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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_phpyNO_Ni_NCS2_140K
_audit_block_doi                 10.5517/ccdc.csd.cc24lhnx
_database_code_depnum_ccdc_archive 'CCDC 1983989'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;UEC Tokyo
Japan
;
_audit_update_record             
;
2020-02-14 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C32 H34 N6 Ni O2 S2'
_chemical_formula_moiety         'C32 H34 N6 Ni O2 S2'
_chemical_formula_weight         657.48
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   19.990(4)
_cell_length_b                   16.865(3)
_cell_length_c                   18.965(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.338(10)
_cell_angle_gamma                90.0000
_cell_volume                     6394(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14879
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    140
#------------------------------------------------------------------------------
_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.071
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2752.00
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_T_max  0.946

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

_diffrn_ambient_temperature      140
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 29.412
_diffrn_reflns_number            32607
_diffrn_reflns_av_R_equivalents  0.1492
_diffrn_reflns_theta_max         25.399
_diffrn_reflns_theta_min         3.057
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             11745
_reflns_number_gt                5664
_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          0.2057
_refine_ls_R_factor_gt           0.0997
_refine_ls_wR_factor_ref         0.2298
_refine_ls_wR_factor_gt          0.1914
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         11745
_refine_ls_number_parameters     775
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0245P)²+63.8805P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.38
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.22956(6) 0.44176(6) 0.53701(6) 0.0244(3) Uani 1 1 d . . . . .
Ni2 Ni 0.73083(6) 0.05702(7) 0.48845(6) 0.0273(3) Uani 1 1 d . . . . .
S1 S 0.04464(15) 0.39098(19) 0.68477(15) 0.0542(8) Uani 1 1 d . . . . .
S2 S 0.32934(14) 0.31806(18) 0.73480(14) 0.0484(8) Uani 1 1 d . . . . .
S3 S 0.58087(15) 0.09765(16) 0.30652(13) 0.0458(7) Uani 1 1 d . . . . .
S4 S 0.82428(15) 0.17260(16) 0.28445(13) 0.0461(7) Uani 1 1 d . . . . .
O1 O 0.3060(3) 0.4317(3) 0.4657(3) 0.0297(15) Uani 1 1 d . . . . .
O2 O 0.1874(3) 0.5273(3) 0.4745(3) 0.0331(16) Uani 1 1 d . . . . .
O3 O 0.8098(3) 0.0706(4) 0.5568(3) 0.0336(16) Uani 1 1 d . . . . .
O4 O 0.6966(3) -0.0319(3) 0.5527(3) 0.0311(15) Uani 1 1 d . . . . .
N1 N 0.2858(3) 0.4090(4) 0.4049(3) 0.0234(17) Uani 1 1 d . . . . .
N2 N 0.1961(3) 0.3610(4) 0.4647(3) 0.0210(16) Uani 1 1 d . . . . .
N3 N 0.1832(4) 0.5950(4) 0.5079(4) 0.0281(18) Uani 1 1 d . . . . .
N4 N 0.2687(3) 0.5440(4) 0.5772(3) 0.0199(16) Uani 1 1 d . . . . .
N5 N 0.1483(4) 0.4395(5) 0.5990(4) 0.0328(19) Uani 1 1 d . . . . .
N6 N 0.2810(4) 0.3702(4) 0.6042(4) 0.0314(19) Uani 1 1 d . . . . .
N7 N 0.7882(4) 0.0914(4) 0.6192(3) 0.0231(17) Uani 1 1 d . . . . .
N8 N 0.6972(4) 0.1388(4) 0.5587(3) 0.0237(17) Uani 1 1 d . . . . .
N9 N 0.6857(4) -0.0958(4) 0.5159(3) 0.0267(18) Uani 1 1 d . . . . .
N10 N 0.7664(4) -0.0445(4) 0.4441(3) 0.0232(17) Uani 1 1 d . . . . .
N11 N 0.6464(4) 0.0556(5) 0.4296(4) 0.038(2) Uani 1 1 d . . . . .
N12 N 0.7765(4) 0.1285(4) 0.4181(4) 0.032(2) Uani 1 1 d . . . . .
C1 C 0.2307(4) 0.3554(5) 0.4056(4) 0.021(2) Uani 1 1 d . . . . .
C2 C 0.2160(4) 0.3002(5) 0.3527(4) 0.027(2) Uani 1 1 d . . . . .
H2 H 0.2412 0.2982 0.3104 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1631(4) 0.2485(5) 0.3644(4) 0.024(2) Uani 1 1 d . . . . .
H3 H 0.1523 0.2101 0.3296 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1257(4) 0.2517(5) 0.4255(4) 0.022(2) Uani 1 1 d . . . . .
C5 C 0.1443(4) 0.3111(5) 0.4733(4) 0.028(2) Uani 1 1 d . . . . .
H5 H 0.1184 0.3166 0.5149 0.033 Uiso 1 1 calc R U . . .
C6 C 0.0693(4) 0.1979(5) 0.4396(5) 0.025(2) Uani 1 1 d . . . . .
C7 C 0.0339(4) 0.1622(5) 0.3838(5) 0.029(2) Uani 1 1 d . . . . .
H7 H 0.0456 0.1730 0.3363 0.035 Uiso 1 1 calc R U . . .
C8 C -0.0189(5) 0.1107(5) 0.3990(6) 0.038(3) Uani 1 1 d . . . . .
H8 H -0.0425 0.0859 0.3613 0.046 Uiso 1 1 calc R U . . .
C9 C -0.0370(5) 0.0952(6) 0.4666(6) 0.038(3) Uani 1 1 d . . . . .
H9 H -0.0739 0.0613 0.4758 0.046 Uiso 1 1 calc R U . . .
C10 C -0.0022(5) 0.1285(6) 0.5218(5) 0.038(3) Uani 1 1 d . . . . .
H10 H -0.0139 0.1162 0.5691 0.045 Uiso 1 1 calc R U . . .
C11 C 0.0503(5) 0.1804(5) 0.5083(5) 0.032(2) Uani 1 1 d . . . . .
H11 H 0.0736 0.2042 0.5466 0.038 Uiso 1 1 calc R U . . .
C12 C 0.3160(4) 0.4555(5) 0.3432(4) 0.026(2) Uani 1 1 d . . . . .
C13 C 0.3907(5) 0.4603(7) 0.3606(5) 0.048(3) Uani 1 1 d . . . . .
H13A H 0.3968 0.4857 0.4067 0.058 Uiso 1 1 calc R U . . .
H13B H 0.4096 0.4068 0.3619 0.058 Uiso 1 1 calc R U . . .
H13C H 0.4134 0.4916 0.3244 0.058 Uiso 1 1 calc R U . . .
C14 C 0.2851(6) 0.5375(5) 0.3451(5) 0.045(3) Uani 1 1 d . . . . .
H14A H 0.2928 0.5614 0.3915 0.054 Uiso 1 1 calc R U . . .
H14B H 0.3055 0.5708 0.3087 0.054 Uiso 1 1 calc R U . . .
H14C H 0.2368 0.5335 0.3362 0.054 Uiso 1 1 calc R U . . .
C15 C 0.3054(5) 0.4174(6) 0.2737(4) 0.037(2) Uani 1 1 d . . . . .
H15A H 0.3258 0.3646 0.2739 0.045 Uiso 1 1 calc R U . . .
H15B H 0.2573 0.4125 0.2644 0.045 Uiso 1 1 calc R U . . .
H15C H 0.3260 0.4498 0.2369 0.045 Uiso 1 1 calc R U . . .
C16 C 0.2373(4) 0.6106(5) 0.5542(4) 0.020(2) Uani 1 1 d . . . . .
C17 C 0.2591(4) 0.6861(5) 0.5741(5) 0.028(2) Uani 1 1 d . . . . .
H17 H 0.2370 0.7321 0.5568 0.033 Uiso 1 1 calc R U . . .
C18 C 0.3113(5) 0.6927(5) 0.6176(5) 0.029(2) Uani 1 1 d . . . . .
H18 H 0.3255 0.7440 0.6320 0.035 Uiso 1 1 calc R U . . .
