# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_50K_2
_database_code_depnum_ccdc_archive 'CCDC 1063807'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C46 N6 Ni2 O2 S10'
_chemical_formula_moiety         'C46 N6 Ni2 O2 S10'
_chemical_formula_weight         1106.55
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.877(3)
_cell_length_b                   19.073(5)
_cell_length_c                   13.930(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.607(7)
_cell_angle_gamma                90.0000
_cell_volume                     2880.4(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4422
_cell_measurement_theta_min      1.05
_cell_measurement_theta_max      27.26
_cell_measurement_temperature    50
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_T_max  1.000

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

_diffrn_ambient_temperature      50
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.69960
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.706
_diffrn_reflns_number            18425
_diffrn_reflns_av_R_equivalents  0.1462
_diffrn_reflns_theta_max         27.020
_diffrn_reflns_theta_min         1.786
_diffrn_reflns_theta_full        27.020
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             6536
_reflns_number_gt                5027
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0866
_refine_ls_wR_factor_ref         0.2407
_refine_ls_wR_factor_gt          0.2212
_refine_ls_number_restraints     0
_refine_ls_number_reflns         6536
_refine_ls_number_parameters     298
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0993P)²+18.6465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.92
_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 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.07814(6) 0.11886(3) 0.63017(5) 0.0144(2) Uani 1 4 d . . .
S1 S 1.25403(12) 0.15581(7) 0.68989(10) 0.0169(3) Uani 1 4 d . . .
S2 S 0.98310(12) 0.20661(7) 0.68538(10) 0.0168(3) Uani 1 4 d . . .
S3 S 1.16828(12) 0.02651(7) 0.58040(10) 0.0163(3) Uani 1 4 d . . .
S4 S 0.90677(12) 0.08764(7) 0.55483(10) 0.0165(3) Uani 1 4 d . . .
S5 S 1.15263(15) -0.02600(8) 0.89273(11) 0.0269(4) Uani 1 4 d . . .
O30 O 1.1797(4) -0.0471(2) 0.9955(3) 0.0309(10) Uani 1 4 d . . .
N1 N 1.0685(5) 0.3188(2) 0.7819(3) 0.0200(10) Uani 1 4 d . . .
N25 N 1.3145(5) 0.2732(2) 0.7833(4) 0.0206(10) Uani 1 4 d . . .
N29 N 0.6873(4) 0.2165(2) 0.8971(3) 0.0132(8) Uani 1 4 d . . .
C2 C 0.7833(5) 0.2162(3) 0.9820(4) 0.0157(10) Uani 1 4 d . . .
C3 C 1.2211(5) 0.2358(3) 0.7434(4) 0.0179(11) Uani 1 4 d . . .
C4 C 0.6949(5) 0.2810(3) 0.8351(4) 0.0170(11) Uani 1 4 d . . .
C5 C 0.5610(5) 0.2144(3) 0.9366(4) 0.0179(11) Uani 1 4 d . . .
C6 C 1.1633(6) 0.3565(3) 0.8219(4) 0.0229(12) Uani 1 4 d . . .
C8 C 0.9139(5) 0.2320(3) 0.9570(4) 0.0173(10) Uani 1 4 d . . .
C9 C 0.5410(5) 0.1505(3) 0.9980(4) 0.0195(11) Uani 1 4 d . . .
C10 C 0.6139(6) 0.4290(3) 0.7521(4) 0.0233(12) Uani 1 4 d . . .
C11 C 0.7065(5) 0.1516(3) 0.8344(4) 0.0153(10) Uani 1 4 d . . .
C12 C 0.9992(5) 0.2220(3) 1.0486(4) 0.0208(11) Uani 1 4 d . . .
C13 C 0.6334(5) 0.0693(3) 0.7073(4) 0.0203(11) Uani 1 4 d . . .
C14 C 1.0615(5) -0.0140(3) 0.5061(4) 0.0166(10) Uani 1 4 d . . .
C15 C 0.7187(5) 0.4118(3) 0.8277(4) 0.0166(10) Uani 1 4 d . . .
C16 C 1.0994(5) 0.2580(3) 0.7414(4) 0.0181(11) Uani 1 4 d . . .
C17 C 1.2836(6) 0.3346(3) 0.8219(4) 0.0216(11) Uani 1 4 d . . .
C18 C 0.5358(6) 0.0499(3) 0.6270(5) 0.0301(14) Uani 1 4 d . . .
C19 C 0.4039(6) 0.1485(3) 1.0171(5) 0.0252(13) Uani 1 4 d . . .
C20 C 0.6018(5) 0.1360(3) 0.7601(4) 0.0193(11) Uani 1 4 d . . .
C21 C 1.2972(6) -0.0038(3) 0.8484(4) 0.0274(13) Uani 1 4 d . . .
C22 C 1.1304(6) 0.2472(4) 1.0353(5) 0.0270(13) Uani 1 4 d . . .
C23 C 0.3773(6) 0.0910(4) 1.0885(5) 0.0328(15) Uani 1 4 d . . .
C24 C 1.0876(6) 0.0600(3) 0.8959(5) 0.0273(13) Uani 1 4 d . . .
C28 C 0.6895(5) 0.3494(3) 0.8922(4) 0.0170(11) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S1 2.1431(15) yes . .
Ni1 S2 2.1422(15) yes . .
Ni1 S3 2.1572(15) yes . .
Ni1 S4 2.1485(15) yes . .
S1 C3 1.747(6) yes . .
S2 C16 1.735(6) yes . .
S3 C14 1.681(5) yes . .
S4 C14 1.691(6) yes . 3_756
S5 O30 1.494(5) yes . .
S5 C21 1.786(7) yes . .
S5 C24 1.789(6) yes . .
N1 C6 1.341(8) yes . .
N1 C16 1.344(7) yes . .
N25 C3 1.326(7) yes . .
N25 C17 1.344(7) yes . .
N29 C2 1.513(7) yes . .
N29 C4 1.509(7) yes . .
N29 C5 1.520(7) yes . .
N29 C11 1.539(7) yes . .
C2 C8 1.520(8) yes . .
C3 C16 1.388(8) yes . .
C4 C28 1.531(7) yes . .
C5 C9 1.513(8) yes . .
C6 C17 1.374(9) yes . .
C8 C12 1.528(8) yes . .
C9 C19 1.536(8) yes . .
C10 C15 1.523(8) yes . .
C11 C20 1.506(7) yes . .
C12 C22 1.531(9) yes . .
C13 C18 1.525(8) yes . .
C13 C20 1.523(8) yes . .
C14 C14 1.438(8) yes . 3_756
C15 C28 1.540(7) yes . .
C19 C23 1.524(10) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Ni1 S2 92.59(6) yes . . .
S1 Ni1 S3 88.78(6) yes . . .
S1 Ni1 S4 173.27(6) yes . . .
S2 Ni1 S3 176.55(6) yes . . .
S2 Ni1 S4 88.12(6) yes . . .
S3 Ni1 S4 90.89(6) yes . . .
Ni1 S1 C3 104.2(2) yes . . .
Ni1 S2 C16 104.3(2) yes . . .
Ni1 S3 C14 105.3(2) yes . . .
Ni1 S4 C14 105.74(19) yes . . 3_756
O30 S5 C21 106.5(3) yes . . .
O30 S5 C24 105.7(3) yes . . .
C21 S5 C24 98.7(3) yes . . .
C6 N1 C16 115.4(5) yes . . .
C3 N25 C17 115.4(5) yes . . .
C2 N29 C4 112.6(4) yes . . .
C2 N29 C5 107.7(4) yes . . .
C2 N29 C11 108.9(4) yes . . .
C4 N29 C5 108.8(4) yes . . .
C4 N29 C11 108.3(4) yes . . .
C5 N29 C11 110.6(4) yes . . .
N29 C2 C8 114.8(4) yes . . .
S1 C3 N25 118.1(4) yes . . .
S1 C3 C16 119.0(4) yes . . .
N25 C3 C16 122.8(5) yes . . .
N29 C4 C28 113.0(4) yes . . .
N29 C5 C9 113.6(4) yes . . .
N1 C6 C17 122.5(5) yes . . .
C2 C8 C12 107.4(5) yes . . .
C5 C9 C19 107.7(5) yes . . .
N29 C11 C20 114.8(4) yes . . .
C8 C12 C22 111.7(5) yes . . .
C18 C13 C20 112.8(5) yes . . .
S3 C14 S4 122.2(3) yes . . 3_756
S3 C14 C14 119.5(4) yes . . 3_756
S4 C14 C14 118.4(4) yes 3_756 . 3_756
C10 C15 C28 113.1(5) yes . . .
S2 C16 N1 118.6(4) yes . . .
S2 C16 C3 119.8(4) yes . . .
N1 C16 C3 121.6(5) yes . . .
N25 C17 C6 122.3(5) yes . . .
C9 C19 C23 111.7(5) yes . . .
C11 C20 C13 108.1(4) yes . . .
C4 C28 C15 109.7(4) yes . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S1 Ni1 S2 C16 2.14(7) no . . . .
S2 Ni1 S1 C3 -2.36(7) no . . . .
S1 Ni1 S3 C14 -169.16(7) no . . . .
S3 Ni1 S1 C3 -179.20(7) no . . . .
S2 Ni1 S4 C14 179.38(7) no . . . 3_756
S4 Ni1 S2 C16 -171.17(7) no . . . .
S3 Ni1 S4 C14 -3.92(7) no . . . 3_756
S4 Ni1 S3 C14 4.12(7) no . . . .
Ni1 S1 C3 N25 -177.0(3) no . . . .
Ni1 S1 C3 C16 2.2(4) no . . . .
Ni1 S2 C16 N1 178.4(3) no . . . .
Ni1 S2 C16 C3 -1.4(4) no . . . .
Ni1 S3 C14 S4 177.0(3) no . . . 3_756
Ni1 S3 C14 C14 -3.6(4) no . . . 3_756
Ni1 S4 C14 S3 -176.6(3) no . . 3_756 3_756
Ni1 S4 C14 C14 2.9(4) no . . 3_756 .
C6 N1 C16 S2 -178.5(4) no . . . .
C6 N1 C16 C3 1.3(7) no . . . .
C16 N1 C6 C17 -0.2(8) no . . . .
C3 N25 C17 C6 1.3(8) no . . . .
C17 N25 C3 S1 179.0(4) no . . . .
C17 N25 C3 C16 -0.2(8) no . . . .
C2 N29 C4 C28 -53.9(5) no . . . .
C4 N29 C2 C8 -49.1(5) no . . . .
C2 N29 C5 C9 -59.4(5) no . . . .
C5 N29 C2 C8 -169.0(4) no . . . .
C2 N29 C11 C20 167.0(4) no . . . .
C11 N29 C2 C8 71.1(5) no . . . .
C4 N29 C5 C9 178.3(4) no . . . .
C5 N29 C4 C28 65.3(5) no . . . .
C4 N29 C11 C20 -70.3(5) no . . . .
C11 N29 C4 C28 -174.5(4) no . . . .
C5 N29 C11 C20 48.8(5) no . . . .
C11 N29 C5 C9 59.5(5) no . . . .
N29 C2 C8 C12 -174.2(4) no . . . .
S1 C3 C16 S2 -0.6(7) no . . . .
S1 C3 C16 N1 179.7(3) no . . . .
N25 C3 C16 S2 178.6(4) no . . . .
N25 C3 C16 N1 -1.2(8) no . . . .
N29 C4 C28 C15 170.9(4) no . . . .
N29 C5 C9 C19 -169.9(4) no . . . .
N1 C6 C17 N25 -1.2(9) no . . . .
C2 C8 C12 C22 -171.4(4) no . . . .
C5 C9 C19 C23 -173.1(4) no . . . .
N29 C11 C20 C13 -178.1(4) no . . . .
C18 C13 C20 C11 -177.7(4) no . . . .
S3 C14 C14 S3 180.0(3) no . . 3_756 3_756
S3 C14 C14 S4 0.5(6) no . . 3_756 .
S4 C14 C14 S3 -0.5(6) no 3_756 . 3_756 3_756
S4 C14 C14 S4 -180.0(3) no 3_756 . 3_756 .
C10 C15 C28 C4 73.2(5) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N1 N25 2.812(7) no . .
C2 C9 2.942(8) no . .
C2 C28 2.975(7) no . .
C3 C6 2.647(8) no . .
C4 C8 2.963(8) no . .
C4 C10 3.150(8) no . .
C4 C20 3.097(7) no . .
C5 C20 2.940(8) no . .
C5 C28 3.018(8) no . .
C8 C11 3.121(7) no . .
C8 C28 3.380(8) no . .
C9 C11 3.014(8) no . .
C9 C20 3.441(8) no . .
C16 C17 2.656(8) no . .
S3 C28 3.553(5) no . 4_554
S5 C10 3.503(6) no . 2_646
O30 C2 3.264(7) no . 3_757
O30 C11 3.263(7) no . 3_757
O30 C23 3.575(8) no . 1_655
O30 C24 3.392(8) no . 3_757
N1 C8 3.490(7) no . .
N25 C5 3.476(7) no . 1_655
C2 O30 3.264(7) no . 3_757
C5 N25 3.476(7) no . 1_455
C8 N1 3.490(7) no . .
C10 S5 3.503(6) no . 2_656
C11 O30 3.263(7) no . 3_757
C13 C15 3.461(8) no . 2_646
C15 C13 3.461(8) no . 2_656
C19 C22 3.547(9) no . 1_455
C22 C19 3.547(9) no . 1_655
C23 O30 3.575(8) no . 1_455
C24 O30 3.392(8) no . 3_757
C28 S3 3.553(5) no . 4_455

