C2 S2 172.6(2) . . . . ?
C13 C8 C9 C10 -1.1(6) . . . . ?
P1 C8 C9 C10 -176.9(3) . . . . ?
C8 C9 C10 C11 1.5(7) . . . . ?
C9 C10 C11 C12 -1.1(7) . . . . ?
C10 C11 C12 C13 0.4(7) . . . . ?
C9 C8 C13 C12 0.3(6) . . . . ?
P1 C8 C13 C12 176.1(4) . . . . ?
C11 C12 C13 C8 0.0(7) . . . . ?
C19 C14 C15 C16 0.7(6) . . . . ?
P1 C14 C15 C16 178.4(3) . . . . ?
C14 C15 C16 C17 -1.8(7) . . . . ?
C15 C16 C17 C18 1.6(7) . . . . ?
C16 C17 C18 C19 -0.3(8) . . . . ?
C15 C14 C19 C18 0.6(6) . . . . ?
P1 C14 C19 C18 -177.0(4) . . . . ?
C17 C18 C19 C14 -0.9(7) . . . . ?
C1 C2 N1 C3B -2.7(10) . . . . ?
S2 C2 N1 C3B -177.2(9) . . . . ?
C1 C2 N1 C3 9.3(7) . . . . ?
S2 C2 N1 C3 -165.3(6) . . . . ?
C1 C2 N1 C4 -171.6(5) . . . . ?
S2 C2 N1 C4 13.8(7) . . . . ?
C5 C4 N1 C3B -148.1(12) . . . . ?
C7 C4 N1 C3B 86.7(12) . . . . ?
C6 C4 N1 C3B -24.5(13) . . . . ?
C5 C4 N1 C3 -161.6(9) . . . . ?
C7 C4 N1 C3 73.2(9) . . . . ?
C6 C4 N1 C3 -38.0(9) . . . . ?
C5 C4 N1 C2 19.4(10) . . . . ?
C7 C4 N1 C2 -105.8(6) . . . . ?
C6 C4 N1 C2 143.0(5) . . . . ?
C13 C8 P1 C8 -123.9(4) . . . 2_756 ?
C9 C8 P1 C8 51.9(3) . . . 2_756 ?
C13 C8 P1 C14 -3.3(4) . . . . ?
C9 C8 P1 C14 172.5(3) . . . . ?
C13 C8 P1 C14 115.5(3) . . . 2_756 ?
C9 C8 P1 C14 -68.7(3) . . . 2_756 ?
C19 C14 P1 C8 -113.1(3) . . . . ?
C15 C14 P1 C8 69.3(3) . . . . ?
C19 C14 P1 C8 4.6(4) . . . 2_756 ?
C15 C14 P1 C8 -173.0(3) . . . 2_756 ?
C19 C14 P1 C14 125.8(4) . . . 2_756 ?
C15 C14 P1 C14 -51.8(3) . . . 2_756 ?
C2 C1 S1 Ni1 5.0(4) . . . . ?
S3 C1 S1 Ni1 -169.8(2) . . . . ?
C1 C2 S2 Ni1 -1.0(3) . . . . ?
N1 C2 S2 Ni1 173.3(3) . . . . ?
C2 C1 S3 C3B 5.5(7) . . . . ?
S1 C1 S3 C3B -179.1(7) . . . . ?
C2 C1 S3 C3 -3.5(5) . . . . ?
S1 C1 S3 C3 171.9(5) . . . . ?
C2 N1 C3 S4 168.6(8) . . . . ?
C4 N1 C3 S4 -10.5(14) . . . . ?
C2 N1 C3 S3 -11.6(8) . . . . ?
C4 N1 C3 S3 169.3(5) . . . . ?
C1 S3 C3 N1 8.7(7) . . . . ?
C1 S3 C3 S4 -171.4(6) . . . . ?
C2 N1 C3B S4B -173.9(12) . . . . ?
