# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_SY80325_DMSOH2O_rt
_database_code_depnum_ccdc_archive 'CCDC 2065214'
loop_
_audit_author_name
_audit_author_address
'So Yokomori'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C38 H34 Ni O5 P S5'
_chemical_formula_moiety         'C38 H34 Ni O5 P S5'
_chemical_formula_weight         820.66
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.188(2)
_cell_length_b                   13.333(3)
_cell_length_c                   13.778(3)
_cell_angle_alpha                92.947(3)
_cell_angle_beta                 99.616(4)
_cell_angle_gamma                94.177(4)
_cell_volume                     1836.5(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4218
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    293
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             850.00
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.835

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

_diffrn_ambient_temperature      293
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            12683
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.070
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6948
_reflns_number_gt                5304
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1361
_refine_ls_wR_factor_gt          0.1213
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6948
_refine_ls_number_parameters     460
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0693P)²+0.5539P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.49
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.500000 0.500000 0.500000 0.04121(17) Uani 1 2 d S . P . .
Ni2 Ni 1.000000 0.000000 0.000000 0.04364(18) Uani 1 2 d S . P . .
S1 S 1.29482(9) 0.53187(7) 0.50085(6) 0.0473(2) Uani 1 1 d . . . . .
S2 S 1.47803(9) 0.51534(8) 0.34459(6) 0.0515(2) Uani 1 1 d . . . . .
S3 S 1.01957(9) 0.16251(6) 0.00782(7) 0.0480(2) Uani 1 1 d . . . . .
S4 S 1.18998(10) -0.00685(6) -0.04809(8) 0.0545(3) Uani 1 1 d . . . . .
S5 S 0.80098(10) 0.38339(8) 0.13157(7) 0.0557(3) Uani 1 1 d . . . . .
P1 P 0.73837(8) 0.08768(6) 0.42516(6) 0.0382(2) Uani 1 1 d . . . . .
O1 O 0.9273(2) 0.6200(2) 0.22372(18) 0.0576(7) Uani 1 1 d . . . . .
H1 H 0.914416 0.627668 0.164320 0.069 Uiso 1 1 calc R U . . .
O2 O 1.0707(2) 0.5816(2) 0.08547(17) 0.0589(7) Uani 1 1 d . . . . .
H2A H 1.126045 0.579040 0.048651 0.071 Uiso 1 1 calc R U . . .
O3 O 1.4138(3) 0.41390(18) -0.0394(3) 0.0682(8) Uani 1 1 d . . . . .
H3 H 1.361407 0.455847 -0.030114 0.082 Uiso 1 1 calc R U . . .
O4 O 1.5503(3) 0.2649(2) -0.0946(2) 0.0709(8) Uani 1 1 d . . . . .
H4 H 1.572821 0.324968 -0.081368 0.085 Uiso 1 1 calc R U . . .
O5 O 0.7481(2) 0.43011(19) 0.03546(18) 0.0558(6) Uani 1 1 d . . . . .
C1 C 1.2302(3) 0.5504(2) 0.3781(2) 0.0382(7) Uani 1 1 d . . . . .
C2 C 1.0993(3) 0.5772(2) 0.3492(2) 0.0416(7) Uani 1 1 d . . . . .
H2 H 1.044507 0.586666 0.396000 0.050 Uiso 1 1 calc R U . . .
C3 C 1.0527(3) 0.5895(2) 0.2517(2) 0.0409(7) Uani 1 1 d . . . . .
C4 C 1.1311(3) 0.5707(2) 0.1798(2) 0.0409(7) Uani 1 1 d . . . . .
C5 C 1.2598(3) 0.5453(2) 0.2067(2) 0.0431(8) Uani 1 1 d . . . . .
H5 H 1.312362 0.533247 0.158947 0.052 Uiso 1 1 calc R U . . .
C6 C 1.3118(3) 0.5375(2) 0.3075(2) 0.0384(7) Uani 1 1 d . . . . .
C7 C 1.1753(3) 0.1948(2) -0.0219(2) 0.0389(7) Uani 1 1 d . . . . .
C8 C 1.2278(3) 0.2964(2) -0.0180(2) 0.0416(8) Uani 1 1 d . . . . .
H8 H 1.177987 0.347787 0.000168 0.050 Uiso 1 1 calc R U . . .
C9 C 1.3516(4) 0.3191(2) -0.0410(3) 0.0465(8) Uani 1 1 d . . . . .
C10 C 1.4279(4) 0.2419(3) -0.0684(3) 0.0489(8) Uani 1 1 d . . . . .
C11 C 1.3792(4) 0.1430(3) -0.0706(3) 0.0493(8) Uani 1 1 d . . . . .
H11 H 1.430693 0.092090 -0.087416 0.059 Uiso 1 1 calc R U . . .
C12 C 1.2531(3) 0.1182(2) -0.0477(2) 0.0412(7) Uani 1 1 d . . . . .
C13 C 0.7423(3) 0.1257(2) 0.5521(2) 0.0419(7) Uani 1 1 d . . . . .
C14 C 0.6372(3) 0.1681(3) 0.5859(3) 0.0487(8) Uani 1 1 d . . . . .
H14 H 0.559710 0.177436 0.542197 0.058 Uiso 1 1 calc R U . . .
C15 C 0.6476(4) 0.1968(3) 0.6858(3) 0.0578(10) Uani 1 1 d . . . . .
H15 H 0.577583 0.226513 0.708376 0.069 Uiso 1 1 calc R U . . .
C16 C 0.7592(4) 0.1817(3) 0.7502(3) 0.0608(11) Uani 1 1 d . . . . .
H16 H 0.764095 0.199221 0.816991 0.073 Uiso 1 1 calc R U . . .
C17 C 0.8659(4) 0.1406(3) 0.7175(3) 0.0629(11) Uani 1 1 d . . . . .
H17 H 0.942492 0.130957 0.762014 0.075 Uiso 1 1 calc R U . . .
C18 C 0.8584(4) 0.1139(3) 0.6188(3) 0.0561(10) Uani 1 1 d . . . . .
H18 H 0.931044 0.087942 0.596411 0.067 Uiso 1 1 calc R U . . .
C19 C 0.8764(3) 0.1603(2) 0.3864(2) 0.0416(7) Uani 1 1 d . . . . .
C20 C 0.9052(4) 0.2580(3) 0.4252(3) 0.0629(10) Uani 1 1 d . . . . .
H20 H 0.862256 0.281528 0.475306 0.076 Uiso 1 1 calc R U . . .
C21 C 0.9973(4) 0.3212(3) 0.3904(4) 0.0753(13) Uani 1 1 d . . . . .
H21 H 1.014830 0.387528 0.416493 0.090 Uiso 1 1 calc R U . . .
C22 C 1.0623(4) 0.2879(4) 0.3188(3) 0.0706(12) Uani 1 1 d . . . . .
H22 H 1.123860 0.331034 0.295157 0.085 Uiso 1 1 calc R U . . .
C23 C 1.0365(4) 0.1903(4) 0.2816(3) 0.0787(14) Uani 1 1 d . . . . .
H23 H 1.082138 0.166941 0.232971 0.094 Uiso 1 1 calc R U . . .
C24 C 0.9437(4) 0.1252(3) 0.3148(3) 0.0616(10) Uani 1 1 d . . . . .
H24 H 0.927343 0.058742 0.289017 0.074 Uiso 1 1 calc R U . . .
C25 C 0.7494(3) -0.0462(2) 0.4127(2) 0.0424(8) Uani 1 1 d . . . . .
C26 C 0.7648(4) -0.0934(3) 0.3226(3) 0.0564(9) Uani 1 1 d . . . . .
H26 H 0.774521 -0.055046 0.269390 0.068 Uiso 1 1 calc R U . . .
C27 C 0.7655(4) -0.1968(3) 0.3128(3) 0.0641(11) Uani 1 1 d . . . . .
H27 H 0.777714 -0.227827 0.253274 0.077 Uiso 1 1 calc R U . . .
C28 C 0.7484(4) -0.2545(3) 0.3906(3) 0.0653(11) Uani 1 1 d . . . . .
H28 H 0.749214 -0.324238 0.383670 0.078 Uiso 1 1 calc R U . . .
C29 C 0.7300(4) -0.2090(3) 0.4783(3) 0.0640(11) Uani 1 1 d . . . . .
H29 H 0.716765 -0.248263 0.530252 0.077 Uiso 1 1 calc R U . . .
C30 C 0.7309(4) -0.1046(3) 0.4906(3) 0.0523(9) Uani 1 1 d . . . . .
H30 H 0.719237 -0.074189 0.550514 0.063 Uiso 1 1 calc R U . . .
C31 C 0.5876(3) 0.1176(2) 0.3484(2) 0.0410(7) Uani 1 1 d . . . . .
C32 C 0.5070(4) 0.0437(3) 0.2860(3) 0.0542(9) Uani 1 1 d . . . . .
H32 H 0.526134 -0.023375 0.288514 0.065 Uiso 1 1 calc R U . . .
C33 C 0.3991(4) 0.0697(3) 0.2204(3) 0.0647(11) Uani 1 1 d . . . . .
H33 H 0.347076 0.020493 0.177598 0.078 Uiso 1 1 calc R U . . .
C34 C 0.3684(4) 0.1683(3) 0.2182(3) 0.0630(11) Uani 1 1 d . . . . .
H34 H 0.295912 0.185585 0.173518 0.076 Uiso 1 1 calc R U . . .
C35 C 0.4440(4) 0.2413(3) 0.2816(3) 0.0590(10) Uani 1 1 d . . . . .
H35 H 0.421144 0.307576 0.281199 0.071 Uiso 1 1 calc R U . . .
C36 C 0.5539(3) 0.2165(3) 0.3460(3) 0.0494(8) Uani 1 1 d . . . . .
H36 H 0.605782 0.266411 0.388023 0.059 Uiso 1 1 calc R U . . .
C37 C 0.7103(5) 0.4314(4) 0.2180(3) 0.0853(15) Uani 1 1 d . . . . .
H37A H 0.616393 0.418673 0.193094 0.102 Uiso 1 1 calc R U . . .
H37B H 0.732528 0.502665 0.229644 0.102 Uiso 1 1 calc R U . . .
H37C H 0.732036 0.399123 0.278639 0.102 Uiso 1 1 calc R U . . .
C38 C 0.7274(5) 0.2577(3) 0.1198(3) 0.0793(13) Uani 1 1 d . . . . .
H38A H 0.762703 0.219670 0.070449 0.095 Uiso 1 1 calc R U . . .
H38B H 0.632352 0.257705 0.100808 0.095 Uiso 1 1 calc R U . . .
H38C H 0.747319 0.227582 0.181847 0.095 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S2 2.1374(10) . ?
Ni1 S2 2.1374(10) 2_866 ?
Ni1 S1 2.1649(10) 2_866 ?
Ni1 S1 2.1650(10) . ?
Ni2 S4 2.1544(11) 2_755 ?
Ni2 S4 2.1544(11) . ?
Ni2 S3 2.1568(10) 2_755 ?
Ni2 S3 2.1569(10) . ?
S1 C1 1.747(3) . ?
S2 C6 1.736(3) . ?
S3 C7 1.734(3) . ?
S4 C12 1.742(3) . ?
S5 O5 1.525(2) . ?
S5 C37 1.748(4) . ?
S5 C38 1.774(4) . ?
P1 C13 1.788(3) . ?
P1 C31 1.796(3) . ?
P1 C25 1.799(3) . ?
P1 C19 1.818(3) . ?
O1 C3 1.370(4) . ?
O1 H1 0.8200 . ?
O2 C4 1.361(4) . ?
O2 H2A 0.8200 . ?
O3 C9 1.369(4) . ?
O3 H3 0.8200 . ?
O4 C10 1.373(4) . ?
O4 H4 0.8200 . ?
C1 C6 1.393(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.369(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.397(4) . ?
C4 C5 1.374(5) . ?
C5 C6 1.413(4) . ?
C5 H5 0.9300 . ?
C7 C12 1.404(4) . ?
C7 C8 1.414(4) . ?
C8 C9 1.367(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.408(5) . ?
C10 C11 1.373(5) . ?
C11 C12 1.395(5) . ?
C11 H11 0.9300 . ?
C13 C14 1.383(5) . ?
C13 C18 1.396(5) . ?
C14 C15 1.394(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.354(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C24 1.374(5) . ?
C19 C20 1.375(5) . ?
C20 C21 1.377(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.351(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.365(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.386(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.387(5) . ?
C25 C26 1.400(5) . ?
C26 C27 1.379(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.379(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.372(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.393(5) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C36 1.388(4) . ?
C31 C32 1.394(4) . ?
C32 C33 1.379(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.373(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.379(5) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S2 180.0 . 2_866 ?
S2 Ni1 S1 88.36(3) . 2_866 ?
S2 Ni1 S1 91.64(3) 2_866 2_866 ?
S2 Ni1 S1 91.64(3) . . ?
S2 Ni1 S1 88.36(3) 2_866 . ?
S1 Ni1 S1 180.0 2_866 . ?
S4 Ni2 S4 180.0 2_755 . ?
S4 Ni2 S3 91.55(3) 2_755 2_755 ?
S4 Ni2 S3 88.45(3) . 2_755 ?
S4 Ni2 S3 88.45(3) 2_755 . ?
S4 Ni2 S3 91.55(3) . . ?
S3 Ni2 S3 180.00(5) 2_755 . ?
C1 S1 Ni1 104.83(11) . . ?
C6 S2 Ni1 105.27(11) . . ?
C7 S3 Ni2 105.14(11) . . ?
C12 S4 Ni2 105.20(12) . . ?
O5 S5 C37 105.3(2) . . ?
O5 S5 C38 106.03(19) . . ?
C37 S5 C38 97.7(2) . . ?
C13 P1 C31 112.02(15) . . ?
C13 P1 C25 109.37(16) . . ?
C31 P1 C25 108.46(15) . . ?
C13 P1 C19 106.49(15) . . ?
C31 P1 C19 107.24(15) . . ?
C25 P1 C19 113.30(16) . . ?
C3 O1 H1 109.5 . . ?
C4 O2 H2A 109.5 . . ?
C9 O3 H3 109.5 . . ?
C10 O4 H4 109.5 . . ?
C6 C1 C2 119.7(3) . . ?
C6 C1 S1 118.4(2) . . ?
C2 C1 S1 121.9(2) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 O1 119.9(3) . . ?
C2 C3 C4 121.0(3) . . ?
O1 C3 C4 119.1(3) . . ?
O2 C4 C5 124.9(3) . . ?
O2 C4 C3 115.0(3) . . ?
C5 C4 C3 120.1(3) . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 119.8(3) . . ?
C1 C6 S2 119.6(2) . . ?
C5 C6 S2 120.6(2) . . ?
C12 C7 C8 119.1(3) . . ?
C12 C7 S3 119.3(2) . . ?
C8 C7 S3 121.6(3) . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 O3 125.8(3) . . ?
C8 C9 C10 120.5(3) . . ?
O3 C9 C10 113.8(3) . . ?
C11 C10 O4 119.5(3) . . ?
C11 C10 C9 120.0(3) . . ?
O4 C10 C9 120.5(3) . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 119.9(3) . . ?
C11 C12 S4 121.3(3) . . ?
C7 C12 S4 118.7(3) . . ?
C14 C13 C18 119.1(3) . . ?
C14 C13 P1 123.0(3) . . ?
C18 C13 P1 117.9(3) . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.3(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.6(4) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 119.8(4) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C13 120.3(4) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C24 C19 C20 119.3(3) . . ?
C24 C19 P1 123.2(3) . . ?
C20 C19 P1 117.2(3) . . ?
C19 C20 C21 120.4(4) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 120.6(4) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 119.2(4) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C22 C23 C24 121.3(4) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C19 C24 C23 119.0(4) . . ?
C19 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C30 C25 C26 119.4(3) . . ?
C30 C25 P1 119.6(3) . . ?
C26 C25 P1 120.8(3) . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 120.4(4) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 119.9(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.8(4) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C25 C30 C29 119.4(4) . . ?
C25 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C36 C31 C32 118.8(3) . . ?
C36 C31 P1 120.1(3) . . ?
C32 C31 P1 121.0(3) . . ?
C33 C32 C31 120.2(4) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C33 C32 120.1(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 C33 120.3(4) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.0(4) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 120.5(3) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
S5 C37 H37A 109.5 . . ?
S5 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
S5 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
S5 C38 H38A 109.5 . . ?
S5 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
S5 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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 S1 C1 C6 3.0(3) . . . . ?
Ni1 S1 C1 C2 -177.3(2) . . . . ?
C6 C1 C2 C3 0.7(5) . . . . ?
S1 C1 C2 C3 -179.1(2) . . . . ?
C1 C2 C3 O1 -177.1(3) . . . . ?
C1 C2 C3 C4 3.2(5) . . . . ?
C2 C3 C4 O2 177.3(3) . . . . ?
O1 C3 C4 O2 -2.4(4) . . . . ?
C2 C3 C4 C5 -3.8(5) . . . . ?
O1 C3 C4 C5 176.5(3) . . . . ?
O2 C4 C5 C6 179.2(3) . . . . ?
C3 C4 C5 C6 0.4(5) . . . . ?
C2 C1 C6 C5 -4.0(5) . . . . ?
S1 C1 C6 C5 175.8(2) . . . . ?
C2 C1 C6 S2 174.3(2) . . . . ?
S1 C1 C6 S2 -5.9(4) . . . . ?
C4 C5 C6 C1 3.4(5) . . . . ?
C4 C5 C6 S2 -174.9(2) . . . . ?
Ni1 S2 C6 C1 5.7(3) . . . . ?
Ni1 S2 C6 C5 -176.0(2) . . . . ?
Ni2 S3 C7 C12 2.4(3) . . . . ?
Ni2 S3 C7 C8 -175.7(2) . . . . ?
C12 C7 C8 C9 1.2(5) . . . . ?
S3 C7 C8 C9 179.3(3) . . . . ?
C7 C8 C9 O3 -179.5(3) . . . . ?
C7 C8 C9 C10 -0.1(5) . . . . ?
C8 C9 C10 C11 -1.2(5) . . . . ?
O3 C9 C10 C11 178.3(3) . . . . ?
C8 C9 C10 O4 177.8(3) . . . . ?
O3 C9 C10 O4 -2.7(5) . . . . ?
O4 C10 C11 C12 -177.7(3) . . . . ?
C9 C10 C11 C12 1.3(5) . . . . ?
C10 C11 C12 C7 -0.2(5) . . . . ?
C10 C11 C12 S4 -179.1(3) . . . . ?
C8 C7 C12 C11 -1.1(5) . . . . ?
S3 C7 C12 C11 -179.2(2) . . . . ?
C8 C7 C12 S4 177.8(2) . . . . ?
S3 C7 C12 S4 -0.3(4) . . . . ?
Ni2 S4 C12 C11 176.9(3) . . . . ?
Ni2 S4 C12 C7 -2.0(3) . . . . ?
C31 P1 C13 C14 3.2(4) . . . . ?
C25 P1 C13 C14 -117.1(3) . . . . ?
C19 P1 C13 C14 120.1(3) . . . . ?
C31 P1 C13 C18 -175.2(3) . . . . ?
C25 P1 C13 C18 64.5(3) . . . . ?
C19 P1 C13 C18 -58.3(3) . . . . ?
C18 C13 C14 C15 -1.0(5) . . . . ?
P1 C13 C14 C15 -179.4(3) . . . . ?
C13 C14 C15 C16 -1.2(6) . . . . ?
C14 C15 C16 C17 2.0(6) . . . . ?
C15 C16 C17 C18 -0.5(6) . . . . ?
C16 C17 C18 C13 -1.8(6) . . . . ?
C14 C13 C18 C17 2.5(6) . . . . ?
P1 C13 C18 C17 -179.0(3) . . . . ?
C13 P1 C19 C24 149.7(3) . . . . ?
C31 P1 C19 C24 -90.2(3) . . . . ?
C25 P1 C19 C24 29.5(4) . . . . ?
C13 P1 C19 C20 -36.2(3) . . . . ?
C31 P1 C19 C20 83.9(3) . . . . ?
C25 P1 C19 C20 -156.5(3) . . . . ?
C24 C19 C20 C21 2.2(6) . . . . ?
P1 C19 C20 C21 -172.1(3) . . . . ?
C19 C20 C21 C22 -1.1(7) . . . . ?
C20 C21 C22 C23 -0.5(7) . . . . ?
C21 C22 C23 C24 0.9(7) . . . . ?
C20 C19 C24 C23 -1.8(6) . . . . ?
P1 C19 C24 C23 172.2(3) . . . . ?
C22 C23 C24 C19 0.2(6) . . . . ?
C13 P1 C25 C30 13.4(3) . . . . ?
C31 P1 C25 C30 -109.0(3) . . . . ?
C19 P1 C25 C30 132.0(3) . . . . ?
C13 P1 C25 C26 -172.2(3) . . . . ?
C31 P1 C25 C26 65.4(3) . . . . ?
C19 P1 C25 C26 -53.5(3) . . . . ?
C30 C25 C26 C27 -1.9(5) . . . . ?
P1 C25 C26 C27 -176.4(3) . . . . ?
C25 C26 C27 C28 1.4(6) . . . . ?
C26 C27 C28 C29 0.2(6) . . . . ?
C27 C28 C29 C30 -1.2(6) . . . . ?
C26 C25 C30 C29 1.0(5) . . . . ?
P1 C25 C30 C29 175.4(3) . . . . ?
C28 C29 C30 C25 0.6(6) . . . . ?
C13 P1 C31 C36 58.0(3) . . . . ?
C25 P1 C31 C36 178.8(3) . . . . ?
C19 P1 C31 C36 -58.4(3) . . . . ?
C13 P1 C31 C32 -126.0(3) . . . . ?
C25 P1 C31 C32 -5.2(3) . . . . ?
C19 P1 C31 C32 117.5(3) . . . . ?
C36 C31 C32 C33 2.5(6) . . . . ?
P1 C31 C32 C33 -173.4(3) . . . . ?
C31 C32 C33 C34 -1.8(6) . . . . ?
C32 C33 C34 C35 -0.5(7) . . . . ?
C33 C34 C35 C36 1.9(6) . . . . ?
C34 C35 C36 C31 -1.1(6) . . . . ?
C32 C31 C36 C35 -1.1(5) . . . . ?
P1 C31 C36 C35 174.9(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O2 . . . 2.639(4) 0.820 2.179 115.7 no
O2 H2A O5 . . 2_765 2.692(4) 0.820 1.873 178.6 no
O3 H3 O5 . . 2_765 2.751(4) 0.820 1.948 166.0 no
O4 H4 O3 . . . 2.658(4) 0.820 2.211 114.5 no