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

#==============================================================================
# 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
#==============================================================================
_chemical_name_systematic        1_50K
####################################################################### 
# 
# 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_100k_2
_database_code_depnum_ccdc_archive 'CCDC 1063808'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C46 N6 Ni2 O2 S10'
_chemical_formula_moiety         'C46 N6 Ni2 O2 S10'
_chemical_formula_weight         1106.55
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.895(3)
_cell_length_b                   19.189(5)
_cell_length_c                   13.957(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.674(7)
_cell_angle_gamma                90.0000
_cell_volume                     2908.3(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4497
_cell_measurement_theta_min      1.04
_cell_measurement_theta_max      27.23
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      100
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.69960
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.706
_diffrn_reflns_number            18421
_diffrn_reflns_av_R_equivalents  0.1471
_diffrn_reflns_theta_max         27.020
_diffrn_reflns_theta_min         1.780
_diffrn_reflns_theta_full        27.020
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             6562
_reflns_number_gt                4723
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0878
_refine_ls_wR_factor_ref         0.2485
_refine_ls_wR_factor_gt          0.2259
_refine_ls_number_restraints     0
_refine_ls_number_reflns         6562
_refine_ls_number_parameters     298
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1121P)²+12.5696P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.84
_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 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.07815(6) 0.11861(4) 0.12954(5) 0.0214(2) Uani 1 4 d . . .
S1 S 0.25370(13) 0.15531(7) 0.18953(11) 0.0253(3) Uani 1 4 d . . .
S2 S -0.01663(13) 0.20603(7) 0.18411(10) 0.0248(3) Uani 1 4 d . . .
S3 S -0.09323(13) 0.08719(7) 0.05449(10) 0.0246(3) Uani 1 4 d . . .
S4 S 0.16847(13) 0.02675(7) 0.07993(10) 0.0240(3) Uani 1 4 d . . .
S5 S 0.34819(18) 0.47393(9) 0.10798(14) 0.0442(5) Uani 1 4 d . . .
O27 O 0.3209(5) 0.4532(3) 0.0050(4) 0.0502(14) Uani 1 4 d . . .
N1 N 0.0678(5) 0.3176(3) 0.2805(4) 0.0285(11) Uani 1 4 d . . .
N8 N 0.1880(4) 0.2842(2) -0.1029(3) 0.0194(9) Uani 1 4 d . . .
N30 N 0.3138(5) 0.2720(3) 0.2836(4) 0.0305(11) Uani 1 4 d . . .
C2 C 0.2213(6) 0.2348(3) 0.2429(4) 0.0265(12) Uani 1 4 d . . .
C3 C 0.0616(5) 0.2865(3) -0.0636(4) 0.0248(12) Uani 1 4 d . . .
C4 C 0.1957(6) 0.2201(3) -0.1658(4) 0.0241(11) Uani 1 4 d . . .
C5 C -0.0613(5) 0.0135(3) -0.0057(4) 0.0244(11) Uani 1 4 d . . .
C6 C 0.1634(7) 0.3550(3) 0.3211(5) 0.0358(15) Uani 1 4 d . . .
C9 C 0.2080(5) 0.3484(3) -0.1654(4) 0.0211(11) Uani 1 4 d . . .
C10 C 0.4149(5) 0.2684(3) -0.0432(4) 0.0241(11) Uani 1 4 d . . .
C11 C 0.0425(5) 0.3499(3) -0.0015(5) 0.0280(13) Uani 1 4 d . . .
C12 C 0.0990(6) 0.2570(3) 0.2404(4) 0.0250(12) Uani 1 4 d . . .
C13 C 0.4995(6) 0.2774(3) 0.0494(5) 0.0304(13) Uani 1 4 d . . .
C14 C 0.2192(5) 0.0896(3) -0.1727(4) 0.0251(11) Uani 1 4 d . . .
C15 C 0.1142(6) 0.0732(3) -0.2484(5) 0.0339(14) Uani 1 4 d . . .
C16 C 0.1347(6) 0.4309(3) -0.2922(4) 0.0293(13) Uani 1 4 d . . .
C17 C 0.2829(6) 0.3337(3) 0.3218(5) 0.0339(14) Uani 1 4 d . . .
C18 C -0.0947(6) 0.3522(4) 0.0166(5) 0.0358(15) Uani 1 4 d . . .
C19 C 0.1047(6) 0.3638(3) -0.2404(4) 0.0299(13) Uani 1 4 d . . .
C20 C 0.0382(7) 0.4490(4) -0.3742(5) 0.0443(17) Uani 1 4 d . . .
C21 C 0.6309(6) 0.2538(4) 0.0351(5) 0.0390(16) Uani 1 4 d . . .
C22 C 0.2036(7) 0.4960(4) 0.1523(5) 0.0427(17) Uani 1 4 d . . .
C23 C -0.1206(7) 0.4091(5) 0.0880(5) 0.0485(19) Uani 1 4 d . . .
C24 C 0.4123(7) 0.5596(4) 0.1045(5) 0.0419(16) Uani 1 4 d . . .
C28 C 0.1903(6) 0.1519(3) -0.1076(4) 0.0242(11) Uani 1 4 d . . .
C29 C 0.2844(5) 0.2845(3) -0.0181(4) 0.0216(11) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S1 2.1434(16) yes . .
Ni1 S2 2.1421(16) yes . .
Ni1 S3 2.1514(16) yes . .
Ni1 S4 2.1601(16) yes . .
S1 C2 1.745(6) yes . .
S2 C12 1.732(6) yes . .
S3 C5 1.695(6) yes . .
S4 C5 1.684(6) yes . 3_555
S5 O27 1.497(6) yes . .
S5 C22 1.790(8) yes . .
S5 C24 1.788(7) yes . .
N1 C6 1.351(8) yes . .
N1 C12 1.347(7) yes . .
N8 C3 1.524(7) yes . .
N8 C4 1.516(7) yes . .
N8 C9 1.536(7) yes . .
N8 C29 1.517(7) yes . .
N30 C2 1.325(8) yes . .
N30 C17 1.353(8) yes . .
C2 C12 1.397(9) yes . .
C3 C11 1.518(8) yes . .
C4 C28 1.543(7) yes . .
C5 C5 1.430(8) yes . 3_555
C6 C17 1.364(10) yes . .
C9 C19 1.502(8) yes . .
C10 C13 1.534(8) yes . .
C10 C29 1.524(8) yes . .
C11 C18 1.537(9) yes . .
C13 C21 1.531(9) yes . .
C14 C15 1.525(8) yes . .
C14 C28 1.550(8) yes . .
C16 C19 1.524(9) yes . .
C16 C20 1.529(9) yes . .
C18 C23 1.520(11) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Ni1 S2 92.55(6) yes . . .
S1 Ni1 S3 173.57(7) yes . . .
S1 Ni1 S4 88.74(6) yes . . .
S2 Ni1 S3 88.17(6) yes . . .
S2 Ni1 S4 176.78(7) yes . . .
S3 Ni1 S4 90.87(6) yes . . .
Ni1 S1 C2 104.4(2) yes . . .
Ni1 S2 C12 104.5(2) yes . . .
Ni1 S3 C5 105.7(2) yes . . .
Ni1 S4 C5 105.1(2) yes . . 3_555
O27 S5 C22 106.4(3) yes . . .
O27 S5 C24 105.4(3) yes . . .
C22 S5 C24 98.6(3) yes . . .
C6 N1 C12 114.9(5) yes . . .
C3 N8 C4 109.1(4) yes . . .
C3 N8 C9 110.8(4) yes . . .
C3 N8 C29 107.9(4) yes . . .
C4 N8 C9 107.8(4) yes . . .
C4 N8 C29 112.8(4) yes . . .
C9 N8 C29 108.6(4) yes . . .
C2 N30 C17 115.8(5) yes . . .
S1 C2 N30 118.7(5) yes . . .
S1 C2 C12 118.8(4) yes . . .
N30 C2 C12 122.5(5) yes . . .
N8 C3 C11 113.5(4) yes . . .
N8 C4 C28 112.1(4) yes . . .
S3 C5 S4 121.9(3) yes . . 3_555
S3 C5 C5 118.4(4) yes . . 3_555
S4 C5 C5 119.8(4) yes 3_555 . 3_555
N1 C6 C17 123.2(6) yes . . .
N8 C9 C19 114.9(4) yes . . .
C13 C10 C29 106.9(5) yes . . .
C3 C11 C18 107.3(5) yes . . .
S2 C12 N1 118.5(5) yes . . .
S2 C12 C2 119.7(4) yes . . .
N1 C12 C2 121.8(5) yes . . .
C10 C13 C21 111.1(5) yes . . .
C15 C14 C28 112.8(5) yes . . .
C19 C16 C20 112.7(5) yes . . .
N30 C17 C6 121.8(6) yes . . .
C11 C18 C23 111.3(5) yes . . .
C9 C19 C16 108.6(5) yes . . .
C4 C28 C14 109.1(5) yes . . .
N8 C29 C10 114.8(4) yes . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S1 Ni1 S2 C12 2.02(8) no . . . .
S2 Ni1 S1 C2 -2.24(8) no . . . .
S1 Ni1 S4 C5 -169.34(7) no . . . 3_555
S4 Ni1 S1 C2 -179.29(7) no . . . .
S2 Ni1 S3 C5 179.50(7) no . . . .
S3 Ni1 S2 C12 -171.58(7) no . . . .
S3 Ni1 S4 C5 4.24(8) no . . . 3_555
S4 Ni1 S3 C5 -3.58(8) no . . . .
Ni1 S1 C2 N30 -177.5(3) no . . . .
Ni1 S1 C2 C12 2.1(4) no . . . .
Ni1 S2 C12 N1 178.5(3) no . . . .
Ni1 S2 C12 C2 -1.3(4) no . . . .
Ni1 S3 C5 S4 -176.3(3) no . . . 3_555
Ni1 S3 C5 C5 2.0(4) no . . . 3_555
Ni1 S4 C5 S3 177.4(3) no . . 3_555 3_555
Ni1 S4 C5 C5 -4.3(4) no . . 3_555 .
C6 N1 C12 S2 -178.6(4) no . . . .
C6 N1 C12 C2 1.1(8) no . . . .
C12 N1 C6 C17 0.2(8) no . . . .
C3 N8 C4 C28 -65.6(5) no . . . .
C4 N8 C3 C11 -178.4(4) no . . . .
C3 N8 C9 C19 -49.5(5) no . . . .
C9 N8 C3 C11 -60.0(5) no . . . .
C3 N8 C29 C10 168.8(4) no . . . .
C29 N8 C3 C11 58.7(5) no . . . .
C4 N8 C9 C19 69.8(5) no . . . .
C9 N8 C4 C28 174.1(4) no . . . .
C4 N8 C29 C10 48.3(5) no . . . .
C29 N8 C4 C28 54.3(5) no . . . .
C9 N8 C29 C10 -71.1(5) no . . . .
C29 N8 C9 C19 -167.8(4) no . . . .
C2 N30 C17 C6 2.2(8) no . . . .
C17 N30 C2 S1 178.6(4) no . . . .
C17 N30 C2 C12 -1.0(8) no . . . .
S1 C2 C12 S2 -0.5(7) no . . . .
S1 C2 C12 N1 179.7(4) no . . . .
N30 C2 C12 S2 179.0(5) no . . . .
N30 C2 C12 N1 -0.7(9) no . . . .
N8 C3 C11 C18 169.6(4) no . . . .
N8 C4 C28 C14 -171.1(4) no . . . .
S3 C5 C5 S3 180.0(3) no . . 3_555 3_555
S3 C5 C5 S4 1.6(7) no . . 3_555 .
S4 C5 C5 S3 -1.6(7) no 3_555 . 3_555 3_555
S4 C5 C5 S4 180.0(3) no 3_555 . 3_555 .
N1 C6 C17 N30 -2.0(10) no . . . .
N8 C9 C19 C16 176.8(4) no . . . .
C13 C10 C29 N8 175.3(4) no . . . .
C29 C10 C13 C21 173.1(4) no . . . .
C3 C11 C18 C23 173.3(4) no . . . .
C15 C14 C28 C4 -72.8(6) no . . . .
C20 C16 C19 C9 176.8(5) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N1 N30 2.818(7) no . .
C2 C6 2.650(9) no . .
C3 C19 2.949(9) no . .
C3 C28 3.025(8) no . .
C4 C10 2.971(8) no . .
C4 C15 3.146(8) no . .
C4 C19 3.082(8) no . .
C9 C10 3.118(8) no . .
C9 C11 3.025(9) no . .
C10 C28 3.382(8) no . .
C11 C19 3.466(9) no . .
C11 C29 2.946(8) no . .
C12 C17 2.665(9) no . .
C28 C29 2.980(8) no . .
S4 C28 3.575(6) no . .
S5 C15 3.506(7) no . 4_555
O27 C9 3.277(7) no . .
O27 C24 3.400(9) no . 3_665
O27 C29 3.274(8) no . .
N1 C10 3.495(8) no . 4_455
N30 C3 3.487(7) no . 4_555
C3 N30 3.487(7) no . 4_454
C9 O27 3.277(7) no . .
C10 N1 3.495(8) no . 4_554
C14 C16 3.490(8) no . 2_544
C15 S5 3.506(7) no . 4_454
C16 C14 3.490(8) no . 2_554
C18 C21 3.563(10) no . 1_455
C21 C18 3.563(10) no . 1_655