C4 N1 C3B S4B -4.9(15) . . . . ?
C2 N1 C3B S3 7.0(15) . . . . ?
C4 N1 C3B S3 176.1(7) . . . . ?
C1 S3 C3B N1 -7.3(13) . . . . ?
C1 S3 C3B S4B 173.8(14) . . . . ?

####################################################################### 
# 
# 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_tppSEt
_database_code_depnum_ccdc_archive 'CCDC 1826893'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;

_audit_creation_date             2018-03-21T15:39:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C24 H20 P, C10 H10 N2 Ni S8'
_chemical_formula_sum            'C34 H30 N2 Ni P S8'
_chemical_formula_weight         812.76
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                             UNIT CELL INFORMATION                          #
#----------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.574(3)
_cell_length_b                   18.701(2)
_cell_length_c                   9.9430(15)
_cell_angle_alpha                90
_cell_angle_beta                 103.080(6)
_cell_angle_gamma                90
_cell_volume                     3545.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    8635
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.49
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                              CRYSTAL INFORMATION                           #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1676
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                             ABSORPTION CORRECTION                          #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_T_max  0.896



#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_ub_11      -0.025318
_diffrn_orient_matrix_ub_12      0.001513
_diffrn_orient_matrix_ub_13      0.076752
_diffrn_orient_matrix_ub_21      -0.032112
_diffrn_orient_matrix_ub_22      0.037631
_diffrn_orient_matrix_ub_23      -0.050555
_diffrn_orient_matrix_ub_31      -0.032842
_diffrn_orient_matrix_ub_32      -0.03796
_diffrn_orient_matrix_ub_33      -0.047057
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_number            12752
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.394
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_reflns_Friedel_coverage         0
_reflns_number_total             4082
_reflns_number_gt                3501
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+24.2830P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4082
_refine_ls_number_parameters     290
_refine_ls_number_restraints     230
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1431
_refine_ls_wR_factor_gt          0.136
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.121

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.25 0.25 1 0.01393(16) Uani 1 2 d S . P . .
S1 S 0.17994(4) 0.33888(4) 0.93181(9) 0.01811(19) Uani 1 1 d . . . . .
S2 S 0.28338(4) 0.24352(4) 0.80609(8) 0.01786(19) Uani 1 1 d . . . . .
S3 S 0.23240(5) 0.33662(5) 0.54325(9) 0.0215(2) Uani 1 1 d . . . . .
S4 S 0.13796(7) 0.46131(7) 0.42451(14) 0.0492(4) Uani 1 1 d . . . . .
C1 C 0.23523(17) 0.31110(17) 0.7128(3) 0.0166(6) Uani 1 1 d . . . . .
C2 C 0.18908(17) 0.35259(17) 0.7647(3) 0.0168(6) Uani 1 1 d . . . . .
N3 N 0.15228(16) 0.40365(16) 0.6775(3) 0.0208(6) Uani 1 1 d . . . . .
C4 C 0.16940(19) 0.40141(18) 0.5591(4) 0.0212(7) Uani 1 1 d . . . . .