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



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

data_sy01013_thfsalt_afterannealing
_database_code_depnum_ccdc_archive 'CCDC 2065216'
loop_
_audit_author_name
_audit_author_address
'So Yokomori'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;
_audit_creation_date             2020-11-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H7 Ni O4 S4, C24 H20 P, 0.5(C4 H8 O)'
_chemical_formula_sum            'C38 H29.50 Ni O4.50 P S4'
_chemical_formula_weight         776.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
# start Validation Reply Form
_vrf_PLAT420_sy01013_thfsalt_afterannealing 
;
PROBLEM: D-H Without Acceptor       O4       --H4A      .     Please Check 
RESPONSE:
The H4A atom was positionally disordered. One have proton acceptor
and the other have no proton acceptor, where there is space
available to place hydrogen atom. Thus, the results of this
analysis are not necessarily wrong.
;
# end Validation Reply Form
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3243(3)
_cell_length_b                   12.8682(3)
_cell_length_c                   13.4352(3)
_cell_angle_alpha                80.715(2)
_cell_angle_beta                 69.202(2)
_cell_angle_gamma                69.820(2)
_cell_volume                     1716.21(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10295
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5050
_cell_measurement_theta_min      2.1590
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Dark_Green
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             801
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14894
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.597
_diffrn_reflns_theta_min         2.147
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   60.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   60.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0370501000
_diffrn_orient_matrix_UB_12      0.0388041000
_diffrn_orient_matrix_UB_13      -0.0303673000
_diffrn_orient_matrix_UB_21      0.0459837000
_diffrn_orient_matrix_UB_22      -0.0264671000
_diffrn_orient_matrix_UB_23      -0.0472726000
_diffrn_orient_matrix_UB_31      -0.0385412000
_diffrn_orient_matrix_UB_32      -0.0353435000
_diffrn_orient_matrix_UB_33      0.0062225000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6830
_reflns_number_total             8604
_reflns_odcompleteness_completeness 81.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.53
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8604
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0368
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0410P)²+0.9474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O5-C37 = O5-C40
 1.44 with sigma of 0.02
 C37-C38 = C39-C40
 1.53 with sigma of 0.02
 C38-C39
 1.54 with sigma of 0.02
 O5-C38 = O5-C39 = C37-C39 = C38-C40
 2.38 with sigma of 0.04
 O5-C37 \\sim O5-C40
 with sigma of 0.02
 C37-C38 \\sim C38-C39 \\sim C39-C40
 with sigma of 0.02
 C38-C40 \\sim C37-C39
 with sigma of 0.04
 O5-C38 \\sim O5-C39
 with sigma of 0.04
 O4-H4A \\sim O4-H4B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O5, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H1(0.5) H3(0.5) H4A(0.5) O5(0.5) C37(0.5) H37A(0.5) H37B(0.5)
 C38(0.5) H38A(0.5) H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H4B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C36(H36), C5(H5), C33(H33), C8(H8), C11(H11), C00R(H00R), C34(H34),
 C28(H28), C35(H35), C22(H22), C26(H26), C20(H20), C27(H27), C30(H30), C16(H16),
  C18(H18), C29(H29), C14(H14), C15(H15), C21(H21), C24(H24), C23(H23), C17(H17)
6.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1), O3(H3), O4(H4A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.36011(2) 0.88624(2) 0.92238(2) 0.03273(8) Uani 1 1 d . . . . .
S4 S 0.30027(5) 0.88554(5) 0.78773(4) 0.03731(12) Uani 1 1 d . . . . .
S1 S 0.16159(5) 0.90141(5) 1.02825(4) 0.03917(12) Uani 1 1 d . . . . .
S2 S 0.42768(5) 0.88448(5) 1.05179(4) 0.03816(12) Uani 1 1 d . . . . .
P005 P 0.73313(5) 0.49242(4) 0.16810(4) 0.03556(12) Uani 1 1 d . . . . .
S3 S 0.55937(5) 0.87299(5) 0.82256(4) 0.04219(13) Uani 1 1 d . . . . .
O2 O 0.20557(16) 0.89726(16) 1.45280(12) 0.0513(4) Uani 1 1 d . . . . .
H2 H 0.135134 0.935298 1.492423 0.077 Uiso 1 1 calc R U . A 1
O1 O -0.03156(17) 0.91370(17) 1.43710(12) 0.0562(5) Uani 1 1 d . . . . .
H1 H -0.084907 0.888251 1.429638 0.084 Uiso 0.5 1 calc R U P . .
O3 O 0.77670(17) 0.86189(17) 0.41687(12) 0.0555(4) Uani 1 1 d . . . . .
H3 H 0.837093 0.870705 0.431256 0.083 Uiso 0.5 1 calc R U P . .
O4 O 0.56184(19) 0.85515(18) 0.38951(13) 0.0572(5) Uani 1 1 d D . . . .
H4A H 0.488980 0.856444 0.389397 0.086 Uiso 0.5 1 calc DR U P B 1
C31 C 0.7814(2) 0.61220(17) 0.16314(16) 0.0374(4) Uani 1 1 d . . . . .
C2 C 0.0597(2) 0.9073(2) 1.24686(17) 0.0417(5) Uani 1 1 d . . . . .
H2A H -0.021584 0.913194 1.240650 0.050 Uiso 1 1 calc R U . . .
C36 C 0.8946(2) 0.60607(19) 0.18503(18) 0.0441(5) Uani 1 1 d . . . . .
H36 H 0.948439 0.538086 0.203113 0.053 Uiso 1 1 calc R U . . .
C1 C 0.17012(19) 0.89931(16) 1.15505(15) 0.0332(4) Uani 1 1 d . . . . .
C4 C 0.1949(2) 0.89913(18) 1.35501(16) 0.0375(4) Uani 1 1 d . . . . .
C3 C 0.0692(2) 0.90649(19) 1.34692(17) 0.0403(5) Uani 1 1 d . . . . .
C5 C 0.3039(2) 0.89156(17) 1.26642(16) 0.0366(4) Uani 1 1 d . . . . .
H5 H 0.384769 0.886614 1.272960 0.044 Uiso 1 1 calc R U . . .
C33 C 0.7006(2) 0.71529(18) 0.13731(19) 0.0446(5) Uani 1 1 d . . . . .
H33 H 0.624120 0.719993 0.123273 0.054 Uiso 1 1 calc R U . . .
C13 C 0.8558(2) 0.36903(17) 0.19416(16) 0.0379(4) Uani 1 1 d . . . . .
C8 C 0.6759(2) 0.8663(2) 0.60751(17) 0.0426(5) Uani 1 1 d . . . . .
H8 H 0.753024 0.864914 0.618532 0.051 Uiso 1 1 calc R U . . .
C25 C 0.5793(2) 0.50423(17) 0.27606(17) 0.0397(5) Uani 1 1 d . . . . .
C12 C 0.4416(2) 0.87487(16) 0.67832(15) 0.0340(4) Uani 1 1 d . . . . .
C19 C 0.7152(2) 0.48382(18) 0.04183(17) 0.0395(5) Uani 1 1 d . . . . .
C6 C 0.29371(18) 0.89124(16) 1.16505(15) 0.0314(4) Uani 1 1 d . . . . .
C11 C 0.4417(2) 0.86946(18) 0.57426(17) 0.0390(5) Uani 1 1 d . . . . .
H11 H 0.365012 0.870717 0.562569 0.047 Uiso 1 1 calc R U . . .
C7 C 0.5606(2) 0.87093(17) 0.69446(16) 0.0355(4) Uani 1 1 d . . . . .
C00R C 0.7335(2) 0.80953(19) 0.13256(19) 0.0470(5) Uani 1 1 d . . . . .
H00R H 0.679369 0.877898 0.115466 0.056 Uiso 1 1 calc R U . . .
C34 C 0.8468(3) 0.8026(2) 0.1532(2) 0.0506(6) Uani 1 1 d . . . . .
H34 H 0.869688 0.866369 0.149103 0.061 Uiso 1 1 calc R U . . .
C28 C 0.3435(3) 0.5170(2) 0.4398(2) 0.0593(7) Uani 1 1 d . . . . .
H28 H 0.263511 0.521711 0.494153 0.071 Uiso 1 1 calc R U . . .
C9 C 0.6752(2) 0.86377(19) 0.50514(17) 0.0417(5) Uani 1 1 d . . . . .
C35 C 0.9268(3) 0.7014(2) 0.1798(2) 0.0544(6) Uani 1 1 d . . . . .
H35 H 1.002639 0.697467 0.194352 0.065 Uiso 1 1 calc R U . . .
C10 C 0.5563(2) 0.86233(19) 0.49099(16) 0.0407(5) Uani 1 1 d . . . . .
C22 C 0.6938(3) 0.4611(2) -0.1515(2) 0.0641(7) Uani 1 1 d . . . . .
H22 H 0.687799 0.453069 -0.216968 0.077 Uiso 1 1 calc R U . . .
C26 C 0.5341(3) 0.4129(2) 0.3079(2) 0.0557(6) Uani 1 1 d . . . . .
H26 H 0.583576 0.346528 0.273943 0.067 Uiso 1 1 calc R U . . .
C20 C 0.7509(3) 0.5547(2) -0.0440(2) 0.0575(7) Uani 1 1 d . . . . .
H20 H 0.782806 0.609773 -0.036822 0.069 Uiso 1 1 calc R U . . .
C27 C 0.4166(3) 0.4199(2) 0.3893(2) 0.0624(7) Uani 1 1 d . . . . .
H27 H 0.386701 0.358387 0.409992 0.075 Uiso 1 1 calc R U . . .
C30 C 0.5060(3) 0.6018(2) 0.3293(2) 0.0515(6) Uani 1 1 d . . . . .
H30 H 0.536145 0.663146 0.310395 0.062 Uiso 1 1 calc R U . . .
C16 C 1.0494(3) 0.1845(2) 0.2369(2) 0.0572(6) Uani 1 1 d . . . . .
H16 H 1.116479 0.123786 0.250712 0.069 Uiso 1 1 calc R U . . .
C18 C 0.9512(3) 0.3046(2) 0.11308(19) 0.0632(8) Uani 1 1 d . . . . .
H18 H 0.951195 0.322667 0.043216 0.076 Uiso 1 1 calc R U . . .
C29 C 0.3877(3) 0.6071(2) 0.4107(2) 0.0613(7) Uani 1 1 d . . . . .
H29 H 0.337915 0.672709 0.445865 0.074 Uiso 1 1 calc R U . . .
C14 C 0.8554(3) 0.3376(2) 0.2974(2) 0.0659(8) Uani 1 1 d . . . . .
H14 H 0.788936 0.378732 0.353412 0.079 Uiso 1 1 calc R U . . .
C15 C 0.9525(3) 0.2456(2) 0.3183(2) 0.0707(8) Uani 1 1 d . . . . .
H15 H 0.951754 0.225426 0.388112 0.085 Uiso 1 1 calc R U . . .
C21 C 0.7393(4) 0.5438(3) -0.1405(2) 0.0734(9) Uani 1 1 d . . . . .
H21 H 0.762184 0.592195 -0.197944 0.088 Uiso 1 1 calc R U . . .
C24 C 0.6674(3) 0.4027(2) 0.0294(2) 0.0588(7) Uani 1 1 d . . . . .
H24 H 0.641642 0.355377 0.087024 0.071 Uiso 1 1 calc R U . . .
C23 C 0.6577(3) 0.3915(2) -0.0676(2) 0.0643(8) Uani 1 1 d . . . . .
H23 H 0.626480 0.336236 -0.075387 0.077 Uiso 1 1 calc R U . . .
C17 C 1.0478(3) 0.2123(2) 0.1358(2) 0.0782(10) Uani 1 1 d . . . . .
H17 H 1.112480 0.168756 0.080618 0.094 Uiso 1 1 calc R U . . .
O5 O 0.0134(8) 0.5118(9) 0.5946(5) 0.118(2) Uani 0.5 1 d D U P C -1
C37 C -0.048(2) 0.6022(10) 0.5346(15) 0.115(4) Uani 0.5 1 d D U P C -1
H37A H -0.019791 0.665800 0.532015 0.138 Uiso 0.5 1 calc R U P C -1
H37B H -0.144451 0.623552 0.565904 0.138 Uiso 0.5 1 calc R U P C -1
C38 C -0.006(2) 0.5617(15) 0.4287(13) 0.125(5) Uani 0.5 1 d D U P C -1
H38A H 0.058543 0.594986 0.379162 0.150 Uiso 0.5 1 calc R U P C -1
H38B H -0.081532 0.580086 0.403562 0.150 Uiso 0.5 1 calc R U P C -1
C39 C 0.0543(19) 0.4393(14) 0.4371(13) 0.117(4) Uani 0.5 1 d D U P C -1
H39A H 0.011145 0.402527 0.409753 0.141 Uiso 0.5 1 calc R U P C -1
H39B H 0.148226 0.417914 0.396016 0.141 Uiso 0.5 1 calc R U P C -1
C40 C 0.0360(19) 0.4080(10) 0.5504(13) 0.123(5) Uani 0.5 1 d D U P C -1
H40A H -0.039883 0.380923 0.582810 0.147 Uiso 0.5 1 calc R U P C -1
H40B H 0.114654 0.351642 0.559921 0.147 Uiso 0.5 1 calc R U P C -1
H4B H 0.637(2) 0.861(3) 0.354(3) 0.020(9) Uiso 0.5 1 d D . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1474(6) . ?
Ni1 S1 2.1520(6) . ?
Ni1 S2 2.1282(6) . ?
Ni1 S3 2.1398(6) . ?
S4 C12 1.727(2) . ?
S1 C1 1.736(2) . ?
S2 C6 1.7137(19) . ?
P005 C31 1.789(2) . ?
P005 C13 1.794(2) . ?
P005 C25 1.805(2) . ?
P005 C19 1.803(2) . ?
S3 C7 1.720(2) . ?
O2 H2 0.8200 . ?
O2 C4 1.357(2) . ?
O1 H1 0.8200 . ?
O1 C3 1.327(2) . ?
O3 H3 0.8200 . ?
O3 C9 1.323(2) . ?
O4 H4A 0.8200 . ?
O4 C10 1.359(3) . ?
O4 H4B 0.835(19) . ?
C31 C36 1.388(3) . ?
C31 C33 1.399(3) . ?
C2 H2A 0.9300 . ?
C2 C1 1.397(3) . ?
C2 C3 1.384(3) . ?
C36 H36 0.9300 . ?
C36 C35 1.380(3) . ?
C1 C6 1.420(3) . ?
C4 C3 1.435(3) . ?
C4 C5 1.364(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.408(3) . ?
C33 H33 0.9300 . ?
C33 C00R 1.372(3) . ?
C13 C18 1.371(3) . ?
C13 C14 1.379(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.399(3) . ?
C8 C9 1.384(3) . ?
C25 C26 1.387(3) . ?
C25 C30 1.387(3) . ?
C12 C11 1.411(3) . ?
C12 C7 1.422(3) . ?
C19 C20 1.382(3) . ?
C19 C24 1.386(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.366(3) . ?
C00R H00R 0.9300 . ?
C00R C34 1.378(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.383(4) . ?
C28 H28 0.9300 . ?
C28 C27 1.367(4) . ?
C28 C29 1.365(4) . ?
C9 C10 1.432(3) . ?
C35 H35 0.9300 . ?
C22 H22 0.9300 . ?
C22 C21 1.380(4) . ?
C22 C23 1.357(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.375(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.382(4) . ?
C27 H27 0.9300 . ?
C30 H30 0.9300 . ?
C30 C29 1.384(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.359(4) . ?
C16 C17 1.353(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.387(4) . ?
C29 H29 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.380(4) . ?
C15 H15 0.9300 . ?
C21 H21 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.380(4) . ?
C23 H23 0.9300 . ?
C17 H17 0.9300 . ?
O5 C37 1.424(11) . ?
O5 C40 1.455(11) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.452(10) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.488(11) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.469(10) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ni1 S1 90.59(2) . . ?
S2 Ni1 S4 177.65(2) . . ?
S2 Ni1 S1 91.68(2) . . ?
S2 Ni1 S3 85.94(2) . . ?
S3 Ni1 S4 91.79(2) . . ?
S3 Ni1 S1 177.55(2) . . ?
C12 S4 Ni1 105.17(7) . . ?
C1 S1 Ni1 104.97(7) . . ?
C6 S2 Ni1 106.13(7) . . ?
C31 P005 C13 110.68(10) . . ?
C31 P005 C25 108.61(10) . . ?
C31 P005 C19 108.84(10) . . ?
C13 P005 C25 107.83(10) . . ?
C13 P005 C19 109.42(10) . . ?
C19 P005 C25 111.45(10) . . ?
C7 S3 Ni1 105.61(7) . . ?
C4 O2 H2 109.5 . . ?
C3 O1 H1 109.5 . . ?
C9 O3 H3 109.5 . . ?
C10 O4 H4A 109.5 . . ?
C10 O4 H4B 102(3) . . ?
C36 C31 P005 122.29(17) . . ?
C36 C31 C33 119.4(2) . . ?
C33 C31 P005 118.27(16) . . ?
C1 C2 H2A 119.4 . . ?
C3 C2 H2A 119.4 . . ?
C3 C2 C1 121.18(19) . . ?
C31 C36 H36 120.2 . . ?
C35 C36 C31 119.7(2) . . ?
C35 C36 H36 120.2 . . ?
C2 C1 S1 122.47(15) . . ?
C2 C1 C6 119.12(18) . . ?
C6 C1 S1 118.40(14) . . ?
O2 C4 C3 119.16(18) . . ?
O2 C4 C5 119.74(19) . . ?
C5 C4 C3 121.09(19) . . ?
O1 C3 C2 124.2(2) . . ?
O1 C3 C4 117.10(19) . . ?
C2 C3 C4 118.72(18) . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.81(18) . . ?
C6 C5 H5 120.1 . . ?
C31 C33 H33 119.8 . . ?
C00R C33 C31 120.4(2) . . ?
C00R C33 H33 119.8 . . ?
C18 C13 P005 121.27(17) . . ?
C18 C13 C14 118.8(2) . . ?
C14 C13 P005 119.96(17) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C9 C8 C7 120.0(2) . . ?
C26 C25 P005 119.16(17) . . ?
C26 C25 C30 119.1(2) . . ?
C30 C25 P005 121.75(17) . . ?
C11 C12 S4 121.68(16) . . ?
C11 C12 C7 119.60(18) . . ?
C7 C12 S4 118.72(15) . . ?
C20 C19 P005 121.56(18) . . ?
C20 C19 C24 119.0(2) . . ?
C24 C19 P005 119.44(18) . . ?
C1 C6 S2 118.78(15) . . ?
C5 C6 S2 121.13(15) . . ?
C5 C6 C1 120.07(17) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 C12 118.81(19) . . ?
C10 C11 H11 120.6 . . ?
C8 C7 S3 120.90(16) . . ?
C8 C7 C12 120.41(18) . . ?
C12 C7 S3 118.68(15) . . ?
C33 C00R H00R 120.1 . . ?
C33 C00R C34 119.8(2) . . ?
C34 C00R H00R 120.1 . . ?
C00R C34 H34 119.8 . . ?
C00R C34 C35 120.3(2) . . ?
C35 C34 H34 119.8 . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C29 C28 C27 120.2(2) . . ?
O3 C9 C8 125.5(2) . . ?
O3 C9 C10 115.78(19) . . ?
C8 C9 C10 118.68(19) . . ?
C36 C35 C34 120.4(2) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
O4 C10 C11 120.9(2) . . ?
O4 C10 C9 116.69(19) . . ?
C11 C10 C9 122.35(19) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C23 C22 C21 120.5(3) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.4(2) . . ?
C27 C26 H26 119.8 . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 120.0(3) . . ?
C21 C20 H20 120.0 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C25 C30 H30 120.2 . . ?
C29 C30 C25 119.6(2) . . ?
C29 C30 H30 120.2 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C17 C16 C15 119.7(2) . . ?
C13 C18 H18 120.2 . . ?
C13 C18 C17 119.7(2) . . ?
C17 C18 H18 120.2 . . ?
C28 C29 C30 120.6(2) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(2) . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 120.1(2) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C19 C24 H24 119.7 . . ?
C23 C24 C19 120.6(2) . . ?
C23 C24 H24 119.7 . . ?
C22 C23 C24 119.9(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C16 C17 C18 121.1(2) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C37 O5 C40 109.6(12) . . ?
O5 C37 H37A 110.7 . . ?
O5 C37 H37B 110.7 . . ?
O5 C37 C38 105.1(10) . . ?
H37A C37 H37B 108.8 . . ?
C38 C37 H37A 110.7 . . ?
C38 C37 H37B 110.7 . . ?
C37 C38 H38A 110.3 . . ?
C37 C38 H38B 110.3 . . ?
C37 C38 C39 107.0(8) . . ?
H38A C38 H38B 108.6 . . ?
C39 C38 H38A 110.3 . . ?
C39 C38 H38B 110.3 . . ?
C38 C39 H39A 110.3 . . ?
C38 C39 H39B 110.3 . . ?
H39A C39 H39B 108.5 . . ?
C40 C39 C38 107.2(8) . . ?
C40 C39 H39A 110.3 . . ?
C40 C39 H39B 110.3 . . ?
O5 C40 C39 102.6(10) . . ?
O5 C40 H40A 111.2 . . ?
O5 C40 H40B 111.2 . . ?
C39 C40 H40A 111.2 . . ?
C39 C40 H40B 111.2 . . ?
H40A C40 H40B 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_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 S4 C12 C11 178.59(16) . . . . ?
Ni1 S4 C12 C7 -1.09(18) . . . . ?
Ni1 S1 C1 C2 -179.93(17) . . . . ?
Ni1 S1 C1 C6 1.26(17) . . . . ?
Ni1 S2 C6 C1 -1.61(17) . . . . ?
Ni1 S2 C6 C5 179.92(15) . . . . ?
Ni1 S3 C7 C8 177.96(16) . . . . ?
Ni1 S3 C7 C12 -1.58(18) . . . . ?
S4 C12 C11 C10 179.27(17) . . . . ?
S4 C12 C7 S3 1.8(2) . . . . ?
S4 C12 C7 C8 -177.71(17) . . . . ?
S1 C1 C6 S2 0.2(2) . . . . ?
S1 C1 C6 C5 178.71(15) . . . . ?
P005 C31 C36 C35 179.95(18) . . . . ?
P005 C31 C33 C00R 179.98(18) . . . . ?
P005 C13 C18 C17 177.3(3) . . . . ?
P005 C13 C14 C15 -177.1(3) . . . . ?
P005 C25 C26 C27 -179.4(2) . . . . ?
P005 C25 C30 C29 179.2(2) . . . . ?
P005 C19 C20 C21 178.2(2) . . . . ?
P005 C19 C24 C23 -177.4(2) . . . . ?
O2 C4 C3 O1 1.5(3) . . . . ?
O2 C4 C3 C2 -179.4(2) . . . . ?
O2 C4 C5 C6 178.72(19) . . . . ?
O3 C9 C10 O4 2.3(3) . . . . ?
O3 C9 C10 C11 -176.7(2) . . . . ?
C31 P005 C13 C18 -97.2(2) . . . . ?
C31 P005 C13 C14 82.7(2) . . . . ?
C31 P005 C25 C26 -168.7(2) . . . . ?
C31 P005 C25 C30 10.2(2) . . . . ?
C31 P005 C19 C20 6.9(2) . . . . ?
C31 P005 C19 C24 -174.6(2) . . . . ?
C31 C36 C35 C34 0.1(4) . . . . ?
C31 C33 C00R C34 0.1(4) . . . . ?
C2 C1 C6 S2 -178.63(16) . . . . ?
C2 C1 C6 C5 -0.1(3) . . . . ?
C36 C31 C33 C00R 0.6(3) . . . . ?
C1 C2 C3 O1 -180.0(2) . . . . ?
C1 C2 C3 C4 1.0(3) . . . . ?
C4 C5 C6 S2 178.75(16) . . . . ?
C4 C5 C6 C1 0.3(3) . . . . ?
C3 C2 C1 S1 -179.33(17) . . . . ?
C3 C2 C1 C6 -0.5(3) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C5 C4 C3 O1 -179.9(2) . . . . ?
C5 C4 C3 C2 -0.8(3) . . . . ?
C33 C31 C36 C35 -0.8(3) . . . . ?
C33 C00R C34 C35 -0.8(4) . . . . ?
C13 P005 C31 C36 -4.4(2) . . . . ?
C13 P005 C31 C33 176.32(17) . . . . ?
C13 P005 C25 C26 -48.7(2) . . . . ?
C13 P005 C25 C30 130.2(2) . . . . ?
C13 P005 C19 C20 -114.1(2) . . . . ?
C13 P005 C19 C24 64.3(2) . . . . ?
C13 C18 C17 C16 0.1(5) . . . . ?
C13 C14 C15 C16 -0.5(5) . . . . ?
C8 C9 C10 O4 -177.3(2) . . . . ?
C8 C9 C10 C11 3.7(4) . . . . ?
C25 P005 C31 C36 113.82(19) . . . . ?
C25 P005 C31 C33 -65.5(2) . . . . ?
C25 P005 C13 C18 144.1(2) . . . . ?
C25 P005 C13 C14 -36.0(2) . . . . ?
C25 P005 C19 C20 126.7(2) . . . . ?
C25 P005 C19 C24 -54.8(2) . . . . ?
C25 C26 C27 C28 -0.3(5) . . . . ?
C25 C30 C29 C28 0.8(4) . . . . ?
C12 C11 C10 O4 179.0(2) . . . . ?
C12 C11 C10 C9 -2.1(3) . . . . ?
C19 P005 C31 C36 -124.66(19) . . . . ?
C19 P005 C31 C33 56.0(2) . . . . ?
C19 P005 C13 C18 22.7(3) . . . . ?
C19 P005 C13 C14 -157.4(2) . . . . ?
C19 P005 C25 C26 71.4(2) . . . . ?
C19 P005 C25 C30 -109.7(2) . . . . ?
C19 C20 C21 C22 -0.9(5) . . . . ?
C19 C24 C23 C22 -0.7(4) . . . . ?
C11 C12 C7 S3 -177.85(16) . . . . ?
C11 C12 C7 C8 2.6(3) . . . . ?
C7 C8 C9 O3 178.4(2) . . . . ?
C7 C8 C9 C10 -2.0(3) . . . . ?
C7 C12 C11 C10 -1.1(3) . . . . ?
C00R C34 C35 C36 0.7(4) . . . . ?
C9 C8 C7 S3 179.46(18) . . . . ?
C9 C8 C7 C12 -1.0(3) . . . . ?
C26 C25 C30 C29 -1.9(4) . . . . ?
C20 C19 C24 C23 1.1(4) . . . . ?
C27 C28 C29 C30 0.6(5) . . . . ?
C30 C25 C26 C27 1.6(4) . . . . ?
C18 C13 C14 C15 2.8(5) . . . . ?
C29 C28 C27 C26 -0.9(5) . . . . ?
C14 C13 C18 C17 -2.5(5) . . . . ?
C15 C16 C17 C18 2.2(5) . . . . ?
C21 C22 C23 C24 -0.5(5) . . . . ?
C24 C19 C20 C21 -0.3(4) . . . . ?
C23 C22 C21 C20 1.3(5) . . . . ?
C17 C16 C15 C14 -2.0(5) . . . . ?
O5 C37 C38 C39 13(2) . . . . ?
C37 O5 C40 C39 29.8(15) . . . . ?
C37 C38 C39 C40 5(3) . . . . ?
C38 C39 C40 O5 -20(2) . . . . ?
C40 O5 C37 C38 -27.2(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.876
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran. acetic acid, and hexane'
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 2065218'
loop_
_audit_author_name
_audit_author_address
'So Yokomori'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;
_audit_creation_date             2021-02-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'4(Br), C12 H8 Ni O4 S4, 4(C24 H20 P), 2(C3 H7 N O), 2(O)'
_chemical_formula_sum            'C114 H102 Br4 N2 Ni O8 P4 S4'
_chemical_formula_weight         2258.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
# start Validation Reply Form
_vrf_PLAT260_shelxl              
;
PROBLEM: Large Average Ueq of Residue Including        O4      0.771 Check 
RESPONSE:
This alert was due to the serious disordering of water molecule by
caused by thermal vibration. This disordering of water molecules
taken in as a crystal solvent was often observed. This arert is no
problem for discussing molecular and crystal structures except for
the location of water molecule.
;
_vrf_PLAT306_shelxl              
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O4 Check 
RESPONSE:
This O4 atom belongs to water molecule. In this crystal, due to the
serious disorder of teh water molecule above-mentioned, the position
of the hydrogen atoms cannot be determined.
;
# end Validation Reply Form
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4401(18)
_cell_length_b                   14.660(3)
_cell_length_c                   21.242(4)
_cell_angle_alpha                83.678(7)
_cell_angle_beta                 77.178(6)
_cell_angle_gamma                77.841(6)
_cell_volume                     2795.9(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.08
_shelx_estimated_absorpt_T_max   0.716
_shelx_estimated_absorpt_T_min   0.716
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.8148
_exptl_absorpt_correction_T_min  0.8148
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17805
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.076
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6590
_reflns_number_total             9594
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9594
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0642
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1156P)²+0.3439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2084
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Uiso: H1(0.10659) H2A(0.0792) H2(0.10239) H5(0.0736) H8(0.08709)
 H9(0.10689) H10(0.11549) H11(0.11689) H12(0.09439) H14(0.09099) H15(0.11849)
 H16(0.10239) H17(0.09709) H18(0.0755) H20(0.0802) H21(0.09399) H22(0.09579)
 H23(0.09349) H24(0.0778) H26(0.08729) H27(0.11679) H28(0.10549) H29(0.10369)
 H30(0.08709) H32(0.0757) H33(0.0843) H34(0.09089) H35(0.08779) H36(0.0786)
 H38(0.0735) H39(0.08969) H40(0.10289) H41(0.09239) H42(0.0795) H44(0.08549)
 H45(0.11999) H46(0.12299) H47(0.11599) H48(0.09399) H50(0.08629) H51(0.09829)
 H52(0.10299) H53(0.09849) H54(0.0774) H55(0.21859)
 Fixed X: Ni1(1) H1(1.17844) H2A(1.095921) H2(1.236488) H5(1.17433)
 H8(0.496559) H9(0.36631) H10(0.492439) H11(0.7459) H12(0.87396) H14(1.036399)
 H15(1.28178) H16(1.38464) H17(1.2433) H18(0.992909) H20(0.667991)
 H21(0.597529) H22(0.61503) H23(0.68801) H24(0.756949) H26(0.568351)
 H27(0.55517) H28(0.763181) H29(0.98893) H30(1.001161) H32(0.875489)
 H33(0.987419) H34(0.863911) H35(0.61471) H36(0.501841) H38(0.37296)
 H39(0.118791) H40(-0.01012) H41(0.121262) H42(0.37512) H44(0.445729)
 H45(0.5127) H46(0.75011) H47(0.917089) H48(0.85027) H50(0.611311)
 H51(0.703469) H52(0.81771) H53(0.85422) H54(0.75726) H55(0.19997)
 Fixed Y: Ni1(0) H1(0.00466) H2A(0.067321) H2(-0.276899) H5(-0.24401)
 H8(0.39591) H9(0.29519) H10(0.16765) H11(0.123211) H12(0.218161) H14(0.32553)
 H15(0.25586) H16(0.22159) H17(0.26294) H18(0.32962) H20(0.271029) H21(0.28139)
 H22(0.409689) H23(0.53616) H24(0.53156) H26(0.52415) H27(0.67866) H28(0.74326)
 H29(0.65617) H30(0.509469) H32(0.592529) H33(0.449479) H34(0.328331)
 H35(0.35002) H36(0.49169) H38(0.6422) H39(0.661222) H40(0.70916) H41(0.73394)
 H42(0.716519) H44(0.80715) H45(0.934129) H46(0.95797) H47(0.868661)
 H48(0.744929) H50(0.79612) H51(0.79197) H52(0.653381) H53(0.51821) H54(0.5193)
 H55(0.95976)
 Fixed Z: Ni1(0) H1(0.29358) H2A(0.20129) H2(0.25092) H5(0.151701) H8(0.18358)
 H9(0.258961) H10(0.30494) H11(0.27236) H12(0.198501) H14(0.189569)
 H15(0.158941) H16(0.05323) H17(-0.022561) H18(0.00509) H20(0.061761) H21(-
 0.03692) H22(-0.106639) H23(-0.07701) H24(0.01926) H26(0.193641) H27(0.216249)
 H28(0.19204) H29(0.14556) H30(0.11408) H32(0.328891) H33(0.29159) H34(0.30462)
 H35(0.35652) H36(0.401489) H38(0.34758) H39(0.373449) H40(0.475639)
 H41(0.55076) H42(0.52389) H44(0.332589) H45(0.26714) H46(0.248489) H47(0.3048)
 H48(0.3734) H50(0.494619) H51(0.5879) H52(0.63075) H53(0.57872) H54(0.48704)
 H55(0.61541)
3.a Everything fixed:
 H1, H2A, H2, H5, H8, H9, H10, H11, H12, H14, H15, H16, H17, H18, H20, H21,
 H22, H23, H24, H26, H27, H28, H29, H30, H32, H33, H34, H35, H36, H38, H39, H40,
  H41, H42, H44, H45, H46, H47, H48, H50, H51, H52, H53, H54, H55
3.b Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.23722(6) -0.43680(4) 0.24552(3) 0.0733(2) Uani 1 1 d . . . . .
Br2 Br -0.11492(8) 0.83643(4) 0.68442(3) 0.0891(3) Uani 1 1 d . . . . .
Ni1 Ni 1.000000 0.000000 0.000000 0.1057(5) Uani 1 2 d S . P . .
S1 S 1.0215(3) 0.07132(9) 0.07888(8) 0.0979(6) Uani 1 1 d . . . . .
S2 S 1.0624(3) -0.13393(10) 0.04775(8) 0.1032(7) Uani 1 1 d . . . . .
P1 P 0.79664(13) 0.38905(8) 0.12223(6) 0.0503(3) Uani 1 1 d . . . . .
P2 P 0.59757(13) 0.66269(9) 0.41103(6) 0.0507(3) Uani 1 1 d . . . . .
O1 O 1.1995(5) -0.0515(3) 0.28788(19) 0.0901(13) Uani 1 1 d . . . . .
O2 O 1.2429(5) -0.2250(2) 0.25993(19) 0.0842(12) Uani 1 1 d . . . . .
O3 O 0.3556(14) 0.8781(11) 0.5743(6) 0.287(6) Uani 1 1 d . . . . .
N1 N 0.2255(10) 0.9897(5) 0.5221(5) 0.141(3) Uani 1 1 d . . . . .
C1 C 1.0807(7) -0.0155(3) 0.1329(2) 0.0673(14) Uani 1 1 d . . . . .
C2 C 1.1129(6) 0.0049(3) 0.1906(2) 0.0635(13) Uani 1 1 d . . . . .
C3 C 1.1675(6) -0.0653(4) 0.2321(2) 0.0619(13) Uani 1 1 d . . . . .
C4 C 1.1905(6) -0.1609(3) 0.2166(2) 0.0589(12) Uani 1 1 d . . . . .
C5 C 1.1574(6) -0.1811(3) 0.1610(2) 0.0612(13) Uani 1 1 d . . . . .
C6 C 1.1012(6) -0.1098(3) 0.1187(2) 0.0641(14) Uani 1 1 d . . . . .
C7 C 0.6978(6) 0.3156(4) 0.1817(2) 0.0566(12) Uani 1 1 d . . . . .
C8 C 0.5447(6) 0.3408(4) 0.2012(3) 0.0718(15) Uani 1 1 d . . . . .
C9 C 0.4693(7) 0.2816(6) 0.2467(3) 0.0868(19) Uani 1 1 d . . . . .
C10 C 0.5412(9) 0.2042(5) 0.2730(3) 0.093(2) Uani 1 1 d . . . . .
C11 C 0.6924(10) 0.1785(4) 0.2557(3) 0.100(2) Uani 1 1 d . . . . .
C12 C 0.7715(7) 0.2346(4) 0.2093(3) 0.0760(16) Uani 1 1 d . . . . .
C13 C 0.9865(5) 0.3355(3) 0.1004(2) 0.0546(11) Uani 1 1 d . . . . .
C14 C 1.0757(6) 0.3130(4) 0.1465(3) 0.0744(15) Uani 1 1 d . . . . .
C15 C 1.2223(7) 0.2698(5) 0.1291(4) 0.093(2) Uani 1 1 d . . . . .
C16 C 1.2834(7) 0.2514(5) 0.0652(4) 0.0871(18) Uani 1 1 d . . . . .
C17 C 1.2000(7) 0.2750(4) 0.0196(3) 0.0785(16) Uani 1 1 d . . . . .
C18 C 1.0494(6) 0.3159(3) 0.0368(2) 0.0615(12) Uani 1 1 d . . . . .
C19 C 0.7198(5) 0.4012(3) 0.0516(2) 0.0542(11) Uani 1 1 d . . . . .
C20 C 0.6704(6) 0.3257(4) 0.0339(2) 0.0635(13) Uani 1 1 d . . . . .
C21 C 0.6312(7) 0.3304(5) -0.0246(3) 0.0768(16) Uani 1 1 d . . . . .
C22 C 0.6383(7) 0.4074(5) -0.0664(3) 0.0804(17) Uani 1 1 d . . . . .
C23 C 0.6854(6) 0.4833(5) -0.0496(3) 0.0778(17) Uani 1 1 d . . . . .
C24 C 0.7262(6) 0.4806(4) 0.0087(3) 0.0650(13) Uani 1 1 d . . . . .
C25 C 0.7859(5) 0.5031(3) 0.1489(2) 0.0543(11) Uani 1 1 d . . . . .
C26 C 0.6521(6) 0.5532(4) 0.1811(3) 0.0707(14) Uani 1 1 d . . . . .
C27 C 0.6453(7) 0.6434(5) 0.1964(4) 0.0893(19) Uani 1 1 d . . . . .
C28 C 0.7694(9) 0.6816(4) 0.1828(3) 0.0856(18) Uani 1 1 d . . . . .
C29 C 0.9016(7) 0.6318(5) 0.1533(3) 0.0880(19) Uani 1 1 d . . . . .
C30 C 0.9103(6) 0.5424(4) 0.1356(3) 0.0722(15) Uani 1 1 d . . . . .
C31 C 0.6770(5) 0.5563(3) 0.3711(2) 0.0513(11) Uani 1 1 d . . . . .
C32 C 0.8233(5) 0.5430(4) 0.3365(2) 0.0609(12) Uani 1 1 d . . . . .
C33 C 0.8887(6) 0.4585(4) 0.3130(3) 0.0689(14) Uani 1 1 d . . . . .
C34 C 0.8140(7) 0.3863(4) 0.3207(3) 0.0739(15) Uani 1 1 d . . . . .
C35 C 0.6682(7) 0.3990(4) 0.3521(3) 0.0730(15) Uani 1 1 d . . . . .
C36 C 0.6004(6) 0.4834(4) 0.3783(2) 0.0634(13) Uani 1 1 d . . . . .
C37 C 0.4001(5) 0.6752(3) 0.4335(2) 0.0515(11) Uani 1 1 d . . . . .
C38 C 0.3217(5) 0.6599(4) 0.3887(2) 0.0612(13) Uani 1 1 d . . . . .
C39 C 0.1688(6) 0.6726(4) 0.4046(3) 0.0732(15) Uani 1 1 d . . . . .
C40 C 0.0949(6) 0.7007(5) 0.4646(3) 0.0827(18) Uani 1 1 d . . . . .
C41 C 0.1714(6) 0.7164(5) 0.5091(3) 0.0771(16) Uani 1 1 d . . . . .
C42 C 0.3242(6) 0.7046(4) 0.4936(2) 0.0659(13) Uani 1 1 d . . . . .
C43 C 0.6414(5) 0.7625(3) 0.3595(2) 0.0547(11) Uani 1 1 d . . . . .
C44 C 0.5407(6) 0.8189(4) 0.3281(3) 0.0696(14) Uani 1 1 d . . . . .
C45 C 0.5809(9) 0.8944(5) 0.2872(4) 0.098(2) Uani 1 1 d . . . . .
C46 C 0.7224(10) 0.9107(5) 0.2777(4) 0.102(2) Uani 1 1 d . . . . .
C47 C 0.8234(8) 0.8563(5) 0.3102(4) 0.098(2) Uani 1 1 d . . . . .
C48 C 0.7840(6) 0.7814(4) 0.3506(3) 0.0769(16) Uani 1 1 d . . . . .
C49 C 0.6746(5) 0.6579(4) 0.4817(2) 0.0569(12) Uani 1 1 d . . . . .
C50 C 0.6584(6) 0.7395(4) 0.5122(3) 0.0697(14) Uani 1 1 d . . . . .
C51 C 0.7130(6) 0.7375(5) 0.5674(3) 0.0797(17) Uani 1 1 d . . . . .
C52 C 0.7839(7) 0.6552(6) 0.5922(3) 0.0854(19) Uani 1 1 d . . . . .
C53 C 0.8028(7) 0.5736(5) 0.5623(3) 0.0806(17) Uani 1 1 d . . . . .
C54 C 0.7476(6) 0.5744(4) 0.5066(3) 0.0627(13) Uani 1 1 d . . . . .
C55 C 0.2553(16) 0.9424(10) 0.5740(7) 0.186(6) Uani 1 1 d . . . . .
C56 C 0.0889(17) 1.0627(9) 0.5346(8) 0.244(8) Uani 1 1 d . . . . .
H56A H 0.003731 1.034282 0.540143 0.366 Uiso 1 1 calc R U . . .
H56B H 0.089474 1.108466 0.498659 0.366 Uiso 1 1 calc R U . . .
H56C H 0.085208 1.092388 0.573197 0.366 Uiso 1 1 calc R U . . .
C57 C 0.332(2) 0.9693(12) 0.4612(6) 0.253(9) Uani 1 1 d . . . . .
H57A H 0.395308 1.014490 0.451356 0.380 Uiso 1 1 calc R U . . .
H57B H 0.279403 0.972296 0.426907 0.380 Uiso 1 1 calc R U . . .
H57C H 0.390573 0.907815 0.465433 0.380 Uiso 1 1 calc R U . . .
H1 H 1.178440 0.004660 0.293580 0.107 Uiso 1 1 d . U . . .
H2A H 1.095921 0.067321 0.201290 0.079 Uiso 1 1 d . U . . .
H2 H 1.236488 -0.276899 0.250920 0.102 Uiso 1 1 d . U . . .
H5 H 1.174330 -0.244010 0.151701 0.074 Uiso 1 1 d . U . . .
H8 H 0.496559 0.395910 0.183580 0.087 Uiso 1 1 d . U . . .
H9 H 0.366310 0.295190 0.258961 0.107 Uiso 1 1 d . U . . .
H10 H 0.492439 0.167650 0.304940 0.115 Uiso 1 1 d . U . . .
H11 H 0.745900 0.123211 0.272360 0.117 Uiso 1 1 d . U . . .
H12 H 0.873960 0.218161 0.198501 0.094 Uiso 1 1 d . U . . .
H14 H 1.036400 0.325530 0.189569 0.091 Uiso 1 1 d . U . . .
H15 H 1.281780 0.255860 0.158941 0.118 Uiso 1 1 d . U . . .
H16 H 1.384640 0.221590 0.053230 0.102 Uiso 1 1 d . U . . .
H17 H 1.243301 0.262940 -0.022561 0.097 Uiso 1 1 d . U . . .
H18 H 0.992909 0.329620 0.005090 0.075 Uiso 1 1 d . U . . .
H20 H 0.667991 0.271029 0.061761 0.080 Uiso 1 1 d . U . . .
H21 H 0.597529 0.281390 -0.036920 0.094 Uiso 1 1 d . U . . .
H22 H 0.615030 0.409689 -0.106639 0.096 Uiso 1 1 d . U . . .
H23 H 0.688010 0.536160 -0.077010 0.093 Uiso 1 1 d . U . . .
H24 H 0.756949 0.531560 0.019260 0.078 Uiso 1 1 d . U . . .
H26 H 0.568351 0.524150 0.193641 0.087 Uiso 1 1 d . U . . .
H27 H 0.555170 0.678660 0.216249 0.117 Uiso 1 1 d . U . . .
H28 H 0.763181 0.743260 0.192040 0.105 Uiso 1 1 d . U . . .
H29 H 0.988930 0.656170 0.145560 0.104 Uiso 1 1 d . U . . .
H30 H 1.001160 0.509469 0.114080 0.087 Uiso 1 1 d . U . . .
H32 H 0.875489 0.592529 0.328891 0.076 Uiso 1 1 d . U . . .
H33 H 0.987419 0.449479 0.291590 0.084 Uiso 1 1 d . U . . .
H34 H 0.863911 0.328331 0.304620 0.091 Uiso 1 1 d . U . . .
H35 H 0.614710 0.350020 0.356520 0.088 Uiso 1 1 d . U . . .
H36 H 0.501841 0.491690 0.401489 0.079 Uiso 1 1 d . U . . .
H38 H 0.372960 0.642200 0.347580 0.073 Uiso 1 1 d . U . . .
H39 H 0.118791 0.661222 0.373449 0.090 Uiso 1 1 d . U . . .
H40 H -0.010120 0.709160 0.475639 0.103 Uiso 1 1 d . U . . .
H41 H 0.121262 0.733940 0.550760 0.092 Uiso 1 1 d . U . . .
H42 H 0.375120 0.716519 0.523890 0.079 Uiso 1 1 d . U . . .
H44 H 0.445729 0.807150 0.332589 0.085 Uiso 1 1 d . U . . .
H45 H 0.512700 0.934129 0.267140 0.120 Uiso 1 1 d . U . . .
H46 H 0.750110 0.957970 0.248489 0.123 Uiso 1 1 d . U . . .
H47 H 0.917089 0.868661 0.304800 0.116 Uiso 1 1 d . U . . .
H48 H 0.850270 0.744929 0.373400 0.094 Uiso 1 1 d . U . . .
H50 H 0.611311 0.796120 0.494619 0.086 Uiso 1 1 d . U . . .
H51 H 0.703469 0.791970 0.587900 0.098 Uiso 1 1 d . U . . .
H52 H 0.817710 0.653381 0.630750 0.103 Uiso 1 1 d . U . . .
H53 H 0.854220 0.518210 0.578720 0.098 Uiso 1 1 d . U . . .
H54 H 0.757260 0.519300 0.487040 0.077 Uiso 1 1 d . U . . .
H55 H 0.199970 0.959760 0.615410 0.219 Uiso 1 1 d . U . . .
O4 O 0.5355(13) 0.985(2) 0.1065(8) 0.77(3) Uani 1 1 d . . . . .


