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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_kw131_twin3
_database_code_depnum_ccdc_archive 'CCDC 1539266'
_audit_update_record             
;
2017-03-21 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H28 Cl2 N4 Ni O9 S2'
_chemical_formula_weight         590.13

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   12.3784(2)
_cell_length_b                   19.1075(3)
_cell_length_c                   21.1751(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.0587(7)
_cell_angle_gamma                90
_cell_volume                     5008.34(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      25.39

_exptl_crystal_description       rod
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             2448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.204
_shelx_estimated_absorpt_T_min   0.671
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.677578
_exptl_absorpt_correction_T_max  0.745210
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47955
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.859
_diffrn_reflns_theta_max         25.178
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             4464
_reflns_number_gt                4169
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
 The strcture is a pseudo-merohedral twin in space group I2/a.
One perchlorate is disordered and it was treated as edge-sharing
alternative tetrahedra.
Residual electron density along a line (water) was treated as three
alternative sites from one water oxygen with SUMP
The macrocyclic ligand is disordered,
with propylene versus ethylene bridges. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0754P)²+94.9081P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4464
_refine_ls_number_parameters     258
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.1919
_refine_ls_wR_factor_gt          0.1859
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.00022(6) 0.22417(2) 0.17360(2) 0.01646(9) Uani 1 1 d . . . . .
S1A S 0.19178(13) 0.24684(8) 0.17022(7) 0.0224(3) Uani 0.6694(16) 1 d D . P A 1
S2A S -0.18700(14) 0.20425(8) 0.18024(8) 0.0270(4) Uani 0.6694(16) 1 d D . P A
1
N1A N -0.0018(3) 0.28543(15) 0.08911(14) 0.0269(3) Uiso 0.6694(16) 1 d D U P A
1
N2A N 0.0065(3) 0.12849(15) 0.12372(14) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
C1A C 0.1968(5) 0.2792(3) 0.0895(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H1A H 0.2649 0.3052 0.0822 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H1B H 0.1933 0.2397 0.0593 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C2A C 0.1007(4) 0.3269(3) 0.0809(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H2A H 0.1034 0.3652 0.1124 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H2B H 0.1024 0.3481 0.0382 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C3A C -0.0958(4) 0.3326(3) 0.0824(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H3A H -0.0861 0.3598 0.0431 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H3B H -0.0938 0.3662 0.1179 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C4A C -0.2091(5) 0.2999(3) 0.0807(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H4A H -0.2589 0.3346 0.0617 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H4B H -0.2067 0.2591 0.0519 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C5A C -0.2577(5) 0.2757(3) 0.1430(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H5A H -0.3334 0.2613 0.1354 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H5B H -0.2590 0.3159 0.1725 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C6A C -0.1924(5) 0.1333(3) 0.1238(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H6A H -0.2606 0.1068 0.1283 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H6B H -0.1876 0.1515 0.0801 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C7A C -0.0961(5) 0.0870(3) 0.1387(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H7A H -0.0989 0.0439 0.1128 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H7B H -0.0969 0.0735 0.1838 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C8A C 0.1035(5) 0.0839(3) 0.1394(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H8A H 0.1059 0.0779 0.1858 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H8B H 0.0919 0.0370 0.1207 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C9A C 0.2126(5) 0.1099(3) 0.1182(3) 0.0269(3) Uiso 0.6694(16) 1 d . U P A 1
