# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_jj_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1435763'
_audit_update_record             
;
2015-11-07 deposited with the CCDC.
2015-12-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Ni3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H42 N24 Ni3 O6 S6'
_chemical_formula_sum            'C18 H42 N24 Ni3 O6 S6'
_chemical_formula_weight         1059.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '
_symmetry_space_group_name_Hall  '-C 2yc  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.7049(17)
_cell_length_b                   14.1790(12)
_cell_length_c                   23.480(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.644(5)
_cell_angle_gamma                90.00
_cell_volume                     6317.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      27.690

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3828
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24785
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         27.69
_reflns_number_total             7140
_reflns_number_gt                4772
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7140
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1161
_refine_ls_wR_factor_ref         0.3421
_refine_ls_wR_factor_gt          0.3246
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_restrained_S_all      1.242
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3519(4) 0.7833(6) 0.1232(3) 0.0409(16) Uani 1 1 d . . .
C2 C 0.3337(5) 0.6660(6) 0.1762(3) 0.0486(19) Uani 1 1 d . . .
C3 C 0.4294(7) 0.9356(9) 0.1741(5) 0.080(3) Uani 1 1 d . . .
H3A H 0.3957 0.9550 0.1946 0.119 Uiso 1 1 calc R . .
H3B H 0.4569 0.9891 0.1686 0.119 Uiso 1 1 calc R . .
H3C H 0.4600 0.8886 0.1970 0.119 Uiso 1 1 calc R . .
C4 C 0.2859(4) 0.5790(5) -0.0697(3) 0.0374(15) Uani 1 1 d . . .
C5 C 0.2761(4) 0.4568(5) -0.0179(4) 0.0419(17) Uani 1 1 d . . .
C6 C 0.2930(9) 0.5721(9) -0.1843(5) 0.088(4) Uani 1 1 d . . .
H6A H 0.3073 0.5098 -0.1701 0.131 Uiso 1 1 calc R . .
H6B H 0.3209 0.5928 -0.2097 0.131 Uiso 1 1 calc R . .
H6C H 0.2441 0.5714 -0.2061 0.131 Uiso 1 1 calc R . .
C7 C 0.0795(4) 0.6261(6) 0.0476(4) 0.0463(18) Uani 1 1 d . . .
C8 C 0.0903(4) 0.7537(5) 0.0011(4) 0.0395(16) Uani 1 1 d . . .
C9 C -0.0208(6) 0.8680(9) -0.0446(7) 0.095(4) Uani 1 1 d . . .
H9A H -0.0306 0.8579 -0.0071 0.142 Uiso 1 1 calc R . .
H9B H -0.0443 0.8206 -0.0721 0.142 Uiso 1 1 calc R . .
H9C H -0.0375 0.9292 -0.0594 0.142 Uiso 1 1 calc R . .
N1 N 0.3078(3) 0.7271(4) 0.0880(2) 0.0329(12) Uani 1 1 d . . .
N2 N 0.2953(3) 0.6514(4) 0.1210(3) 0.0371(13) Uani 1 1 d . . .
N3 N 0.3707(4) 0.7463(5) 0.1807(3) 0.0509(17) Uani 1 1 d . . .
N4 N 0.3354(5) 0.6063(6) 0.2240(3) 0.061(2) Uani 1 1 d . . .
H4A H 0.2975 0.5694 0.2152 0.091 Uiso 1 1 calc R . .
H4B H 0.3358 0.6407 0.2558 0.091 Uiso 1 1 calc R . .
H4C H 0.3741 0.5708 0.2314 0.091 Uiso 1 1 calc R . .
N5 N 0.2686(3) 0.6093(4) -0.0243(2) 0.0307(12) Uani 1 1 d . . .
N6 N 0.2625(3) 0.5346(4) 0.0109(3) 0.0325(12) Uani 1 1 d . . .
N7 N 0.2912(3) 0.4838(5) -0.0671(3) 0.0424(14) Uani 1 1 d . . .
N8 N 0.2734(4) 0.3671(4) 0.0014(3) 0.0497(16) Uani 1 1 d . . .