_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 2.1375(14) 2_755 ?
Ni1 S1 2.1375(14) . ?
Ni1 S2 2.1378(14) 2_755 ?
Ni1 S2 2.1378(14) . ?
S1 C1 1.706(5) . ?
S2 C6 1.716(5) . ?
P1 C7 1.797(5) . ?
P1 C13 1.779(5) . ?
P1 C19 1.784(5) . ?
P1 C25 1.799(5) . ?
P2 C31 1.798(5) . ?
P2 C37 1.794(4) . ?
P2 C43 1.793(5) . ?
P2 C49 1.798(5) . ?
O1 C3 1.332(6) . ?
O1 H1 0.8217 . ?
O2 C4 1.339(5) . ?
O2 H2 0.8218 . ?
O3 C55 1.187(13) . ?
N1 C55 1.289(15) . ?
N1 C56 1.486(13) . ?
N1 C57 1.468(15) . ?
C1 C2 1.405(7) . ?
C1 C6 1.412(7) . ?
C2 C3 1.371(7) . ?
C2 H2A 0.9388 . ?
C3 C4 1.436(7) . ?
C4 C5 1.362(7) . ?
C5 C6 1.398(6) . ?
C5 H5 0.9381 . ?
C7 C8 1.392(7) . ?
C7 C12 1.384(8) . ?
C8 C9 1.402(8) . ?
C8 H8 0.9233 . ?
C9 C10 1.329(10) . ?
C9 H9 0.9327 . ?
C10 C11 1.373(10) . ?
C10 H10 0.9190 . ?
C11 C12 1.399(8) . ?
C11 H11 0.9386 . ?
C12 H12 0.9282 . ?
C13 C14 1.398(7) . ?
C13 C18 1.383(7) . ?
C14 C15 1.381(9) . ?
C14 H14 0.9307 . ?
C15 C16 1.385(10) . ?
C15 H15 0.9165 . ?
C16 C17 1.352(9) . ?
C16 H16 0.9535 . ?
C17 C18 1.405(8) . ?
C17 H17 0.9171 . ?
C18 H18 0.9298 . ?
C19 C20 1.403(7) . ?
C19 C24 1.399(7) . ?
C20 C21 1.363(7) . ?
C20 H20 0.9437 . ?
C21 C22 1.362(9) . ?
C21 H21 0.9282 . ?
C22 C23 1.388(9) . ?
C22 H22 0.9238 . ?
C23 C24 1.372(8) . ?
C23 H23 0.9176 . ?
C24 H24 0.9212 . ?
C25 C26 1.393(7) . ?
C25 C30 1.376(7) . ?
C26 C27 1.380(8) . ?
C26 H26 0.9492 . ?
C27 C28 1.364(9) . ?
C27 H27 0.9340 . ?
C28 C29 1.362(9) . ?
C28 H28 0.9331 . ?
C29 C30 1.383(8) . ?
C29 H29 0.9416 . ?
C30 H30 0.9367 . ?
C31 C32 1.398(7) . ?
C31 C36 1.388(7) . ?
C32 C33 1.357(8) . ?
C32 H32 0.9408 . ?
C33 C34 1.367(8) . ?
C33 H33 0.9307 . ?
C34 C35 1.373(8) . ?
C34 H34 0.9407 . ?
C35 C36 1.381(8) . ?
C35 H35 0.9476 . ?
C36 H36 0.9407 . ?
C37 C38 1.391(7) . ?
C37 C42 1.384(7) . ?
C38 C39 1.384(7) . ?
C38 H38 0.9349 . ?
C39 C40 1.372(8) . ?
C39 H39 0.9407 . ?
C40 C41 1.374(8) . ?
C40 H40 0.9510 . ?
C41 C42 1.384(7) . ?
C41 H41 0.9406 . ?
C42 H42 0.9342 . ?
C43 C44 1.364(7) . ?
C43 C48 1.399(7) . ?
C44 C45 1.393(8) . ?
C44 H44 0.9304 . ?
C45 C46 1.373(10) . ?
C45 H45 0.9196 . ?
C46 C47 1.369(10) . ?
C46 H46 0.9183 . ?
C47 C48 1.379(8) . ?
C47 H47 0.9198 . ?
C48 H48 0.9216 . ?
C49 C50 1.386(7) . ?
C49 C54 1.384(7) . ?
C50 C51 1.377(7) . ?
C50 H50 0.9367 . ?
C51 C52 1.363(9) . ?
C51 H51 0.9292 . ?
C52 C53 1.376(9) . ?
C52 H52 0.9386 . ?
C53 C54 1.392(7) . ?
C53 H53 0.9291 . ?
C54 H54 0.9280 . ?
C55 H55 0.9493 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S1 180.0 2_755 . ?
S1 Ni1 S2 87.89(5) 2_755 . ?
S1 Ni1 S2 92.11(5) . . ?
S1 Ni1 S2 92.11(5) 2_755 2_755 ?
S1 Ni1 S2 87.89(5) . 2_755 ?
S2 Ni1 S2 180.0 2_755 . ?
C1 S1 Ni1 104.76(18) . . ?
C6 S2 Ni1 104.76(17) . . ?
C7 P1 C25 113.2(2) . . ?
C13 P1 C7 110.5(2) . . ?
C13 P1 C19 107.6(2) . . ?
C13 P1 C25 108.4(2) . . ?
C19 P1 C7 107.7(2) . . ?
C19 P1 C25 109.3(2) . . ?
C37 P2 C31 110.3(2) . . ?
C37 P2 C49 110.2(2) . . ?
C43 P2 C31 111.0(2) . . ?
C43 P2 C37 108.7(2) . . ?
C43 P2 C49 108.4(2) . . ?
C49 P2 C31 108.2(2) . . ?
C3 O1 H1 109.2 . . ?
C4 O2 H2 108.6 . . ?
C55 N1 C56 113.0(11) . . ?
C55 N1 C57 117.5(11) . . ?
C57 N1 C56 129.4(12) . . ?
C2 C1 S1 121.3(4) . . ?
C2 C1 C6 119.2(4) . . ?
C6 C1 S1 119.5(4) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 C1 120.8(4) . . ?
C3 C2 H2A 119.5 . . ?
O1 C3 C2 124.2(5) . . ?
O1 C3 C4 116.2(4) . . ?
C2 C3 C4 119.6(4) . . ?
O2 C4 C3 115.6(4) . . ?
O2 C4 C5 124.5(4) . . ?
C5 C4 C3 119.8(4) . . ?
C4 C5 C6 120.9(4) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 120.8 . . ?
C1 C6 S2 118.8(4) . . ?
C5 C6 S2 121.4(4) . . ?
C5 C6 C1 119.8(4) . . ?
C8 C7 P1 119.6(4) . . ?
C12 C7 P1 121.1(4) . . ?
C12 C7 C8 119.3(5) . . ?
C7 C8 C9 118.8(6) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 122.3 . . ?
C8 C9 H9 120.7 . . ?
C10 C9 C8 121.4(6) . . ?
C10 C9 H9 117.9 . . ?
C9 C10 C11 121.0(6) . . ?
C9 C10 H10 121.4 . . ?
C11 C10 H10 117.5 . . ?
C10 C11 C12 119.3(6) . . ?
C10 C11 H11 122.9 . . ?
C12 C11 H11 117.7 . . ?
C7 C12 C11 120.1(6) . . ?
C7 C12 H12 120.5 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 P1 121.1(4) . . ?
C18 C13 P1 120.4(4) . . ?
C18 C13 C14 118.6(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 C13 120.5(6) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C16 120.0(6) . . ?
C14 C15 H15 121.0 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.3(6) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C18 120.4(6) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 H17 120.9 . . ?
C13 C18 C17 120.2(5) . . ?
C13 C18 H18 120.6 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 P1 119.9(4) . . ?
C24 C19 P1 120.6(4) . . ?
C24 C19 C20 119.0(5) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 119.7(5) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 121.0 . . ?
C22 C21 C20 121.3(5) . . ?
C22 C21 H21 117.8 . . ?
C21 C22 C23 119.9(5) . . ?
C21 C22 H22 121.2 . . ?
C23 C22 H22 118.9 . . ?
C22 C23 H23 120.6 . . ?
C24 C23 C22 120.3(5) . . ?
C24 C23 H23 119.2 . . ?
C19 C24 H24 120.9 . . ?
C23 C24 C19 119.8(5) . . ?
C23 C24 H24 119.3 . . ?
C26 C25 P1 120.8(4) . . ?
C30 C25 P1 119.6(4) . . ?
C30 C25 C26 119.6(5) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 C25 119.2(5) . . ?
C27 C26 H26 121.2 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.5(6) . . ?
C28 C27 H27 119.5 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.5(5) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 C30 120.1(5) . . ?
C28 C29 H29 121.3 . . ?
C30 C29 H29 118.6 . . ?
C25 C30 C29 120.0(5) . . ?
C25 C30 H30 120.6 . . ?
C29 C30 H30 119.4 . . ?
C32 C31 P2 119.5(4) . . ?
C36 C31 P2 121.3(4) . . ?
C36 C31 C32 118.9(5) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 C31 119.4(5) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 C34 121.8(5) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 119.4 . . ?
C33 C34 C35 119.8(5) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 H34 121.0 . . ?
C34 C35 C36 119.6(5) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 H36 119.5 . . ?
C35 C36 C31 120.5(5) . . ?
C35 C36 H36 120.0 . . ?
C38 C37 P2 119.5(3) . . ?
C42 C37 P2 120.9(4) . . ?
C42 C37 C38 119.6(4) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 C37 120.1(5) . . ?
C39 C38 H38 120.4 . . ?
C38 C39 H39 118.2 . . ?
C40 C39 C38 119.8(5) . . ?
C40 C39 H39 122.0 . . ?
C39 C40 C41 120.5(5) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C42 120.2(5) . . ?
C40 C41 H41 120.7 . . ?
C42 C41 H41 119.0 . . ?
C37 C42 C41 119.8(5) . . ?
C37 C42 H42 120.6 . . ?
C41 C42 H42 119.6 . . ?
C44 C43 P2 121.8(4) . . ?
C44 C43 C48 119.6(5) . . ?
C48 C43 P2 118.6(4) . . ?
C43 C44 C45 119.8(6) . . ?
C43 C44 H44 121.2 . . ?
C45 C44 H44 119.0 . . ?
C44 C45 H45 120.3 . . ?
C46 C45 C44 120.0(6) . . ?
C46 C45 H45 119.6 . . ?
C45 C46 H46 119.5 . . ?
C47 C46 C45 120.9(6) . . ?
C47 C46 H46 119.6 . . ?
C46 C47 C48 119.2(6) . . ?
C46 C47 H47 120.7 . . ?
C48 C47 H47 120.2 . . ?
C43 C48 H48 119.4 . . ?
C47 C48 C43 120.5(6) . . ?
C47 C48 H48 120.1 . . ?
C50 C49 P2 119.0(4) . . ?
C54 C49 P2 121.3(4) . . ?
C54 C49 C50 119.7(4) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 C49 120.3(5) . . ?
C51 C50 H50 120.2 . . ?
C50 C51 H51 120.9 . . ?
C52 C51 C50 120.0(6) . . ?
C52 C51 H51 119.2 . . ?
C51 C52 C53 120.7(5) . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 119.3 . . ?
C52 C53 C54 120.0(6) . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C49 C54 C53 119.4(5) . . ?
C49 C54 H54 120.3 . . ?
C53 C54 H54 120.3 . . ?
O3 C55 N1 123.7(15) . . ?
O3 C55 H55 115.2 . . ?
N1 C55 H55 120.9 . . ?
N1 C56 H56A 109.5 . . ?
N1 C56 H56B 109.5 . . ?
N1 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N1 C57 H57A 109.5 . . ?
N1 C57 H57B 109.5 . . ?
N1 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 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 S1 C1 C2 177.6(5) . . . . ?
Ni1 S1 C1 C6 -0.9(6) . . . . ?
Ni1 S2 C6 C1 2.6(5) . . . . ?
Ni1 S2 C6 C5 -175.0(5) . . . . ?
S1 C1 C2 C3 -176.7(5) . . . . ?
S1 C1 C6 S2 -1.1(7) . . . . ?
S1 C1 C6 C5 176.5(5) . . . . ?
P1 C7 C8 C9 178.7(4) . . . . ?
P1 C7 C12 C11 179.7(5) . . . . ?
P1 C13 C14 C15 178.8(5) . . . . ?
P1 C13 C18 C17 179.0(4) . . . . ?
P1 C19 C20 C21 -170.8(4) . . . . ?
P1 C19 C24 C23 171.0(4) . . . . ?
P1 C25 C26 C27 -174.9(5) . . . . ?
P1 C25 C30 C29 177.0(5) . . . . ?
P2 C31 C32 C33 172.1(4) . . . . ?
P2 C31 C36 C35 -174.0(4) . . . . ?
P2 C37 C38 C39 -177.7(4) . . . . ?
P2 C37 C42 C41 178.1(4) . . . . ?
P2 C43 C44 C45 -178.4(5) . . . . ?
P2 C43 C48 C47 178.6(5) . . . . ?
P2 C49 C50 C51 178.4(4) . . . . ?
P2 C49 C54 C53 -178.7(4) . . . . ?
O1 C3 C4 O2 -0.6(7) . . . . ?
O1 C3 C4 C5 178.6(5) . . . . ?
O2 C4 C5 C6 179.1(5) . . . . ?
C1 C2 C3 O1 -179.4(6) . . . . ?
C1 C2 C3 C4 -0.7(9) . . . . ?
C2 C1 C6 S2 -179.6(5) . . . . ?
C2 C1 C6 C5 -2.1(9) . . . . ?
C2 C3 C4 O2 -179.5(5) . . . . ?
C2 C3 C4 C5 -0.3(8) . . . . ?
C3 C4 C5 C6 0.0(8) . . . . ?
C4 C5 C6 S2 178.7(4) . . . . ?
C4 C5 C6 C1 1.2(9) . . . . ?
C6 C1 C2 C3 1.8(9) . . . . ?
C7 P1 C13 C14 -60.0(5) . . . . ?
C7 P1 C13 C18 120.6(4) . . . . ?
C7 P1 C19 C20 -35.6(5) . . . . ?
C7 P1 C19 C24 153.1(4) . . . . ?
C7 P1 C25 C26 -44.0(5) . . . . ?
C7 P1 C25 C30 138.1(4) . . . . ?
C7 C8 C9 C10 2.5(9) . . . . ?
C8 C7 C12 C11 0.5(9) . . . . ?
C8 C9 C10 C11 -1.2(11) . . . . ?
C9 C10 C11 C12 -0.4(11) . . . . ?
C10 C11 C12 C7 0.8(10) . . . . ?
C12 C7 C8 C9 -2.1(8) . . . . ?
C13 P1 C7 C8 -174.3(4) . . . . ?
C13 P1 C7 C12 6.5(5) . . . . ?
C13 P1 C19 C20 83.6(4) . . . . ?
C13 P1 C19 C24 -87.7(4) . . . . ?
C13 P1 C25 C26 -167.0(4) . . . . ?
C13 P1 C25 C30 15.1(5) . . . . ?
C13 C14 C15 C16 2.3(10) . . . . ?
C14 C13 C18 C17 -0.5(8) . . . . ?
C14 C15 C16 C17 -0.4(11) . . . . ?
C15 C16 C17 C18 -1.8(10) . . . . ?
C16 C17 C18 C13 2.3(9) . . . . ?
C18 C13 C14 C15 -1.8(9) . . . . ?
C19 P1 C7 C8 -57.0(5) . . . . ?
C19 P1 C7 C12 123.7(4) . . . . ?
C19 P1 C13 C14 -177.3(4) . . . . ?
C19 P1 C13 C18 3.3(5) . . . . ?
C19 P1 C25 C26 76.1(5) . . . . ?
C19 P1 C25 C30 -101.8(4) . . . . ?
C19 C20 C21 C22 -0.3(9) . . . . ?
C20 C19 C24 C23 -0.4(7) . . . . ?
C20 C21 C22 C23 -0.3(9) . . . . ?
C21 C22 C23 C24 0.6(9) . . . . ?
C22 C23 C24 C19 -0.3(8) . . . . ?
C24 C19 C20 C21 0.7(8) . . . . ?
C25 P1 C7 C8 63.9(5) . . . . ?
C25 P1 C7 C12 -115.3(4) . . . . ?
C25 P1 C13 C14 64.6(5) . . . . ?
C25 P1 C13 C18 -114.8(4) . . . . ?
C25 P1 C19 C20 -158.9(4) . . . . ?
C25 P1 C19 C24 29.7(5) . . . . ?
C25 C26 C27 C28 -2.9(10) . . . . ?
C26 C25 C30 C29 -0.9(9) . . . . ?
C26 C27 C28 C29 0.7(11) . . . . ?
C27 C28 C29 C30 1.3(11) . . . . ?
C28 C29 C30 C25 -1.2(10) . . . . ?
C30 C25 C26 C27 3.0(9) . . . . ?
C31 P2 C37 C38 -46.5(5) . . . . ?
C31 P2 C37 C42 136.7(4) . . . . ?
C31 P2 C43 C44 102.6(5) . . . . ?
C31 P2 C43 C48 -76.2(5) . . . . ?
C31 P2 C49 C50 165.0(4) . . . . ?
C31 P2 C49 C54 -16.0(5) . . . . ?
C31 C32 C33 C34 1.7(8) . . . . ?
C32 C31 C36 C35 0.4(7) . . . . ?
C32 C33 C34 C35 1.0(8) . . . . ?
C33 C34 C35 C36 -3.0(8) . . . . ?
C34 C35 C36 C31 2.3(8) . . . . ?
C36 C31 C32 C33 -2.3(7) . . . . ?
C37 P2 C31 C32 165.3(4) . . . . ?
C37 P2 C31 C36 -20.3(5) . . . . ?
C37 P2 C43 C44 -18.9(5) . . . . ?
C37 P2 C43 C48 162.4(4) . . . . ?
C37 P2 C49 C50 -74.4(5) . . . . ?
C37 P2 C49 C54 104.7(4) . . . . ?
C37 C38 C39 C40 0.2(9) . . . . ?
C38 C37 C42 C41 1.4(8) . . . . ?
C38 C39 C40 C41 0.0(10) . . . . ?
C39 C40 C41 C42 0.5(10) . . . . ?
C40 C41 C42 C37 -1.2(9) . . . . ?
C42 C37 C38 C39 -0.9(8) . . . . ?
C43 P2 C31 C32 44.7(4) . . . . ?
C43 P2 C31 C36 -140.9(4) . . . . ?
C43 P2 C37 C38 75.4(5) . . . . ?
C43 P2 C37 C42 -101.3(4) . . . . ?
C43 P2 C49 C50 44.5(5) . . . . ?
C43 P2 C49 C54 -136.5(4) . . . . ?
C43 C44 C45 C46 1.3(10) . . . . ?
C44 C43 C48 C47 -0.2(9) . . . . ?
C44 C45 C46 C47 -3.1(12) . . . . ?
C45 C46 C47 C48 3.2(12) . . . . ?
C46 C47 C48 C43 -1.6(10) . . . . ?
C48 C43 C44 C45 0.3(8) . . . . ?
C49 P2 C31 C32 -74.1(4) . . . . ?
C49 P2 C31 C36 100.3(4) . . . . ?
C49 P2 C37 C38 -165.9(4) . . . . ?
C49 P2 C37 C42 17.3(5) . . . . ?
C49 P2 C43 C44 -138.7(4) . . . . ?
C49 P2 C43 C48 42.6(5) . . . . ?
C49 C50 C51 C52 0.3(9) . . . . ?
C50 C49 C54 C53 0.4(8) . . . . ?
C50 C51 C52 C53 0.5(10) . . . . ?
C51 C52 C53 C54 -0.8(10) . . . . ?
C52 C53 C54 C49 0.4(9) . . . . ?
C54 C49 C50 C51 -0.7(8) . . . . ?
C56 N1 C55 O3 176.3(17) . . . . ?
C57 N1 C55 O3 -7(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylformamide and diethyl ether'
####################################################################### 
# 
# 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_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2065217'
loop_
_audit_author_name
_audit_author_address
'So Yokomori'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H46 Ni O6 P2 S4'
_chemical_formula_weight         1111.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0081 0.0036 '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'
Ni Ni 0.1008 2.0460 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0239 0.0131 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1765 0.1900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.2048 0.2425 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