H9A H 0.2056 0.1310 0.0757 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H9B H 0.2628 0.0697 0.1149 0.032 Uiso 0.6694(16) 1 calc R U P A 1
C10A C 0.2601(5) 0.1638(3) 0.1632(3) 0.0269(3) Uiso 0.6694(16) 1 d D U P A 1
H10A H 0.3354 0.1732 0.1499 0.032 Uiso 0.6694(16) 1 calc R U P A 1
H10B H 0.2634 0.1425 0.2058 0.032 Uiso 0.6694(16) 1 calc R U P A 1
S1B S 0.1862(2) 0.20038(17) 0.17574(16) 0.0276(8) Uani 0.3306(16) 1 d D . P A 2
S2B S -0.1939(2) 0.24708(16) 0.17365(14) 0.0195(7) Uani 0.3306(16) 1 d D . P A
2
N1B N -0.0018(3) 0.28543(15) 0.08911(14) 0.0269(3) Uiso 0.3306(16) 1 d D U P A
2
N2B N 0.0065(3) 0.12849(15) 0.12372(14) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
C1B C 0.2475(9) 0.2734(5) 0.1354(4) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H1B1 H 0.2547 0.3117 0.1666 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H1B2 H 0.3218 0.2590 0.1238 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C2B C 0.1965(7) 0.3046(6) 0.0769(5) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H2B1 H 0.2447 0.3424 0.0618 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H2B2 H 0.1960 0.2678 0.0439 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C3B C 0.0838(7) 0.3343(5) 0.0808(7) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H3B1 H 0.0817 0.3679 0.1164 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H3B2 H 0.0697 0.3611 0.0416 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C4B C -0.1000(7) 0.3264(5) 0.0821(7) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H4B1 H -0.1038 0.3458 0.0388 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H4B2 H -0.0987 0.3661 0.1122 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C5B C -0.1993(8) 0.2815(6) 0.0946(4) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H5B1 H -0.2020 0.2425 0.0639 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H5B2 H -0.2654 0.3101 0.0892 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C6B C -0.2646(9) 0.1635(4) 0.1713(5) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H6B1 H -0.2657 0.1439 0.2145 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H6B2 H -0.3405 0.1724 0.1588 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C7B C -0.2189(7) 0.1094(6) 0.1277(5) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H7B1 H -0.2401 0.1232 0.0844 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H7B2 H -0.2574 0.0651 0.1370 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C8B C -0.0960(6) 0.0913(6) 0.1254(6) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H8B1 H -0.0870 0.0598 0.1621 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H8B2 H -0.0911 0.0604 0.0879 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C9B C 0.0837(8) 0.0787(6) 0.1268(6) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H9B1 H 0.0764 0.0424 0.0938 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H9B2 H 0.0901 0.0570 0.1691 0.032 Uiso 0.3306(16) 1 calc R U P A 2
C10B C 0.1744(11) 0.1327(5) 0.1127(5) 0.0269(3) Uiso 0.3306(16) 1 d D U P A 2
H10C H 0.1591 0.1559 0.0719 0.032 Uiso 0.3306(16) 1 calc R U P A 2
H10D H 0.2442 0.1077 0.1087 0.032 Uiso 0.3306(16) 1 calc R U P A 2
N4 N 0.0083(5) 0.17050(16) 0.25971(14) 0.0382(10) Uani 1 1 d . . . . .
N3A N -0.0193(5) 0.3139(3) 0.2239(3) 0.0089(12) Uiso 0.471(6) 1 d . . P A 1
C11A C -0.0244(5) 0.3696(3) 0.2490(3) 0.0134(15) Uiso 0.471(6) 1 d D . P A 1
C12A C -0.0553(8) 0.4368(4) 0.2779(4) 0.0273(19) Uiso 0.471(6) 1 d D . P A 1
H12D H -0.0347 0.4753 0.2498 0.041 Uiso 0.471(6) 1 calc R U P A 1
H12E H -0.0180 0.4421 0.3185 0.041 Uiso 0.471(6) 1 calc R U P A 1
H12F H -0.1335 0.4377 0.2848 0.041 Uiso 0.471(6) 1 calc R U P A 1
N3B N 0.0127(7) 0.3163(3) 0.2235(3) 0.0316(15) Uiso 0.529(6) 1 d . . P A 2
C11B C 0.0264(6) 0.3673(4) 0.2471(4) 0.0299(19) Uiso 0.529(6) 1 d D . P A 2
C12B C 0.0152(9) 0.4369(4) 0.2790(4) 0.043(2) Uiso 0.529(6) 1 d D . P A 2
H12A H 0.0836 0.4494 0.2994 0.064 Uiso 0.529(6) 1 calc R U P A 2
H12B H -0.0420 0.4343 0.3109 0.064 Uiso 0.529(6) 1 calc R U P A 2
H12C H -0.0035 0.4726 0.2476 0.064 Uiso 0.529(6) 1 calc R U P A 2
C13 C 0.0092(6) 0.1511(2) 0.31026(18) 0.0397(12) Uani 1 1 d . . . . .