C24 O27 3.400(9) no . 3_665
C28 S4 3.575(6) no . .
C29 O27 3.274(8) 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
#==============================================================================
_chemical_name_systematic        1_100K
####################################################################### 
# 
# 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_150k_2
_database_code_depnum_ccdc_archive 'CCDC 1063809'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C46 N6 Ni2 O2 S10'
_chemical_formula_moiety         'C46 N6 Ni2 O2 S10'
_chemical_formula_weight         1106.55
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.885(4)
_cell_length_b                   19.278(6)
_cell_length_c                   13.961(5)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.810(7)
_cell_angle_gamma                90.0000
_cell_volume                     2919.1(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3769
_cell_measurement_theta_min      1.44
_cell_measurement_theta_max      27.28
_cell_measurement_temperature    150
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      150
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.69960
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.706
_diffrn_reflns_number            18395
_diffrn_reflns_av_R_equivalents  0.1558
_diffrn_reflns_theta_max         27.020
_diffrn_reflns_theta_min         1.777
_diffrn_reflns_theta_full        27.020
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             6572
_reflns_number_gt                3976
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0911
_refine_ls_wR_factor_ref         0.2719
_refine_ls_wR_factor_gt          0.2372
_refine_ls_number_restraints     0
_refine_ls_number_reflns         6572
_refine_ls_number_parameters     298
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1423P)²+3.6912P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.89
_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 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.92178(7) 0.11825(4) 0.37128(6) 0.0277(3) Uani 1 4 d . . .
S1 S 1.01643(15) 0.20532(8) 0.31703(12) 0.0325(4) Uani 1 4 d . . .
S2 S 0.74658(15) 0.15492(8) 0.31087(13) 0.0329(4) Uani 1 4 d . . .
S3 S 0.83134(14) 0.02707(8) 0.42082(12) 0.0315(4) Uani 1 4 d . . .
S4 S 1.09311(15) 0.08666(8) 0.44598(12) 0.0319(4) Uani 1 4 d . . .
S16 S 1.1508(2) 0.02616(10) 0.89110(19) 0.0656(7) Uani 1 4 d . . .
O23 O 1.1778(6) 0.0462(3) 0.9945(5) 0.0720(19) Uani 1 4 d . . .
N1 N 0.8112(5) 0.2850(2) 0.6027(4) 0.0253(11) Uani 1 4 d . . .
N3 N 0.9322(6) 0.3158(3) 0.2208(4) 0.0388(14) Uani 1 4 d . . .
N28 N 0.6863(6) 0.2708(3) 0.2166(4) 0.0394(14) Uani 1 4 d . . .
C2 C 0.9393(6) -0.0135(3) 0.4944(5) 0.0293(13) Uani 1 4 d . . .
C3 C 0.8035(6) 0.2217(3) 0.6652(5) 0.0314(14) Uani 1 4 d . . .
C4 C 0.8089(6) 0.1531(3) 0.6072(5) 0.0320(14) Uani 1 4 d . . .
C5 C 0.7790(6) 0.2340(3) 0.2578(5) 0.0329(14) Uani 1 4 d . . .
C6 C 0.7152(6) 0.2851(3) 0.5175(4) 0.0275(13) Uani 1 4 d . . .
C7 C 0.7903(6) 0.3492(3) 0.6654(5) 0.0272(13) Uani 1 4 d . . .
C8 C 0.9379(6) 0.2871(3) 0.5639(5) 0.0312(14) Uani 1 4 d . . .
C9 C 0.5850(6) 0.2695(3) 0.5433(5) 0.0333(14) Uani 1 4 d . . .
C10 C 0.9015(6) 0.2560(3) 0.2608(5) 0.0327(15) Uani 1 4 d . . .
C11 C 0.7791(6) 0.0917(3) 0.6726(5) 0.0341(15) Uani 1 4 d . . .
C12 C 0.9555(6) 0.3506(3) 0.5016(6) 0.0394(17) Uani 1 4 d . . .
C13 C 0.5002(6) 0.2771(4) 0.4499(5) 0.0403(16) Uani 1 4 d . . .
C14 C 0.8848(8) 0.0763(4) 0.7483(6) 0.050(2) Uani 1 4 d . . .
C15 C 0.8363(8) 0.3534(4) 0.1783(5) 0.0447(18) Uani 1 4 d . . .
C17 C 0.8927(7) 0.3635(3) 0.7413(5) 0.0398(17) Uani 1 4 d . . .
C18 C 0.7172(8) 0.3321(4) 0.1785(5) 0.0443(18) Uani 1 4 d . . .
C19 C 1.0940(7) 0.3530(4) 0.4839(6) 0.048(2) Uani 1 4 d . . .
C20 C 0.8640(6) 0.4302(4) 0.7922(5) 0.0410(17) Uani 1 4 d . . .
C21 C 0.3679(7) 0.2554(5) 0.4650(6) 0.051(2) Uani 1 4 d . . .
C22 C 0.9590(8) 0.4485(4) 0.8756(7) 0.062(2) Uani 1 4 d . . .
C24 C 1.0872(8) -0.0592(4) 0.8941(7) 0.058(2) Uani 1 4 d . . .
C25 C 1.1197(8) 0.4097(5) 0.4131(6) 0.063(3) Uani 1 4 d . . .
C26 C 1.2953(9) 0.0041(4) 0.8470(6) 0.058(2) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S1 2.1409(19) yes . .
Ni1 S2 2.1397(19) yes . .
Ni1 S3 2.1567(18) yes . .
Ni1 S4 2.1472(18) yes . .
S1 C10 1.723(7) yes . .
S2 C5 1.743(6) yes . .
S3 C2 1.686(6) yes . .
S4 C2 1.691(6) yes . 3_756
S16 O23 1.499(7) yes . .
S16 C24 1.788(8) yes . .
S16 C26 1.788(10) yes . .
N1 C3 1.506(7) yes . .
N1 C6 1.516(8) yes . .
N1 C7 1.546(8) yes . .
N1 C8 1.523(8) yes . .
N3 C10 1.337(8) yes . .
N3 C15 1.365(10) yes . .
N28 C5 1.325(9) yes . .
N28 C18 1.350(9) yes . .
C2 C2 1.417(9) yes . 3_756
C3 C4 1.554(8) yes . .
C4 C11 1.546(9) yes . .
C5 C10 1.397(10) yes . .
C6 C9 1.522(9) yes . .
C7 C17 1.497(9) yes . .
C8 C12 1.524(9) yes . .
C9 C13 1.539(9) yes . .
C11 C14 1.525(10) yes . .
C12 C19 1.548(10) yes . .
C13 C21 1.532(11) yes . .
C15 C18 1.360(12) yes . .
C17 C20 1.513(10) yes . .
C19 C25 1.515(12) yes . .
C20 C22 1.532(11) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Ni1 S2 92.35(7) yes . . .
S1 Ni1 S3 176.96(8) yes . . .
S1 Ni1 S4 88.28(7) yes . . .
S2 Ni1 S3 88.85(7) yes . . .
S2 Ni1 S4 173.87(8) yes . . .
S3 Ni1 S4 90.82(7) yes . . .
Ni1 S1 C10 104.6(2) yes . . .
Ni1 S2 C5 104.5(2) yes . . .
Ni1 S3 C2 105.0(2) yes . . .
Ni1 S4 C2 105.5(2) yes . . 3_756
O23 S16 C24 105.1(4) yes . . .
O23 S16 C26 106.6(4) yes . . .
C24 S16 C26 98.2(4) yes . . .
C3 N1 C6 112.8(4) yes . . .
C3 N1 C7 107.6(4) yes . . .
C3 N1 C8 108.9(5) yes . . .
C6 N1 C7 108.6(4) yes . . .
C6 N1 C8 107.8(5) yes . . .
C7 N1 C8 111.1(4) yes . . .
C10 N3 C15 115.5(6) yes . . .
C5 N28 C18 115.7(6) yes . . .
S3 C2 S4 121.6(4) yes . . 3_756
S3 C2 C2 119.6(5) yes . . 3_756
S4 C2 C2 118.8(5) yes 3_756 . 3_756
N1 C3 C4 112.4(5) yes . . .
C3 C4 C11 109.0(5) yes . . .
S2 C5 N28 118.6(5) yes . . .
S2 C5 C10 118.6(5) yes . . .
N28 C5 C10 122.7(6) yes . . .
N1 C6 C9 114.1(5) yes . . .
N1 C7 C17 114.4(5) yes . . .
N1 C8 C12 112.7(5) yes . . .
C6 C9 C13 106.5(5) yes . . .
S1 C10 N3 118.8(5) yes . . .
S1 C10 C5 119.8(5) yes . . .
N3 C10 C5 121.4(6) yes . . .
C4 C11 C14 112.0(6) yes . . .
C8 C12 C19 106.7(5) yes . . .
C9 C13 C21 111.1(6) yes . . .
N3 C15 C18 122.2(6) yes . . .
C7 C17 C20 108.5(5) yes . . .
N28 C18 C15 122.3(7) yes . . .
C12 C19 C25 111.2(6) yes . . .
C17 C20 C22 113.6(6) yes . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S1 Ni1 S2 C5 -2.27(9) no . . . .
S2 Ni1 S1 C10 2.06(9) no . . . .
S1 Ni1 S4 C2 179.42(9) no . . . 3_756
S4 Ni1 S1 C10 -171.84(8) no . . . .
S2 Ni1 S3 C2 -170.00(9) no . . . .
S3 Ni1 S2 C5 -179.48(9) no . . . .
S3 Ni1 S4 C2 -3.48(9) no . . . 3_756
S4 Ni1 S3 C2 3.88(9) no . . . .
Ni1 S1 C10 N3 178.7(4) no . . . .
Ni1 S1 C10 C5 -1.3(5) no . . . .
Ni1 S2 C5 N28 -177.8(4) no . . . .
Ni1 S2 C5 C10 2.1(5) no . . . .
Ni1 S3 C2 S4 177.4(3) no . . . 3_756
Ni1 S3 C2 C2 -3.7(5) no . . . 3_756
Ni1 S4 C2 S3 -176.7(3) no . . 3_756 3_756
Ni1 S4 C2 C2 2.3(5) no . . 3_756 .
C3 N1 C6 C9 48.8(6) no . . . .
C6 N1 C3 C4 54.0(6) no . . . .
C3 N1 C7 C17 69.0(6) no . . . .
C7 N1 C3 C4 173.8(4) no . . . .
C3 N1 C8 C12 -178.6(4) no . . . .
C8 N1 C3 C4 -65.7(6) no . . . .
C6 N1 C7 C17 -168.6(4) no . . . .
C7 N1 C6 C9 -70.5(5) no . . . .
C6 N1 C8 C12 58.7(5) no . . . .
C8 N1 C6 C9 169.0(4) no . . . .
C7 N1 C8 C12 -60.2(6) no . . . .
C8 N1 C7 C17 -50.1(6) no . . . .
C10 N3 C15 C18 1.2(10) no . . . .
C15 N3 C10 S1 -179.4(5) no . . . .
C15 N3 C10 C5 0.6(9) no . . . .
C5 N28 C18 C15 2.9(10) no . . . .
C18 N28 C5 S2 178.8(5) no . . . .
C18 N28 C5 C10 -1.1(9) no . . . .
S3 C2 C2 S3 180.0(4) no . . 3_756 3_756
S3 C2 C2 S4 1.0(8) no . . 3_756 .
S4 C2 C2 S3 -1.0(8) no 3_756 . 3_756 3_756
S4 C2 C2 S4 180.0(4) no 3_756 . 3_756 .
N1 C3 C4 C11 -170.8(4) no . . . .
C3 C4 C11 C14 -72.9(6) no . . . .
S2 C5 C10 S1 -0.5(8) no . . . .
S2 C5 C10 N3 179.5(4) no . . . .
N28 C5 C10 S1 179.3(5) no . . . .
N28 C5 C10 N3 -0.7(10) no . . . .
N1 C6 C9 C13 176.0(4) no . . . .
N1 C7 C17 C20 176.1(4) no . . . .
N1 C8 C12 C19 169.5(4) no . . . .
C6 C9 C13 C21 174.3(5) no . . . .
C8 C12 C19 C25 173.5(5) no . . . .
N3 C15 C18 N28 -3.2(11) no . . . .
C7 C17 C20 C22 176.9(5) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N3 N28 2.810(9) no . .
C3 C9 2.954(9) no . .
C3 C14 3.133(9) no . .
C3 C17 3.062(9) no . .
C4 C6 2.979(8) no . .
C4 C8 3.025(9) no . .
C4 C9 3.378(9) no . .
C5 C15 2.653(9) no . .
C6 C12 2.929(9) no . .
C7 C9 3.103(9) no . .
C7 C12 3.026(10) no . .
C8 C17 2.959(10) no . .
C10 C18 2.667(10) no . .
C12 C17 3.481(11) no . .
S3 C4 3.584(7) no . .
S16 C14 3.511(8) no . .
O23 C6 3.289(9) no . 4_555
O23 C7 3.282(9) no . 4_555
O23 C24 3.400(11) no . 3_757
N3 C9 3.507(9) no . 4_554
N28 C8 3.483(8) no . 4_454
C4 S3 3.584(7) no . .
C6 O23 3.289(9) no . 4_454
C7 O23 3.282(9) no . 4_454
C8 N28 3.483(8) no . 4_555
C9 N3 3.507(9) no . 4_455
C11 C20 3.534(9) no . 2_646
C14 S16 3.511(8) no . .
C19 C21 3.554(11) no . 1_655
C20 C11 3.534(9) no . 2_656
C21 C19 3.554(11) no . 1_455
C24 O23 3.400(11) no . 3_757