C19 C 0.3465(4) 0.6251(5) 0.6431(5) 0.029(2) Uani 1 1 d . . . . .
C20 C 0.3217(5) 0.5521(5) 0.6186(4) 0.027(2) Uani 1 1 d . . . . .
H20 H 0.3446 0.5054 0.6329 0.033 Uiso 1 1 calc R U . . .
C21 C 0.4046(4) 0.6303(5) 0.6899(5) 0.029(2) Uani 1 1 d . . . . .
C22 C 0.4488(5) 0.6945(6) 0.6825(5) 0.035(2) Uani 1 1 d . . . . .
H22 H 0.4401 0.7338 0.6476 0.042 Uiso 1 1 calc R U . . .
C23 C 0.5053(5) 0.7014(7) 0.7257(5) 0.047(3) Uani 1 1 d . . . . .
H23 H 0.5351 0.7447 0.7196 0.057 Uiso 1 1 calc R U . . .
C24 C 0.5180(6) 0.6455(8) 0.7773(6) 0.056(3) Uani 1 1 d . . . . .
H24 H 0.5560 0.6508 0.8072 0.067 Uiso 1 1 calc R U . . .
C25 C 0.4749(6) 0.5816(7) 0.7854(5) 0.049(3) Uani 1 1 d . . . . .
H25 H 0.4836 0.5430 0.8208 0.059 Uiso 1 1 calc R U . . .
C26 C 0.4181(5) 0.5736(6) 0.7410(5) 0.040(3) Uani 1 1 d . . . . .
H26 H 0.3892 0.5293 0.7462 0.048 Uiso 1 1 calc R U . . .
C27 C 0.1204(5) 0.6429(5) 0.4979(5) 0.030(2) Uani 1 1 d . . . . .
C28 C 0.0651(6) 0.5867(7) 0.4820(7) 0.071(4) Uani 1 1 d . . . . .
H28A H 0.0234 0.6162 0.4752 0.085 Uiso 1 1 calc R U . . .
H28B H 0.0755 0.5571 0.4389 0.085 Uiso 1 1 calc R U . . .
H28C H 0.0601 0.5495 0.5214 0.085 Uiso 1 1 calc R U . . .
C29 C 0.1321(7) 0.6984(8) 0.4348(6) 0.087(5) Uani 1 1 d . . . . .
H29A H 0.1687 0.7352 0.4460 0.104 Uiso 1 1 calc R U . . .
H29B H 0.1440 0.6669 0.3933 0.104 Uiso 1 1 calc R U . . .
H29C H 0.0912 0.7286 0.4250 0.104 Uiso 1 1 calc R U . . .
C30 C 0.1048(5) 0.6882(7) 0.5652(5) 0.050(3) Uani 1 1 d . . . . .
H30A H 0.1412 0.7253 0.5756 0.060 Uiso 1 1 calc R U . . .
H30B H 0.0629 0.7178 0.5589 0.060 Uiso 1 1 calc R U . . .
H30C H 0.1000 0.6508 0.6043 0.060 Uiso 1 1 calc R U . . .
C31 C 0.1062(5) 0.4193(5) 0.6343(5) 0.030(2) Uani 1 1 d . . . . .
C32 C 0.3005(4) 0.3488(5) 0.6596(5) 0.028(2) Uani 1 1 d . . . . .
C33 C 0.7349(4) 0.1437(5) 0.6177(4) 0.024(2) Uani 1 1 d . . . . .
C34 C 0.7191(4) 0.1984(5) 0.6715(4) 0.021(2) Uani 1 1 d . . . . .
H34 H 0.7447 0.1997 0.7138 0.026 Uiso 1 1 calc R U . . .
C35 C 0.6666(4) 0.2493(5) 0.6619(4) 0.026(2) Uani 1 1 d . . . . .
H35 H 0.6560 0.2867 0.6976 0.031 Uiso 1 1 calc R U . . .
C36 C 0.6285(4) 0.2468(5) 0.6000(4) 0.023(2) Uani 1 1 d . . . . .
C37 C 0.6466(4) 0.1896(5) 0.5502(5) 0.028(2) Uani 1 1 d . . . . .
H37 H 0.6214 0.1868 0.5077 0.034 Uiso 1 1 calc R U . . .
C38 C 0.5720(4) 0.3020(5) 0.5842(4) 0.022(2) Uani 1 1 d . . . . .
C39 C 0.5304(4) 0.3303(5) 0.6369(5) 0.027(2) Uani 1 1 d . . . . .
H39 H 0.5387 0.3151 0.6843 0.033 Uiso 1 1 calc R U . . .
C40 C 0.4768(5) 0.3806(5) 0.6220(5) 0.036(2) Uani 1 1 d . . . . .
H40 H 0.4486 0.3987 0.6588 0.043 Uiso 1 1 calc R U . . .
C41 C 0.4654(5) 0.4035(6) 0.5541(5) 0.034(2) Uani 1 1 d . . . . .
H41 H 0.4292 0.4380 0.5436 0.041 Uiso 1 1 calc R U . . .
C42 C 0.5063(5) 0.3768(6) 0.4996(5) 0.044(3) Uani 1 1 d . . . . .
H42 H 0.4980 0.3925 0.4523 0.053 Uiso 1 1 calc R U . . .
C43 C 0.5586(5) 0.3275(5) 0.5156(4) 0.033(2) Uani 1 1 d . . . . .
H43 H 0.5868 0.3101 0.4786 0.039 Uiso 1 1 calc R U . . .
C44 C 0.8205(4) 0.0501(5) 0.6810(5) 0.028(2) Uani 1 1 d . . . . .
C45 C 0.8549(8) -0.0207(8) 0.6539(6) 0.100(6) Uani 1 1 d . . . . .
H45A H 0.8898 -0.0045 0.6208 0.120 Uiso 1 1 calc R U . . .
H45B H 0.8753 -0.0498 0.6933 0.120 Uiso 1 1 calc R U . . .
H45C H 0.8225 -0.0549 0.6296 0.120 Uiso 1 1 calc R U . . .
C46 C 0.8701(7) 0.1069(8) 0.7142(8) 0.106(6) Uani 1 1 d . . . . .
H46A H 0.8463 0.1536 0.7319 0.127 Uiso 1 1 calc R U . . .
H46B H 0.8933 0.0806 0.7534 0.127 Uiso 1 1 calc R U . . .
H46C H 0.9028 0.1234 0.6788 0.127 Uiso 1 1 calc R U . . .
C47 C 0.7668(7) 0.0287(9) 0.7317(7) 0.100(6) Uani 1 1 d . . . . .
H47A H 0.7450 0.0771 0.7487 0.120 Uiso 1 1 calc R U . . .
H47B H 0.7336 -0.0051 0.7082 0.120 Uiso 1 1 calc R U . . .
H47C H 0.7864 0.0001 0.7718 0.120 Uiso 1 1 calc R U . . .
C48 C 0.7338(4) -0.1093(5) 0.4623(4) 0.026(2) Uani 1 1 d . . . . .
C49 C 0.7485(5) -0.1846(5) 0.4329(4) 0.029(2) Uani 1 1 d . . . . .
H49 H 0.7263 -0.2312 0.4483 0.035 Uiso 1 1 calc R U . . .
C50 C 0.7960(5) -0.1871(5) 0.3813(5) 0.032(2) Uani 1 1 d . . . . .
H50 H 0.8059 -0.2364 0.3596 0.039 Uiso 1 1 calc R U . . .
C51 C 0.8296(4) -0.1206(5) 0.3600(4) 0.024(2) Uani 1 1 d . . . . .
C52 C 0.8138(4) -0.0495(5) 0.3950(4) 0.026(2) Uani 1 1 d . . . . .
H52 H 0.8380 -0.0029 0.3831 0.031 Uiso 1 1 calc R U . . .
C53 C 0.8783(5) -0.1196(6) 0.3029(5) 0.032(2) Uani 1 1 d . . . . .
C54 C 0.9228(5) -0.1808(7) 0.2920(5) 0.045(3) Uani 1 1 d . . . . .
H54 H 0.9215 -0.2259 0.3219 0.054 Uiso 1 1 calc R U . . .
C55 C 0.9700(6) -0.1778(8) 0.2377(6) 0.062(4) Uani 1 1 d . . . . .