H8A H 0.2291 0.3467 -0.0094 0.074 Uiso 1 1 calc R . .
H8B H 0.2894 0.3656 0.0407 0.074 Uiso 1 1 calc R . .
H8C H 0.3001 0.3301 -0.0143 0.074 Uiso 1 1 calc R . .
N9 N 0.1458(3) 0.6291(4) 0.0470(2) 0.0343(12) Uani 1 1 d . . .
N10 N 0.1535(3) 0.7122(4) 0.0173(2) 0.0329(12) Uani 1 1 d . . .
N11 N 0.0443(3) 0.7019(5) 0.0207(3) 0.0495(16) Uani 1 1 d . . .
N12 N 0.0485(4) 0.5554(6) 0.0734(4) 0.064(2) Uani 1 1 d . . .
H12D H 0.0112 0.5322 0.0467 0.096 Uiso 1 1 calc R . .
H12E H 0.0348 0.5794 0.1036 0.096 Uiso 1 1 calc R . .
H12F H 0.0796 0.5095 0.0865 0.096 Uiso 1 1 calc R . .
Ni1 Ni 0.22795(4) 0.54269(6) 0.08611(4) 0.0331(3) Uani 1 1 d . . .
Ni2 Ni 0.2500 0.7500 0.0000 0.0270(3) Uani 1 2 d S . .
O1 O 0.1959(3) 0.5351(4) 0.1649(3) 0.0544(15) Uani 1 1 d . . .
H1 H 0.2302 0.5240 0.1928 0.082 Uiso 1 1 calc R . .
O2 O 0.3035(3) 0.4423(4) 0.1283(3) 0.0539(15) Uani 1 1 d . . .
H2 H 0.3021 0.3971 0.1062 0.081 Uiso 1 1 calc R . .
O3 O 0.1581(3) 0.4288(4) 0.0549(3) 0.0464(12) Uani 1 1 d . . .
H3 H 0.1759 0.3797 0.0704 0.070 Uiso 1 1 calc R . .
S1 S 0.38527(14) 0.88853(18) 0.10514(10) 0.0624(7) Uani 1 1 d . . .
S2 S 0.30469(14) 0.64796(15) -0.12534(10) 0.0563(6) Uani 1 1 d . . .
S3 S 0.07196(11) 0.86096(17) -0.03543(13) 0.0624(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.299(10) . ?
C1 N3 1.401(10) . ?
C1 S1 1.729(8) . ?
C2 N2 1.328(10) . ?
C2 N3 1.340(11) . ?
C2 N4 1.401(10) . ?
C3 S1 1.751(10) . ?
C4 N5 1.279(9) . ?
C4 N7 1.354(9) . ?
C4 S2 1.748(7) . ?
C5 N7 1.326(10) . ?
C5 N8 1.357(9) . ?
C5 N6 1.358(10) . ?
C6 S2 1.719(11) . ?
C7 N9 1.311(10) . ?
C7 N11 1.341(11) . ?
C7 N12 1.396(10) . ?
C8 N10 1.336(9) . ?
C8 N11 1.342(10) . ?
C8 S3 1.735(7) . ?
C9 S3 1.786(12) . ?
N1 N2 1.384(8) . ?
N1 Ni2 2.098(6) . ?
N2 Ni1 2.055(6) . ?
N5 N6 1.368(8) . ?
N5 Ni2 2.134(5) . ?
N6 Ni1 2.059(6) . ?
N9 N10 1.397(8) . ?
N9 Ni1 2.041(6) . ?
N10 Ni2 2.119(5) . ?
Ni1 O2 2.104(5) . ?
Ni1 O1 2.112(6) . ?
Ni1 O3 2.120(5) . ?
Ni2 N1 2.098(6) 7_565 ?
Ni2 N10 2.119(6) 7_565 ?
Ni2 N5 2.134(5) 7_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N3 110.0(6) . . ?
N1 C1 S1 127.3(6) . . ?
N3 C1 S1 122.7(6) . . ?
N2 C2 N3 111.4(6) . . ?