C5 C 0.1297(4) 0.4196(4) 0.2810(7) 0.0227(14) Uani 0.5 1 d . . P A -1
H5A H 0.12 0.4544 0.2039 0.027 Uiso 0.5 1 calc R U P A -1
H5B H 0.1741 0.3947 0.2791 0.027 Uiso 0.5 1 calc R U P A -1
C6 C 0.0707(5) 0.3657(4) 0.2617(10) 0.036(2) Uani 0.5 1 d . . P A -1
H6A H 0.0845 0.3261 0.3266 0.055 Uiso 0.5 1 calc R U P A -1
H6B H 0.0609 0.3474 0.1669 0.055 Uiso 0.5 1 calc R U P A -1
H6C H 0.0286 0.3888 0.279 0.055 Uiso 0.5 1 calc R U P A -1
C7 C 0.0650(4) 0.4989(4) 0.4724(8) 0.0265(16) Uani 0.5 1 d . . P A -2
H7A H 0.0353 0.4603 0.4968 0.032 Uiso 0.5 1 calc R U P A -2
H7B H 0.0809 0.5295 0.5548 0.032 Uiso 0.5 1 calc R U P A -2
C8 C 0.0217(4) 0.5437(4) 0.3543(9) 0.0276(16) Uani 0.5 1 d . . P A -2
H8A H 0.052 0.5792 0.3246 0.041 Uiso 0.5 1 calc R U P A -2
H8B H -0.016 0.5682 0.3863 0.041 Uiso 0.5 1 calc R U P A -2
H8C H 0.0013 0.5124 0.2765 0.041 Uiso 0.5 1 calc R U P A -2
P1 P 0.5 0.40807(7) 0.75 0.0242(3) Uani 1 2 d DS T P . .
C11A C 0.4831(4) 0.3436(3) 0.6201(6) 0.022(2) Uani 0.5 1 d DG U P B 1
C12A C 0.5308(3) 0.2880(3) 0.6266(5) 0.0233(15) Uani 0.5 1 d G U P B 1
H12A H 0.5712 0.2858 0.7006 0.028 Uiso 0.5 1 calc R U P B 1
C13A C 0.5196(3) 0.2355(3) 0.5250(6) 0.0277(15) Uani 0.5 1 d G U P B 1
H13A H 0.5522 0.1975 0.5295 0.033 Uiso 0.5 1 calc R U P B 1
C14A C 0.4606(3) 0.2386(3) 0.4168(6) 0.0277(15) Uani 0.5 1 d G U P B 1
H14A H 0.4529 0.2027 0.3474 0.033 Uiso 0.5 1 calc R U P B 1
C15A C 0.4128(3) 0.2943(3) 0.4103(6) 0.0269(17) Uani 0.5 1 d G U P B 1
H15A H 0.3725 0.2964 0.3363 0.032 Uiso 0.5 1 calc R U P B 1
C16A C 0.4241(4) 0.3467(3) 0.5119(7) 0.026(2) Uani 0.5 1 d G U P B 1
H16A H 0.3915 0.3848 0.5074 0.031 Uiso 0.5 1 calc R U P B 1
C11B C 0.4822(4) 0.3567(3) 0.5861(6) 0.0197(19) Uani 0.5 1 d DG U P B 2
C12B C 0.5283(3) 0.3038(3) 0.5645(5) 0.0231(16) Uani 0.5 1 d G U P B 2
H12B H 0.5719 0.2975 0.6287 0.028 Uiso 0.5 1 calc R U P B 2
C13B C 0.5108(3) 0.2600(3) 0.4488(6) 0.0280(16) Uani 0.5 1 d G U P B 2
H13B H 0.5424 0.2238 0.4341 0.034 Uiso 0.5 1 calc R U P B 2
C14B C 0.4471(3) 0.2691(3) 0.3548(6) 0.0274(16) Uani 0.5 1 d G U P B 2
H14B H 0.4351 0.2392 0.2757 0.033 Uiso 0.5 1 calc R U P B 2
C15B C 0.4009(3) 0.3221(3) 0.3764(6) 0.0260(18) Uani 0.5 1 d G U P B 2
H15B H 0.3573 0.3284 0.3121 0.031 Uiso 0.5 1 calc R U P B 2
C16B C 0.4184(3) 0.3659(3) 0.4920(7) 0.0187(18) Uani 0.5 1 d G U P B 2