H55 H 1.0010 -0.2200 0.2316 0.074 Uiso 1 1 calc R U . . .
C56 C 0.9712(6) -0.1138(9) 0.1938(7) 0.068(4) Uani 1 1 d . . . . .
H56 H 1.0028 -0.1118 0.1567 0.082 Uiso 1 1 calc R U . . .
C57 C 0.9274(6) -0.0524(7) 0.2026(6) 0.061(3) Uani 1 1 d . . . . .
H57 H 0.9277 -0.0090 0.1706 0.073 Uiso 1 1 calc R U . . .
C58 C 0.8826(6) -0.0534(7) 0.2577(5) 0.050(3) Uani 1 1 d . . . . .
H58 H 0.8545 -0.0089 0.2654 0.060 Uiso 1 1 calc R U . . .
C59 C 0.6197(5) -0.1416(6) 0.5251(5) 0.034(2) Uani 1 1 d . . . . .
C60 C 0.5765(5) -0.0878(6) 0.5694(6) 0.054(3) Uani 1 1 d . . . . .
H60A H 0.5975 -0.0803 0.6157 0.065 Uiso 1 1 calc R U . . .
H60B H 0.5719 -0.0363 0.5459 0.065 Uiso 1 1 calc R U . . .
H60C H 0.5323 -0.1118 0.5752 0.065 Uiso 1 1 calc R U . . .
C61 C 0.5897(5) -0.1554(6) 0.4522(5) 0.047(3) Uani 1 1 d . . . . .
H61A H 0.6191 -0.1905 0.4253 0.056 Uiso 1 1 calc R U . . .
H61B H 0.5456 -0.1801 0.4569 0.056 Uiso 1 1 calc R U . . .
H61C H 0.5852 -0.1046 0.4276 0.056 Uiso 1 1 calc R U . . .
C62 C 0.6343(5) -0.2199(6) 0.5627(5) 0.047(3) Uani 1 1 d . . . . .
H62A H 0.6624 -0.2533 0.5326 0.056 Uiso 1 1 calc R U . . .
H62B H 0.6578 -0.2094 0.6072 0.056 Uiso 1 1 calc R U . . .
H62C H 0.5922 -0.2474 0.5724 0.056 Uiso 1 1 calc R U . . .
C63 C 0.6205(4) 0.0730(5) 0.3793(5) 0.025(2) Uani 1 1 d . . . . .
C64 C 0.7960(5) 0.1451(5) 0.3626(5) 0.030(2) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.1'

#==============================================================================
# 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 N5 2.012(8) . ?
Ni1 N6 2.030(8) . ?
Ni1 N4 2.039(6) . ?
Ni1 N2 2.042(7) . ?
Ni1 O2 2.046(6) . ?
Ni1 O1 2.053(6) . ?
Ni2 N11 2.019(9) . ?
Ni2 N12 2.020(8) . ?
Ni2 N8 2.034(7) . ?
Ni2 N10 2.039(7) . ?
Ni2 O3 2.049(6) . ?
Ni2 O4 2.052(6) . ?
S1 C31 1.635(11) . ?
S2 C32 1.620(10) . ?
S3 C63 1.640(10) . ?
S4 C64 1.655(11) . ?
O1 N1 1.278(8) . ?
O2 N3 1.309(8) . ?
O3 N7 1.312(8) . ?
O4 N9 1.302(8) . ?
N1 C1 1.424(10) . ?
N1 C12 1.536(10) . ?
N2 C1 1.324(10) . ?
N2 C5 1.346(11) . ?
N3 C16 1.414(10) . ?
N3 C27 1.503(11) . ?
N4 C20 1.323(10) . ?
N4 C16 1.358(10) . ?
N5 C31 1.130(11) . ?
N6 C32 1.176(11) . ?
N7 C33 1.383(10) . ?
N7 C44 1.505(10) . ?
N8 C37 1.335(10) . ?
N8 C33 1.348(10) . ?
N9 C48 1.422(11) . ?
N9 C59 1.540(12) . ?
N10 C48 1.320(10) . ?
N10 C52 1.336(10) . ?
N11 C63 1.121(10) . ?
N12 C64 1.160(11) . ?
C1 C2 1.399(11) . ?
C2 C3 1.390(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.400(11) . ?
C4 C6 1.475(12) . ?
C5 H5 0.9500 . ?
C6 C11 1.390(12) . ?
C6 C7 1.405(12) . ?
C7 C8 1.398(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.361(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.373(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(12) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C15 1.480(11) . ?
C12 C14 1.516(12) . ?
C12 C13 1.529(12) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.397(11) . ?
C17 C18 1.331(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.423(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.405(12) . ?
C19 C21 1.461(12) . ?
C20 H20 0.9500 . ?
C21 C26 1.385(13) . ?
C21 C22 1.406(13) . ?
C22 C23 1.397(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(15) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(15) . ?
C24 H24 0.9500 . ?
C25 C26 1.416(13) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.486(14) . ?
C27 C30 1.521(12) . ?
C27 C29 1.538(13) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C33 C34 1.411(11) . ?
C34 C35 1.369(11) . ?
C34 H34 0.9500 . ?
C35 C36 1.396(11) . ?
C35 H35 0.9500 . ?
C36 C37 1.399(11) . ?
C36 C38 1.492(11) . ?
C37 H37 0.9500 . ?
C38 C39 1.390(11) . ?
C38 C43 1.395(11) . ?
C39 C40 1.393(12) . ?
C39 H39 0.9500 . ?
C40 C41 1.363(12) . ?
C40 H40 0.9500 . ?
C41 C42 1.396(13) . ?
C41 H41 0.9500 . ?
C42 C43 1.367(12) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.471(14) . ?
C44 C47 1.491(14) . ?
C44 C46 1.514(15) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.418(12) . ?
C49 C50 1.368(12) . ?
C49 H49 0.9500 . ?
C50 C51 1.371(12) . ?
C50 H50 0.9500 . ?
C51 C52 1.407(11) . ?
C51 C53 1.460(12) . ?
C52 H52 0.9500 . ?
C53 C54 1.380(13) . ?
C53 C58 1.410(13) . ?
C54 C55 1.401(15) . ?
C54 H54 0.9500 . ?
C55 C56 1.363(17) . ?
C55 H55 0.9500 . ?
C56 C57 1.366(17) . ?
C56 H56 0.9500 . ?
C57 C58 1.380(14) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C60 1.509(13) . ?
C59 C61 1.522(12) . ?
C59 C62 1.529(13) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N6 91.7(3) . . ?
N5 Ni1 N4 96.2(3) . . ?
N6 Ni1 N4 94.4(3) . . ?
N5 Ni1 N2 96.7(3) . . ?
N6 Ni1 N2 100.8(3) . . ?
N4 Ni1 N2 159.7(3) . . ?
N5 Ni1 O2 91.2(3) . . ?
N6 Ni1 O2 171.2(3) . . ?
N4 Ni1 O2 77.1(2) . . ?
N2 Ni1 O2 87.1(2) . . ?
N5 Ni1 O1 171.9(3) . . ?
N6 Ni1 O1 89.4(3) . . ?
N4 Ni1 O1 91.8(2) . . ?
N2 Ni1 O1 75.2(3) . . ?
O2 Ni1 O1 88.9(2) . . ?
N11 Ni2 N12 91.2(3) . . ?
N11 Ni2 N8 95.3(3) . . ?
N12 Ni2 N8 100.4(3) . . ?
N11 Ni2 N10 93.1(3) . . ?
N12 Ni2 N10 93.9(3) . . ?
N8 Ni2 N10 163.2(3) . . ?
N11 Ni2 O3 171.8(3) . . ?
N12 Ni2 O3 90.1(3) . . ?
N8 Ni2 O3 76.5(3) . . ?
N10 Ni2 O3 94.9(3) . . ?
N11 Ni2 O4 92.3(3) . . ?
N12 Ni2 O4 169.0(3) . . ?
N8 Ni2 O4 89.7(2) . . ?
N10 Ni2 O4 75.5(3) . . ?
O3 Ni2 O4 88.0(2) . . ?