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

#==============================================================================
# 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
#==============================================================================
_chemical_name_systematic        1_150K
####################################################################### 
# 
# 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_200k_2
_database_code_depnum_ccdc_archive 'CCDC 1063810'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C46 N6 Ni2 O2 S10'
_chemical_formula_moiety         'C46 N6 Ni2 O2 S10'
_chemical_formula_weight         1106.55
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.7705(17)
_cell_length_b                   19.924(3)
_cell_length_c                   13.848(2)
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.499(7)
_cell_angle_gamma                90.0000
_cell_volume                     2952.6(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11812
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      27.29
_cell_measurement_temperature    200
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_T_max  1.000

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

_diffrn_ambient_temperature      200
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.69960
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.706
_diffrn_reflns_number            19126
_diffrn_reflns_av_R_equivalents  0.1462
_diffrn_reflns_theta_max         27.020
_diffrn_reflns_theta_min         1.770
_diffrn_reflns_theta_full        27.020
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             6721
_reflns_number_gt                3080
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1762
_refine_ls_R_factor_gt           0.0902
_refine_ls_wR_factor_ref         0.2933
_refine_ls_wR_factor_gt          0.2462
_refine_ls_number_restraints     23
_refine_ls_number_reflns         6721
_refine_ls_number_parameters     298
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1556P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.002
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.60
_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 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.57725(8) 0.11812(4) 0.62436(7) 0.0466(3) Uani 1 4 d . . .
S1 S 0.67264(16) 0.03152(9) 0.57572(14) 0.0528(5) Uani 1 4 d . . .
S2 S 0.40323(16) 0.08306(9) 0.55102(14) 0.0538(5) Uani 1 4 d . . .
S3 S 0.47822(17) 0.20136(10) 0.67579(14) 0.0556(5) Uani 1 4 d . . .
S4 S 0.75370(16) 0.15635(9) 0.68782(15) 0.0551(5) Uani 1 4 d . . .
S21 S 0.3496(6) 0.0233(3) 0.1159(5) 0.213(3) Uani 1 4 d . . .
O31 O 0.3996(15) -0.0464(8) 0.0999(12) 0.278(9) Uani 1 4 d . . .
N6 N 0.5603(6) 0.3098(3) 0.7743(5) 0.0643(17) Uani 1 4 d . . .
N29 N 0.8106(6) 0.2695(4) 0.7832(5) 0.0688(18) Uani 1 4 d . . .
N30 N 0.6886(6) 0.2915(3) 0.4013(4) 0.0578(16) Uani 1 4 d . . .
C3 C 0.5617(6) -0.0114(3) 0.5061(5) 0.0468(16) Uani 1 4 d . . .
C5 C 0.5918(7) 0.2517(3) 0.7350(5) 0.0563(19) Uani 1 4 d . . .
C7 C 0.7874(7) 0.2899(4) 0.4870(5) 0.0589(19) Uani 1 4 d . . .
C8 C 0.7178(7) 0.2318(3) 0.7392(5) 0.0502(17) Uani 1 4 d . . .
C10 C 0.6069(8) 0.3678(5) 0.2607(7) 0.086(3) Uani 1 4 d . . .
C11 C 0.6531(11) 0.3472(4) 0.8167(7) 0.081(3) Uani 1 4 d . . .
C12 C 0.5503(8) 0.3583(6) 0.5012(8) 0.092(3) Uani 1 4 d . . .
C13 C 0.9164(7) 0.2737(4) 0.4595(6) 0.066(2) Uani 1 4 d . . .
C14 C 0.6919(10) 0.2298(4) 0.3368(6) 0.080(3) Uani 1 4 d . . .
C15 C 0.5612(8) 0.2961(5) 0.4392(7) 0.081(3) Uani 1 4 d . . .
C16 C 0.7767(9) 0.3274(5) 0.8206(6) 0.074(2) Uani 1 4 d . . .
C17 C 0.6396(8) 0.4302(5) 0.2044(7) 0.087(3) Uani 1 4 d . . .
C18 C 1.0080(9) 0.2779(5) 0.5560(7) 0.084(3) Uani 1 4 d . . .
C19 C 1.1378(9) 0.2571(7) 0.5374(8) 0.116(4) Uani 1 4 d . . .
C20 C 0.7229(16) 0.1016(5) 0.3248(7) 0.138(5) Uani 1 4 d . . .
C22 C 0.6767(14) 0.1645(5) 0.3934(8) 0.127(4) Uani 1 4 d . . .
C23 C 0.5436(10) 0.4462(7) 0.1203(9) 0.129(5) Uani 1 4 d . . .
C24 C 0.4138(10) 0.3624(8) 0.5227(10) 0.139(6) Uani 1 4 d . . .
C25 C 0.623(2) 0.0905(9) 0.2625(13) 0.197(8) Uani 1 4 d . . .
C26 C 0.3958(13) 0.4203(9) 0.5906(10) 0.176(8) Uani 1 4 d . . .
C27 C 0.3366(9) 0.0456(4) 0.0124(7) 0.086(3) Uani 1 4 d . . .
C28 C 0.2075(14) 0.0026(7) 0.1599(10) 0.136(5) Uani 1 4 d . . .
C32 C 0.7120(7) 0.3535(4) 0.3388(5) 0.0541(18) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'