# start Validation Reply Form
_vrf_PLAT029_shelxl              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.716 Why?  
RESPONSE:
The data have been collected on 1-circle goniometer with IP area
detector diffractometer. It is only the very high angle data that
is incomplete due to the shape of the area detector,
and we have almost 100% coverage in the low angle data.
This will always be a problem with area detector data that is
not truncated. The obtained analysis was sufficient to elucidate
the molecular and crystal structure of this compound.
;
_vrf_PLAT026_shelxl              
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        36% Check 
RESPONSE:
The data have been collected on 1-circle goniometer with IP area
detector diffractometer. In addition, because this crystal is too
small, the observed reflections were relatively less in the very
high-angle region. However, the obtained analysis was sufficient
to elucidate the molecular and crystal structure of this compound.
;
_vrf_PLAT110_shelxl              
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check 
RESPONSE:
The crystal structural analysis using the suggested lattice and
space group failed due to too high Rint value.
Thus, I adopt this lattice and space group.
;
_vrf_PLAT112_shelxl              
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem       a/2        100 %Fit  
RESPONSE:
The crystal structural analysis using the suggested lattice and
space group failed due to too high Rint value.
Thus, I adopt this lattice and space group.
;
_vrf_PLAT113_shelxl              
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check 
RESPONSE:
The crystal structural analysis using the suggested lattice and
space group failed due to too high Rint value.
Thus, I adopt this lattice and space group.
;
_vrf_PLAT306_shelxl              
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check 
RESPONSE:
This O5 and O6 atoms belong to water molecule. In this crystal,
due to the serious disorder of the hydrogen atoms of the water
molecule, the position of the hydrogen atoms cannot be determined.
;
_vrf_PLAT430_shelxl              
;
PROBLEM: Short Inter D...A Contact  O3       ..O6       .       2.80 Ang.  
RESPONSE:
This alert is due to hydrogen-atom missing of the water molecule.
The reason of the hydrogen-atom missing is as described above.
;
# end Validation Reply Form

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.9446(3)
_cell_length_b                   12.5782(3)
_cell_length_c                   17.5902(7)
_cell_angle_alpha                70.3620(10)
_cell_angle_beta                 76.0230(10)
_cell_angle_gamma                104.3310(10)
_cell_volume                     2631.12(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5551
_cell_measurement_theta_min      3.702
_cell_measurement_theta_max      41.122