N1 O1 Ni1 112.8(5) . . ?
N3 O2 Ni1 111.2(5) . . ?
N7 O3 Ni2 110.1(5) . . ?
N9 O4 Ni2 110.0(5) . . ?
O1 N1 C1 114.9(6) . . ?
O1 N1 C12 114.2(6) . . ?
C1 N1 C12 129.7(6) . . ?
C1 N2 C5 117.7(7) . . ?
C1 N2 Ni1 116.5(6) . . ?
C5 N2 Ni1 125.8(6) . . ?
O2 N3 C16 114.4(7) . . ?
O2 N3 C27 117.6(7) . . ?
C16 N3 C27 127.8(7) . . ?
C20 N4 C16 118.1(7) . . ?
C20 N4 Ni1 127.9(6) . . ?
C16 N4 Ni1 113.8(5) . . ?
C31 N5 Ni1 163.4(8) . . ?
C32 N6 Ni1 155.2(7) . . ?
O3 N7 C33 114.2(6) . . ?
O3 N7 C44 115.8(6) . . ?
C33 N7 C44 129.7(7) . . ?
C37 N8 C33 118.7(7) . . ?
C37 N8 Ni2 127.6(6) . . ?
C33 N8 Ni2 113.6(5) . . ?
O4 N9 C48 113.8(7) . . ?
O4 N9 C59 119.7(7) . . ?
C48 N9 C59 125.8(7) . . ?
C48 N10 C52 119.0(7) . . ?
C48 N10 Ni2 114.4(6) . . ?
C52 N10 Ni2 126.3(6) . . ?
C63 N11 Ni2 148.0(8) . . ?
C64 N12 Ni2 154.1(7) . . ?
N2 C1 C2 123.1(8) . . ?
N2 C1 N1 111.8(7) . . ?
C2 C1 N1 125.0(8) . . ?
C3 C2 C1 117.3(8) . . ?
C3 C2 H2 121.3 . . ?
C1 C2 H2 121.3 . . ?
C4 C3 C2 121.7(8) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 115.4(8) . . ?
C3 C4 C6 123.1(8) . . ?
C5 C4 C6 121.5(8) . . ?
N2 C5 C4 124.8(8) . . ?
N2 C5 H5 117.6 . . ?
C4 C5 H5 117.6 . . ?
C11 C6 C7 118.4(8) . . ?
C11 C6 C4 121.0(8) . . ?
C7 C6 C4 120.6(8) . . ?
C8 C7 C6 119.2(9) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 121.2(9) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 120.3(9) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 119.7(9) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C6 C11 C10 121.2(8) . . ?
C6 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C15 C12 C14 111.2(8) . . ?
C15 C12 C13 110.5(8) . . ?
C14 C12 C13 110.1(8) . . ?
C15 C12 N1 113.6(7) . . ?
C14 C12 N1 106.6(7) . . ?
C13 C12 N1 104.5(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 C17 121.7(8) . . ?
N4 C16 N3 113.3(7) . . ?
C17 C16 N3 125.0(8) . . ?
C18 C17 C16 119.0(8) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 121.9(8) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C20 C19 C18 114.7(8) . . ?
C20 C19 C21 122.0(8) . . ?
C18 C19 C21 123.3(8) . . ?
N4 C20 C19 124.6(8) . . ?
N4 C20 H20 117.7 . . ?
C19 C20 H20 117.7 . . ?
C26 C21 C22 118.8(9) . . ?
C26 C21 C19 122.4(9) . . ?
C22 C21 C19 118.9(8) . . ?
C23 C22 C21 120.7(9) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C22 120.2(11) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.8(11) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 120.2(10) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 120.2(10) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C28 C27 N3 107.6(8) . . ?
C28 C27 C30 109.5(9) . . ?
N3 C27 C30 109.9(7) . . ?
C28 C27 C29 110.3(9) . . ?
N3 C27 C29 107.1(8) . . ?
C30 C27 C29 112.3(9) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 S1 179.2(10) . . ?
N6 C32 S2 178.3(9) . . ?
N8 C33 N7 113.9(7) . . ?
N8 C33 C34 121.0(7) . . ?
N7 C33 C34 125.2(8) . . ?
C35 C34 C33 119.2(8) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 120.5(8) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C37 116.5(8) . . ?
C35 C36 C38 124.0(7) . . ?
C37 C36 C38 119.5(7) . . ?
N8 C37 C36 124.1(8) . . ?
N8 C37 H37 118.0 . . ?
C36 C37 H37 118.0 . . ?
C39 C38 C43 116.8(8) . . ?
C39 C38 C36 121.7(7) . . ?
C43 C38 C36 121.5(8) . . ?
C38 C39 C40 121.8(8) . . ?
C38 C39 H39 119.1 . . ?
C40 C39 H39 119.1 . . ?
C41 C40 C39 119.2(9) . . ?
C41 C40 H40 120.4 . . ?
C39 C40 H40 120.4 . . ?
C40 C41 C42 120.9(9) . . ?
C40 C41 H41 119.6 . . ?
C42 C41 H41 119.6 . . ?
C43 C42 C41 118.9(9) . . ?
C43 C42 H42 120.6 . . ?
C41 C42 H42 120.6 . . ?
C42 C43 C38 122.5(9) . . ?
C42 C43 H43 118.8 . . ?
C38 C43 H43 118.8 . . ?
C45 C44 C47 111.7(10) . . ?
C45 C44 N7 107.7(8) . . ?
C47 C44 N7 107.8(8) . . ?
C45 C44 C46 110.7(11) . . ?
C47 C44 C46 110.9(11) . . ?
N7 C44 C46 107.9(8) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N10 C48 C49 122.3(8) . . ?
N10 C48 N9 113.1(7) . . ?
C49 C48 N9 124.6(8) . . ?
C50 C49 C48 117.1(8) . . ?
C50 C49 H49 121.5 . . ?
C48 C49 H49 121.5 . . ?
C49 C50 C51 122.0(8) . . ?
C49 C50 H50 119.0 . . ?
C51 C50 H50 119.0 . . ?
C50 C51 C52 116.5(8) . . ?
C50 C51 C53 124.0(8) . . ?
C52 C51 C53 119.5(8) . . ?
N10 C52 C51 123.0(8) . . ?
N10 C52 H52 118.5 . . ?
C51 C52 H52 118.5 . . ?
C54 C53 C58 117.3(9) . . ?
C54 C53 C51 122.4(9) . . ?
C58 C53 C51 120.2(9) . . ?
C53 C54 C55 121.4(11) . . ?
C53 C54 H54 119.3 . . ?
C55 C54 H54 119.3 . . ?
C56 C55 C54 119.3(12) . . ?
C56 C55 H55 120.3 . . ?
C54 C55 H55 120.3 . . ?
C55 C56 C57 120.8(12) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 H56 119.6 . . ?
C56 C57 C58 120.1(12) . . ?
C56 C57 H57 119.9 . . ?
C58 C57 H57 119.9 . . ?
C57 C58 C53 120.8(11) . . ?
C57 C58 H58 119.6 . . ?
C53 C58 H58 119.6 . . ?
C60 C59 C61 112.0(9) . . ?
C60 C59 C62 111.7(8) . . ?
C61 C59 C62 111.3(8) . . ?
C60 C59 N9 104.8(8) . . ?
C61 C59 N9 107.9(7) . . ?
C62 C59 N9 108.9(8) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N11 C63 S3 178.6(9) . . ?
N12 C64 S4 177.6(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 O1 N1 C1 -33.7(8) . . . . ?
Ni1 O1 N1 C12 135.3(5) . . . . ?
Ni1 O2 N3 C16 35.8(8) . . . . ?
Ni1 O2 N3 C27 -139.1(6) . . . . ?
Ni2 O3 N7 C33 -38.2(8) . . . . ?
Ni2 O3 N7 C44 136.8(6) . . . . ?
Ni2 O4 N9 C48 38.2(7) . . . . ?
Ni2 O4 N9 C59 -132.6(6) . . . . ?
C5 N2 C1 C2 -0.4(12) . . . . ?
Ni1 N2 C1 C2 176.7(6) . . . . ?
C5 N2 C1 N1 -177.3(7) . . . . ?