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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S1 2.155(2) yes . .
Ni1 S2 2.1451(19) yes . .
Ni1 S3 2.137(2) yes . .
Ni1 S4 2.1415(19) yes . .
S1 C3 1.681(6) yes . .
S2 C3 1.696(7) yes . 3_656
S3 C5 1.717(7) yes . .
S4 C8 1.726(7) yes . .
S21 O31 1.516(17) yes . .
S21 C27 1.491(12) yes . .
S21 C28 1.759(17) yes . .
N6 C5 1.338(10) yes . .
N6 C11 1.328(12) yes . .
N29 C8 1.340(9) yes . .
N29 C16 1.332(12) yes . .
N30 C7 1.502(9) yes . .
N30 C14 1.522(10) yes . .
N30 C15 1.527(11) yes . .
N30 C32 1.545(9) yes . .
C3 C3 1.397(9) yes . 3_656
C5 C8 1.410(11) yes . .
C7 C13 1.516(11) yes . .
C10 C17 1.529(14) yes . .
C10 C32 1.501(11) yes . .
C11 C16 1.384(15) yes . .
C12 C15 1.521(15) yes . .
C12 C24 1.534(15) yes . .
C13 C18 1.570(12) yes . .
C14 C22 1.537(13) yes . .
C17 C23 1.502(14) yes . .
C18 C19 1.508(14) yes . .
C20 C22 1.681(16) yes . .
C20 C25 1.32(2) yes . .
C24 C26 1.51(2) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Ni1 S2 90.76(7) yes . . .
S1 Ni1 S3 177.68(9) yes . . .
S1 Ni1 S4 88.89(7) yes . . .
S2 Ni1 S3 88.18(8) yes . . .
S2 Ni1 S4 175.84(9) yes . . .
S3 Ni1 S4 92.32(8) yes . . .
Ni1 S1 C3 104.7(2) yes . . .
Ni1 S2 C3 105.5(2) yes . . 3_656
Ni1 S3 C5 104.9(3) yes . . .
Ni1 S4 C8 104.4(2) yes . . .
O31 S21 C27 97.4(8) yes . . .
O31 S21 C28 100.0(8) yes . . .
C27 S21 C28 114.4(7) yes . . .
C5 N6 C11 116.9(7) yes . . .
C8 N29 C16 116.1(7) yes . . .
C7 N30 C14 112.7(6) yes . . .
C7 N30 C15 108.3(6) yes . . .
C7 N30 C32 108.3(5) yes . . .
C14 N30 C15 109.4(6) yes . . .
C14 N30 C32 107.5(6) yes . . .
C15 N30 C32 110.7(6) yes . . .
S1 C3 S2 121.0(4) yes . . 3_656
S1 C3 C3 120.6(5) yes . . 3_656
S2 C3 C3 118.4(5) yes 3_656 . 3_656
S3 C5 N6 120.0(6) yes . . .
S3 C5 C8 119.1(5) yes . . .
N6 C5 C8 120.9(6) yes . . .
N30 C7 C13 113.1(6) yes . . .
S4 C8 N29 119.1(6) yes . . .
S4 C8 C5 119.2(5) yes . . .
N29 C8 C5 121.8(6) yes . . .
C17 C10 C32 108.8(7) yes . . .
N6 C11 C16 122.1(8) yes . . .
C15 C12 C24 106.8(9) yes . . .
C7 C13 C18 106.3(7) yes . . .
N30 C14 C22 112.0(7) yes . . .
N30 C15 C12 111.9(7) yes . . .
N29 C16 C11 122.4(8) yes . . .
C10 C17 C23 113.0(8) yes . . .
C13 C18 C19 110.2(8) yes . . .
C22 C20 C25 102.9(13) yes . . .
C14 C22 C20 106.7(9) yes . . .
C12 C24 C26 110.7(11) yes . . .
N30 C32 C10 113.4(6) yes . . .