C14 C 0.0096(7) 0.1274(2) 0.37610(18) 0.0443(13) Uani 1 1 d . . . . .
H14A H -0.0129 0.1660 0.4037 0.067 Uiso 1 1 calc R U . . .
H14B H 0.0826 0.1124 0.3878 0.067 Uiso 1 1 calc R U . . .
H14C H -0.0406 0.0881 0.3809 0.067 Uiso 1 1 calc R U . . .
Cl1 Cl 0.50246(12) 0.16145(4) 0.05366(4) 0.0275(2) Uani 1 1 d . . . . .
O1 O 0.4131(4) 0.1904(3) 0.0254(2) 0.1174(18) Uani 1 1 d . . . . .
O2 O 0.5953(4) 0.1810(3) 0.0173(2) 0.0837(17) Uani 1 1 d . . . . .
O3 O 0.5187(7) 0.1826(3) 0.11718(17) 0.103(2) Uani 1 1 d . . . . .
O4 O 0.4919(8) 0.0893(2) 0.0533(3) 0.125(2) Uani 1 1 d . . . . .
Cl2A Cl 0.22758(14) 0.49725(10) 0.19235(8) 0.0260(4) Uiso 0.563(3) 1 d D . P B
1
O7A O 0.2302(9) 0.5013(6) 0.2599(3) 0.080(2) Uiso 0.563(3) 1 d D . P B 1
O8A O 0.1329(6) 0.4839(6) 0.1602(5) 0.098(3) Uiso 0.563(3) 1 d D . P B 1
Cl2B Cl 0.2925(2) 0.50656(14) 0.18770(13) 0.0400(6) Uiso 0.437(3) 1 d D . P B 2
O7B O 0.3973(5) 0.5147(5) 0.1661(4) 0.051(2) Uiso 0.437(3) 1 d D . P B 2
O8B O 0.2983(8) 0.5048(5) 0.2553(3) 0.053(2) Uiso 0.437(3) 1 d D . P B 2
O5 O 0.2319(8) 0.5632(4) 0.1674(5) 0.211(5) Uiso 1 1 d D . . . .
O6 O 0.2556(5) 0.4347(2) 0.1720(3) 0.0868(16) Uiso 1 1 d D . . . .
O10 O 0.2500 0.4992(9) 0.0000 0.088(3) Uiso 0.698(9) 2 d S . P . .
O11 O 0.0000 0.5000 0.0000 0.065(2) Uiso 0.689(9) 2 d S . P . .
O12 O 0.3924(8) 0.4990(9) 0.0000(9) 0.044(2) Uiso 0.322(5) 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3A 2.033(6) . ?
Ni1 N3B 2.060(7) . ?
Ni1 N4 2.094(3) . ?
Ni1 N2A 2.113(3) . ?
Ni1 N1A 2.138(3) . ?
Ni1 S1B 2.346(3) . ?
Ni1 S2A 2.3528(18) . ?
Ni1 S1A 2.4116(17) . ?
Ni1 S2B 2.443(3) . ?
S1A C10A 1.804(6) . ?
S1A C1A 1.819(6) . ?
S2A C5A 1.803(6) . ?
S2A C6A 1.808(6) . ?