Ni1 N2 C1 N1 -0.1(9) . . . . ?
O1 N1 C1 N2 22.6(10) . . . . ?
C12 N1 C1 N2 -144.5(8) . . . . ?
O1 N1 C1 C2 -154.2(8) . . . . ?
C12 N1 C1 C2 38.7(13) . . . . ?
N2 C1 C2 C3 -1.1(13) . . . . ?
N1 C1 C2 C3 175.3(8) . . . . ?
C1 C2 C3 C4 0.7(13) . . . . ?
C2 C3 C4 C5 1.1(12) . . . . ?
C2 C3 C4 C6 180.0(8) . . . . ?
C1 N2 C5 C4 2.5(12) . . . . ?
Ni1 N2 C5 C4 -174.3(6) . . . . ?
C3 C4 C5 N2 -2.8(12) . . . . ?
C6 C4 C5 N2 178.3(8) . . . . ?
C3 C4 C6 C11 154.2(8) . . . . ?
C5 C4 C6 C11 -27.0(12) . . . . ?
C3 C4 C6 C7 -24.9(12) . . . . ?
C5 C4 C6 C7 153.8(8) . . . . ?
C11 C6 C7 C8 0.0(13) . . . . ?
C4 C6 C7 C8 179.2(8) . . . . ?
C6 C7 C8 C9 0.8(14) . . . . ?
C7 C8 C9 C10 -2.0(15) . . . . ?
C8 C9 C10 C11 2.3(15) . . . . ?
C7 C6 C11 C10 0.3(13) . . . . ?
C4 C6 C11 C10 -178.8(8) . . . . ?
C9 C10 C11 C6 -1.5(14) . . . . ?
O1 N1 C12 C15 166.3(7) . . . . ?
C1 N1 C12 C15 -26.6(12) . . . . ?
O1 N1 C12 C14 -70.9(9) . . . . ?
C1 N1 C12 C14 96.2(10) . . . . ?
O1 N1 C12 C13 45.7(9) . . . . ?
C1 N1 C12 C13 -147.2(8) . . . . ?
C20 N4 C16 C17 -0.8(12) . . . . ?
Ni1 N4 C16 C17 -177.4(6) . . . . ?
C20 N4 C16 N3 177.4(7) . . . . ?
Ni1 N4 C16 N3 0.8(8) . . . . ?
O2 N3 C16 N4 -24.6(10) . . . . ?
C27 N3 C16 N4 149.7(8) . . . . ?
O2 N3 C16 C17 153.6(8) . . . . ?
C27 N3 C16 C17 -32.1(13) . . . . ?
N4 C16 C17 C18 -1.2(13) . . . . ?
N3 C16 C17 C18 -179.2(8) . . . . ?
C16 C17 C18 C19 1.5(14) . . . . ?
C17 C18 C19 C20 0.1(13) . . . . ?
C17 C18 C19 C21 179.0(9) . . . . ?
C16 N4 C20 C19 2.6(12) . . . . ?
Ni1 N4 C20 C19 178.7(6) . . . . ?
C18 C19 C20 N4 -2.3(13) . . . . ?
C21 C19 C20 N4 178.9(8) . . . . ?
C20 C19 C21 C26 -34.5(13) . . . . ?
C18 C19 C21 C26 146.7(9) . . . . ?
C20 C19 C21 C22 144.9(9) . . . . ?
C18 C19 C21 C22 -33.9(13) . . . . ?
C26 C21 C22 C23 0.0(14) . . . . ?
C19 C21 C22 C23 -179.4(8) . . . . ?
C21 C22 C23 C24 -1.0(15) . . . . ?
C22 C23 C24 C25 1.1(16) . . . . ?
C23 C24 C25 C26 -0.1(15) . . . . ?
C22 C21 C26 C25 1.0(14) . . . . ?
C19 C21 C26 C25 -179.6(8) . . . . ?
C24 C25 C26 C21 -1.0(15) . . . . ?
O2 N3 C27 C28 28.0(11) . . . . ?
C16 N3 C27 C28 -146.1(9) . . . . ?
O2 N3 C27 C30 147.2(8) . . . . ?
C16 N3 C27 C30 -26.9(12) . . . . ?
O2 N3 C27 C29 -90.5(10) . . . . ?
C16 N3 C27 C29 95.4(11) . . . . ?
C37 N8 C33 N7 -176.5(7) . . . . ?
Ni2 N8 C33 N7 -0.9(9) . . . . ?
C37 N8 C33 C34 3.5(12) . . . . ?
Ni2 N8 C33 C34 179.1(6) . . . . ?
O3 N7 C33 N8 26.4(10) . . . . ?
C44 N7 C33 N8 -147.7(8) . . . . ?
O3 N7 C33 C34 -153.6(8) . . . . ?
C44 N7 C33 C34 32.3(14) . . . . ?
N8 C33 C34 C35 -2.9(13) . . . . ?
N7 C33 C34 C35 177.1(8) . . . . ?
C33 C34 C35 C36 0.7(13) . . . . ?
C34 C35 C36 C37 0.8(12) . . . . ?
C34 C35 C36 C38 -177.7(8) . . . . ?
C33 N8 C37 C36 -2.0(13) . . . . ?
Ni2 N8 C37 C36 -176.9(6) . . . . ?
C35 C36 C37 N8 -0.1(13) . . . . ?
C38 C36 C37 N8 178.5(8) . . . . ?
C35 C36 C38 C39 -34.3(13) . . . . ?
C37 C36 C38 C39 147.3(9) . . . . ?
C35 C36 C38 C43 145.7(9) . . . . ?
C37 C36 C38 C43 -32.8(12) . . . . ?
C43 C38 C39 C40 1.4(13) . . . . ?
C36 C38 C39 C40 -178.7(8) . . . . ?
C38 C39 C40 C41 -0.9(14) . . . . ?
C39 C40 C41 C42 0.5(15) . . . . ?
C40 C41 C42 C43 -0.5(16) . . . . ?
C41 C42 C43 C38 1.0(15) . . . . ?
C39 C38 C43 C42 -1.4(14) . . . . ?
C36 C38 C43 C42 178.7(9) . . . . ?
O3 N7 C44 C45 -16.5(12) . . . . ?
C33 N7 C44 C45 157.5(10) . . . . ?
O3 N7 C44 C47 -137.1(9) . . . . ?
C33 N7 C44 C47 36.9(13) . . . . ?
O3 N7 C44 C46 103.0(10) . . . . ?
C33 N7 C44 C46 -83.0(12) . . . . ?
C52 N10 C48 C49 1.7(12) . . . . ?
Ni2 N10 C48 C49 175.5(6) . . . . ?
C52 N10 C48 N9 178.9(7) . . . . ?
Ni2 N10 C48 N9 -7.3(9) . . . . ?
O4 N9 C48 N10 -21.1(10) . . . . ?
C59 N9 C48 N10 149.1(8) . . . . ?
O4 N9 C48 C49 156.1(8) . . . . ?
C59 N9 C48 C49 -33.7(13) . . . . ?
N10 C48 C49 C50 -3.4(13) . . . . ?
N9 C48 C49 C50 179.6(8) . . . . ?
C48 C49 C50 C51 1.8(13) . . . . ?
C49 C50 C51 C52 1.3(13) . . . . ?
C49 C50 C51 C53 -176.9(8) . . . . ?
C48 N10 C52 C51 1.8(12) . . . . ?
Ni2 N10 C52 C51 -171.2(6) . . . . ?
C50 C51 C52 N10 -3.3(12) . . . . ?
C53 C51 C52 N10 175.0(8) . . . . ?
C50 C51 C53 C54 -38.3(13) . . . . ?
C52 C51 C53 C54 143.5(9) . . . . ?
C50 C51 C53 C58 143.9(9) . . . . ?
C52 C51 C53 C58 -34.3(12) . . . . ?
C58 C53 C54 C55 -0.8(14) . . . . ?
C51 C53 C54 C55 -178.6(9) . . . . ?
C53 C54 C55 C56 -1.3(16) . . . . ?
C54 C55 C56 C57 0.6(18) . . . . ?
C55 C56 C57 C58 2.2(18) . . . . ?