H16B H 0.3869 0.4021 0.5068 0.022 Uiso 0.5 1 calc R U P B 2
C17A C 0.4202(4) 0.4604(4) 0.7445(9) 0.0294(18) Uani 0.5 1 d DG U P B 1
C18A C 0.4053(4) 0.5148(4) 0.6469(8) 0.0375(18) Uani 0.5 1 d G U P B 1
H18A H 0.4378 0.5259 0.5919 0.045 Uiso 0.5 1 calc R U P B 1
C19A C 0.3430(4) 0.5530(4) 0.6299(8) 0.0448(19) Uani 0.5 1 d G U P B 1
H19A H 0.3329 0.5901 0.5633 0.054 Uiso 0.5 1 calc R U P B 1
C20A C 0.2956(3) 0.5367(4) 0.7104(10) 0.039(2) Uani 0.5 1 d G U P B 1
H20A H 0.253 0.5628 0.6988 0.047 Uiso 0.5 1 calc R U P B 1
C21A C 0.3105(5) 0.4823(5) 0.8080(10) 0.034(2) Uani 0.5 1 d G U P B 1
H21A H 0.278 0.4712 0.863 0.04 Uiso 0.5 1 calc R U P B 1
C22A C 0.3728(6) 0.4442(5) 0.8250(10) 0.029(2) Uani 0.5 1 d G U P B 1
H22A H 0.383 0.407 0.8917 0.035 Uiso 0.5 1 calc R U P B 1
C17B C 0.4290(4) 0.4673(4) 0.7425(9) 0.0272(18) Uani 0.5 1 d DG U P B 2
C18B C 0.4289(3) 0.5338(4) 0.6800(8) 0.0322(17) Uani 0.5 1 d G U P B 2
H18B H 0.4686 0.5488 0.6474 0.039 Uiso 0.5 1 calc R U P B 2
C19B C 0.3707(4) 0.5782(3) 0.6650(8) 0.047(3) Uani 0.5 1 d G U P B 2
H19B H 0.3707 0.6236 0.6223 0.056 Uiso 0.5 1 calc R U P B 2
C20B C 0.3126(4) 0.5561(4) 0.7126(10) 0.044(3) Uani 0.5 1 d G U P B 2
H20B H 0.2729 0.5865 0.7024 0.052 Uiso 0.5 1 calc R U P B 2
C21B C 0.3127(5) 0.4896(5) 0.7752(11) 0.036(3) Uani 0.5 1 d G U P B 2
H21B H 0.273 0.4746 0.8077 0.043 Uiso 0.5 1 calc R U P B 2
C22B C 0.3708(6) 0.4452(4) 0.7901(11) 0.029(2) Uani 0.5 1 d G U P B 2
H22B H 0.3709 0.3998 0.8329 0.035 Uiso 0.5 1 calc R U P B 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 S1 2.1640(8) . ?
Ni1 S1 2.1640(8) 7_557 ?
Ni1 S2 2.1746(9) . ?
Ni1 S2 2.1746(9) 7_557 ?
S1 C2 1.730(3) . ?
S2 C1 1.718(3) . ?
S3 C1 1.741(3) . ?
S3 C4 1.761(4) . ?
S4 C5 1.602(7) . ?
S4 C4 1.747(4) . ?
S4 C7 1.752(7) . ?
C1 C2 1.377(5) . ?
C2 N3 1.379(4) . ?
N3 C4 1.295(5) . ?
C5 C6 1.511(11) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.533(11) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
P1 C11A 1.743(4) 2_656 ?
P1 C11A 1.743(4) . ?
P1 C17B 1.766(6) . ?
P1 C17B 1.766(6) 2_656 ?
P1 C17A 1.833(7) 2_656 ?
P1 C17A 1.833(7) . ?
P1 C11B 1.856(4) 2_656 ?
P1 C11B 1.856(4) . ?
C11A C12A 1.39 . ?
C11A C16A 1.39 . ?
C12A C13A 1.39 . ?
C12A H12A 0.95 . ?
C13A C14A 1.39 . ?
C13A H13A 0.95 . ?
C14A C15A 1.39 . ?
C14A H14A 0.95 . ?
C15A C16A 1.39 . ?
C15A H15A 0.95 . ?