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

#==============================================================================
# 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
#==============================================================================
_chemical_name_systematic        1_200K
####################################################################### 
# 
# 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_250k_2
_database_code_depnum_ccdc_archive 'CCDC 1063811'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C46 N6 Ni2 O2 S10'
_chemical_formula_moiety         'C46 N6 Ni2 O2 S10'
_chemical_formula_weight         1106.55
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.7047(15)
_cell_length_b                   20.555(3)
_cell_length_c                   13.8324(19)
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.106(7)
_cell_angle_gamma                90.0000
_cell_volume                     3013.2(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12556
_cell_measurement_theta_min      0.97
_cell_measurement_theta_max      27.30
_cell_measurement_temperature    250
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      250
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.69960
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.706
_diffrn_reflns_number            19540
_diffrn_reflns_av_R_equivalents  0.1452
_diffrn_reflns_theta_max         27.020
_diffrn_reflns_theta_min         1.759
_diffrn_reflns_theta_full        27.020
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             6859
_reflns_number_gt                2811
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1949
_refine_ls_R_factor_gt           0.0901
_refine_ls_wR_factor_ref         0.2863
_refine_ls_wR_factor_gt          0.2340
_refine_ls_number_restraints     15
_refine_ls_number_reflns         6859
_refine_ls_number_parameters     298
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1541P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.07590(8) 0.11782(4) 0.62050(7) 0.0572(3) Uani 1 4 d . . .
S1 S -0.10017(16) 0.08022(10) 0.54713(15) 0.0659(5) Uani 1 4 d . . .
S2 S 0.25358(17) 0.15652(10) 0.68692(16) 0.0689(6) Uani 1 4 d . . .
S3 S 0.17526(16) 0.03512(10) 0.57187(15) 0.0668(6) Uani 1 4 d . . .
S4 S -0.02663(18) 0.19772(10) 0.66987(16) 0.0689(6) Uani 1 4 d . . .
S15 S 0.1389(6) -0.0068(4) 0.8970(5) 0.274(4) Uani 1 4 d . . .
O26 O 0.1516(8) -0.0463(4) 0.9778(6) 0.150(3) Uani 1 4 d . . .
N6 N 0.0538(7) 0.3033(4) 0.7694(5) 0.082(2) Uani 1 4 d . . .
N30 N 0.1833(6) 0.2980(3) 0.4040(4) 0.0641(16) Uani 1 4 d . . .
N31 N 0.3072(7) 0.2670(4) 0.7821(5) 0.085(2) Uani 1 4 d . . .
C4 C -0.0638(6) 0.0102(3) 0.4935(5) 0.0554(17) Uani 1 4 d . . .
C5 C 0.2120(7) 0.3562(3) 0.3429(5) 0.0580(18) Uani 1 4 d . . .
C7 C 0.0883(7) 0.2481(4) 0.7314(5) 0.068(2) Uani 1 4 d . . .
C8 C 0.0559(8) 0.3056(4) 0.4421(6) 0.079(2) Uani 1 4 d . . .
C9 C 0.2150(7) 0.2302(4) 0.7379(6) 0.0643(19) Uani 1 4 d . . .
C10 C 0.2896(7) 0.2918(4) 0.4908(5) 0.066(2) Uani 1 4 d . . .
C11 C 0.1046(8) 0.3738(4) 0.2635(6) 0.082(3) Uani 1 4 d . . .
C12 C 0.1448(8) 0.4304(5) 0.2049(7) 0.090(3) Uani 1 4 d . . .
C13 C 0.1765(10) 0.2379(4) 0.3377(6) 0.089(3) Uani 1 4 d . . .
C14 C 0.1455(11) 0.3419(5) 0.8149(7) 0.097(3) Uani 1 4 d . . .
C16 C 0.4143(8) 0.2759(4) 0.4611(6) 0.079(2) Uani 1 4 d . . .
C17 C 0.5104(8) 0.2758(5) 0.5587(7) 0.099(3) Uani 1 4 d . . .
C18 C 0.2729(10) 0.3228(5) 0.8193(7) 0.095(3) Uani 1 4 d . . .
C19 C 0.0558(9) 0.3675(5) 0.5060(8) 0.096(3) Uani 1 4 d . . .
C20 C 0.1283(17) 0.1196(7) 0.3196(11) 0.158(6) Uani 1 4 d . . .
C21 C 0.6379(10) 0.2552(7) 0.5407(8) 0.131(4) Uani 1 4 d . . .
C22 C 0.0493(10) 0.4481(6) 0.1177(9) 0.134(5) Uani 1 4 d . . .
C23 C -0.0823(11) 0.3746(7) 0.5294(10) 0.134(5) Uani 1 4 d . . .
C24 C 0.1501(13) 0.1764(4) 0.3936(8) 0.124(4) Uani 1 4 d . . .
C25 C -0.0916(13) 0.4331(8) 0.5960(10) 0.167(6) Uani 1 4 d . . .
C27 C 0.2568(17) -0.0087(9) 0.8298(11) 0.243(11) Uani 1 4 d . . .
C28 C 0.0534(18) 0.0536(10) 0.8770(15) 0.282(14) Uani 1 4 d . . .
C29 C 0.237(2) 0.1064(6) 0.2977(18) 0.262(13) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S1 2.1541(19) yes . .
Ni1 S2 2.145(2) yes . .
Ni1 S3 2.162(2) yes . .
Ni1 S4 2.140(2) yes . .
S1 C4 1.690(7) yes . .
S2 C9 1.745(8) yes . .
S3 C4 1.675(6) yes . 3_556
S4 C7 1.737(8) yes . .
S15 O26 1.371(11) yes . .
S15 C27 1.67(2) yes . .
S15 C28 1.54(2) yes . .
N6 C7 1.324(11) yes . .
N6 C14 1.347(13) yes . .
N30 C5 1.520(9) yes . .
N30 C8 1.538(11) yes . .
N30 C10 1.539(9) yes . .
N30 C13 1.534(10) yes . .
N31 C9 1.324(10) yes . .
N31 C18 1.329(13) yes . .
C4 C4 1.415(9) yes . 3_556
C5 C11 1.518(10) yes . .
C7 C9 1.396(11) yes . .
C8 C19 1.549(13) yes . .
C10 C16 1.488(12) yes . .
C11 C12 1.516(13) yes . .
C12 C22 1.511(14) yes . .
C13 C24 1.529(13) yes . .
C14 C18 1.412(16) yes . .
C16 C17 1.578(11) yes . .
C17 C21 1.484(15) yes . .
C19 C23 1.564(15) yes . .
C20 C24 1.549(17) yes . .
C20 C29 1.27(3) yes . .
C23 C25 1.53(2) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Ni1 S2 177.28(10) yes . . .
S1 Ni1 S3 90.43(8) yes . . .
S1 Ni1 S4 88.38(8) yes . . .
S2 Ni1 S3 88.82(8) yes . . .
S2 Ni1 S4 92.43(8) yes . . .
S3 Ni1 S4 178.28(9) yes . . .
Ni1 S1 C4 105.8(2) yes . . .
Ni1 S2 C9 104.4(3) yes . . .
Ni1 S3 C4 105.1(2) yes . . 3_556
Ni1 S4 C7 104.8(3) yes . . .
O26 S15 C27 116.3(8) yes . . .
O26 S15 C28 127.6(10) yes . . .
C27 S15 C28 113.2(11) yes . . .
C7 N6 C14 117.7(8) yes . . .
C5 N30 C8 111.7(6) yes . . .
C5 N30 C10 108.3(5) yes . . .
C5 N30 C13 107.3(5) yes . . .
C8 N30 C10 109.6(6) yes . . .
C8 N30 C13 108.5(6) yes . . .
C10 N30 C13 111.5(6) yes . . .
C9 N31 C18 116.3(8) yes . . .
S1 C4 S3 121.3(4) yes . . 3_556
S1 C4 C4 118.3(5) yes . . 3_556
S3 C4 C4 120.3(5) yes 3_556 . 3_556
N30 C5 C11 113.5(6) yes . . .
S4 C7 N6 119.2(6) yes . . .
S4 C7 C9 119.2(6) yes . . .
N6 C7 C9 121.5(7) yes . . .
N30 C8 C19 110.5(7) yes . . .
S2 C9 N31 118.6(6) yes . . .
S2 C9 C7 119.1(6) yes . . .
N31 C9 C7 122.2(7) yes . . .
N30 C10 C16 113.3(6) yes . . .
C5 C11 C12 109.1(7) yes . . .
C11 C12 C22 113.6(8) yes . . .
N30 C13 C24 111.1(7) yes . . .
N6 C14 C18 119.5(9) yes . . .
C10 C16 C17 105.4(7) yes . . .
C16 C17 C21 111.1(8) yes . . .
N31 C18 C14 122.7(9) yes . . .
C8 C19 C23 105.8(8) yes . . .
C24 C20 C29 105.2(15) yes . . .
C19 C23 C25 110.0(10) yes . . .
C13 C24 C20 108.1(9) yes . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S1 Ni1 S3 C4 0.11(11) no . . . 3_556
S3 Ni1 S1 C4 -0.59(11) no . . . .
S1 Ni1 S4 C7 -176.09(11) no . . . .
S4 Ni1 S1 C4 -179.36(11) no . . . .
S2 Ni1 S3 C4 -177.28(11) no . . . 3_556
S3 Ni1 S2 C9 179.14(11) no . . . .
S2 Ni1 S4 C7 1.31(12) no . . . .
S4 Ni1 S2 C9 -2.04(11) no . . . .
Ni1 S1 C4 S3 179.9(4) no . . . 3_556
Ni1 S1 C4 C4 1.1(5) no . . . 3_556
Ni1 S2 C9 N31 -177.9(5) no . . . .
Ni1 S2 C9 C7 2.6(6) no . . . .
Ni1 S3 C4 S1 179.4(4) no . . 3_556 3_556
Ni1 S3 C4 C4 0.6(5) no . . 3_556 .
Ni1 S4 C7 N6 178.7(5) no . . . .
Ni1 S4 C7 C9 -0.0(6) no . . . .
C7 N6 C14 C18 0.8(12) no . . . .
C14 N6 C7 S4 -178.7(7) no . . . .
C14 N6 C7 C9 -0.1(12) no . . . .
C5 N30 C8 C19 -59.5(7) no . . . .
C8 N30 C5 C11 -50.6(7) no . . . .
C5 N30 C10 C16 -65.3(7) no . . . .
C10 N30 C5 C11 -171.3(5) no . . . .
C5 N30 C13 C24 179.0(6) no . . . .
C13 N30 C5 C11 68.1(7) no . . . .
C8 N30 C10 C16 172.7(5) no . . . .
C10 N30 C8 C19 60.4(7) no . . . .
C8 N30 C13 C24 -60.2(8) no . . . .
C13 N30 C8 C19 -177.6(5) no . . . .
C10 N30 C13 C24 60.6(8) no . . . .
C13 N30 C10 C16 52.6(8) no . . . .
C9 N31 C18 C14 1.6(13) no . . . .
C18 N31 C9 S2 179.7(7) no . . . .
C18 N31 C9 C7 -0.8(12) no . . . .
S1 C4 C4 S1 -180.0(4) no . . 3_556 3_556
S1 C4 C4 S3 -1.2(8) no . . 3_556 .
S3 C4 C4 S1 1.2(8) no 3_556 . 3_556 3_556
S3 C4 C4 S3 180.0(4) no 3_556 . 3_556 .
N30 C5 C11 C12 -177.9(5) no . . . .
S4 C7 C9 S2 -1.8(9) no . . . .
S4 C7 C9 N31 178.7(5) no . . . .
N6 C7 C9 S2 179.5(6) no . . . .
N6 C7 C9 N31 0.1(12) no . . . .
N30 C8 C19 C23 173.2(6) no . . . .
N30 C10 C16 C17 176.7(5) no . . . .
C5 C11 C12 C22 174.6(6) no . . . .
N30 C13 C24 C20 173.2(7) no . . . .
N6 C14 C18 N31 -1.6(14) no . . . .
C10 C16 C17 C21 175.3(7) no . . . .
C8 C19 C23 C25 177.8(8) no . . . .
C29 C20 C24 C13 73.1(15) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N6 N31 2.795(10) no . .
C5 C16 3.015(10) no . .
C5 C19 3.000(13) no . .
C7 C18 2.658(13) no . .
C8 C11 2.949(13) no . .
C8 C24 2.951(13) no . .
C9 C14 2.680(13) no . .
C10 C19 2.979(12) no . .
C10 C24 3.017(12) no . .
C11 C13 3.037(11) no . .
C11 C19 3.469(14) no . .
C13 C16 2.963(12) no . .
C13 C29 2.851(17) no . .
C16 C24 3.508(15) no . .
Ni1 C24 3.555(11) no . .
O26 C5 3.360(10) no . 2_546
O26 C10 3.404(11) no . 2_546
O26 C19 3.579(12) no . 2_546
O26 C28 3.18(2) no . 3_557
N31 C8 3.542(11) no . 4_555
C5 O26 3.360(10) no . 2_556
C8 N31 3.542(11) no . 4_454
C10 O26 3.404(11) no . 2_556
C19 O26 3.579(12) no . 2_556
C24 Ni1 3.555(11) no . .
C28 O26 3.18(2) no . 3_557