C56 C57 C58 C53 -4.3(16) . . . . ?
C54 C53 C58 C57 3.6(14) . . . . ?
C51 C53 C58 C57 -178.5(9) . . . . ?
O4 N9 C59 C60 10.1(10) . . . . ?
C48 N9 C59 C60 -159.6(8) . . . . ?
O4 N9 C59 C61 129.5(8) . . . . ?
C48 N9 C59 C61 -40.2(11) . . . . ?
O4 N9 C59 C62 -109.6(8) . . . . ?
C48 N9 C59 C62 80.8(10) . . . . ?

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



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        '[Ni(phpyNO)2(NCS)2]'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_phpyNO_Ni_NCS2_400K
_audit_block_doi                 10.5517/ccdc.csd.cc24lhpy
_database_code_depnum_ccdc_archive 'CCDC 1983990'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;UEC Tokyo
Japan
;
_audit_update_record             
;
2020-02-14 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C32 H34 N6 Ni O2 S2'
_chemical_formula_moiety         'C32 H34 N6 Ni O2 S2'
_chemical_formula_weight         657.48
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_IT_number           61
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,-Z
3 -X,1/2+Y,1/2-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,+Z
7 +X,-1/2-Y,-1/2+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   17.0732(19)
_cell_length_b                   19.194(3)
_cell_length_c                   20.667(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     6772.7(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    25622
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.56
_cell_measurement_temperature    400
#------------------------------------------------------------------------------
_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.177
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2752.00
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.878

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

_diffrn_ambient_temperature      400
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 29.412
_diffrn_reflns_number            75566
_diffrn_reflns_av_R_equivalents  0.1293
_diffrn_reflns_theta_max         26.596
_diffrn_reflns_theta_min         3.095
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7078
_reflns_number_gt                3016
_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          0.1954
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.1563
_refine_ls_wR_factor_gt          0.1227
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7078
_refine_ls_number_parameters     416
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0514P)²+2.6054P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.43367(3) 0.46961(3) 0.76739(3) 0.0862(2) Uani 1 1 d . . . . .
S1 S 0.40775(13) 0.31016(9) 0.93669(9) 0.1727(8) Uani 1 1 d . . . . .
S2 S 0.32127(10) 0.27768(9) 0.66660(10) 0.1611(7) Uani 1 1 d . . . . .
O1 O 0.43302(18) 0.54378(16) 0.69652(15) 0.1056(10) Uani 1 1 d . . . . .
O2 O 0.51809(19) 0.52715(16) 0.81512(17) 0.1170(11) Uani 1 1 d . . . . .
N1 N 0.40647(19) 0.60340(19) 0.71475(16) 0.0820(9) Uani 1 1 d . . . . .
N2 N 0.35283(18) 0.54160(18) 0.79902(17) 0.0787(9) Uani 1 1 d . . . . .
N3 N 0.5850(2) 0.4959(2) 0.8188(2) 0.0920(10) Uani 1 1 d . . . . .
N4 N 0.53781(17) 0.42899(18) 0.73573(18) 0.0792(9) Uani 1 1 d . . . . .
N5 N 0.4252(2) 0.4068(2) 0.8441(2) 0.1206(15) Uani 1 1 d . . . . .
N6 N 0.3658(2) 0.4058(2) 0.7127(2) 0.1054(13) Uani 1 1 d . . . . .
C1 C 0.3526(2) 0.6021(2) 0.7667(2) 0.0757(11) Uani 1 1 d . . . . .
C2 C 0.3007(2) 0.6544(2) 0.7819(2) 0.0883(12) Uani 1 1 d . . . . .
H2 H 0.2998 0.6955 0.7581 0.106 Uiso 1 1 calc R U . . .
C3 C 0.2498(2) 0.6446(2) 0.8332(2) 0.0868(12) Uani 1 1 d . . . . .
H3 H 0.2150 0.6799 0.8443 0.104 Uiso 1 1 calc R U . . .
C4 C 0.2500(2) 0.5836(2) 0.8680(2) 0.0738(11) Uani 1 1 d . . . . .
C5 C 0.3036(2) 0.5341(2) 0.8482(2) 0.0819(12) Uani 1 1 d . . . . .
H5 H 0.3052 0.4923 0.8709 0.098 Uiso 1 1 calc R U . . .
C6 C 0.1971(2) 0.5705(2) 0.9233(2) 0.0757(11) Uani 1 1 d . . . . .
C7 C 0.1680(3) 0.6230(3) 0.9604(2) 0.1005(14) Uani 1 1 d . . . . .
H7 H 0.1808 0.6688 0.9503 0.121 Uiso 1 1 calc R U . . .
C8 C 0.1199(3) 0.6099(4) 1.0127(3) 0.1255(18) Uani 1 1 d . . . . .
H8 H 0.1011 0.6466 1.0376 0.151 Uiso 1 1 calc R U . . .
C9 C 0.1001(3) 0.5435(4) 1.0277(3) 0.130(2) Uani 1 1 d . . . . .
H9 H 0.0677 0.5345 1.0629 0.156 Uiso 1 1 calc R U . . .
C10 C 0.1275(4) 0.4907(3) 0.9914(3) 0.141(2) Uani 1 1 d . . . . .
H10 H 0.1141 0.4450 1.0014 0.169 Uiso 1 1 calc R U . . .
C11 C 0.1755(3) 0.5044(3) 0.9393(2) 0.1138(16) Uani 1 1 d . . . . .
H11 H 0.1937 0.4674 0.9144 0.137 Uiso 1 1 calc R U . . .
C12 C 0.4446(3) 0.6646(3) 0.6831(3) 0.0988(14) Uani 1 1 d . . . . .
C16 C 0.6011(2) 0.4481(2) 0.7698(2) 0.0776(11) Uani 1 1 d . . . . .
C17 C 0.6751(2) 0.4233(3) 0.7550(2) 0.0939(13) Uani 1 1 d . . . . .
H17 H 0.7185 0.4374 0.7788 0.113 Uiso 1 1 calc R U . . .
C18 C 0.6829(2) 0.3781(2) 0.7049(2) 0.0928(13) Uani 1 1 d . . . . .
H18 H 0.7323 0.3605 0.6953 0.111 Uiso 1 1 calc R U . . .
C19 C 0.6197(2) 0.3576(2) 0.6679(2) 0.0788(11) Uani 1 1 d . . . . .
C20 C 0.5480(2) 0.3857(2) 0.6864(2) 0.0824(12) Uani 1 1 d . . . . .
H20 H 0.5041 0.3733 0.6625 0.099 Uiso 1 1 calc R U . . .
C21 C 0.6262(3) 0.3104(3) 0.6130(2) 0.0962(14) Uani 1 1 d . . . . .
C22 C 0.6927(3) 0.3090(3) 0.5743(3) 0.1204(18) Uani 1 1 d . . . . .
H22 H 0.7345 0.3384 0.5836 0.144 Uiso 1 1 calc R U . . .
C23 C 0.6972(5) 0.2645(4) 0.5224(4) 0.158(3) Uani 1 1 d . . . . .
H23 H 0.7415 0.2647 0.4963 0.190 Uiso 1 1 calc R U . . .
C24 C 0.6382(8) 0.2209(5) 0.5091(5) 0.184(4) Uani 1 1 d . . . . .
H24 H 0.6421 0.1905 0.4742 0.220 Uiso 1 1 calc R U . . .
C25 C 0.5720(6) 0.2210(5) 0.5469(5) 0.179(3) Uani 1 1 d . . . . .
H25 H 0.5313 0.1904 0.5377 0.215 Uiso 1 1 calc R U . . .
C26 C 0.5659(4) 0.2664(3) 0.5984(3) 0.1289(19) Uani 1 1 d . . . . .
H26 H 0.5205 0.2670 0.6232 0.155 Uiso 1 1 calc R U . . .
C27 C 0.6340(3) 0.5126(3) 0.8770(3) 0.1108(15) Uani 1 1 d . . . . .
C28 C 0.5841(5) 0.5502(5) 0.9229(3) 0.254(5) Uani 1 1 d . . . . .
H28A H 0.6139 0.5616 0.9608 0.305 Uiso 1 1 calc R U . . .