C16A H16A 0.95 . ?
C11B C12B 1.39 . ?
C11B C16B 1.39 . ?
C12B C13B 1.39 . ?
C12B H12B 0.95 . ?
C13B C14B 1.39 . ?
C13B H13B 0.95 . ?
C14B C15B 1.39 . ?
C14B H14B 0.95 . ?
C15B C16B 1.39 . ?
C15B H15B 0.95 . ?
C16B H16B 0.95 . ?
C17A C18A 1.39 . ?
C17A C22A 1.39 . ?
C18A C19A 1.39 . ?
C18A H18A 0.95 . ?
C19A C20A 1.39 . ?
C19A H19A 0.95 . ?
C20A C21A 1.39 . ?
C20A H20A 0.95 . ?
C21A C22A 1.39 . ?
C21A H21A 0.95 . ?
C22A H22A 0.95 . ?
C17B C18B 1.39 . ?
C17B C22B 1.39 . ?
C18B C19B 1.39 . ?
C18B H18B 0.95 . ?
C19B C20B 1.39 . ?
C19B H19B 0.95 . ?
C20B C21B 1.39 . ?
C20B H20B 0.95 . ?
C21B C22B 1.39 . ?
C21B H21B 0.95 . ?
C22B H22B 0.95 . ?

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
S1 Ni1 S1 180 . 7_557 ?
S1 Ni1 S2 93.51(3) . . ?
S1 Ni1 S2 86.49(3) 7_557 . ?
S1 Ni1 S2 86.49(3) . 7_557 ?
S1 Ni1 S2 93.51(3) 7_557 7_557 ?
S2 Ni1 S2 180.00(4) . 7_557 ?
C2 S1 Ni1 102.63(12) . . ?
C1 S2 Ni1 101.52(11) . . ?
C1 S3 C4 88.37(16) . . ?
C5 S4 C4 108.5(3) . . ?
C4 S4 C7 102.5(3) . . ?
C2 C1 S2 122.6(3) . . ?
C2 C1 S3 109.2(2) . . ?
S2 C1 S3 128.2(2) . . ?
C1 C2 N3 116.6(3) . . ?
C1 C2 S1 119.7(3) . . ?
N3 C2 S1 123.7(3) . . ?
C4 N3 C2 110.1(3) . . ?
N3 C4 S4 123.8(3) . . ?
N3 C4 S3 115.7(3) . . ?
S4 C4 S3 120.3(2) . . ?
C6 C5 S4 111.0(6) . . ?
C6 C5 H5A 109.4 . . ?
S4 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
S4 C5 H5B 109.4 . . ?
H5A C5 H5B 108 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 S4 110.8(5) . . ?
C8 C7 H7A 109.5 . . ?
S4 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
S4 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11A P1 C11A 92.5(5) 2_656 . ?
C17B P1 C17B 102.3(6) . 2_656 ?
C11A P1 C17A 109.2(4) 2_656 2_656 ?
C11A P1 C17A 114.1(4) . 2_656 ?
C11A P1 C17A 114.1(4) 2_656 . ?
C11A P1 C17A 109.2(4) . . ?
C17A P1 C17A 115.4(6) 2_656 . ?
C17B P1 C11B 110.6(4) . 2_656 ?
C17B P1 C11B 107.3(3) 2_656 2_656 ?
C17B P1 C11B 107.3(4) . . ?
C17B P1 C11B 110.6(4) 2_656 . ?
C11B P1 C11B 117.7(4) 2_656 . ?
C12A C11A C16A 120 . . ?
C12A C11A P1 118.0(4) . . ?
C16A C11A P1 122.0(4) . . ?
C13A C12A C11A 120 . . ?
C13A C12A H12A 120 . . ?
C11A C12A H12A 120 . . ?
C14A C13A C12A 120 . . ?
C14A C13A H13A 120 . . ?
C12A C13A H13A 120 . . ?