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.643
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.99968
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku IPDSC'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11763
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.702
_diffrn_reflns_theta_max         41.122
_diffrn_reflns_theta_full        36.856
_diffrn_measured_fraction_theta_max 0.649
_diffrn_measured_fraction_theta_full 0.716
_diffrn_reflns_Laue_measured_fraction_max 0.649
_diffrn_reflns_Laue_measured_fraction_full 0.716
_diffrn_reflns_point_group_measured_fraction_max 0.649
_diffrn_reflns_point_group_measured_fraction_full 0.716
_reflns_number_total             8152
_reflns_number_gt                2967
_reflns_threshold_expression     'I > 2σ(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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0634P)²] 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         8152
_refine_ls_number_parameters     660
_refine_ls_number_restraints     438
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1074
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   0.740
_refine_ls_restrained_S_all      0.736
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.25006(13) 0.50018(14) 0.50003(9) 0.04271(14) Uani 1 1 d . U . . .
S2 S 0.40970(18) 0.5406(2) 0.42093(14) 0.0529(7) Uani 1 1 d . U . . .
P2 P 0.4552(2) 1.2430(2) 0.24653(13) 0.0443(6) Uani 1 1 d . U . . .
P3 P 0.0453(2) -0.2430(2) 0.75331(13) 0.0431(6) Uani 1 1 d . U . . .
S4 S 0.26792(19) 0.3609(2) 0.60059(14) 0.0547(7) Uani 1 1 d . U . . .
S3 S 0.09069(18) 0.4599(2) 0.57874(12) 0.0496(6) Uani 1 1 d . U . . .
S1 S 0.23201(19) 0.6391(2) 0.39956(14) 0.0572(7) Uani 1 1 d . U . . .
O1 O 0.4759(5) 0.9176(5) 0.0873(3) 0.068(2) Uani 1 1 d . U . . .
H1 H 0.425010 0.938953 0.086840 0.102 Uiso 1 1 calc R U . . .
O2 O 0.6332(5) 0.8373(5) 0.1095(3) 0.0665(18) Uani 1 1 d . U . . .
H2 H 0.621734 0.857551 0.064156 0.100 Uiso 1 1 calc R U . . .
O6 O 0.1665(5) -0.0206(6) 0.9382(4) 0.074(2) Uani 1 1 d . U . . .
O5 O 0.3327(5) 1.0225(6) 0.0627(4) 0.072(2) Uani 1 1 d . U . . .
O3 O -0.1355(5) 0.1632(6) 0.8905(4) 0.078(2) Uani 1 1 d . U . . .
O4 O 0.0238(4) 0.0828(5) 0.9119(3) 0.0645(19) Uani 1 1 d . U . . .
C30 C 0.3036(8) 1.0201(9) 0.3690(6) 0.058(3) Uani 1 1 d . U . . .
H30 H 0.341224 1.026945 0.405242 0.070 Uiso 1 1 calc R U . . .
C40 C 0.3387(8) 0.0921(9) 0.6569(6) 0.065(3) Uani 1 1 d . U . . .
H40 H 0.398518 0.160385 0.638239 0.078 Uiso 1 1 calc R U . . .
C37 C 0.1610(7) -0.1113(8) 0.7129(5) 0.043(2) Uani 1 1 d . U . . .
C36 C 0.5032(6) 1.3240(7) 0.3651(5) 0.052(2) Uani 1 1 d . U . . .
H36 H 0.474841 1.382263 0.343728 0.063 Uiso 1 1 calc R U . . .
C55 C -0.0578(7) -0.2456(8) 0.8399(5) 0.042(2) Uani 1 1 d . U . . .
C43 C -0.0057(7) -0.2449(7) 0.6693(5) 0.044(2) Uani 1 1 d . U . . .
C29 C 0.2141(9) 0.9207(10) 0.3975(6) 0.071(3) Uani 1 1 d . U . . .
H29 H 0.189709 0.862088 0.453852 0.085 Uiso 1 1 calc R U . . .
C54 C 0.0249(8) -0.4668(8) 0.8740(5) 0.059(3) Uani 1 1 d . U . . .
H54 H -0.032018 -0.462061 0.911484 0.071 Uiso 1 1 calc R U . . .
C48 C -0.0057(7) -0.3277(7) 0.6333(5) 0.053(2) Uani 1 1 d . U . . .
H48 H 0.020241 -0.388787 0.653733 0.064 Uiso 1 1 calc R U . . .
C60 C -0.0398(7) -0.1669(7) 0.8784(5) 0.052(2) Uani 1 1 d . U . . .
H60 H 0.027042 -0.109080 0.860485 0.062 Uiso 1 1 calc R U . . .
C31 C 0.5054(6) 1.2391(7) 0.3318(5) 0.041(2) Uani 1 1 d . U . . .
C25 C 0.3382(7) 1.1103(7) 0.2863(5) 0.044(2) Uani 1 1 d . U . . .
C2 C 0.3647(7) 0.7934(7) 0.2359(5) 0.046(2) Uani 1 1 d . U . . .
H2A H 0.312138 0.824835 0.228881 0.055 Uiso 1 1 calc R U . . .
C14 C 0.3360(6) 1.3839(8) 0.2644(5) 0.048(2) Uani 1 1 d . U . . .
H14 H 0.297856 1.322657 0.319691 0.057 Uiso 1 1 calc R U . . .
C4 C 0.5418(8) 0.7966(9) 0.1766(5) 0.059(3) Uani 1 1 d . U . . .
C49 C 0.0805(7) -0.3732(8) 0.7917(5) 0.044(2) Uani 1 1 d . U . . .
C1 C 0.3476(7) 0.7023(7) 0.3168(5) 0.051(2) Uani 1 1 d . U . . .
C24 C 0.5413(7) 1.1671(8) 0.1232(5) 0.060(3) Uani 1 1 d . U . . .
H24 H 0.475187 1.107142 0.142992 0.072 Uiso 1 1 calc R U . . .
C32 C 0.5495(6) 1.1525(7) 0.3632(5) 0.055(2) Uani 1 1 d . U . . .
H32 H 0.553383 1.096181 0.340372 0.066 Uiso 1 1 calc R U . . .
C28 C 0.1600(8) 0.9067(8) 0.3436(6) 0.059(3) Uani 1 1 d . U . . .
H28 H 0.100980 0.837428 0.362625 0.071 Uiso 1 1 calc R U . . .
C19 C 0.5585(7) 1.2472(8) 0.1604(5) 0.043(2) Uani 1 1 d . U . . .
C5 C 0.5288(8) 0.7010(8) 0.2560(5) 0.056(2) Uani 1 1 d . U . . .
H5 H 0.580920 0.668626 0.262922 0.067 Uiso 1 1 calc R U . . .
C58 C -0.2224(8) -0.2644(9) 0.9732(5) 0.061(3) Uani 1 1 d . U . . .
H58 H -0.278210 -0.271261 1.018245 0.073 Uiso 1 1 calc R U . . .
C6 C 0.4317(7) 0.6611(7) 0.3217(4) 0.047(2) Uani 1 1 d . U . . .
C8 C -0.0297(7) 0.2924(7) 0.7458(5) 0.047(2) Uani 1 1 d . U . . .
H8 H -0.085590 0.317204 0.738199 0.057 Uiso 1 1 calc R U . . .
C9 C -0.0467(7) 0.2068(8) 0.8255(5) 0.047(2) Uani 1 1 d . U . . .
C12 C 0.1462(6) 0.2965(7) 0.6875(4) 0.039(2) Uani 1 1 d . U . . .
C7 C 0.0662(6) 0.3459(7) 0.6741(5) 0.039(2) Uani 1 1 d . U . . .
C57 C -0.2377(7) -0.3434(9) 0.9339(5) 0.063(3) Uani 1 1 d . U . . .
H57 H -0.303468 -0.403938 0.953596 0.075 Uiso 1 1 calc R U . . .
C26 C 0.2817(7) 1.0984(9) 0.2327(5) 0.051(2) Uani 1 1 d . U . . .
H26 H 0.302598 1.158874 0.177448 0.061 Uiso 1 1 calc R U . . .
C22 C 0.7225(9) 1.2620(9) 0.0273(5) 0.063(3) Uani 1 1 d . U . . .
H22 H 0.777530 1.265392 -0.016712 0.075 Uiso 1 1 calc R U . . .
C13 C 0.4214(7) 1.3761(7) 0.2077(5) 0.046(2) Uani 1 1 d . U . . .
C38 C 0.2146(8) -0.1005(9) 0.7669(6) 0.057(3) Uani 1 1 d . U . . .
H38 H 0.191184 -0.161263 0.822400 0.068 Uiso 1 1 calc R U . . .
C44 C -0.0467(7) -0.1581(8) 0.6394(5) 0.058(3) Uani 1 1 d . U . . .
H44 H -0.046510 -0.102354 0.663260 0.069 Uiso 1 1 calc R U . . .
C27 C 0.1931(8) 0.9938(9) 0.2633(6) 0.062(3) Uani 1 1 d . U . . .
H27 H 0.155985 0.984137 0.227240 0.074 Uiso 1 1 calc R U . . .
C42 C 0.1956(8) -0.0207(8) 0.6299(5) 0.050(2) Uani 1 1 d . U . . .
H42 H 0.159542 -0.028478 0.592782 0.060 Uiso 1 1 calc R U . . .
C39 C 0.3036(8) 0.0008(9) 0.7391(6) 0.060(3) Uani 1 1 d . U . . .
H39 H 0.340272 0.007643 0.775907 0.073 Uiso 1 1 calc R U . . .
C15 C 0.3106(8) 1.4876(9) 0.2344(7) 0.066(3) Uani 1 1 d . U . . .
H15 H 0.256527 1.497406 0.271069 0.079 Uiso 1 1 calc R U . . .
C10 C 0.0371(7) 0.1617(7) 0.8370(4) 0.047(2) Uani 1 1 d . U . . .
C59 C -0.1253(9) -0.1767(10) 0.9455(6) 0.071(3) Uani 1 1 d . U . . .
H59 H -0.115658 -0.123152 0.971234 0.085 Uiso 1 1 calc R U . . .
C34 C 0.5850(7) 1.2389(8) 0.4621(5) 0.067(3) Uani 1 1 d . U . . .
H34 H 0.611906 1.238947 0.505527 0.080 Uiso 1 1 calc R U . . .
C45 C -0.0888(7) -0.1503(8) 0.5745(5) 0.065(3) Uani 1 1 d . U . . .
H45 H -0.118282 -0.092020 0.556085 0.078 Uiso 1 1 calc R U . . .
C35 C 0.5429(7) 1.3225(8) 0.4299(5) 0.063(3) Uani 1 1 d . U . . .
H35 H 0.540733 1.379824 0.451982 0.076 Uiso 1 1 calc R U . . .
C3 C 0.4565(7) 0.8355(8) 0.1684(5) 0.055(2) Uani 1 1 d . U . . .
C21 C 0.7400(7) 1.3409(8) 0.0632(5) 0.060(3) Uani 1 1 d . U . . .
H21 H 0.806671 1.400113 0.042913 0.072 Uiso 1 1 calc R U . . .
C56 C -0.1563(8) -0.3323(9) 0.8664(5) 0.056(3) Uani 1 1 d . U . . .
H56 H -0.167393 -0.382918 0.838654 0.067 Uiso 1 1 calc R U . . .
C11 C 0.1311(7) 0.2068(8) 0.7646(5) 0.056(3) Uani 1 1 d . U . . .
H11 H 0.183873 0.174684 0.769514 0.067 Uiso 1 1 calc R U . . .
C50 C 0.1634(7) -0.3833(9) 0.7378(6) 0.061(3) Uani 1 1 d . U . . .
H50 H 0.200998 -0.320983 0.682907 0.073 Uiso 1 1 calc R U . . .
C20 C 0.6589(8) 1.3339(9) 0.1301(5) 0.058(3) Uani 1 1 d . U . . .
H20 H 0.671774 1.387862 0.155048 0.069 Uiso 1 1 calc R U . . .
C46 C -0.0856(6) -0.2311(8) 0.5387(5) 0.058(2) Uani 1 1 d . U . . .
H46 H -0.111753 -0.226626 0.494332 0.070 Uiso 1 1 calc R U . . .
C23 C 0.6243(9) 1.1775(9) 0.0558(6) 0.064(3) Uani 1 1 d . U . . .
H23 H 0.612384 1.125297 0.029269 0.077 Uiso 1 1 calc R U . . .
C33 C 0.5874(7) 1.1530(8) 0.4292(5) 0.057(2) Uani 1 1 d . U . . .
H33 H 0.614928 1.094557 0.451924 0.068 Uiso 1 1 calc R U . . .
C51 C 0.1935(8) -0.4838(9) 0.7623(6) 0.063(3) Uani 1 1 d . U . . .
H51 H 0.249381 -0.489359 0.724406 0.076 Uiso 1 1 calc R U . . .
C17 C 0.4452(8) 1.5641(9) 0.0994(6) 0.072(3) Uani 1 1 d . U . . .
H17 H 0.482039 1.625057 0.043896 0.087 Uiso 1 1 calc R U . . .
C52 C 0.1385(8) -0.5740(8) 0.8438(6) 0.062(3) Uani 1 1 d . U . . .
H52 H 0.158309 -0.641142 0.861293 0.074 Uiso 1 1 calc R U . . .
C47 C -0.0440(7) -0.3190(8) 0.5676(5) 0.064(3) Uani 1 1 d . U . . .
H47 H -0.042024 -0.372877 0.542297 0.077 Uiso 1 1 calc R U . . .
C41 C 0.2833(9) 0.0803(9) 0.6031(6) 0.065(3) Uani 1 1 d . U . . .
H41 H 0.305842 0.141604 0.547957 0.078 Uiso 1 1 calc R U . . .
C53 C 0.0546(8) -0.5680(8) 0.9004(6) 0.067(3) Uani 1 1 d . U . . .
H53 H 0.018202 -0.630230 0.955498 0.080 Uiso 1 1 calc R U . . .
C16 C 0.3638(9) 1.5738(9) 0.1526(7) 0.071(3) Uani 1 1 d . U . . .
H16 H 0.343919 1.640422 0.133042 0.085 Uiso 1 1 calc R U . . .
C18 C 0.4748(7) 1.4643(8) 0.1264(5) 0.056(2) Uani 1 1 d . U . . .
H18 H 0.530606 1.457790 0.089028 0.067 Uiso 1 1 calc R U . . .


_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 2.144(3) . ?
Ni1 S3 2.144(3) . ?
Ni1 S4 2.146(2) . ?
Ni1 S2 2.149(3) . ?
S2 C6 1.780(7) . ?
P2 C31 1.793(8) . ?
P2 C19 1.796(8) . ?
P2 C25 1.803(9) . ?
P2 C13 1.809(8) . ?
P3 C37 1.784(9) . ?
P3 C49 1.786(8) . ?
P3 C43 1.793(8) . ?
P3 C55 1.810(7) . ?
S4 C12 1.763(7) . ?
S3 C7 1.689(8) . ?
S1 C1 1.674(8) . ?
O1 C3 1.364(9) . ?
O1 H1 0.8200 . ?
O2 C4 1.350(9) . ?
O2 H2 0.8200 . ?
O3 C9 1.304(9) . ?
O4 C10 1.292(8) . ?
C30 C29 1.369(11) . ?
C30 C25 1.384(11) . ?
C30 H30 0.9300 . ?
C40 C41 1.379(12) . ?
C40 C39 1.383(12) . ?
C40 H40 0.9300 . ?
C37 C38 1.363(11) . ?
C37 C42 1.390(10) . ?
C36 C35 1.380(10) . ?
C36 C31 1.383(10) . ?
C36 H36 0.9300 . ?
C55 C56 1.378(11) . ?
C55 C60 1.383(10) . ?
C43 C44 1.366(10) . ?
C43 C48 1.388(10) . ?
C29 C28 1.375(12) . ?
C29 H29 0.9300 . ?
C54 C49 1.394(11) . ?
C54 C53 1.402(11) . ?
C54 H54 0.9300 . ?
C48 C47 1.370(10) . ?
C48 H48 0.9300 . ?
C60 C59 1.407(11) . ?
C60 H60 0.9300 . ?
C31 C32 1.400(10) . ?
C25 C26 1.389(11) . ?
C2 C3 1.355(11) . ?
C2 C1 1.414(10) . ?
C2 H2A 0.9300 . ?
C14 C15 1.401(10) . ?
C14 C13 1.404(10) . ?
C14 H14 0.9300 . ?
C4 C3 1.413(11) . ?
C4 C5 1.440(11) . ?
C49 C50 1.370(11) . ?
C1 C6 1.404(11) . ?
C24 C19 1.378(11) . ?
C24 C23 1.385(11) . ?
C24 H24 0.9300 . ?
C32 C33 1.388(11) . ?
C32 H32 0.9300 . ?
C28 C27 1.342(12) . ?
C28 H28 0.9300 . ?
C19 C20 1.388(11) . ?
C5 C6 1.392(10) . ?
C5 H5 0.9300 . ?
C58 C59 1.367(12) . ?
C58 C57 1.392(11) . ?
C58 H58 0.9300 . ?
C8 C9 1.371(10) . ?
C8 C7 1.414(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.447(10) . ?
C12 C11 1.368(10) . ?
C12 C7 1.435(9) . ?
C57 C56 1.370(11) . ?
C57 H57 0.9300 . ?
C26 C27 1.395(11) . ?
C26 H26 0.9300 . ?
C22 C21 1.348(11) . ?
C22 C23 1.360(11) . ?
C22 H22 0.9300 . ?
C13 C18 1.357(11) . ?
C38 C39 1.382(11) . ?
C38 H38 0.9300 . ?
C44 C45 1.391(11) . ?
C44 H44 0.9300 . ?
C27 H27 0.9300 . ?
C42 C41 1.372(11) . ?
C42 H42 0.9300 . ?
C39 H39 0.9300 . ?
C15 C16 1.353(12) . ?
C15 H15 0.9300 . ?
C10 C11 1.415(10) . ?
C59 H59 0.9300 . ?
C34 C35 1.355(11) . ?
C34 C33 1.389(11) . ?
C34 H34 0.9300 . ?
C45 C46 1.367(11) . ?
C45 H45 0.9300 . ?
C35 H35 0.9300 . ?
C21 C20 1.381(10) . ?
C21 H21 0.9300 . ?
C56 H56 0.9300 . ?
C11 H11 0.9300 . ?
C50 C51 1.393(11) . ?
C50 H50 0.9300 . ?
C20 H20 0.9300 . ?
C46 C47 1.378(11) . ?
C46 H46 0.9300 . ?
C23 H23 0.9300 . ?
C33 H33 0.9300 . ?
C51 C52 1.369(11) . ?
C51 H51 0.9300 . ?
C17 C16 1.346(12) . ?
C17 C18 1.386(11) . ?
C17 H17 0.9300 . ?
C52 C53 1.379(11) . ?
C52 H52 0.9300 . ?
C47 H47 0.9300 . ?
C41 H41 0.9300 . ?
C53 H53 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S3 88.31(9) . . ?
S1 Ni1 S4 179.91(18) . . ?
S3 Ni1 S4 91.64(9) . . ?
S1 Ni1 S2 91.60(10) . . ?
S3 Ni1 S2 179.89(15) . . ?
S4 Ni1 S2 88.45(10) . . ?
C6 S2 Ni1 104.5(3) . . ?
C31 P2 C19 107.0(4) . . ?
C31 P2 C25 109.3(4) . . ?
C19 P2 C25 111.4(4) . . ?
C31 P2 C13 111.0(4) . . ?
C19 P2 C13 109.4(4) . . ?
C25 P2 C13 108.9(4) . . ?
C37 P3 C49 108.3(4) . . ?
C37 P3 C43 110.2(4) . . ?
C49 P3 C43 109.6(4) . . ?
C37 P3 C55 111.0(4) . . ?
C49 P3 C55 109.9(4) . . ?
C43 P3 C55 107.7(4) . . ?
C12 S4 Ni1 105.4(3) . . ?
C7 S3 Ni1 106.2(3) . . ?
C1 S1 Ni1 105.9(3) . . ?
C3 O1 H1 109.5 . . ?
C4 O2 H2 109.5 . . ?
C29 C30 C25 120.1(9) . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
C41 C40 C39 118.9(10) . . ?
C41 C40 H40 120.6 . . ?
C39 C40 H40 120.6 . . ?
C38 C37 C42 120.3(9) . . ?
C38 C37 P3 117.7(7) . . ?
C42 C37 P3 122.0(7) . . ?
C35 C36 C31 120.2(7) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C56 C55 C60 121.5(8) . . ?
C56 C55 P3 115.9(6) . . ?
C60 C55 P3 122.6(7) . . ?
C44 C43 C48 118.8(8) . . ?
C44 C43 P3 116.8(6) . . ?
C48 C43 P3 124.4(6) . . ?
C30 C29 C28 120.7(10) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C49 C54 C53 120.2(8) . . ?
C49 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C47 C48 C43 119.7(8) . . ?
C47 C48 H48 120.2 . . ?
C43 C48 H48 120.2 . . ?
C55 C60 C59 118.2(9) . . ?
C55 C60 H60 120.9 . . ?
C59 C60 H60 120.9 . . ?
C36 C31 C32 119.8(7) . . ?
C36 C31 P2 119.9(6) . . ?
C32 C31 P2 120.3(6) . . ?
C30 C25 C26 119.3(9) . . ?
C30 C25 P2 121.5(7) . . ?
C26 C25 P2 119.2(7) . . ?
C3 C2 C1 121.1(8) . . ?
C3 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
C15 C14 C13 117.3(8) . . ?
C15 C14 H14 121.4 . . ?
C13 C14 H14 121.4 . . ?
O2 C4 C3 122.5(8) . . ?
O2 C4 C5 117.4(8) . . ?
C3 C4 C5 119.8(9) . . ?
C50 C49 C54 118.5(8) . . ?
C50 C49 P3 119.1(7) . . ?
C54 C49 P3 122.4(6) . . ?
C6 C1 C2 115.5(7) . . ?
C6 C1 S1 121.4(6) . . ?
C2 C1 S1 122.9(6) . . ?
C19 C24 C23 118.9(9) . . ?
C19 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C33 C32 C31 118.2(7) . . ?
C33 C32 H32 120.9 . . ?
C31 C32 H32 120.9 . . ?
C27 C28 C29 119.5(10) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C24 C19 C20 118.7(8) . . ?
C24 C19 P2 122.2(8) . . ?
C20 C19 P2 119.1(6) . . ?
C6 C5 C4 114.4(8) . . ?
C6 C5 H5 122.8 . . ?
C4 C5 H5 122.8 . . ?
C59 C58 C57 120.1(9) . . ?
C59 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C5 C6 C1 126.8(7) . . ?
C5 C6 S2 116.6(6) . . ?
C1 C6 S2 116.5(6) . . ?
C9 C8 C7 125.1(8) . . ?
C9 C8 H8 117.5 . . ?
C7 C8 H8 117.5 . . ?
O3 C9 C8 122.8(8) . . ?
O3 C9 C10 118.9(7) . . ?
C8 C9 C10 118.3(8) . . ?
C11 C12 C7 122.2(7) . . ?
C11 C12 S4 121.1(6) . . ?
C7 C12 S4 116.6(5) . . ?
C8 C7 C12 114.8(6) . . ?
C8 C7 S3 125.0(5) . . ?
C12 C7 S3 120.2(5) . . ?
C56 C57 C58 120.3(9) . . ?
C56 C57 H57 119.9 . . ?
C58 C57 H57 119.9 . . ?
C25 C26 C27 118.7(8) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
C21 C22 C23 119.8(9) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C18 C13 C14 121.0(8) . . ?
C18 C13 P2 121.5(6) . . ?
C14 C13 P2 117.5(6) . . ?
C37 C38 C39 119.9(9) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C43 C44 C45 122.2(7) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C28 C27 C26 121.6(9) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C41 C42 C37 119.4(8) . . ?
C41 C42 H42 120.3 . . ?
C37 C42 H42 120.3 . . ?
C38 C39 C40 120.6(9) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C16 C15 C14 120.9(9) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O4 C10 C11 122.7(8) . . ?
O4 C10 C9 119.4(7) . . ?
C11 C10 C9 117.9(7) . . ?
C58 C59 C60 120.4(9) . . ?
C58 C59 H59 119.8 . . ?
C60 C59 H59 119.8 . . ?
C35 C34 C33 119.1(8) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C46 C45 C44 117.9(8) . . ?
C46 C45 H45 121.1 . . ?
C44 C45 H45 121.1 . . ?
C34 C35 C36 121.1(8) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C2 C3 O1 124.3(8) . . ?
C2 C3 C4 122.0(8) . . ?
O1 C3 C4 113.7(8) . . ?
C22 C21 C20 120.1(9) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C57 C56 C55 119.6(8) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C12 C11 C10 121.5(8) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C49 C50 C51 122.3(9) . . ?
C49 C50 H50 118.8 . . ?
C51 C50 H50 118.8 . . ?
C21 C20 C19 120.8(8) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C45 C46 C47 120.8(8) . . ?
C45 C46 H46 119.6 . . ?
C47 C46 H46 119.6 . . ?
C22 C23 C24 121.7(9) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C32 C33 C34 121.5(7) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C52 C51 C50 118.2(9) . . ?
C52 C51 H51 120.9 . . ?
C50 C51 H51 120.9 . . ?
C16 C17 C18 120.8(9) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C51 C52 C53 121.7(9) . . ?
C51 C52 H52 119.2 . . ?
C53 C52 H52 119.2 . . ?
C48 C47 C46 120.6(8) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C42 C41 C40 120.9(9) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C52 C53 C54 119.2(9) . . ?
C52 C53 H53 120.4 . . ?
C54 C53 H53 120.4 . . ?
C17 C16 C15 120.7(9) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C13 C18 C17 119.4(8) . . ?
C13 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?