N1A C3A 1.478(7) . ?
N1A C2A 1.507(7) . ?
N2A C8A 1.509(7) . ?
N2A C7A 1.531(7) . ?
C1A C2A 1.510(8) . ?
C1A H1A 0.9900 . ?
C1A H1B 0.9900 . ?
C2A H2A 0.9900 . ?
C2A H2B 0.9900 . ?
C3A C4A 1.535(8) . ?
C3A H3A 0.9900 . ?
C3A H3B 0.9900 . ?
C4A C5A 1.522(8) . ?
C4A H4A 0.9900 . ?
C4A H4B 0.9900 . ?
C5A H5A 0.9900 . ?
C5A H5B 0.9900 . ?
C6A C7A 1.516(8) . ?
C6A H6A 0.9900 . ?
C6A H6B 0.9900 . ?
C7A H7A 0.9900 . ?
C7A H7B 0.9900 . ?
C8A C9A 1.508(9) . ?
C8A H8A 0.9900 . ?
C8A H8B 0.9900 . ?
C9A C10A 1.521(9) . ?
C9A H9A 0.9900 . ?
C9A H9B 0.9900 . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
S1B C1B 1.805(10) . ?
S1B C10B 1.864(10) . ?
S2B C5B 1.800(9) . ?
S2B C6B 1.821(9) . ?
C1B C2B 1.512(12) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B C3B 1.509(11) . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B C5B 1.522(12) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C5B H5B1 0.9900 . ?
C5B H5B2 0.9900 . ?
C6B C7B 1.497(12) . ?
C6B H6B1 0.9900 . ?
C6B H6B2 0.9900 . ?
C7B C8B 1.561(11) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
C9B C10B 1.553(16) . ?
C9B H9B1 0.9900 . ?
C9B H9B2 0.9900 . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
N4 C13 1.133(5) . ?
N3A C11A 1.191(9) . ?
C11A C12A 1.473(9) . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
N3B C11B 1.108(10) . ?
C11B C12B 1.498(10) . ?
C12B H12A 0.9800 . ?
C12B H12B 0.9800 . ?
C12B H12C 0.9800 . ?
C13 C14 1.466(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
Cl1 O1 1.373(5) . ?
Cl1 O4 1.385(4) . ?
Cl1 O3 1.418(4) . ?
Cl1 O2 1.434(5) . ?
Cl2A O6 1.317(5) . ?
Cl2A O5 1.367(7) . ?
Cl2A O8A 1.378(8) . ?
Cl2A O7A 1.434(6) . ?
O8A O6 1.803(10) . ?
Cl2B O7B 1.384(7) . ?
Cl2B O5 1.384(8) . ?
Cl2B O8B 1.434(7) . ?
Cl2B O6 1.485(5) . ?
O10 O12 1.762(10) . ?
O10 O12 1.762(10) 2 ?
O11 O12 1.332(10) 6_565 ?
O11 O12 1.332(10) 2 ?
O12 O11 1.332(10) 2 ?

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
N3A Ni1 N4 87.85(18) . . ?
N3B Ni1 N4 88.2(2) . . ?
N3A Ni1 N2A 174.94(19) . . ?
N4 Ni1 N2A 90.56(12) . . ?
N3A Ni1 N1A 88.60(17) . . ?
N4 Ni1 N1A 175.64(15) . . ?
N2A Ni1 N1A 93.19(11) . . ?
N3B Ni1 S1B 94.7(2) . . ?
N4 Ni1 S1B 80.93(19) . . ?
N3A Ni1 S2A 89.28(17) . . ?
N4 Ni1 S2A 85.12(18) . . ?
N2A Ni1 S2A 85.79(12) . . ?
N1A Ni1 S2A 97.35(12) . . ?
N3A Ni1 S1A 88.95(17) . . ?
N4 Ni1 S1A 93.88(18) . . ?