N2 C2 N4 124.8(8) . . ?
N3 C2 N4 123.7(8) . . ?
N5 C4 N7 109.4(6) . . ?
N5 C4 S2 126.4(5) . . ?
N7 C4 S2 124.2(6) . . ?
N7 C5 N8 126.9(7) . . ?
N7 C5 N6 108.7(6) . . ?
N8 C5 N6 124.4(7) . . ?
N9 C7 N11 111.1(7) . . ?
N9 C7 N12 125.6(8) . . ?
N11 C7 N12 123.3(7) . . ?
N10 C8 N11 108.9(6) . . ?
N10 C8 S3 125.5(5) . . ?
N11 C8 S3 125.4(6) . . ?
C1 N1 N2 108.0(6) . . ?
C1 N1 Ni2 128.7(5) . . ?
N2 N1 Ni2 122.7(4) . . ?
C2 N2 N1 106.5(6) . . ?
C2 N2 Ni1 130.0(5) . . ?
N1 N2 Ni1 123.5(4) . . ?
C2 N3 C1 104.1(6) . . ?
C4 N5 N6 109.4(5) . . ?
C4 N5 Ni2 129.8(5) . . ?
N6 N5 Ni2 120.8(4) . . ?
C5 N6 N5 105.4(5) . . ?
C5 N6 Ni1 128.9(5) . . ?
N5 N6 Ni1 125.4(4) . . ?
C5 N7 C4 107.1(6) . . ?
C7 N9 N10 106.0(6) . . ?
C7 N9 Ni1 130.4(5) . . ?
N10 N9 Ni1 123.4(4) . . ?
C8 N10 N9 107.2(5) . . ?
C8 N10 Ni2 130.5(5) . . ?
N9 N10 Ni2 122.2(4) . . ?
C7 N11 C8 106.8(6) . . ?
N9 Ni1 N2 94.5(2) . . ?
N9 Ni1 N6 93.0(2) . . ?
N2 Ni1 N6 93.2(2) . . ?
N9 Ni1 O2 173.1(2) . . ?
N2 Ni1 O2 91.2(2) . . ?
N6 Ni1 O2 90.6(2) . . ?
N9 Ni1 O1 92.1(2) . . ?
N2 Ni1 O1 90.1(2) . . ?
N6 Ni1 O1 173.6(2) . . ?
O2 Ni1 O1 83.9(3) . . ?
N9 Ni1 O3 86.5(2) . . ?
N2 Ni1 O3 176.9(2) . . ?
N6 Ni1 O3 89.7(2) . . ?
O2 Ni1 O3 87.6(2) . . ?
O1 Ni1 O3 86.8(2) . . ?
N1 Ni2 N1 180.0(3) 7_565 . ?
N1 Ni2 N10 92.8(2) 7_565 7_565 ?
N1 Ni2 N10 87.2(2) . 7_565 ?
N1 Ni2 N10 87.2(2) 7_565 . ?
N1 Ni2 N10 92.8(2) . . ?
N10 Ni2 N10 180.0(3) 7_565 . ?
N1 Ni2 N5 91.8(2) 7_565 7_565 ?
N1 Ni2 N5 88.2(2) . 7_565 ?
N10 Ni2 N5 92.4(2) 7_565 7_565 ?
N10 Ni2 N5 87.6(2) . 7_565 ?
N1 Ni2 N5 88.2(2) 7_565 . ?
N1 Ni2 N5 91.8(2) . . ?
N10 Ni2 N5 87.6(2) 7_565 . ?
N10 Ni2 N5 92.4(2) . . ?
N5 Ni2 N5 180.0(3) 7_565 . ?
C1 S1 C3 103.2(5) . . ?
C6 S2 C4 104.0(5) . . ?
C8 S3 C9 100.3(4) . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.052 -0.010 0.250 1295 744 ' '
2 0.070 -0.004 0.750 1294 757 ' '
_platon_squeeze_details          ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        27.69
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.267
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF/CH3OH'
_chemical_properties_physical    Heat-sensitive
_exptl_crystal_preparation       'Magnetic properties'