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
C49 P3 C37 C38 -55.1(7) . . . . ?
C43 P3 C37 C38 -175.1(6) . . . . ?
C55 P3 C37 C38 65.7(7) . . . . ?
C49 P3 C37 C42 126.0(7) . . . . ?
C43 P3 C37 C42 6.1(8) . . . . ?
C55 P3 C37 C42 -113.1(7) . . . . ?
C37 P3 C55 C56 169.7(6) . . . . ?
C49 P3 C55 C56 -70.4(7) . . . . ?
C43 P3 C55 C56 48.9(7) . . . . ?
C37 P3 C55 C60 -11.0(8) . . . . ?
C49 P3 C55 C60 108.8(7) . . . . ?
C43 P3 C55 C60 -131.8(7) . . . . ?
C37 P3 C43 C44 -67.6(7) . . . . ?
C49 P3 C43 C44 173.2(7) . . . . ?
C55 P3 C43 C44 53.7(8) . . . . ?
C37 P3 C43 C48 112.2(8) . . . . ?
C49 P3 C43 C48 -7.0(9) . . . . ?
C55 P3 C43 C48 -126.6(8) . . . . ?
C25 C30 C29 C28 2.7(13) . . . . ?
C44 C43 C48 C47 1.6(13) . . . . ?
P3 C43 C48 C47 -178.2(7) . . . . ?
C56 C55 C60 C59 -0.5(12) . . . . ?
P3 C55 C60 C59 -179.7(6) . . . . ?
C35 C36 C31 C32 -0.9(13) . . . . ?
C35 C36 C31 P2 -179.2(7) . . . . ?
C19 P2 C31 C36 126.1(7) . . . . ?
C25 P2 C31 C36 -113.2(7) . . . . ?
C13 P2 C31 C36 6.8(8) . . . . ?
C19 P2 C31 C32 -52.2(8) . . . . ?
C25 P2 C31 C32 68.5(7) . . . . ?
C13 P2 C31 C32 -171.4(7) . . . . ?
C29 C30 C25 C26 -0.5(12) . . . . ?
C29 C30 C25 P2 179.7(6) . . . . ?
C31 P2 C25 C30 -4.5(8) . . . . ?
C19 P2 C25 C30 113.5(7) . . . . ?
C13 P2 C25 C30 -125.8(7) . . . . ?
C31 P2 C25 C26 175.7(6) . . . . ?
C19 P2 C25 C26 -66.3(7) . . . . ?
C13 P2 C25 C26 54.4(7) . . . . ?
C53 C54 C49 C50 0.5(14) . . . . ?
C53 C54 C49 P3 178.9(7) . . . . ?
C37 P3 C49 C50 -53.2(8) . . . . ?
C43 P3 C49 C50 67.1(8) . . . . ?
C55 P3 C49 C50 -174.7(7) . . . . ?
C37 P3 C49 C54 128.4(8) . . . . ?
C43 P3 C49 C54 -111.3(8) . . . . ?
C55 P3 C49 C54 6.9(9) . . . . ?
C3 C2 C1 C6 0.6(12) . . . . ?
C3 C2 C1 S1 -174.8(7) . . . . ?
Ni1 S1 C1 C6 0.8(8) . . . . ?
Ni1 S1 C1 C2 176.0(6) . . . . ?
C36 C31 C32 C33 1.7(12) . . . . ?
P2 C31 C32 C33 180.0(6) . . . . ?
C30 C29 C28 C27 -2.6(14) . . . . ?
C23 C24 C19 C20 -1.3(12) . . . . ?
C23 C24 C19 P2 178.7(6) . . . . ?
C31 P2 C19 C24 128.2(7) . . . . ?
C25 P2 C19 C24 8.9(8) . . . . ?
C13 P2 C19 C24 -111.5(7) . . . . ?
C31 P2 C19 C20 -51.9(7) . . . . ?
C25 P2 C19 C20 -171.2(6) . . . . ?
C13 P2 C19 C20 68.4(8) . . . . ?
O2 C4 C5 C6 -178.3(8) . . . . ?
C3 C4 C5 C6 -4.7(13) . . . . ?
C4 C5 C6 C1 1.6(13) . . . . ?
C4 C5 C6 S2 178.7(6) . . . . ?
C2 C1 C6 C5 0.5(13) . . . . ?
S1 C1 C6 C5 175.9(7) . . . . ?
C2 C1 C6 S2 -176.7(6) . . . . ?
S1 C1 C6 S2 -1.2(10) . . . . ?
Ni1 S2 C6 C5 -176.5(6) . . . . ?
Ni1 S2 C6 C1 0.9(7) . . . . ?
C7 C8 C9 O3 177.5(8) . . . . ?
C7 C8 C9 C10 -3.7(13) . . . . ?
Ni1 S4 C12 C11 -177.4(6) . . . . ?
Ni1 S4 C12 C7 0.3(6) . . . . ?
C9 C8 C7 C12 5.2(12) . . . . ?
C9 C8 C7 S3 -174.3(7) . . . . ?
C11 C12 C7 C8 -1.7(11) . . . . ?
S4 C12 C7 C8 -179.4(6) . . . . ?
C11 C12 C7 S3 177.9(6) . . . . ?
S4 C12 C7 S3 0.1(9) . . . . ?
Ni1 S3 C7 C8 178.9(6) . . . . ?
Ni1 S3 C7 C12 -0.5(7) . . . . ?
C59 C58 C57 C56 -1.2(13) . . . . ?
C30 C25 C26 C27 -1.6(12) . . . . ?
P2 C25 C26 C27 178.2(6) . . . . ?
C15 C14 C13 C18 -1.9(13) . . . . ?
C15 C14 C13 P2 179.5(6) . . . . ?
C31 P2 C13 C18 114.3(8) . . . . ?
C19 P2 C13 C18 -3.5(9) . . . . ?
C25 P2 C13 C18 -125.4(8) . . . . ?
C31 P2 C13 C14 -67.1(7) . . . . ?
C19 P2 C13 C14 175.1(6) . . . . ?
C25 P2 C13 C14 53.2(7) . . . . ?
C42 C37 C38 C39 -0.1(12) . . . . ?
P3 C37 C38 C39 -178.9(6) . . . . ?
C48 C43 C44 C45 0.3(13) . . . . ?
P3 C43 C44 C45 -179.9(7) . . . . ?
C29 C28 C27 C26 0.4(13) . . . . ?
C25 C26 C27 C28 1.7(13) . . . . ?
C38 C37 C42 C41 -0.7(12) . . . . ?
P3 C37 C42 C41 178.1(6) . . . . ?
C37 C38 C39 C40 0.5(12) . . . . ?
C41 C40 C39 C38 -0.1(13) . . . . ?
C13 C14 C15 C16 2.8(13) . . . . ?
O3 C9 C10 O4 -2.5(13) . . . . ?
C8 C9 C10 O4 178.6(8) . . . . ?
O3 C9 C10 C11 177.5(8) . . . . ?
C8 C9 C10 C11 -1.4(12) . . . . ?
C57 C58 C59 C60 -1.1(14) . . . . ?
C55 C60 C59 C58 2.0(13) . . . . ?
C43 C44 C45 C46 -1.8(14) . . . . ?
C33 C34 C35 C36 -0.4(14) . . . . ?
C31 C36 C35 C34 0.2(14) . . . . ?
C1 C2 C3 O1 175.8(7) . . . . ?
C1 C2 C3 C4 -3.9(14) . . . . ?
O2 C4 C3 C2 179.4(8) . . . . ?
C5 C4 C3 C2 6.1(14) . . . . ?
O2 C4 C3 O1 -0.4(13) . . . . ?
C5 C4 C3 O1 -173.6(8) . . . . ?
C23 C22 C21 C20 1.6(14) . . . . ?
C58 C57 C56 C55 2.7(13) . . . . ?
C60 C55 C56 C57 -1.8(13) . . . . ?
P3 C55 C56 C57 177.4(6) . . . . ?
C7 C12 C11 C10 -3.1(13) . . . . ?
S4 C12 C11 C10 174.5(7) . . . . ?
O4 C10 C11 C12 -175.3(8) . . . . ?
C9 C10 C11 C12 4.6(13) . . . . ?
C54 C49 C50 C51 0.3(14) . . . . ?
P3 C49 C50 C51 -178.1(7) . . . . ?
C22 C21 C20 C19 -0.9(13) . . . . ?
C24 C19 C20 C21 0.7(12) . . . . ?
P2 C19 C20 C21 -179.2(6) . . . . ?
C44 C45 C46 C47 1.5(13) . . . . ?
C21 C22 C23 C24 -2.2(14) . . . . ?
C19 C24 C23 C22 2.0(14) . . . . ?
C31 C32 C33 C34 -1.9(13) . . . . ?
C35 C34 C33 C32 1.3(14) . . . . ?
C49 C50 C51 C52 -1.0(14) . . . . ?
C50 C51 C52 C53 0.8(14) . . . . ?
C43 C48 C47 C46 -2.0(14) . . . . ?
C45 C46 C47 C48 0.4(14) . . . . ?
C37 C42 C41 C40 1.1(13) . . . . ?
C39 C40 C41 C42 -0.7(13) . . . . ?
C51 C52 C53 C54 0.0(14) . . . . ?
C49 C54 C53 C52 -0.6(14) . . . . ?
C18 C17 C16 C15 1.6(15) . . . . ?
C14 C15 C16 C17 -2.7(15) . . . . ?
C14 C13 C18 C17 0.9(14) . . . . ?
P2 C13 C18 C17 179.4(7) . . . . ?
C16 C17 C18 C13 -0.7(14) . . . . ?

_refine_diff_density_max         0.526
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.050