N2A Ni1 S1A 95.96(12) . . ?
N1A Ni1 S1A 83.53(12) . . ?
S2A Ni1 S1A 178.00(6) . . ?
N3B Ni1 S2B 85.4(2) . . ?
N4 Ni1 S2B 97.67(19) . . ?
S1B Ni1 S2B 178.59(11) . . ?
C10A S1A C1A 101.8(3) . . ?
C10A S1A Ni1 107.8(2) . . ?
C1A S1A Ni1 97.1(2) . . ?
C5A S2A C6A 105.1(3) . . ?
C5A S2A Ni1 109.2(2) . . ?
C6A S2A Ni1 96.7(2) . . ?
C3A N1A C2A 109.3(4) . . ?
C3A N1A Ni1 115.0(3) . . ?
C2A N1A Ni1 112.1(3) . . ?
C8A N2A C7A 108.8(4) . . ?
C8A N2A Ni1 114.1(3) . . ?
C7A N2A Ni1 108.3(3) . . ?
C2A C1A S1A 106.9(4) . . ?
C2A C1A H1A 110.3 . . ?
S1A C1A H1A 110.3 . . ?
C2A C1A H1B 110.3 . . ?
S1A C1A H1B 110.3 . . ?
H1A C1A H1B 108.6 . . ?
N1A C2A C1A 109.4(5) . . ?
N1A C2A H2A 109.8 . . ?
C1A C2A H2A 109.8 . . ?
N1A C2A H2B 109.8 . . ?
C1A C2A H2B 109.8 . . ?
H2A C2A H2B 108.3 . . ?
N1A C3A C4A 118.3(5) . . ?
N1A C3A H3A 107.7 . . ?
C4A C3A H3A 107.7 . . ?
N1A C3A H3B 107.7 . . ?
C4A C3A H3B 107.7 . . ?
H3A C3A H3B 107.1 . . ?
C5A C4A C3A 117.6(5) . . ?
C5A C4A H4A 107.9 . . ?
C3A C4A H4A 107.9 . . ?
C5A C4A H4B 107.9 . . ?
C3A C4A H4B 107.9 . . ?
H4A C4A H4B 107.2 . . ?
C4A C5A S2A 114.7(4) . . ?
C4A C5A H5A 108.6 . . ?
S2A C5A H5A 108.6 . . ?
C4A C5A H5B 108.6 . . ?
S2A C5A H5B 108.6 . . ?
H5A C5A H5B 107.6 . . ?
C7A C6A S2A 105.8(4) . . ?
C7A C6A H6A 110.6 . . ?
S2A C6A H6A 110.6 . . ?
C7A C6A H6B 110.6 . . ?
S2A C6A H6B 110.6 . . ?
H6A C6A H6B 108.7 . . ?
C6A C7A N2A 107.9(5) . . ?
C6A C7A H7A 110.1 . . ?
N2A C7A H7A 110.1 . . ?
C6A C7A H7B 110.1 . . ?
N2A C7A H7B 110.1 . . ?
H7A C7A H7B 108.4 . . ?
C9A C8A N2A 117.5(5) . . ?
C9A C8A H8A 107.9 . . ?
N2A C8A H8A 107.9 . . ?
C9A C8A H8B 107.9 . . ?
N2A C8A H8B 107.9 . . ?
H8A C8A H8B 107.2 . . ?
C8A C9A C10A 112.5(5) . . ?
C8A C9A H9A 109.1 . . ?
C10A C9A H9A 109.1 . . ?
C8A C9A H9B 109.1 . . ?
C10A C9A H9B 109.1 . . ?
H9A C9A H9B 107.8 . . ?
C9A C10A S1A 117.8(5) . . ?
C9A C10A H10A 107.9 . . ?
S1A C10A H10A 107.9 . . ?
C9A C10A H10B 107.9 . . ?
S1A C10A H10B 107.9 . . ?