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

#==============================================================================
# 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
#==============================================================================
_chemical_name_systematic        1_250K
####################################################################### 
# 
# 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_300k_2
_database_code_depnum_ccdc_archive 'CCDC 1063812'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C46 N6 Ni2 O2 S10'
_chemical_formula_moiety         'C46 N6 Ni2 O2 S10'
_chemical_formula_weight         1106.55
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.6962(14)
_cell_length_b                   20.721(3)
_cell_length_c                   13.8764(19)
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.222(7)
_cell_angle_gamma                90.0000
_cell_volume                     3044.0(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11139
_cell_measurement_theta_min      0.96
_cell_measurement_theta_max      27.34
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      296
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.69960
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.706
_diffrn_reflns_number            19774
_diffrn_reflns_av_R_equivalents  0.1386
_diffrn_reflns_theta_max         27.020
_diffrn_reflns_theta_min         1.751
_diffrn_reflns_theta_full        27.020
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             6924
_reflns_number_gt                2380
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.2070
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.2428
_refine_ls_wR_factor_gt          0.1930
_refine_ls_number_restraints     6
_refine_ls_number_reflns         6924
_refine_ls_number_parameters     307
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1229P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.40
_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 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.57498(7) 0.11750(4) 0.61889(6) 0.0682(3) Uani 1 4 d . . .
S1 S 0.39915(15) 0.07954(9) 0.54601(14) 0.0791(5) Uani 1 4 d . . .
S2 S 0.75217(16) 0.15609(10) 0.68576(14) 0.0830(6) Uani 1 4 d . . .
S3 S 0.47172(16) 0.19644(9) 0.66783(14) 0.0835(6) Uani 1 4 d . . .
S4 S 0.67517(15) 0.03597(9) 0.57088(14) 0.0799(6) Uani 1 4 d . . .
S29 S 0.6562(7) 0.0071(4) 0.9133(5) 0.140(2) Uani 0.5 4 d . . .
S31 S 0.6073(10) -0.0286(4) 0.8713(8) 0.210(5) Uani 0.5 4 d . . .
O6 O 0.6517(7) -0.0475(4) 0.9749(6) 0.174(3) Uani 1 4 d . . .
N13 N 0.1824(5) 0.2012(2) 0.9035(4) 0.0696(14) Uani 1 4 d . . .
N28 N 0.5531(7) 0.3011(4) 0.7693(5) 0.101(2) Uani 1 4 d . . .
N30 N 0.8047(6) 0.2655(4) 0.7825(5) 0.0991(19) Uani 1 4 d . . .
C3 C 0.2119(6) 0.1432(3) 0.8424(4) 0.0660(17) Uani 1 4 d . . .
C4 C 0.4358(5) 0.0095(3) 0.4935(4) 0.0658(17) Uani 1 4 d . . .
C5 C 0.6429(11) 0.3394(4) 0.8151(6) 0.117(3) Uani 1 4 d . . .
C7 C 0.5872(7) 0.2467(4) 0.7289(5) 0.080(2) Uani 1 4 d . . .
C8 C 0.0555(7) 0.1928(4) 0.9429(5) 0.086(2) Uani 1 4 d . . .
C9 C 0.2879(6) 0.2077(3) 0.9899(4) 0.0730(18) Uani 1 4 d . . .
C10 C 0.7136(7) 0.2288(3) 0.7373(5) 0.0754(18) Uani 1 4 d . . .
C11 C 0.1044(7) 0.1262(4) 0.7635(5) 0.090(2) Uani 1 4 d . . .
C12 C 0.1436(7) 0.0696(4) 0.7058(6) 0.102(3) Uani 1 4 d . . .
C14 C 0.1754(8) 0.2600(3) 0.8363(5) 0.096(2) Uani 1 4 d . . .
C15 C 0.7714(10) 0.3204(5) 0.8199(6) 0.111(3) Uani 1 4 d . . .
C16 C 0.0538(8) 0.1324(4) 1.0046(6) 0.110(3) Uani 1 4 d . . .
C17 C 0.4125(7) 0.2232(4) 0.9606(5) 0.092(2) Uani 1 4 d . . .
C18 C -0.0830(9) 0.1269(5) 1.0291(8) 0.135(3) Uani 1 4 d . . .
C19 C 0.5089(8) 0.2231(5) 1.0588(6) 0.113(3) Uani 1 4 d . . .
C20 C 0.0477(8) 0.0514(5) 0.6185(7) 0.143(4) Uani 1 4 d . . .
C21 C 0.1517(11) 0.3211(4) 0.8938(7) 0.135(4) Uani 1 4 d . . .
C22 C 0.6367(9) 0.2404(6) 1.0432(7) 0.150(4) Uani 1 4 d . . .
C23 C 0.2410(18) 0.3927(6) 0.8012(14) 0.258(10) Uani 1 4 d . . .
C24 C -0.0918(11) 0.0675(6) 1.0944(8) 0.169(5) Uani 1 4 d . . .
C25 C 0.1286(14) 0.3784(6) 0.8182(9) 0.171(5) Uani 1 4 d . . .
C26 C 0.751(2) -0.0099(9) 0.8278(12) 0.275(10) Uani 1 4 d . . .
C27 C 0.5477(15) 0.0459(8) 0.8680(12) 0.296(12) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S1 2.1528(18) yes . .
Ni1 S2 2.1423(19) yes . .
Ni1 S3 2.138(2) yes . .
Ni1 S4 2.157(2) yes . .
S1 C4 1.695(6) yes . .
S2 C10 1.742(7) yes . .
S3 C7 1.740(7) yes . .
S4 C4 1.671(6) yes . 3_656
S29 O6 1.425(10) yes . .
S29 C26 1.70(2) yes . .
S29 C27 1.476(17) yes . .
S31 O6 1.500(13) yes . .
S31 C26 1.77(2) yes . .
S31 C27 1.669(19) yes . .
N13 C3 1.530(8) yes . .
N13 C8 1.543(9) yes . .
N13 C9 1.530(7) yes . .
N13 C14 1.530(8) yes . .
N28 C5 1.335(12) yes . .
N28 C7 1.334(11) yes . .
N30 C10 1.322(10) yes . .
N30 C15 1.320(13) yes . .
C3 C11 1.512(9) yes . .
C4 C4 1.414(8) yes . 3_656
C5 C15 1.422(16) yes . .
C7 C10 1.391(10) yes . .
C8 C16 1.518(12) yes . .
C9 C17 1.483(10) yes . .
C11 C12 1.512(11) yes . .
C12 C20 1.518(11) yes . .
C14 C21 1.537(11) yes . .
C16 C18 1.553(13) yes . .
C17 C19 1.587(10) yes . .
C18 C24 1.539(16) yes . .
C19 C22 1.458(13) yes . .
C21 C25 1.580(15) yes . .
C23 C25 1.29(2) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Ni1 S2 177.68(9) yes . . .
S1 Ni1 S3 88.42(7) yes . . .
S1 Ni1 S4 90.46(7) yes . . .
S2 Ni1 S3 92.41(8) yes . . .
S2 Ni1 S4 88.76(7) yes . . .
S3 Ni1 S4 178.33(8) yes . . .
Ni1 S1 C4 105.9(2) yes . . .
Ni1 S2 C10 104.7(2) yes . . .
Ni1 S3 C7 104.4(3) yes . . .
Ni1 S4 C4 105.1(2) yes . . 3_656
O6 S29 C26 109.2(8) yes . . .
O6 S29 C27 126.7(9) yes . . .
C26 S29 C27 109.0(10) yes . . .
O6 S31 C26 102.3(8) yes . . .
O6 S31 C27 109.7(9) yes . . .
C26 S31 C27 97.7(10) yes . . .
S29 O6 S31 41.4(5) yes . . .
C3 N13 C8 111.7(5) yes . . .
C3 N13 C9 108.4(4) yes . . .
C3 N13 C14 106.4(5) yes . . .
C8 N13 C9 108.7(5) yes . . .
C8 N13 C14 109.7(5) yes . . .
C9 N13 C14 111.9(5) yes . . .
C5 N28 C7 118.7(8) yes . . .
C10 N30 C15 117.4(7) yes . . .
N13 C3 C11 112.9(5) yes . . .
S1 C4 S4 121.5(3) yes . . 3_656
S1 C4 C4 117.6(4) yes . . 3_656
S4 C4 C4 120.9(5) yes 3_656 . 3_656
N28 C5 C15 118.9(9) yes . . .
S3 C7 N28 119.5(6) yes . . .
S3 C7 C10 119.7(6) yes . . .
N28 C7 C10 120.7(7) yes . . .
N13 C8 C16 112.0(6) yes . . .
N13 C9 C17 113.3(5) yes . . .
S2 C10 N30 119.4(6) yes . . .
S2 C10 C7 118.7(5) yes . . .
N30 C10 C7 121.9(7) yes . . .
C3 C11 C12 109.0(6) yes . . .
C11 C12 C20 114.1(7) yes . . .
N13 C14 C21 109.6(6) yes . . .
N30 C15 C5 122.2(9) yes . . .
C8 C16 C18 105.8(7) yes . . .
C9 C17 C19 105.3(6) yes . . .
C16 C18 C24 109.1(8) yes . . .
C17 C19 C22 112.3(7) yes . . .
C14 C21 C25 107.2(8) yes . . .
C21 C25 C23 103.4(12) yes . . .
S29 C26 S31 34.6(6) yes . . .
S29 C27 S31 37.8(6) yes . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S1 Ni1 S3 C7 -176.09(10) no . . . .
S3 Ni1 S1 C4 -178.77(10) no . . . .
S1 Ni1 S4 C4 -0.11(10) no . . . 3_656
S4 Ni1 S1 C4 -0.00(10) no . . . .
S2 Ni1 S3 C7 1.75(10) no . . . .
S3 Ni1 S2 C10 -1.69(10) no . . . .
S2 Ni1 S4 C4 -177.92(10) no . . . 3_656
S4 Ni1 S2 C10 179.50(10) no . . . .
Ni1 S1 C4 S4 179.9(3) no . . . 3_656
Ni1 S1 C4 C4 0.1(5) no . . . 3_656
Ni1 S2 C10 N30 -178.2(4) no . . . .
Ni1 S2 C10 C7 1.2(5) no . . . .
Ni1 S3 C7 N28 -179.7(4) no . . . .
Ni1 S3 C7 C10 -1.5(5) no . . . .
Ni1 S4 C4 S1 180.0(3) no . . 3_656 3_656
Ni1 S4 C4 C4 0.2(5) no . . 3_656 .
O6 S29 C26 S31 66.5(6) no . . . .
C26 S29 O6 S31 -68.5(8) no . . . .
O6 S29 C27 S31 -61.4(8) no . . . .
C27 S29 O6 S31 64.9(10) no . . . .
C26 S29 C27 S31 72.2(8) no . . . .
C27 S29 C26 S31 -75.5(9) no . . . .
O6 S31 C26 S29 -57.3(6) no . . . .
C26 S31 O6 S29 59.9(8) no . . . .
O6 S31 C27 S29 45.2(7) no . . . .
C27 S31 O6 S29 -43.0(7) no . . . .
C26 S31 C27 S29 -60.8(8) no . . . .
C27 S31 C26 S29 54.8(7) no . . . .
C3 N13 C8 C16 58.2(6) no . . . .
C8 N13 C3 C11 51.7(6) no . . . .
C3 N13 C9 C17 64.7(6) no . . . .
C9 N13 C3 C11 171.4(4) no . . . .
C3 N13 C14 C21 -177.5(5) no . . . .
C14 N13 C3 C11 -68.0(6) no . . . .
C8 N13 C9 C17 -173.6(5) no . . . .
C9 N13 C8 C16 -61.3(6) no . . . .
C8 N13 C14 C21 61.4(6) no . . . .
C14 N13 C8 C16 176.0(4) no . . . .
C9 N13 C14 C21 -59.3(7) no . . . .
C14 N13 C9 C17 -52.3(6) no . . . .
C5 N28 C7 S3 -179.4(6) no . . . .
C5 N28 C7 C10 2.4(11) no . . . .
C7 N28 C5 C15 -0.6(12) no . . . .
C10 N30 C15 C5 1.8(12) no . . . .
C15 N30 C10 S2 179.5(6) no . . . .
C15 N30 C10 C7 0.1(11) no . . . .
N13 C3 C11 C12 178.6(4) no . . . .
S1 C4 C4 S1 180.0(3) no . . 3_656 3_656
S1 C4 C4 S4 -0.3(7) no . . 3_656 .
S4 C4 C4 S1 0.3(7) no 3_656 . 3_656 3_656
S4 C4 C4 S4 180.0(4) no 3_656 . 3_656 .
N28 C5 C15 N30 -1.6(13) no . . . .
S3 C7 C10 S2 0.2(8) no . . . .
S3 C7 C10 N30 179.6(5) no . . . .
N28 C7 C10 S2 178.3(6) no . . . .
N28 C7 C10 N30 -2.3(11) no . . . .
N13 C8 C16 C18 -174.1(5) no . . . .
N13 C9 C17 C19 -176.3(4) no . . . .
C3 C11 C12 C20 -175.0(5) no . . . .
N13 C14 C21 C25 -173.1(6) no . . . .
C8 C16 C18 C24 -178.4(6) no . . . .
C9 C17 C19 C22 -177.6(6) no . . . .
C14 C21 C25 C23 -77.4(10) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N28 N30 2.772(9) no . .
C3 C16 3.011(11) no . .
C3 C17 3.006(9) no . .
C5 C10 2.687(12) no . .
C7 C15 2.665(12) no . .
C8 C11 2.958(11) no . .
C8 C21 2.964(11) no . .
C9 C16 2.982(11) no . .
C9 C21 2.978(10) no . .
C11 C14 3.011(10) no . .
C11 C16 3.466(12) no . .
C14 C17 2.956(10) no . .
C14 C23 2.895(15) no . .
C17 C21 3.467(12) no . .
Ni1 C21 3.575(10) no . 4_554
O6 C3 3.381(9) no . 3_657
O6 C9 3.402(10) no . 3_657
O6 C16 3.583(11) no . 3_657
O6 C27 3.261(19) no . 3_657
N30 C8 3.565(9) no . 1_655
C3 O6 3.381(9) no . 3_657
C8 N30 3.565(9) no . 1_455
C9 O6 3.402(10) no . 3_657
C16 O6 3.583(11) no . 3_657
C21 Ni1 3.575(10) no . 4_455
C27 O6 3.261(19) no . 3_657