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethyl sulfoxide and water'
####################################################################### 
# 
# 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_sy00911_dmsoh2o_blackrod_20201023
_database_code_depnum_ccdc_archive 'CCDC 2065215'
loop_
_audit_author_name
_audit_author_address
'So Yokomori'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;
_audit_creation_date             2021-02-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H7 Ni O4 S4, C24 H20 P, 0.5(O)'
_chemical_formula_sum            'C36 H27 Ni O4.50 P S4'
_chemical_formula_weight         749.49
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
# start Validation Reply Form
_vrf_PLAT417_sy00911_dmsoh2o_blackrod_20201023 
;
PROBLEM: Short Inter D-H..H-D       H4       ..H4       .       1.38 Ang.  
RESPONSE:
In this crystal, due to a disordering of hydrogen atoms of
water molecule, H4 atom would also be disordered. Since the
disordering process of the H4 atom failed, the H4 atom was placed
at the location supported by the difference Fourier analysis.
Although the location of the H4 atom may not always be accurate,
this will not be a problem in discussing molecular and crystal
structures.
;
# end Validation Reply Form
_cell_length_a                   7.1612(5)
_cell_length_b                   16.3222(8)
_cell_length_c                   28.1125(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.563(5)
_cell_angle_gamma                90
_cell_volume                     3285.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.9040
_cell_measurement_theta_min      1.9630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.1278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            26901
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.492
_diffrn_reflns_theta_min         2.506
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   90.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   90.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0777539000
_diffrn_orient_matrix_UB_12      -0.0259970000
_diffrn_orient_matrix_UB_13      -0.0038120000
_diffrn_orient_matrix_UB_21      0.0121582000
_diffrn_orient_matrix_UB_22      -0.0043822000
_diffrn_orient_matrix_UB_23      0.0249498000
_diffrn_orient_matrix_UB_31      -0.0601063000
_diffrn_orient_matrix_UB_32      -0.0345398000
_diffrn_orient_matrix_UB_33      -0.0002943000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4987
_reflns_number_total             8840
_reflns_odcompleteness_completeness 88.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1729
_refine_ls_R_factor_gt           0.0887
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0083P)²+15.7613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1485
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: O5(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C5(H5), C17(H17), C18(H18), C20(H20), C21(H21), C16(H16), C11(H11),
 C23(H23), C2(H2A), C36(H36), C22(H22), C8(H8), C35(H35), C24(H24), C29(H29),
 C27(H27), C14(H14), C32(H32), C28(H28), C30(H30), C34(H34), C15(H15), C33(H33)
3.b Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.24158(10) 0.29673(4) 0.68021(3) 0.02151(17) Uani 1 1 d . . . . .
S3 S -0.02981(19) 0.24463(8) 0.68961(5) 0.0233(3) Uani 1 1 d . . . . .
S2 S 0.51697(19) 0.34639(9) 0.67356(5) 0.0239(3) Uani 1 1 d . . . . .
S1 S 0.20112(19) 0.35844(8) 0.74693(5) 0.0240(3) Uani 1 1 d . . . . .
S4 S 0.27842(19) 0.23637(8) 0.61307(5) 0.0241(3) Uani 1 1 d . . . . .
P1 P 0.6851(2) 0.66032(8) 0.60355(5) 0.0202(3) Uani 1 1 d . . . . .
O1 O 0.6389(5) 0.5445(2) 0.84403(14) 0.0277(9) Uani 1 1 d . . . . .
O3 O -0.4195(5) 0.0503(2) 0.58350(13) 0.0278(9) Uani 1 1 d . . . . .
H3 H -0.482507 0.048292 0.607669 0.042 Uiso 1 1 calc R U . . .
O4 O -0.1522(5) 0.0421(3) 0.51777(13) 0.0309(10) Uani 1 1 d . . . . .
H4 H -0.053798 0.034240 0.503843 0.046 Uiso 1 1 calc R U . . .
O2 O 0.9017(6) 0.5349(3) 0.78075(15) 0.0400(11) Uani 1 1 d . . . . .
H2 H 0.893075 0.557949 0.806540 0.060 Uiso 1 1 calc R U . . .
C13 C 0.5370(7) 0.6404(3) 0.65331(18) 0.0207(11) Uani 1 1 d . . . . .
C19 C 0.8346(7) 0.5740(3) 0.59201(18) 0.0208(11) Uani 1 1 d . . . . .
C26 C 0.5582(8) 0.6355(3) 0.51040(19) 0.0250(12) Uani 1 1 d . . . . .
H26 H 0.649427 0.595217 0.508061 0.030 Uiso 1 1 calc R U . . .
C5 C 0.7234(7) 0.4441(3) 0.73228(19) 0.0224(12) Uani 1 1 d . . . . .
H5 H 0.820256 0.439518 0.710640 0.027 Uiso 1 1 calc R U . . .
C25 C 0.5361(7) 0.6791(3) 0.55268(18) 0.0222(12) Uani 1 1 d . . . . .
C17 C 0.2773(7) 0.5666(3) 0.6858(2) 0.0246(12) Uani 1 1 d . . . . .
H17 H 0.183466 0.527582 0.682583 0.029 Uiso 1 1 calc R U . . .
C18 C 0.3964(7) 0.5818(3) 0.64854(19) 0.0229(12) Uani 1 1 d . . . . .
H18 H 0.382796 0.552909 0.620201 0.027 Uiso 1 1 calc R U . . .
C20 C 0.8048(7) 0.4982(3) 0.61278(19) 0.0228(12) Uani 1 1 d . . . . .
H20 H 0.703090 0.490622 0.632632 0.027 Uiso 1 1 calc R U . . .
C21 C 0.9251(8) 0.4339(3) 0.6042(2) 0.0266(13) Uani 1 1 d . . . . .
H21 H 0.906365 0.383676 0.618969 0.032 Uiso 1 1 calc R U . . .
C7 C -0.0658(7) 0.1858(3) 0.63908(18) 0.0217(12) Uani 1 1 d . . . . .
C1 C 0.4086(8) 0.4084(3) 0.75891(19) 0.0242(12) Uani 1 1 d . . . . .
C16 C 0.2973(8) 0.6091(4) 0.7278(2) 0.0283(13) Uani 1 1 d . . . . .
H16 H 0.217171 0.598596 0.752902 0.034 Uiso 1 1 calc R U . . .
C31 C 0.8345(7) 0.7463(3) 0.61382(18) 0.0226(12) Uani 1 1 d . . . . .
C11 C 0.0446(8) 0.1319(3) 0.56358(19) 0.0234(12) Uani 1 1 d . . . . .
H11 H 0.137317 0.128205 0.540734 0.028 Uiso 1 1 calc R U . . .
C23 C 1.1044(8) 0.5198(3) 0.5522(2) 0.0254(12) Uani 1 1 d . . . . .
H23 H 1.204174 0.526920 0.531677 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4336(8) 0.4538(3) 0.8000(2) 0.0253(12) Uani 1 1 d . . . . .
H2A H 0.339957 0.455049 0.822632 0.030 Uiso 1 1 calc R U . . .
C36 C 0.9759(7) 0.7397(3) 0.6487(2) 0.0261(12) Uani 1 1 d . . . . .
H36 H 0.988282 0.691952 0.666505 0.031 Uiso 1 1 calc R U . . .
C6 C 0.5541(7) 0.4024(3) 0.72409(19) 0.0222(12) Uani 1 1 d . . . . .
C3 C 0.5999(8) 0.4982(3) 0.8078(2) 0.0270(13) Uani 1 1 d . . . . .
C22 C 1.0756(8) 0.4443(3) 0.57319(19) 0.0256(12) Uani 1 1 d . . . . .
H22 H 1.155241 0.400735 0.566810 0.031 Uiso 1 1 calc R U . . .
C8 C -0.2338(8) 0.1420(3) 0.63241(19) 0.0219(12) Uani 1 1 d . . . . .
H8 H -0.326737 0.145246 0.655214 0.026 Uiso 1 1 calc R U . . .
C35 C 1.0966(8) 0.8049(4) 0.6564(2) 0.0330(14) Uani 1 1 d . . . . .
H35 H 1.188270 0.801414 0.679966 0.040 Uiso 1 1 calc R U . . .
C24 C 0.9852(7) 0.5854(3) 0.56151(19) 0.0245(12) Uani 1 1 d . . . . .
H24 H 1.005826 0.636229 0.547558 0.029 Uiso 1 1 calc R U . . .
C29 C 0.2850(8) 0.7561(4) 0.5175(2) 0.0304(13) Uani 1 1 d . . . . .
H29 H 0.193546 0.796352 0.519811 0.036 Uiso 1 1 calc R U . . .
C27 C 0.4415(8) 0.6533(4) 0.47156(19) 0.0280(13) Uani 1 1 d . . . . .
H27 H 0.454157 0.624349 0.443289 0.034 Uiso 1 1 calc R U . . .
C10 C -0.1191(8) 0.0894(3) 0.55750(18) 0.0234(12) Uani 1 1 d . . . . .
C4 C 0.7453(8) 0.4913(3) 0.7721(2) 0.0266(13) Uani 1 1 d . . . . .
C14 C 0.5589(8) 0.6831(3) 0.6963(2) 0.0271(13) Uani 1 1 d . . . . .
H14 H 0.654241 0.721341 0.700056 0.033 Uiso 1 1 calc R U . . .
C32 C 0.8176(8) 0.8174(3) 0.5872(2) 0.0287(13) Uani 1 1 d . . . . .
H32 H 0.724310 0.822274 0.564140 0.034 Uiso 1 1 calc R U . . .
C12 C 0.0735(8) 0.1812(3) 0.60418(19) 0.0229(12) Uani 1 1 d . . . . .
C9 C -0.2619(7) 0.0942(3) 0.59232(19) 0.0221(12) Uani 1 1 d . . . . .
C28 C 0.3070(8) 0.7140(4) 0.4751(2) 0.0306(14) Uani 1 1 d . . . . .
H28 H 0.231416 0.726481 0.449018 0.037 Uiso 1 1 calc R U . . .
C30 C 0.3984(8) 0.7387(3) 0.5564(2) 0.0287(13) Uani 1 1 d . . . . .
H30 H 0.382591 0.766852 0.584812 0.034 Uiso 1 1 calc R U . . .
C34 C 1.0813(9) 0.8749(4) 0.6292(2) 0.0366(15) Uani 1 1 d . . . . .
H34 H 1.165575 0.917581 0.633723 0.044 Uiso 1 1 calc R U . . .
C15 C 0.4366(9) 0.6676(4) 0.7328(2) 0.0330(14) Uani 1 1 d . . . . .
H15 H 0.447765 0.696686 0.761109 0.040 Uiso 1 1 calc R U . . .
C33 C 0.9427(9) 0.8819(4) 0.5955(2) 0.0377(16) Uani 1 1 d . . . . .
H33 H 0.931502 0.930022 0.577984 0.045 Uiso 1 1 calc R U . . .
O5 O -0.4323(12) -0.0592(6) 0.5065(3) 0.045(2) Uani 0.5 1 d . . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S3 2.1401(16) . ?
Ni1 S2 2.1421(16) . ?
Ni1 S1 2.1512(16) . ?
Ni1 S4 2.1477(16) . ?
S3 C7 1.732(5) . ?
S2 C6 1.708(6) . ?
S1 C1 1.725(6) . ?
S4 C12 1.738(6) . ?
P1 C13 1.793(5) . ?
P1 C19 1.802(5) . ?
P1 C25 1.802(5) . ?
P1 C31 1.786(5) . ?
O1 C3 1.297(6) . ?
O3 H3 0.8200 . ?
O3 C9 1.358(6) . ?
O4 H4 0.8200 . ?
O4 C10 1.376(6) . ?
O2 H2 0.8200 . ?
O2 C4 1.347(7) . ?
C13 C18 1.394(7) . ?
C13 C14 1.402(7) . ?
C19 C20 1.384(7) . ?
C19 C24 1.397(7) . ?
C26 H26 0.9300 . ?
C26 C25 1.395(7) . ?
C26 C27 1.399(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.407(7) . ?
C5 C4 1.366(7) . ?
C25 C30 1.390(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.381(7) . ?
C17 C16 1.374(8) . ?
C18 H18 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.381(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.402(7) . ?
C7 C8 1.410(7) . ?
C7 C12 1.408(7) . ?
C1 C2 1.382(7) . ?
C1 C6 1.440(7) . ?
C16 H16 0.9300 . ?
C16 C15 1.387(8) . ?
C31 C36 1.407(8) . ?
C31 C32 1.386(7) . ?
C11 H11 0.9300 . ?
C11 C10 1.371(8) . ?
C11 C12 1.410(7) . ?
C23 H23 0.9300 . ?
C23 C22 1.383(8) . ?
C23 C24 1.396(7) . ?
C2 H2A 0.9300 . ?
C2 C3 1.410(8) . ?
C36 H36 0.9300 . ?
C36 C35 1.387(8) . ?
C3 C4 1.458(8) . ?
C22 H22 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.383(7) . ?
C35 H35 0.9300 . ?
C35 C34 1.378(9) . ?
C24 H24 0.9300 . ?
C29 H29 0.9300 . ?
C29 C28 1.386(8) . ?
C29 C30 1.385(8) . ?
C27 H27 0.9300 . ?
C27 C28 1.386(8) . ?
C10 C9 1.425(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.380(7) . ?
C32 H32 0.9300 . ?
C32 C33 1.400(8) . ?
C28 H28 0.9300 . ?
C30 H30 0.9300 . ?
C34 H34 0.9300 . ?
C34 C33 1.370(9) . ?
C15 H15 0.9300 . ?
C33 H33 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S3 Ni1 S2 177.56(7) . . ?
S3 Ni1 S1 87.03(6) . . ?
S3 Ni1 S4 92.63(6) . . ?
S2 Ni1 S1 91.77(6) . . ?
S2 Ni1 S4 88.61(6) . . ?
S4 Ni1 S1 179.05(7) . . ?
C7 S3 Ni1 104.31(19) . . ?
C6 S2 Ni1 105.42(19) . . ?
C1 S1 Ni1 105.56(19) . . ?
C12 S4 Ni1 104.68(19) . . ?
C13 P1 C19 110.8(2) . . ?
C13 P1 C25 107.5(2) . . ?
C19 P1 C25 109.8(2) . . ?
C31 P1 C13 112.0(2) . . ?
C31 P1 C19 106.7(2) . . ?
C31 P1 C25 110.1(3) . . ?
C9 O3 H3 109.5 . . ?
C10 O4 H4 109.5 . . ?
C4 O2 H2 109.5 . . ?
C18 C13 P1 118.8(4) . . ?
C18 C13 C14 119.9(5) . . ?
C14 C13 P1 121.3(4) . . ?
C20 C19 P1 121.9(4) . . ?
C20 C19 C24 120.1(5) . . ?
C24 C19 P1 118.0(4) . . ?
C25 C26 H26 120.4 . . ?
C25 C26 C27 119.2(5) . . ?
C27 C26 H26 120.4 . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.9(5) . . ?
C26 C25 P1 121.2(4) . . ?
C30 C25 P1 118.3(4) . . ?
C30 C25 C26 120.4(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.1(5) . . ?
C13 C18 H18 120.0 . . ?
C17 C18 C13 120.1(5) . . ?
C17 C18 H18 120.0 . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.4(5) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.1(5) . . ?
C22 C21 H21 119.9 . . ?
C8 C7 S3 120.7(4) . . ?
C12 C7 S3 120.0(4) . . ?
C12 C7 C8 119.3(5) . . ?
C2 C1 S1 121.4(4) . . ?
C2 C1 C6 121.0(5) . . ?
C6 C1 S1 117.6(4) . . ?
C17 C16 H16 119.9 . . ?
C17 C16 C15 120.2(5) . . ?
C15 C16 H16 119.9 . . ?
C36 C31 P1 118.6(4) . . ?
C32 C31 P1 121.5(4) . . ?
C32 C31 C36 119.9(5) . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.5(5) . . ?
C12 C11 H11 119.7 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.6(5) . . ?
C24 C23 H23 119.7 . . ?
C1 C2 H2A 119.7 . . ?
C1 C2 C3 120.6(5) . . ?
C3 C2 H2A 119.7 . . ?
C31 C36 H36 120.2 . . ?
C35 C36 C31 119.6(5) . . ?
C35 C36 H36 120.2 . . ?
C5 C6 S2 121.5(4) . . ?
C5 C6 C1 119.0(5) . . ?
C1 C6 S2 119.6(4) . . ?
O1 C3 C2 126.7(5) . . ?
O1 C3 C4 115.9(5) . . ?
C2 C3 C4 117.4(5) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 C21 119.4(5) . . ?
C23 C22 H22 120.3 . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.7(5) . . ?
C9 C8 H8 119.6 . . ?
C36 C35 H35 119.9 . . ?
C34 C35 C36 120.2(6) . . ?
C34 C35 H35 119.9 . . ?
C19 C24 H24 120.3 . . ?
C23 C24 C19 119.3(5) . . ?
C23 C24 H24 120.3 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C30 C29 C28 120.4(5) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.2(5) . . ?
C28 C27 H27 119.9 . . ?
O4 C10 C9 118.0(5) . . ?
C11 C10 O4 121.7(5) . . ?
C11 C10 C9 120.3(5) . . ?
O2 C4 C5 122.3(5) . . ?
O2 C4 C3 115.6(5) . . ?
C5 C4 C3 122.0(5) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.9(5) . . ?
C15 C14 H14 120.6 . . ?
C31 C32 H32 120.4 . . ?
C31 C32 C33 119.2(6) . . ?
C33 C32 H32 120.4 . . ?
C7 C12 S4 118.4(4) . . ?
C7 C12 C11 119.7(5) . . ?
C11 C12 S4 122.0(4) . . ?
O3 C9 C8 124.1(5) . . ?
O3 C9 C10 116.5(5) . . ?
C8 C9 C10 119.4(5) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 C29 120.1(5) . . ?
C27 C28 H28 119.9 . . ?
C25 C30 H30 120.1 . . ?
C29 C30 C25 119.7(5) . . ?
C29 C30 H30 120.1 . . ?
C35 C34 H34 119.8 . . ?
C33 C34 C35 120.4(6) . . ?
C33 C34 H34 119.8 . . ?
C16 C15 H15 119.6 . . ?
C14 C15 C16 120.8(5) . . ?
C14 C15 H15 119.6 . . ?
C32 C33 H33 119.7 . . ?
C34 C33 C32 120.7(6) . . ?
C34 C33 H33 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S3 C7 C8 -179.4(4) . . . . ?
Ni1 S3 C7 C12 0.7(5) . . . . ?
Ni1 S2 C6 C5 179.6(4) . . . . ?
Ni1 S2 C6 C1 -1.3(5) . . . . ?
Ni1 S1 C1 C2 -179.0(4) . . . . ?
Ni1 S1 C1 C6 2.2(5) . . . . ?
Ni1 S4 C12 C7 0.2(4) . . . . ?
Ni1 S4 C12 C11 -179.2(4) . . . . ?
S3 C7 C8 C9 -179.3(4) . . . . ?
S3 C7 C12 S4 -0.6(6) . . . . ?
S3 C7 C12 C11 178.8(4) . . . . ?
S1 C1 C2 C3 -176.1(4) . . . . ?
S1 C1 C6 S2 -0.6(6) . . . . ?
S1 C1 C6 C5 178.5(4) . . . . ?
P1 C13 C18 C17 -178.4(4) . . . . ?
P1 C13 C14 C15 177.6(4) . . . . ?
P1 C19 C20 C21 -178.2(4) . . . . ?
P1 C19 C24 C23 179.5(4) . . . . ?
P1 C25 C30 C29 178.3(4) . . . . ?
P1 C31 C36 C35 178.3(4) . . . . ?
P1 C31 C32 C33 -177.7(4) . . . . ?
O1 C3 C4 O2 -0.9(7) . . . . ?
O1 C3 C4 C5 179.6(5) . . . . ?
O4 C10 C9 O3 0.9(7) . . . . ?
O4 C10 C9 C8 -179.3(5) . . . . ?
C13 P1 C19 C20 12.9(5) . . . . ?
C13 P1 C19 C24 -166.4(4) . . . . ?
C13 P1 C25 C26 -126.9(4) . . . . ?
C13 P1 C25 C30 53.6(5) . . . . ?
C13 P1 C31 C36 67.6(5) . . . . ?
C13 P1 C31 C32 -114.5(5) . . . . ?
C13 C14 C15 C16 1.8(9) . . . . ?
C19 P1 C13 C18 -68.9(5) . . . . ?
C19 P1 C13 C14 111.9(5) . . . . ?
C19 P1 C25 C26 -6.3(5) . . . . ?
C19 P1 C25 C30 174.2(4) . . . . ?
C19 P1 C31 C36 -53.8(5) . . . . ?
C19 P1 C31 C32 124.0(5) . . . . ?
C19 C20 C21 C22 -1.9(8) . . . . ?
C26 C25 C30 C29 -1.3(8) . . . . ?
C26 C27 C28 C29 -1.4(8) . . . . ?
C25 P1 C13 C18 51.1(5) . . . . ?
C25 P1 C13 C14 -128.1(4) . . . . ?
C25 P1 C19 C20 -105.6(5) . . . . ?
C25 P1 C19 C24 75.1(5) . . . . ?
C25 P1 C31 C36 -172.9(4) . . . . ?
C25 P1 C31 C32 5.0(5) . . . . ?
C25 C26 C27 C28 0.6(8) . . . . ?
C17 C16 C15 C14 -1.1(9) . . . . ?
C18 C13 C14 C15 -1.6(8) . . . . ?
C18 C17 C16 C15 0.2(9) . . . . ?
C20 C19 C24 C23 0.2(8) . . . . ?
C20 C21 C22 C23 1.4(8) . . . . ?
C7 C8 C9 O3 179.9(5) . . . . ?
C7 C8 C9 C10 0.1(8) . . . . ?
C1 C2 C3 O1 178.2(5) . . . . ?
C1 C2 C3 C4 -2.6(8) . . . . ?
C16 C17 C18 C13 -0.1(8) . . . . ?
C31 P1 C13 C18 172.1(4) . . . . ?
C31 P1 C13 C14 -7.1(5) . . . . ?
C31 P1 C19 C20 135.1(5) . . . . ?
C31 P1 C19 C24 -44.2(5) . . . . ?
C31 P1 C25 C26 110.9(5) . . . . ?
C31 P1 C25 C30 -68.6(5) . . . . ?
C31 C36 C35 C34 -1.7(8) . . . . ?
C31 C32 C33 C34 0.5(9) . . . . ?
C11 C10 C9 O3 179.9(5) . . . . ?
C11 C10 C9 C8 -0.2(8) . . . . ?
C2 C1 C6 S2 -179.4(4) . . . . ?
C2 C1 C6 C5 -0.3(8) . . . . ?
C2 C3 C4 O2 179.8(5) . . . . ?
C2 C3 C4 C5 0.2(8) . . . . ?
C36 C31 C32 C33 0.1(8) . . . . ?
C36 C35 C34 C33 2.4(9) . . . . ?
C6 C5 C4 O2 -177.5(5) . . . . ?
C6 C5 C4 C3 2.0(8) . . . . ?
C6 C1 C2 C3 2.6(8) . . . . ?
C22 C23 C24 C19 -0.6(8) . . . . ?
C8 C7 C12 S4 179.5(4) . . . . ?
C8 C7 C12 C11 -1.1(8) . . . . ?
C35 C34 C33 C32 -1.8(9) . . . . ?
C24 C19 C20 C21 1.1(8) . . . . ?
C24 C23 C22 C21 -0.1(8) . . . . ?
C27 C26 C25 P1 -178.8(4) . . . . ?
C27 C26 C25 C30 0.7(8) . . . . ?
C10 C11 C12 S4 -179.7(4) . . . . ?
C10 C11 C12 C7 0.9(8) . . . . ?
C4 C5 C6 S2 177.1(4) . . . . ?
C4 C5 C6 C1 -2.0(8) . . . . ?
C14 C13 C18 C17 0.8(8) . . . . ?
C32 C31 C36 C35 0.4(8) . . . . ?
C12 C7 C8 C9 0.6(8) . . . . ?
C12 C11 C10 O4 178.7(5) . . . . ?
C12 C11 C10 C9 -0.3(8) . . . . ?
C28 C29 C30 C25 0.5(9) . . . . ?
C30 C29 C28 C27 0.8(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.899
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethyl sulfoxide and water'
####################################################################### 
# 
# 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_shelxl_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2065219'
loop_
_audit_author_name
_audit_author_address
'So Yokomori'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;
_audit_creation_date             2020-12-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C12 H7 Ni O4 S4, C6 H4 Ni0.5 O2 S2, C24 H20 P'
_chemical_formula_sum            'C42 H31 Ni1.50 O6 P S6'
_chemical_formula_weight         943.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
# start Validation Reply Form
_vrf_PLAT417_shelxl              
;
PROBLEM: Short Inter D-H..H-D       H2       ..H4       .       1.63 Ang.  
RESPONSE:
This alert is based on serious and complicated disordering of
the H atoms. However, the disordering process is too difficult
and failed due to the complicated hydrogen bonding network.
Therefore, these H atoms were generated geometrically and
refined with limitations on bond length angle. The obtained
structure was sufficient to discuss the molecular and crystal
structure with considering the deviation of bond lengths.
;
_vrf_PLAT026_shelxl              
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        36% Check 
RESPONSE:
This is based on low number of observed reflections in high
angle region due to relatively low crystallinity of this
crystal. The obtained analysis was sufficient to discuss
the molecular and crystal structure with considering the
deviation of bond lengths.
;
_vrf_PLAT084_shelxl              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.40 Report
RESPONSE:
This is due to relatively low crystallinity of this crystal.
However, the obtained structure was sufficient to discuss
the molecular and crystal structure with considering the
deviation of bond lengths.
;
_vrf_PLAT341_shelxl              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01824 Ang.  
RESPONSE:
This is due to relatively low crystallinity of this crystal.
However, the obtained structure was no problem to discuss
the molecular and crystal structure with considering the
deviation of bond lengths.
;
_vrf_PLAT416_shelxl              
;
PROBLEM: Short Intra D-H..H-D       H1       ..H2       .       1.71 Ang.  
RESPONSE:
This alert is based on serious and complicated disordering of
the H atoms. However, the disordering process is too difficult
and failed due to the complicated hydrogen bonding network.
Therefore, these H atoms were generated geometrically and
refined with limitations on bond length angle. The obtained
structure was sufficient to discuss the molecular and crystal
structure with considering the deviation of bond lengths.
;
# end Validation Reply Form

_cell_length_a                   10.770(5)
_cell_length_b                   13.090(6)
_cell_length_c                   15.722(7)
_cell_angle_alpha                71.015(14)
_cell_angle_beta                 84.98(2)
_cell_angle_gamma                87.58(2)
_cell_volume                     2087.6(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      3.100
_shelx_estimated_absorpt_T_max   0.815
_shelx_estimated_absorpt_T_min   0.815
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.8146
_exptl_absorpt_correction_T_min  0.8146
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.1856
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15149
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.058
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3022
_reflns_number_total             8335
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.922
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2365
_refine_ls_R_factor_gt           0.1176
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1963P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2812
_refine_ls_wR_factor_ref         0.3961
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Uiso: H2A(0.062) H5(0.09399) H8(0.071) H11(0.049) H14(0.061) H17(0.059)
 H20(0.055) H21(0.068) H22(0.059) H23(0.061) H24(0.057) H26(0.074) H27(0.077)
 H28(0.076) H29(0.08499) H30(0.064) H32(0.049) H33(0.073) H34(0.075) H35(0.063)
 H36(0.053) H38(0.064) H39(0.058) H40(0.061) H41(0.056) H42(0.064)
 Fixed X: Ni2(0.5) H2A(-0.236799) H5(0.108001) H8(-0.2159) H11(0.1604)
 H14(0.3014) H17(0.7278) H20(0.353601) H21(0.361601) H22(0.5387) H23(0.7042)
 H24(0.695101) H26(0.6774) H27(0.8388) H28(0.928901) H29(0.847) H30(0.6729)
 H32(0.4814) H33(0.3057) H34(0.103801) H35(0.0872) H36(0.2508) H38(0.414399)
 H39(0.3992) H40(0.4871) H41(0.568301) H42(0.5674)
 Fixed Y: Ni2(0) H2A(-0.488999) H5(-0.2657) H8(-0.4401) H11(-0.2613) H14(-
 0.304799) H17(-0.2612) H20(0.195601) H21(0.2823) H22(0.3866) H23(0.3868)
 H24(0.2889) H26(0.0496) H27(-0.0749) H28(-0.1055) H29(-0.023301) H30(0.0897)
 H32(-0.065301) H33(-0.178299) H34(-0.0979) H35(0.0787) H36(0.1867) H38(0.1363)
 H39(0.2453) H40(0.4205) H41(0.486099) H42(0.381901)
 Fixed Z: Ni2(1) H2A(1.2092) H5(1.1098) H8(1.730499) H11(1.638801)
 H14(0.959399) H17(0.8969) H20(0.7607) H21(0.869101) H22(0.859301) H23(0.7541)
 H24(0.656) H26(0.7522) H27(0.7644) H28(0.638201) H29(0.5003) H30(0.492599)
 H32(0.7116) H33(0.7647) H34(0.739699) H35(0.651901) H36(0.607) H38(0.465301)
 H39(0.311901) H40(0.2645) H41(0.3655) H42(0.5185)
3.a Everything fixed:
 H2A, H5, H8, H11, H14, H17, H20, H21, H22, H23, H24, H26, H27, H28, H29, H30,
 H32, H33, H34, H35, H36, H38, H39, H40, H41, H42
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4), O5(H5A), O6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.05473(14) -0.35204(12) 1.41870(10) 0.0444(5) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.000000 1.000000 0.0599(7) Uani 1 2 d S . P . .
S1 S -0.1771(3) -0.4300(3) 1.3593(2) 0.0460(8) Uani 1 1 d . . . . .
S2 S 0.0521(3) -0.2833(3) 1.2937(2) 0.0502(8) Uani 1 1 d . . . . .
S3 S -0.1689(3) -0.4138(3) 1.5430(2) 0.0492(8) Uani 1 1 d . . . . .
S4 S 0.0737(3) -0.2834(2) 1.48066(19) 0.0420(7) Uani 1 1 d . . . . .
S5 S 0.3625(3) -0.1091(3) 0.9923(3) 0.0599(10) Uani 1 1 d . . . . .
S6 S 0.6470(3) -0.0873(3) 0.9520(2) 0.0589(9) Uani 1 1 d . . . . .
P1 P 0.5146(3) 0.1606(2) 0.6190(2) 0.0406(8) Uani 1 1 d . . . . .
O1 O -0.1648(9) -0.4675(8) 1.0444(6) 0.062(2) Uani 1 1 d . . . . .
H1 H -0.128944 -0.444331 0.993842 0.093 Uiso 1 1 calc R U . . .
O2 O 0.0290(14) -0.3218(13) 0.9804(7) 0.126(5) Uani 1 1 d . . . . .
H2 H -0.003763 -0.360808 0.957472 0.189 Uiso 1 1 calc R U . . .
O3 O -0.1168(7) -0.4029(7) 1.8591(5) 0.046(2) Uani 1 1 d . . . . .
O4 O 0.1053(8) -0.3042(8) 1.8083(5) 0.060(2) Uani 1 1 d . . . . .
H4 H 0.059855 -0.314442 1.854824 0.089 Uiso 1 1 calc R U . . .
O5 O 0.4042(8) -0.4603(7) 0.9076(6) 0.055(2) Uani 1 1 d . . . . .
H5A H 0.333439 -0.469517 0.932344 0.082 Uiso 1 1 calc R U . . .
O6 O 0.6470(7) -0.4420(6) 0.8785(6) 0.049(2) Uani 1 1 d . . . . .
H6 H 0.721812 -0.429724 0.867898 0.074 Uiso 1 1 calc R U . . .
C1 C -0.1130(11) -0.3992(10) 1.2480(8) 0.047(3) Uani 1 1 d . . . . .
C2 C -0.1687(11) -0.4431(10) 1.1873(9) 0.050(3) Uani 1 1 d . . . . .
C3 C -0.1171(15) -0.4182(12) 1.1012(9) 0.065(4) Uani 1 1 d . . . . .
C4 C -0.0141(15) -0.3473(14) 1.0689(10) 0.078(5) Uani 1 1 d . . . . .
C5 C 0.0406(16) -0.3092(13) 1.1293(9) 0.078(5) Uani 1 1 d . . . . .
C6 C -0.0139(12) -0.3331(11) 1.2177(9) 0.053(3) Uani 1 1 d . . . . .
C7 C -0.0921(12) -0.3750(9) 1.6191(7) 0.044(3) Uani 1 1 d . . . . .
C8 C -0.1416(12) -0.4046(10) 1.7122(9) 0.052(3) Uani 1 1 d . . . . .
C9 C -0.0755(12) -0.3803(9) 1.7763(8) 0.050(3) Uani 1 1 d . . . . .
C10 C 0.0420(10) -0.3273(9) 1.7448(8) 0.037(3) Uani 1 1 d . . . . .
C11 C 0.0857(10) -0.2959(9) 1.6560(7) 0.041(3) Uani 1 1 d . . . . .
C12 C 0.0196(11) -0.3201(9) 1.5920(8) 0.044(3) Uani 1 1 d . . . . .
C13 C 0.4441(13) -0.2043(9) 0.9555(8) 0.051(3) Uani 1 1 d . . . . .
C14 C 0.3854(11) -0.2954(10) 0.9460(8) 0.051(3) Uani 1 1 d . . . . .
C15 C 0.4526(11) -0.3732(9) 0.9178(7) 0.043(3) Uani 1 1 d . . . . .
C16 C 0.5893(12) -0.3619(11) 0.9019(8) 0.053(3) Uani 1 1 d . . . . .
C17 C 0.6416(11) -0.2711(10) 0.9092(8) 0.051(3) Uani 1 1 d . . . . .
C18 C 0.5723(13) -0.1947(10) 0.9351(9) 0.055(3) Uani 1 1 d . . . . .
C19 C 0.5194(10) 0.2344(9) 0.6957(7) 0.041(3) Uani 1 1 d . . . . .
C20 C 0.4234(10) 0.2345(9) 0.7603(8) 0.044(3) Uani 1 1 d . . . . .
C21 C 0.4265(12) 0.2872(11) 0.8249(8) 0.054(3) Uani 1 1 d . . . . .
C22 C 0.5329(12) 0.3452(9) 0.8209(8) 0.050(3) Uani 1 1 d . . . . .
C23 C 0.6323(12) 0.3480(10) 0.7562(9) 0.053(3) Uani 1 1 d . . . . .
C24 C 0.6280(11) 0.2896(10) 0.6957(8) 0.048(3) Uani 1 1 d . . . . .
C25 C 0.6553(11) 0.0796(9) 0.6218(8) 0.044(3) Uani 1 1 d . . . . .
C26 C 0.7083(11) 0.0319(10) 0.7028(10) 0.057(4) Uani 1 1 d . . . . .
C27 C 0.8076(12) -0.0389(11) 0.7096(10) 0.064(4) Uani 1 1 d . . . . .
C28 C 0.8603(10) -0.0598(12) 0.6349(11) 0.063(4) Uani 1 1 d . . . . .
C29 C 0.8112(12) -0.0120(12) 0.5533(12) 0.071(5) Uani 1 1 d . . . . .
C30 C 0.7081(11) 0.0595(10) 0.5465(9) 0.053(3) Uani 1 1 d . . . . .
C31 C 0.3853(10) 0.0732(9) 0.6521(8) 0.043(3) Uani 1 1 d . . . . .
C32 C 0.4007(10) -0.0366(9) 0.7009(8) 0.041(3) Uani 1 1 d . . . . .
C33 C 0.2969(14) -0.1046(11) 0.7339(9) 0.063(4) Uani 1 1 d . . . . .
C34 C 0.1754(12) -0.0582(11) 0.7193(9) 0.063(4) Uani 1 1 d . . . . .
C35 C 0.1648(10) 0.0490(10) 0.6676(9) 0.052(3) Uani 1 1 d . . . . .
C36 C 0.2655(10) 0.1151(9) 0.6379(8) 0.042(3) Uani 1 1 d . . . . .
C37 C 0.4998(10) 0.2466(8) 0.5066(8) 0.040(3) Uani 1 1 d . . . . .
C38 C 0.4477(11) 0.2063(9) 0.4456(9) 0.050(3) Uani 1 1 d . . . . .
C39 C 0.4375(11) 0.2717(10) 0.3513(9) 0.050(3) Uani 1 1 d . . . . .
C40 C 0.4870(12) 0.3775(9) 0.3251(8) 0.052(3) Uani 1 1 d . . . . .
C41 C 0.5370(10) 0.4151(9) 0.3861(8) 0.045(3) Uani 1 1 d . . . . .
C42 C 0.5426(11) 0.3513(10) 0.4770(9) 0.053(3) Uani 1 1 d . . . . .
H2A H -0.236799 -0.488999 1.209200 0.062 Uiso 1 1 d . U . . .
H5 H 0.108001 -0.265700 1.109800 0.094 Uiso 1 1 d . U . . .
H8 H -0.215900 -0.440100 1.730499 0.071 Uiso 1 1 d . U . . .
H11 H 0.160400 -0.261300 1.638802 0.049 Uiso 1 1 d . U . . .
H14 H 0.301400 -0.304799 0.959399 0.061 Uiso 1 1 d . U . . .
H17 H 0.727800 -0.261200 0.896900 0.059 Uiso 1 1 d . U . . .
H20 H 0.353601 0.195601 0.760700 0.055 Uiso 1 1 d . U . . .
H21 H 0.361601 0.282300 0.869101 0.068 Uiso 1 1 d . U . . .
H22 H 0.538700 0.386600 0.859301 0.059 Uiso 1 1 d . U . . .
H23 H 0.704200 0.386800 0.754100 0.061 Uiso 1 1 d . U . . .
H24 H 0.695101 0.288900 0.656000 0.057 Uiso 1 1 d . U . . .
H26 H 0.677400 0.049600 0.752200 0.074 Uiso 1 1 d . U . . .
H27 H 0.838800 -0.074900 0.764400 0.077 Uiso 1 1 d . U . . .
H28 H 0.928901 -0.105500 0.638201 0.076 Uiso 1 1 d . U . . .
H29 H 0.847000 -0.023301 0.500300 0.085 Uiso 1 1 d . U . . .
H30 H 0.672900 0.089700 0.492599 0.064 Uiso 1 1 d . U . . .
H32 H 0.481400 -0.065301 0.711600 0.049 Uiso 1 1 d . U . . .
H33 H 0.305700 -0.178299 0.764700 0.073 Uiso 1 1 d . U . . .
H34 H 0.103801 -0.097900 0.739699 0.075 Uiso 1 1 d . U . . .
H35 H 0.087200 0.078700 0.651901 0.063 Uiso 1 1 d . U . . .
H36 H 0.250800 0.186700 0.607000 0.053 Uiso 1 1 d . U . . .
H38 H 0.414399 0.136300 0.465301 0.064 Uiso 1 1 d . U . . .
H39 H 0.399200 0.245300 0.311901 0.058 Uiso 1 1 d . U . . .
H40 H 0.487100 0.420500 0.264500 0.061 Uiso 1 1 d . U . . .
H41 H 0.568301 0.486099 0.365500 0.056 Uiso 1 1 d . U . . .
H42 H 0.567400 0.381901 0.518500 0.064 Uiso 1 1 d . U . . .