C15A C14A C13A 120 . . ?
C15A C14A H14A 120 . . ?
C13A C14A H14A 120 . . ?
C14A C15A C16A 120 . . ?
C14A C15A H15A 120 . . ?
C16A C15A H15A 120 . . ?
C15A C16A C11A 120 . . ?
C15A C16A H16A 120 . . ?
C11A C16A H16A 120 . . ?
C12B C11B C16B 120 . . ?
C12B C11B P1 120.3(4) . . ?
C16B C11B P1 119.3(4) . . ?
C13B C12B C11B 120 . . ?
C13B C12B H12B 120 . . ?
C11B C12B H12B 120 . . ?
C12B C13B C14B 120 . . ?
C12B C13B H13B 120 . . ?
C14B C13B H13B 120 . . ?
C15B C14B C13B 120 . . ?
C15B C14B H14B 120 . . ?
C13B C14B H14B 120 . . ?
C14B C15B C16B 120 . . ?
C14B C15B H15B 120 . . ?
C16B C15B H15B 120 . . ?
C15B C16B C11B 120 . . ?
C15B C16B H16B 120 . . ?
C11B C16B H16B 120 . . ?
C18A C17A C22A 120 . . ?
C18A C17A P1 117.0(5) . . ?
C22A C17A P1 122.8(5) . . ?
C17A C18A C19A 120 . . ?
C17A C18A H18A 120 . . ?
C19A C18A H18A 120 . . ?
C20A C19A C18A 120 . . ?
C20A C19A H19A 120 . . ?
C18A C19A H19A 120 . . ?
C19A C20A C21A 120 . . ?
C19A C20A H20A 120 . . ?
C21A C20A H20A 120 . . ?
C22A C21A C20A 120 . . ?
C22A C21A H21A 120 . . ?
C20A C21A H21A 120 . . ?
C21A C22A C17A 120 . . ?
C21A C22A H22A 120 . . ?
C17A C22A H22A 120 . . ?
C18B C17B C22B 120 . . ?
C18B C17B P1 120.0(5) . . ?
C22B C17B P1 119.8(5) . . ?
C17B C18B C19B 120 . . ?
C17B C18B H18B 120 . . ?
C19B C18B H18B 120 . . ?
C20B C19B C18B 120 . . ?
C20B C19B H19B 120 . . ?
C18B C19B H19B 120 . . ?
C19B C20B C21B 120 . . ?
C19B C20B H20B 120 . . ?
C21B C20B H20B 120 . . ?
C22B C21B C20B 120 . . ?
C22B C21B H21B 120 . . ?
C20B C21B H21B 120 . . ?
C21B C22B C17B 120 . . ?
C21B C22B H22B 120 . . ?
C17B C22B H22B 120 . . ?

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
Ni1 S2 C1 C2 -0.7(3) . . . . ?
Ni1 S2 C1 S3 -177.9(2) . . . . ?
C4 S3 C1 C2 0.3(3) . . . . ?
C4 S3 C1 S2 177.9(3) . . . . ?
S2 C1 C2 N3 -178.2(2) . . . . ?
S3 C1 C2 N3 -0.5(4) . . . . ?
S2 C1 C2 S1 1.8(4) . . . . ?
S3 C1 C2 S1 179.49(18) . . . . ?
Ni1 S1 C2 C1 -1.8(3) . . . . ?
Ni1 S1 C2 N3 178.2(3) . . . . ?
C1 C2 N3 C4 0.4(4) . . . . ?
S1 C2 N3 C4 -179.6(3) . . . . ?
C2 N3 C4 S4 -176.0(3) . . . . ?
C2 N3 C4 S3 -0.1(4) . . . . ?
C5 S4 C4 N3 -146.1(4) . . . . ?
C7 S4 C4 N3 -17.2(5) . . . . ?
C5 S4 C4 S3 38.2(4) . . . . ?