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

#==============================================================================
# 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
#==============================================================================
_chemical_name_systematic        1_300K
####################################################################### 
# 
# 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_MH_130704_1_result_4
_database_code_depnum_ccdc_archive 'CCDC 1063813'
_audit_update_record             
;
2015-05-07 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C40 N6 Ni S4'
_chemical_formula_moiety         'C40 N6 Ni S4'
_chemical_formula_weight         751.42
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   7.7723(7)
_cell_length_b                   20.4416(18)
_cell_length_c                   14.1183(12)
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.3700(10)
_cell_angle_gamma                90.0000
_cell_volume                     2229.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748.00
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_type   none

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

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  ?
_diffrn_reflns_number            10920
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_theta_max         25.361
_diffrn_reflns_theta_min         1.760
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# 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).
;
_reflns_number_total             4071
_reflns_number_gt                3862
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1987
_refine_ls_number_restraints     0
_refine_ls_number_reflns         4071
_refine_ls_number_parameters     232
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1237P)²+5.6423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.28
_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)
;
N N 0.0061 0.0033
;
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)
;
Ni Ni 0.3393 1.1124
;
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_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0 0.0 0.0 0.0219(2) Uani 1 2 d . . .
S2 S -0.09219(12) 0.04415(4) 0.12522(6) 0.0262(3) Uani 1 4 d . . .
S3 S 0.03403(12) -0.09474(4) 0.07110(6) 0.0272(3) Uani 1 4 d . . .
N4 N 0.4224(4) 0.14734(14) 0.1877(2) 0.0217(6) Uani 1 4 d . . .
N5 N -0.1506(5) -0.00797(17) 0.2914(3) 0.0315(8) Uani 1 4 d . . .
N6 N -0.0224(4) -0.13200(17) 0.2458(2) 0.0313(7) Uani 1 4 d . . .
C7 C -0.0925(5) -0.01940(19) 0.2074(3) 0.0254(7) Uani 1 4 d . . .
C8 C 0.3842(5) 0.04658(18) 0.2922(3) 0.0274(8) Uani 1 4 d . . .
C9 C -0.0304(4) -0.08230(19) 0.1834(3) 0.0254(7) Uani 1 4 d . . .
C10 C 0.3403(5) 0.21390(17) 0.1634(3) 0.0260(8) Uani 1 4 d . . .
C11 C 0.6118(5) 0.15800(19) 0.2273(3) 0.0284(8) Uani 1 4 d . . .
C12 C 0.4171(5) 0.10337(16) 0.1000(2) 0.0223(7) Uani 1 4 d . . .
C13 C 0.2985(5) 0.02725(18) 0.3807(3) 0.0275(8) Uani 1 4 d . . .
C14 C 0.3213(5) 0.11456(17) 0.2607(3) 0.0243(7) Uani 1 4 d . . .
C15 C 0.4991(6) 0.1165(2) -0.1632(3) 0.0317(8) Uani 1 4 d . . .
C16 C -0.1422(5) -0.0588(2) 0.3534(3) 0.0351(9) Uani 1 4 d . . .
C17 C 0.4821(5) 0.08399(17) -0.0671(2) 0.0233(7) Uani 1 4 d . . .
C18 C 0.0917(6) 0.28126(18) 0.0932(3) 0.0334(9) Uani 1 4 d . . .
C19 C -0.0785(5) -0.1191(2) 0.3312(3) 0.0352(9) Uani 1 4 d . . .
C20 C 0.3412(6) -0.0434(2) 0.4104(3) 0.0357(9) Uani 1 4 d . . .
C21 C 0.1530(5) 0.21163(18) 0.1182(3) 0.0301(8) Uani 1 4 d . . .
C22 C 0.4757(5) 0.13523(18) 0.0117(3) 0.0267(8) Uani 1 4 d . . .
C23 C -0.0954(6) 0.2815(2) 0.0448(4) 0.0449(11) Uani 1 4 d . . .
C24 C 0.6372(7) 0.1959(3) 0.3222(3) 0.0455(11) Uani 1 4 d . . .
C25 C 0.8297(8) 0.2103(3) 0.3503(4) 0.0526(13) Uani 1 4 d . . .
C26 C 0.9322(7) 0.1507(3) 0.3866(4) 0.0571(14) Uani 1 4 d . . .



#==============================================================================
_computing_data_collection       Unknown
_computing_cell_refinement       Unknown
_computing_data_reduction        Unknown
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

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

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 S2 2.1759(9) yes . .
Ni1 S2 2.1759(9) yes . 3_555
Ni1 S3 2.1839(8) yes . .
Ni1 S3 2.1839(8) yes . 3_555
S2 C7 1.742(4) yes . .
S3 C9 1.734(4) yes . .
N4 C10 1.526(5) yes . .
N4 C11 1.531(5) yes . .
N4 C12 1.527(4) yes . .
N4 C14 1.519(5) yes . .
N5 C7 1.335(5) yes . .
N5 C16 1.355(6) yes . .
N6 C9 1.341(5) yes . .
N6 C19 1.352(6) yes . .
C7 C9 1.427(5) yes . .
C8 C13 1.532(6) yes . .
C8 C14 1.523(5) yes . .
C10 C21 1.524(5) yes . .
C11 C24 1.541(6) yes . .
C12 C22 1.521(5) yes . .
C13 C20 1.530(5) yes . .
C15 C17 1.529(5) yes . .
C16 C19 1.378(6) yes . .
C17 C22 1.532(5) yes . .
C18 C21 1.530(5) yes . .
C18 C23 1.537(6) yes . .
C24 C25 1.533(8) yes . .
C25 C26 1.513(8) yes . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S2 Ni1 S2 180.00(5) yes . . 3_555
S2 Ni1 S3 91.63(3) yes . . .
S2 Ni1 S3 88.37(3) yes . . 3_555
S2 Ni1 S3 88.37(3) yes 3_555 . .
S2 Ni1 S3 91.63(3) yes 3_555 . 3_555
S3 Ni1 S3 180.00(5) yes . . 3_555
Ni1 S2 C7 104.89(13) yes . . .
Ni1 S3 C9 104.94(13) yes . . .
C10 N4 C11 108.4(3) yes . . .
C10 N4 C12 111.7(3) yes . . .
C10 N4 C14 108.1(3) yes . . .
C11 N4 C12 108.6(3) yes . . .
C11 N4 C14 111.3(3) yes . . .
C12 N4 C14 108.7(3) yes . . .
C7 N5 C16 116.2(4) yes . . .
C9 N6 C19 116.2(4) yes . . .
S2 C7 N5 119.1(3) yes . . .
S2 C7 C9 119.2(3) yes . . .
N5 C7 C9 121.7(3) yes . . .
C13 C8 C14 108.6(3) yes . . .
S3 C9 N6 119.5(3) yes . . .
S3 C9 C7 119.3(3) yes . . .
N6 C9 C7 121.3(3) yes . . .
N4 C10 C21 115.0(3) yes . . .
N4 C11 C24 114.5(3) yes . . .
N4 C12 C22 115.4(3) yes . . .
C8 C13 C20 111.5(3) yes . . .
N4 C14 C8 115.3(3) yes . . .
N5 C16 C19 122.1(4) yes . . .
C15 C17 C22 111.1(3) yes . . .
C21 C18 C23 111.2(3) yes . . .
N6 C19 C16 122.5(4) yes . . .
C10 C21 C18 109.1(3) yes . . .
C12 C22 C17 109.8(3) yes . . .
C11 C24 C25 110.4(4) yes . . .
C24 C25 C26 113.3(4) yes . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S2 Ni1 S3 C9 0.32(4) no . . . .
S3 Ni1 S2 C7 -1.57(4) no . . . .
S2 Ni1 S3 C9 179.68(4) no . . 3_555 3_555
S3 Ni1 S2 C7 178.43(4) no 3_555 . . .
S2 Ni1 S3 C9 -179.68(4) no 3_555 . . .
S3 Ni1 S2 C7 -178.43(4) no . . 3_555 3_555
S2 Ni1 S3 C9 -0.32(4) no 3_555 . 3_555 3_555
S3 Ni1 S2 C7 1.57(4) no 3_555 . 3_555 3_555
Ni1 S2 C7 N5 -177.2(2) no . . . .
Ni1 S2 C7 C9 2.9(3) no . . . .
Ni1 S3 C9 N6 -179.1(2) no . . . .
Ni1 S3 C9 C7 1.4(3) no . . . .
C10 N4 C11 C24 64.4(3) no . . . .
C11 N4 C10 C21 177.1(3) no . . . .
C10 N4 C12 C22 47.3(4) no . . . .
C12 N4 C10 C21 57.5(4) no . . . .
C10 N4 C14 C8 179.1(2) no . . . .
C14 N4 C10 C21 -62.1(3) no . . . .
C11 N4 C12 C22 -72.2(3) no . . . .
C12 N4 C11 C24 -174.1(2) no . . . .
C11 N4 C14 C8 -61.9(3) no . . . .
C14 N4 C11 C24 -54.5(4) no . . . .
C12 N4 C14 C8 57.7(3) no . . . .
C14 N4 C12 C22 166.5(2) no . . . .
C7 N5 C16 C19 -0.4(5) no . . . .
C16 N5 C7 S2 -177.9(3) no . . . .
C16 N5 C7 C9 2.0(5) no . . . .
C9 N6 C19 C16 0.6(5) no . . . .
C19 N6 C9 S3 -178.5(3) no . . . .
C19 N6 C9 C7 0.9(5) no . . . .
S2 C7 C9 S3 -3.0(4) no . . . .
S2 C7 C9 N6 177.5(2) no . . . .
N5 C7 C9 S3 177.1(3) no . . . .
N5 C7 C9 N6 -2.3(5) no . . . .
C13 C8 C14 N4 167.1(2) no . . . .
C14 C8 C13 C20 174.1(2) no . . . .
N4 C10 C21 C18 -177.1(3) no . . . .
N4 C11 C24 C25 -174.0(3) no . . . .
N4 C12 C22 C17 174.0(2) no . . . .
N5 C16 C19 N6 -0.9(6) no . . . .
C15 C17 C22 C12 166.8(3) no . . . .
C23 C18 C21 C10 178.4(3) no . . . .
C11 C24 C25 C26 -74.1(5) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
Ni1 C7 3.117(4) no . 3_555
Ni1 C9 3.119(4) no . 3_555
N5 N6 2.825(5) no . .
C7 C19 2.679(6) no . .
C8 C11 3.085(5) no . .
C8 C12 2.988(5) no . .
C9 C16 2.684(6) no . .
C10 C22 2.964(5) no . .
C10 C24 3.056(6) no . .
C11 C22 3.145(5) no . .
C11 C26 3.168(6) no . .
C12 C21 3.048(5) no . .
C14 C21 3.018(5) no . .
C14 C24 3.013(6) no . .
C21 C22 3.439(6) no . .
N5 C26 3.543(7) no . 1_455
C26 N5 3.543(7) no . 1_655

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

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