H28B H 0.5653 0.5922 0.9031 0.305 Uiso 1 1 calc R U . . .
H28C H 0.5405 0.5214 0.9348 0.305 Uiso 1 1 calc R U . . .
C29 C 0.6611(4) 0.4449(3) 0.9071(3) 0.176(3) Uani 1 1 d . . . . .
H29A H 0.6938 0.4203 0.8770 0.211 Uiso 1 1 calc R U . . .
H29B H 0.6903 0.4547 0.9458 0.211 Uiso 1 1 calc R U . . .
H29C H 0.6163 0.4168 0.9177 0.211 Uiso 1 1 calc R U . . .
C30 C 0.7040(4) 0.5554(4) 0.8563(4) 0.199(3) Uani 1 1 d . . . . .
H30A H 0.7351 0.5290 0.8263 0.239 Uiso 1 1 calc R U . . .
H30B H 0.6863 0.5974 0.8358 0.239 Uiso 1 1 calc R U . . .
H30C H 0.7350 0.5669 0.8935 0.239 Uiso 1 1 calc R U . . .
C31 C 0.4185(2) 0.3678(2) 0.8817(2) 0.0855(13) Uani 1 1 d . . . . .
C32 C 0.3473(2) 0.3525(3) 0.6939(3) 0.0981(15) Uani 1 1 d . . . . .
C13A C 0.4668(11) 0.7164(8) 0.7342(7) 0.174(9) Uani 0.61(2) 1 d . . P A 1
H13A H 0.4206 0.7316 0.7566 0.209 Uiso 0.61(2) 1 calc R U P A 1
H13B H 0.5021 0.6950 0.7644 0.209 Uiso 0.61(2) 1 calc R U P A 1
H13C H 0.4918 0.7558 0.7144 0.209 Uiso 0.61(2) 1 calc R U P A 1
C14A C 0.5133(9) 0.6389(6) 0.6465(9) 0.172(10) Uani 0.61(2) 1 d . . P A 1
H14A H 0.5389 0.6774 0.6256 0.206 Uiso 0.61(2) 1 calc R U P A 1
H14B H 0.5493 0.6167 0.6756 0.206 Uiso 0.61(2) 1 calc R U P A 1
H14C H 0.4964 0.6060 0.6144 0.206 Uiso 0.61(2) 1 calc R U P A 1
C15A C 0.3845(9) 0.6954(10) 0.6375(8) 0.189(9) Uani 0.61(2) 1 d . . P A 1
H15A H 0.3403 0.7118 0.6619 0.227 Uiso 0.61(2) 1 calc R U P A 1
H15B H 0.4074 0.7335 0.6142 0.227 Uiso 0.61(2) 1 calc R U P A 1
H15C H 0.3676 0.6603 0.6074 0.227 Uiso 0.61(2) 1 calc R U P A 1
C13B C 0.5323(10) 0.6649(11) 0.7081(13) 0.154(12) Uani 0.39(2) 1 d . . P A 2
H13D H 0.5554 0.6200 0.7007 0.185 Uiso 0.39(2) 1 calc R U P A 2
H13E H 0.5616 0.6998 0.6852 0.185 Uiso 0.39(2) 1 calc R U P A 2
H13F H 0.5331 0.6752 0.7536 0.185 Uiso 0.39(2) 1 calc R U P A 2
C14B C 0.4483(17) 0.6509(9) 0.6110(7) 0.133(9) Uani 0.39(2) 1 d . . P A 2
H14D H 0.4707 0.6057 0.6035 0.159 Uiso 0.39(2) 1 calc R U P A 2
H14E H 0.3964 0.6523 0.5932 0.159 Uiso 0.39(2) 1 calc R U P A 2
H14F H 0.4801 0.6858 0.5907 0.159 Uiso 0.39(2) 1 calc R U P A 2
C15B C 0.4098(12) 0.7345(8) 0.6949(12) 0.124(9) Uani 0.39(2) 1 d . . P A 2
H15D H 0.4394 0.7691 0.6720 0.148 Uiso 0.39(2) 1 calc R U P A 2
H15E H 0.3566 0.7350 0.6799 0.148 Uiso 0.39(2) 1 calc R U P A 2
H15F H 0.4109 0.7445 0.7404 0.148 Uiso 0.39(2) 1 calc R U P A 2


#==============================================================================
_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.1'

#==============================================================================
# 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 N5 1.997(4) . ?
Ni1 N6 2.030(4) . ?
Ni1 O1 2.043(3) . ?
Ni1 N4 2.049(3) . ?
Ni1 N2 2.059(3) . ?
Ni1 O2 2.066(3) . ?
S1 C31 1.597(5) . ?
S2 C32 1.606(6) . ?
O1 N1 1.287(4) . ?
O2 N3 1.292(4) . ?
N1 C1 1.413(5) . ?
N1 C12 1.494(5) . ?
N2 C5 1.327(5) . ?
N2 C1 1.339(5) . ?
N3 C16 1.394(5) . ?
N3 C27 1.501(6) . ?
N4 C20 1.326(5) . ?
N4 C16 1.341(5) . ?
N5 C31 1.085(5) . ?
N6 C32 1.139(5) . ?
C1 C2 1.376(5) . ?
C2 C3 1.384(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.374(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(5) . ?
C4 C6 1.478(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.359(5) . ?
C6 C11 1.363(6) . ?
C7 C8 1.381(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.354(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.345(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(6) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C14A 1.481(10) . ?
C12 C15B 1.487(16) . ?
C12 C13A 1.500(12) . ?
C12 C15A 1.513(13) . ?
C12 C14B 1.513(15) . ?
C12 C13B 1.585(15) . ?
C16 C17 1.384(5) . ?
C17 C18 1.356(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.392(5) . ?
C19 C21 1.456(6) . ?
C20 H20 0.9300 . ?
C21 C26 1.365(6) . ?
C21 C22 1.390(6) . ?
C22 C23 1.373(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.337(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.374(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.380(9) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.465(7) . ?
C27 C30 1.512(7) . ?
C27 C29 1.513(7) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C13A H13A 0.9600 . ?
C13A H13B 0.9600 . ?
C13A H13C 0.9600 . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C15A H15A 0.9600 . ?
C15A H15B 0.9600 . ?
C15A H15C 0.9600 . ?
C13B H13D 0.9600 . ?
C13B H13E 0.9600 . ?
C13B H13F 0.9600 . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C15B H15D 0.9600 . ?
C15B H15E 0.9600 . ?
C15B H15F 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
N5 Ni1 N6 92.04(19) . . ?
N5 Ni1 O1 171.77(15) . . ?
N6 Ni1 O1 91.05(16) . . ?
N5 Ni1 N4 94.98(15) . . ?
N6 Ni1 N4 95.04(15) . . ?
O1 Ni1 N4 92.34(13) . . ?
N5 Ni1 N2 96.00(16) . . ?
N6 Ni1 N2 101.48(14) . . ?
O1 Ni1 N2 75.90(13) . . ?
N4 Ni1 N2 159.77(14) . . ?
N5 Ni1 O2 89.70(18) . . ?
N6 Ni1 O2 170.56(14) . . ?
O1 Ni1 O2 88.49(14) . . ?
N4 Ni1 O2 75.56(14) . . ?
N2 Ni1 O2 87.55(13) . . ?
N1 O1 Ni1 114.3(2) . . ?
N3 O2 Ni1 113.3(3) . . ?
O1 N1 C1 115.8(3) . . ?
O1 N1 C12 114.7(3) . . ?
C1 N1 C12 129.1(4) . . ?
C5 N2 C1 118.3(3) . . ?
C5 N2 Ni1 126.5(3) . . ?
C1 N2 Ni1 115.1(3) . . ?
O2 N3 C16 116.0(4) . . ?
O2 N3 C27 116.2(4) . . ?
C16 N3 C27 127.8(4) . . ?
C20 N4 C16 117.9(3) . . ?
C20 N4 Ni1 126.7(3) . . ?
C16 N4 Ni1 115.3(3) . . ?
C31 N5 Ni1 173.1(5) . . ?
C32 N6 Ni1 152.9(4) . . ?
N2 C1 C2 121.3(4) . . ?