C7 S4 C4 S3 167.1(3) . . . . ?
C1 S3 C4 N3 -0.1(3) . . . . ?
C1 S3 C4 S4 175.9(2) . . . . ?
C4 S4 C5 C6 69.0(6) . . . . ?
C4 S4 C7 C8 -169.9(5) . . . . ?
C11A P1 C11A C12A -48.4(3) 2_656 . . . ?
C17A P1 C11A C12A 64.0(5) 2_656 . . . ?
C17A P1 C11A C12A -165.1(5) . . . . ?
C11A P1 C11A C16A 131.8(5) 2_656 . . . ?
C17A P1 C11A C16A -115.8(5) 2_656 . . . ?
C17A P1 C11A C16A 15.1(5) . . . . ?
C16A C11A C12A C13A 0 . . . . ?
P1 C11A C12A C13A -179.8(6) . . . . ?
C11A C12A C13A C14A 0 . . . . ?
C12A C13A C14A C15A 0 . . . . ?
C13A C14A C15A C16A 0 . . . . ?
C14A C15A C16A C11A 0 . . . . ?
C12A C11A C16A C15A 0 . . . . ?
P1 C11A C16A C15A 179.8(6) . . . . ?
C17B P1 C11B C12B -177.7(5) . . . . ?
C17B P1 C11B C12B 71.4(5) 2_656 . . . ?
C11B P1 C11B C12B -52.3(3) 2_656 . . . ?
C17B P1 C11B C16B -5.1(5) . . . . ?
C17B P1 C11B C16B -116.0(4) 2_656 . . . ?
C11B P1 C11B C16B 120.3(4) 2_656 . . . ?
C16B C11B C12B C13B 0 . . . . ?
P1 C11B C12B C13B 172.6(5) . . . . ?
C11B C12B C13B C14B 0 . . . . ?
C12B C13B C14B C15B 0 . . . . ?
C13B C14B C15B C16B 0 . . . . ?
C14B C15B C16B C11B 0 . . . . ?
C12B C11B C16B C15B 0 . . . . ?
P1 C11B C16B C15B -172.6(5) . . . . ?
C11A P1 C17A C18A 177.3(5) 2_656 . . . ?
C11A P1 C17A C18A -80.7(6) . . . . ?
C17A P1 C17A C18A 49.5(4) 2_656 . . . ?
C11A P1 C17A C22A -7.8(5) 2_656 . . . ?
C11A P1 C17A C22A 94.2(5) . . . . ?
C17A P1 C17A C22A -135.6(5) 2_656 . . . ?
C22A C17A C18A C19A 0 . . . . ?
P1 C17A C18A C19A 175.1(6) . . . . ?
C17A C18A C19A C20A 0 . . . . ?
C18A C19A C20A C21A 0 . . . . ?
C19A C20A C21A C22A 0 . . . . ?
C20A C21A C22A C17A 0 . . . . ?
C18A C17A C22A C21A 0 . . . . ?
P1 C17A C22A C21A -174.8(6) . . . . ?
C17B P1 C17B C18B 30.6(4) 2_656 . . . ?
C11B P1 C17B C18B 144.6(5) 2_656 . . . ?
C11B P1 C17B C18B -85.8(6) . . . . ?
C17B P1 C17B C22B -154.1(5) 2_656 . . . ?
C11B P1 C17B C22B -40.1(5) 2_656 . . . ?
C11B P1 C17B C22B 89.4(5) . . . . ?
C22B C17B C18B C19B 0 . . . . ?
P1 C17B C18B C19B 175.3(6) . . . . ?
C17B C18B C19B C20B 0 . . . . ?
C18B C19B C20B C21B 0 . . . . ?
C19B C20B C21B C22B 0 . . . . ?
C20B C21B C22B C17B 0 . . . . ?
C18B C17B C22B C21B 0 . . . . ?
P1 C17B C22B C21B -175.3(6) . . . . ?