_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 2.145(3) . ?
Ni1 S2 2.130(3) . ?
Ni1 S3 2.150(3) . ?
Ni1 S4 2.140(3) . ?
Ni2 S5 2.137(3) 2_657 ?
Ni2 S5 2.137(3) . ?
Ni2 S6 2.141(3) 2_657 ?
Ni2 S6 2.141(3) . ?
S1 C1 1.748(12) . ?
S2 C6 1.747(12) . ?
S3 C7 1.725(12) . ?
S4 C12 1.713(12) . ?
S5 C13 1.717(12) . ?
S6 C18 1.751(12) . ?
P1 C19 1.779(12) . ?
P1 C25 1.809(12) . ?
P1 C31 1.772(12) . ?
P1 C37 1.776(11) . ?
O1 H1 0.8200 . ?
O1 C3 1.400(16) . ?
O2 H2 0.8200 . ?
O2 C4 1.364(17) . ?
O3 C9 1.279(13) . ?
O4 H4 0.8200 . ?
O4 C10 1.372(12) . ?
O5 H5A 0.8200 . ?
O5 C15 1.335(13) . ?
O6 H6 0.8200 . ?
O6 C16 1.333(14) . ?
C1 C2 1.445(16) . ?
C1 C6 1.356(17) . ?
C2 C3 1.358(17) . ?
C2 H2A 0.9361 . ?
C3 C4 1.43(2) . ?
C4 C5 1.388(19) . ?
C5 C6 1.403(17) . ?
C5 H5 0.9094 . ?
C7 C8 1.446(16) . ?
C7 C12 1.389(17) . ?
C8 C9 1.406(17) . ?
C8 H8 0.9177 . ?
C9 C10 1.439(16) . ?
C10 C11 1.367(15) . ?
C11 C12 1.403(15) . ?
C11 H11 0.9158 . ?
C13 C14 1.429(16) . ?
C13 C18 1.392(18) . ?
C14 C15 1.389(16) . ?
C14 H14 0.9149 . ?
C15 C16 1.478(17) . ?
C16 C17 1.379(16) . ?
C17 C18 1.368(17) . ?
C17 H17 0.9374 . ?
C19 C20 1.385(15) . ?
C19 C24 1.400(16) . ?
C20 C21 1.404(16) . ?
C20 H20 0.9241 . ?
C21 C22 1.387(17) . ?
C21 H21 0.9304 . ?
C22 C23 1.404(17) . ?
C22 H22 0.9408 . ?
C23 C24 1.404(16) . ?
C23 H23 0.9363 . ?
C24 H24 0.9147 . ?
C25 C26 1.384(17) . ?
C25 C30 1.367(16) . ?
C26 C27 1.374(17) . ?
C26 H26 0.9118 . ?
C27 C28 1.361(19) . ?
C27 H27 0.9226 . ?
C28 C29 1.37(2) . ?
C28 H28 0.9252 . ?
C29 C30 1.410(17) . ?
C29 H29 0.9409 . ?
C30 H30 0.9181 . ?
C31 C32 1.403(14) . ?
C31 C36 1.388(15) . ?
C32 C33 1.411(17) . ?
C32 H32 0.9394 . ?
C33 C34 1.425(18) . ?
C33 H33 0.9329 . ?
C34 C35 1.380(17) . ?
C34 H34 0.9217 . ?
C35 C36 1.367(15) . ?
C35 H35 0.9260 . ?
C36 H36 0.9184 . ?
C37 C38 1.399(15) . ?
C37 C42 1.381(15) . ?
C38 C39 1.462(17) . ?
C38 H38 0.9426 . ?
C39 C40 1.423(16) . ?
C39 H39 0.9327 . ?
C40 C41 1.368(17) . ?
C40 H40 0.9353 . ?
C41 C42 1.406(16) . ?
C41 H41 0.9458 . ?
C42 H42 0.9315 . ?

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 S3 87.62(13) . . ?
S2 Ni1 S1 92.39(14) . . ?
S2 Ni1 S3 176.93(15) . . ?
S2 Ni1 S4 88.06(13) . . ?
S4 Ni1 S1 176.48(14) . . ?
S4 Ni1 S3 92.12(13) . . ?
S5 Ni2 S5 180.0 2_657 . ?
S5 Ni2 S6 87.88(13) 2_657 . ?
S5 Ni2 S6 92.12(13) 2_657 2_657 ?
S5 Ni2 S6 87.88(13) . 2_657 ?
S5 Ni2 S6 92.12(13) . . ?
S6 Ni2 S6 180.0 2_657 . ?
C1 S1 Ni1 103.3(5) . . ?
C6 S2 Ni1 104.8(5) . . ?
C7 S3 Ni1 103.7(4) . . ?
C12 S4 Ni1 104.9(4) . . ?
C13 S5 Ni2 105.1(5) . . ?
C18 S6 Ni2 104.5(5) . . ?
C19 P1 C25 109.5(6) . . ?
C31 P1 C19 109.2(6) . . ?
C31 P1 C25 108.5(5) . . ?
C31 P1 C37 108.3(5) . . ?
C37 P1 C19 112.3(5) . . ?
C37 P1 C25 109.0(5) . . ?
C3 O1 H1 109.5 . . ?
C4 O2 H2 109.5 . . ?
C10 O4 H4 109.5 . . ?
C15 O5 H5A 109.5 . . ?
C16 O6 H6 109.5 . . ?
C2 C1 S1 119.3(10) . . ?
C6 C1 S1 120.9(10) . . ?
C6 C1 C2 119.9(11) . . ?
C1 C2 H2A 118.9 . . ?
C3 C2 C1 118.2(13) . . ?
C3 C2 H2A 122.8 . . ?
O1 C3 C4 119.8(12) . . ?
C2 C3 O1 118.2(14) . . ?
C2 C3 C4 121.9(14) . . ?
O2 C4 C3 118.7(13) . . ?
O2 C4 C5 122.6(15) . . ?
C5 C4 C3 118.7(14) . . ?
C4 C5 C6 119.2(14) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 121.2 . . ?
C1 C6 S2 118.4(10) . . ?
C1 C6 C5 121.8(12) . . ?
C5 C6 S2 119.7(11) . . ?
C8 C7 S3 119.5(10) . . ?
C12 C7 S3 120.3(9) . . ?
C12 C7 C8 120.2(11) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 C7 120.2(12) . . ?
C9 C8 H8 119.1 . . ?
O3 C9 C8 122.5(12) . . ?
O3 C9 C10 120.5(12) . . ?
C8 C9 C10 117.0(11) . . ?
O4 C10 C9 116.2(10) . . ?
C11 C10 O4 121.4(10) . . ?
C11 C10 C9 122.3(10) . . ?
C10 C11 C12 120.6(11) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 120.0 . . ?
C7 C12 S4 118.9(9) . . ?
C7 C12 C11 119.7(11) . . ?
C11 C12 S4 121.4(9) . . ?
C14 C13 S5 122.4(10) . . ?
C18 C13 S5 119.7(10) . . ?
C18 C13 C14 117.9(11) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 121.9(11) . . ?
C15 C14 H14 117.7 . . ?
O5 C15 C14 125.3(11) . . ?
O5 C15 C16 116.9(11) . . ?
C14 C15 C16 117.8(11) . . ?
O6 C16 C15 113.9(11) . . ?
O6 C16 C17 127.8(12) . . ?
C17 C16 C15 118.2(12) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 122.4(11) . . ?
C18 C17 H17 118.2 . . ?
C13 C18 S6 118.5(10) . . ?
C17 C18 S6 119.7(10) . . ?
C17 C18 C13 121.6(11) . . ?
C20 C19 P1 123.1(9) . . ?
C20 C19 C24 117.6(11) . . ?
C24 C19 P1 119.2(9) . . ?
C19 C20 C21 124.7(11) . . ?
C19 C20 H20 116.4 . . ?
C21 C20 H20 118.9 . . ?
C20 C21 H21 122.0 . . ?
C22 C21 C20 116.6(12) . . ?
C22 C21 H21 121.4 . . ?
C21 C22 C23 120.7(12) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 118.2 . . ?
C22 C23 H23 120.3 . . ?
C24 C23 C22 120.8(11) . . ?
C24 C23 H23 118.8 . . ?
C19 C24 C23 119.4(11) . . ?
C19 C24 H24 120.5 . . ?
C23 C24 H24 120.1 . . ?
C26 C25 P1 119.7(9) . . ?
C30 C25 P1 121.6(10) . . ?
C30 C25 C26 118.6(12) . . ?
C25 C26 H26 118.8 . . ?
C27 C26 C25 121.4(13) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 121.4 . . ?
C28 C27 C26 120.2(13) . . ?
C28 C27 H27 118.4 . . ?
C27 C28 C29 119.5(12) . . ?
C27 C28 H28 121.1 . . ?
C29 C28 H28 119.4 . . ?
C28 C29 C30 120.4(14) . . ?
C28 C29 H29 121.4 . . ?
C30 C29 H29 118.2 . . ?
C25 C30 C29 119.7(13) . . ?
C25 C30 H30 119.4 . . ?
C29 C30 H30 120.8 . . ?
C32 C31 P1 120.9(9) . . ?
C36 C31 P1 119.9(9) . . ?
C36 C31 C32 118.9(11) . . ?
C31 C32 C33 121.1(11) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C34 118.4(12) . . ?
C32 C33 H33 122.1 . . ?
C34 C33 H33 119.5 . . ?
C33 C34 H34 122.7 . . ?
C35 C34 C33 118.5(12) . . ?
C35 C34 H34 118.7 . . ?
C34 C35 H35 119.8 . . ?
C36 C35 C34 122.6(11) . . ?
C36 C35 H35 117.5 . . ?
C31 C36 H36 122.0 . . ?
C35 C36 C31 120.3(11) . . ?
C35 C36 H36 117.8 . . ?
C38 C37 P1 119.4(8) . . ?
C42 C37 P1 121.4(9) . . ?
C42 C37 C38 119.2(11) . . ?
C37 C38 C39 121.9(10) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 117.7 . . ?
C38 C39 H39 121.3 . . ?
C40 C39 C38 115.7(10) . . ?
C40 C39 H39 122.9 . . ?
C39 C40 H40 118.6 . . ?
C41 C40 C39 121.1(11) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 C42 121.9(11) . . ?
C40 C41 H41 118.0 . . ?
C42 C41 H41 120.2 . . ?
C37 C42 C41 120.1(11) . . ?
C37 C42 H42 119.7 . . ?
C41 C42 H42 119.8 . . ?

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 S1 C1 C2 177.3(9) . . . . ?
Ni1 S1 C1 C6 -4.2(11) . . . . ?
Ni1 S2 C6 C1 0.8(11) . . . . ?
Ni1 S2 C6 C5 -175.5(11) . . . . ?
Ni1 S3 C7 C8 -179.0(8) . . . . ?
Ni1 S3 C7 C12 -2.0(10) . . . . ?
Ni1 S4 C12 C7 -4.6(10) . . . . ?
Ni1 S4 C12 C11 175.3(9) . . . . ?
Ni2 S5 C13 C14 176.8(10) . . . . ?
Ni2 S5 C13 C18 -2.3(12) . . . . ?
Ni2 S6 C18 C13 -1.1(11) . . . . ?
Ni2 S6 C18 C17 -176.1(10) . . . . ?
S1 C1 C2 C3 -179.9(9) . . . . ?
S1 C1 C6 S2 2.4(15) . . . . ?
S1 C1 C6 C5 178.6(11) . . . . ?
S3 C7 C8 C9 175.4(9) . . . . ?
S3 C7 C12 S4 4.6(14) . . . . ?
S3 C7 C12 C11 -175.3(8) . . . . ?
S5 C13 C14 C15 -178.7(9) . . . . ?
S5 C13 C18 S6 2.4(15) . . . . ?
S5 C13 C18 C17 177.3(10) . . . . ?
P1 C19 C20 C21 176.7(10) . . . . ?
P1 C19 C24 C23 -180.0(9) . . . . ?
P1 C25 C26 C27 173.3(10) . . . . ?
P1 C25 C30 C29 -174.2(9) . . . . ?
P1 C31 C32 C33 174.7(10) . . . . ?
P1 C31 C36 C35 -176.5(10) . . . . ?
P1 C37 C38 C39 -177.6(9) . . . . ?
P1 C37 C42 C41 175.9(9) . . . . ?
O1 C3 C4 O2 6(2) . . . . ?
O1 C3 C4 C5 -172.7(13) . . . . ?
O2 C4 C5 C6 175.8(16) . . . . ?
O3 C9 C10 O4 0.6(16) . . . . ?
O3 C9 C10 C11 -175.9(10) . . . . ?
O4 C10 C11 C12 -179.8(10) . . . . ?
O5 C15 C16 O6 0.3(15) . . . . ?
O5 C15 C16 C17 178.0(11) . . . . ?
O6 C16 C17 C18 -179.1(12) . . . . ?
C1 C2 C3 O1 175.0(10) . . . . ?
C1 C2 C3 C4 -3(2) . . . . ?
C2 C1 C6 S2 -179.1(9) . . . . ?
C2 C1 C6 C5 -3(2) . . . . ?
C2 C3 C4 O2 -176.8(15) . . . . ?
C2 C3 C4 C5 5(2) . . . . ?
C3 C4 C5 C6 -6(3) . . . . ?
C4 C5 C6 S2 -178.7(13) . . . . ?
C4 C5 C6 C1 5(2) . . . . ?
C6 C1 C2 C3 1.6(18) . . . . ?
C7 C8 C9 O3 178.5(10) . . . . ?
C7 C8 C9 C10 -0.9(17) . . . . ?
C8 C7 C12 S4 -178.5(9) . . . . ?
C8 C7 C12 C11 1.6(17) . . . . ?
C8 C9 C10 O4 180.0(10) . . . . ?
C8 C9 C10 C11 3.5(17) . . . . ?
C9 C10 C11 C12 -3.5(17) . . . . ?
C10 C11 C12 S4 -179.0(9) . . . . ?
C10 C11 C12 C7 0.9(17) . . . . ?
C12 C7 C8 C9 -1.5(17) . . . . ?
C13 C14 C15 O5 179.9(11) . . . . ?
C13 C14 C15 C16 2.8(18) . . . . ?
C14 C13 C18 S6 -176.8(9) . . . . ?
C14 C13 C18 C17 -2(2) . . . . ?
C14 C15 C16 O6 177.6(11) . . . . ?
C14 C15 C16 C17 -4.7(17) . . . . ?
C15 C16 C17 C18 4(2) . . . . ?
C16 C17 C18 S6 174.7(10) . . . . ?
C16 C17 C18 C13 0(2) . . . . ?
C18 C13 C14 C15 0.4(19) . . . . ?
C19 P1 C25 C26 36.9(11) . . . . ?
C19 P1 C25 C30 -146.5(10) . . . . ?
C19 P1 C31 C32 -99.5(10) . . . . ?
C19 P1 C31 C36 74.1(11) . . . . ?
C19 P1 C37 C38 -155.5(9) . . . . ?
C19 P1 C37 C42 26.7(12) . . . . ?
C19 C20 C21 C22 1.7(19) . . . . ?
C20 C19 C24 C23 -4.2(17) . . . . ?
C20 C21 C22 C23 -1.3(18) . . . . ?
C21 C22 C23 C24 -1.9(19) . . . . ?
C22 C23 C24 C19 4.7(19) . . . . ?
C24 C19 C20 C21 1.1(18) . . . . ?
C25 P1 C19 C20 -128.8(10) . . . . ?
C25 P1 C19 C24 46.7(10) . . . . ?
C25 P1 C31 C32 19.8(12) . . . . ?
C25 P1 C31 C36 -166.6(10) . . . . ?
C25 P1 C37 C38 83.0(10) . . . . ?
C25 P1 C37 C42 -94.7(11) . . . . ?
C25 C26 C27 C28 3(2) . . . . ?
C26 C25 C30 C29 2.5(18) . . . . ?
C26 C27 C28 C29 -2(2) . . . . ?
C27 C28 C29 C30 1(2) . . . . ?
C28 C29 C30 C25 -1.3(19) . . . . ?
C30 C25 C26 C27 -3.4(18) . . . . ?
C31 P1 C19 C20 -10.1(12) . . . . ?
C31 P1 C19 C24 165.4(9) . . . . ?
C31 P1 C25 C26 -82.3(10) . . . . ?
C31 P1 C25 C30 94.4(10) . . . . ?
C31 P1 C37 C38 -34.9(11) . . . . ?
C31 P1 C37 C42 147.4(10) . . . . ?
C31 C32 C33 C34 -2.1(19) . . . . ?
C32 C31 C36 C35 -2.8(19) . . . . ?
C32 C33 C34 C35 5(2) . . . . ?
C33 C34 C35 C36 -7(2) . . . . ?
C34 C35 C36 C31 6(2) . . . . ?
C36 C31 C32 C33 1.0(19) . . . . ?
C37 P1 C19 C20 110.1(10) . . . . ?
C37 P1 C19 C24 -74.4(10) . . . . ?
C37 P1 C25 C26 160.0(9) . . . . ?
C37 P1 C25 C30 -23.4(11) . . . . ?
C37 P1 C31 C32 138.0(10) . . . . ?
C37 P1 C31 C36 -48.4(11) . . . . ?
C37 C38 C39 C40 1.7(17) . . . . ?
C38 C37 C42 C41 -1.8(18) . . . . ?
C38 C39 C40 C41 -2.0(18) . . . . ?
C39 C40 C41 C42 0.4(19) . . . . ?
C40 C41 C42 C37 1.6(19) . . . . ?
C42 C37 C38 C39 0.2(18) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 156.3 31.2 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran. acetic acid, and diethyl ether'