N2 C1 N1 113.1(4) . . ?
C2 C1 N1 125.4(4) . . ?
C1 C2 C3 118.7(4) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 115.6(4) . . ?
C3 C4 C6 123.3(4) . . ?
C5 C4 C6 121.1(4) . . ?
N2 C5 C4 124.9(4) . . ?
N2 C5 H5 117.6 . . ?
C4 C5 H5 117.6 . . ?
C7 C6 C11 117.0(4) . . ?
C7 C6 C4 122.2(4) . . ?
C11 C6 C4 120.8(4) . . ?
C6 C7 C8 121.6(5) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 119.9(5) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 119.6(5) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 120.0(5) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C6 C11 C10 121.9(5) . . ?
C6 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C14A C12 N1 107.9(6) . . ?
C15B C12 N1 117.6(7) . . ?
C14A C12 C13A 112.4(9) . . ?
N1 C12 C13A 108.8(6) . . ?
C14A C12 C15A 110.4(9) . . ?
N1 C12 C15A 106.5(6) . . ?
C13A C12 C15A 110.6(10) . . ?
C15B C12 C14B 109.6(12) . . ?
N1 C12 C14B 108.2(7) . . ?
C15B C12 C13B 108.7(12) . . ?
N1 C12 C13B 105.7(7) . . ?
C14B C12 C13B 106.4(13) . . ?
N4 C16 C17 121.7(4) . . ?
N4 C16 N3 113.7(4) . . ?
C17 C16 N3 124.6(4) . . ?
C18 C17 C16 118.5(4) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 122.0(4) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C18 C19 C20 115.0(4) . . ?
C18 C19 C21 123.4(4) . . ?
C20 C19 C21 121.5(4) . . ?
N4 C20 C19 124.8(4) . . ?
N4 C20 H20 117.6 . . ?
C19 C20 H20 117.6 . . ?
C26 C21 C22 118.5(5) . . ?
C26 C21 C19 120.0(5) . . ?
C22 C21 C19 121.4(5) . . ?
C23 C22 C21 120.4(6) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C24 C23 C22 120.6(9) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 120.1(10) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 120.1(9) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 120.3(7) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C28 C27 N3 107.4(5) . . ?
C28 C27 C30 112.0(6) . . ?
N3 C27 C30 109.3(5) . . ?
C28 C27 C29 109.5(6) . . ?
N3 C27 C29 108.5(5) . . ?
C30 C27 C29 110.0(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 S1 179.4(6) . . ?
N6 C32 S2 179.3(6) . . ?
C12 C13A H13A 109.5 . . ?
C12 C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C12 C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C12 C14A H14A 109.5 . . ?
C12 C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C12 C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C12 C15A H15A 109.5 . . ?
C12 C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C12 C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C12 C13B H13D 109.5 . . ?
C12 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C12 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C12 C14B H14D 109.5 . . ?
C12 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C12 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C12 C15B H15D 109.5 . . ?
C12 C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C12 C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 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 O1 N1 C1 -26.8(4) . . . . ?
Ni1 O1 N1 C12 146.2(3) . . . . ?
Ni1 O2 N3 C16 27.3(4) . . . . ?
Ni1 O2 N3 C27 -149.7(3) . . . . ?
C5 N2 C1 C2 -2.6(6) . . . . ?
Ni1 N2 C1 C2 178.8(3) . . . . ?
C5 N2 C1 N1 -178.9(3) . . . . ?
Ni1 N2 C1 N1 2.5(4) . . . . ?
O1 N1 C1 N2 16.0(5) . . . . ?
C12 N1 C1 N2 -155.8(4) . . . . ?
O1 N1 C1 C2 -160.2(4) . . . . ?
C12 N1 C1 C2 28.0(7) . . . . ?
N2 C1 C2 C3 2.3(6) . . . . ?
N1 C1 C2 C3 178.1(4) . . . . ?
C1 C2 C3 C4 -0.9(6) . . . . ?
C2 C3 C4 C5 0.0(6) . . . . ?
C2 C3 C4 C6 179.9(4) . . . . ?
C1 N2 C5 C4 1.6(6) . . . . ?
Ni1 N2 C5 C4 -180.0(3) . . . . ?
C3 C4 C5 N2 -0.3(6) . . . . ?
C6 C4 C5 N2 179.8(4) . . . . ?
C3 C4 C6 C7 -27.2(6) . . . . ?
C5 C4 C6 C7 152.7(4) . . . . ?
C3 C4 C6 C11 153.0(4) . . . . ?
C5 C4 C6 C11 -27.2(6) . . . . ?
C11 C6 C7 C8 1.2(7) . . . . ?
C4 C6 C7 C8 -178.7(4) . . . . ?
C6 C7 C8 C9 -0.6(8) . . . . ?
C7 C8 C9 C10 -0.1(9) . . . . ?
C8 C9 C10 C11 0.1(10) . . . . ?
C7 C6 C11 C10 -1.1(7) . . . . ?
C4 C6 C11 C10 178.7(5) . . . . ?
C9 C10 C11 C6 0.5(9) . . . . ?
O1 N1 C12 C14A -9.5(11) . . . . ?
C1 N1 C12 C14A 162.3(10) . . . . ?
O1 N1 C12 C15B 171.9(14) . . . . ?
C1 N1 C12 C15B -16.3(15) . . . . ?
O1 N1 C12 C13A -131.7(10) . . . . ?
C1 N1 C12 C13A 40.2(11) . . . . ?
O1 N1 C12 C15A 109.1(10) . . . . ?
C1 N1 C12 C15A -79.1(10) . . . . ?
O1 N1 C12 C14B 47.1(13) . . . . ?
C1 N1 C12 C14B -141.1(13) . . . . ?
O1 N1 C12 C13B -66.6(13) . . . . ?
C1 N1 C12 C13B 105.2(13) . . . . ?
C20 N4 C16 C17 -0.7(6) . . . . ?
Ni1 N4 C16 C17 178.3(3) . . . . ?
C20 N4 C16 N3 177.4(3) . . . . ?
Ni1 N4 C16 N3 -3.5(4) . . . . ?
O2 N3 C16 N4 -15.9(5) . . . . ?
C27 N3 C16 N4 160.6(4) . . . . ?
O2 N3 C16 C17 162.2(4) . . . . ?
C27 N3 C16 C17 -21.3(7) . . . . ?
N4 C16 C17 C18 -0.5(7) . . . . ?
N3 C16 C17 C18 -178.5(4) . . . . ?
C16 C17 C18 C19 1.4(7) . . . . ?
C17 C18 C19 C20 -1.0(6) . . . . ?
C17 C18 C19 C21 178.6(4) . . . . ?
C16 N4 C20 C19 1.2(6) . . . . ?
Ni1 N4 C20 C19 -177.8(3) . . . . ?
C18 C19 C20 N4 -0.3(6) . . . . ?
C21 C19 C20 N4 -180.0(4) . . . . ?
C18 C19 C21 C26 148.1(5) . . . . ?
C20 C19 C21 C26 -32.3(6) . . . . ?
C18 C19 C21 C22 -32.3(7) . . . . ?
C20 C19 C21 C22 147.3(4) . . . . ?
C26 C21 C22 C23 0.3(7) . . . . ?
C19 C21 C22 C23 -179.4(4) . . . . ?
C21 C22 C23 C24 -1.3(10) . . . . ?
C22 C23 C24 C25 0.9(13) . . . . ?
C23 C24 C25 C26 0.4(14) . . . . ?
C22 C21 C26 C25 1.1(8) . . . . ?
C19 C21 C26 C25 -179.3(5) . . . . ?
C24 C25 C26 C21 -1.5(12) . . . . ?
O2 N3 C27 C28 12.2(7) . . . . ?
C16 N3 C27 C28 -164.4(5) . . . . ?
O2 N3 C27 C30 -109.6(5) . . . . ?
C16 N3 C27 C30 73.9(6) . . . . ?
O2 N3 C27 C29 130.5(5) . . . . ?
C16 N3 C27 C29 -46.0(6) . . . . ?

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



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        '[Ni(phpyNO)2(NCS)2]'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_preparation       'Magnetic properties'