H10A C10A H10B 107.2 . . ?
C1B S1B C10B 103.4(5) . . ?
C1B S1B Ni1 104.7(4) . . ?
C10B S1B Ni1 92.6(4) . . ?
C5B S2B C6B 106.1(5) . . ?
C5B S2B Ni1 95.8(3) . . ?
C6B S2B Ni1 108.4(4) . . ?
C2B C1B S1B 121.1(8) . . ?
C2B C1B H1B1 107.1 . . ?
S1B C1B H1B1 107.1 . . ?
C2B C1B H1B2 107.1 . . ?
S1B C1B H1B2 107.1 . . ?
H1B1 C1B H1B2 106.8 . . ?
C3B C2B C1B 119.2(10) . . ?
C3B C2B H2B1 107.5 . . ?
C1B C2B H2B1 107.5 . . ?
C3B C2B H2B2 107.5 . . ?
C1B C2B H2B2 107.5 . . ?
H2B1 C2B H2B2 107.0 . . ?
C2B C3B H3B1 108.1 . . ?
C2B C3B H3B2 108.1 . . ?
H3B1 C3B H3B2 107.3 . . ?
C5B C4B H4B1 109.5 . . ?
C5B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 108.1 . . ?
C4B C5B S2B 109.8(8) . . ?
C4B C5B H5B1 109.7 . . ?
S2B C5B H5B1 109.7 . . ?
C4B C5B H5B2 109.7 . . ?
S2B C5B H5B2 109.7 . . ?
H5B1 C5B H5B2 108.2 . . ?
C7B C6B S2B 116.2(8) . . ?
C7B C6B H6B1 108.2 . . ?
S2B C6B H6B1 108.2 . . ?
C7B C6B H6B2 108.2 . . ?
S2B C6B H6B2 108.2 . . ?
H6B1 C6B H6B2 107.4 . . ?
C6B C7B C8B 122.8(9) . . ?
C6B C7B H7B1 106.6 . . ?
C8B C7B H7B1 106.6 . . ?
C6B C7B H7B2 106.6 . . ?
C8B C7B H7B2 106.6 . . ?
H7B1 C7B H7B2 106.6 . . ?
C7B C8B H8B1 102.6 . . ?
C7B C8B H8B2 102.6 . . ?
H8B1 C8B H8B2 105.0 . . ?
C10B C9B H9B1 113.3 . . ?
C10B C9B H9B2 113.3 . . ?
H9B1 C9B H9B2 110.6 . . ?
C9B C10B S1B 112.3(8) . . ?
C9B C10B H10C 109.2 . . ?
S1B C10B H10C 109.2 . . ?
C9B C10B H10D 109.2 . . ?
S1B C10B H10D 109.2 . . ?
H10C C10B H10D 107.9 . . ?
C13 N4 Ni1 169.5(3) . . ?
C11A N3A Ni1 173.5(5) . . ?
N3A C11A C12A 168.0(7) . . ?
C11A C12A H12D 109.5 . . ?
C11A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C11A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C11B N3B Ni1 174.1(7) . . ?
N3B C11B C12B 165.8(9) . . ?
C11B C12B H12A 109.5 . . ?
C11B C12B H12B 109.5 . . ?
H12A C12B H12B 109.5 . . ?
C11B C12B H12C 109.5 . . ?
H12A C12B H12C 109.5 . . ?
H12B C12B H12C 109.5 . . ?
N4 C13 C14 178.9(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 Cl1 O4 108.8(5) . . ?
O1 Cl1 O3 114.3(4) . . ?
O4 Cl1 O3 107.5(3) . . ?
O1 Cl1 O2 107.9(3) . . ?
O4 Cl1 O2 109.4(4) . . ?
O3 Cl1 O2 108.8(4) . . ?
O6 Cl2A O5 134.3(5) . . ?
O6 Cl2A O8A 83.9(5) . . ?
O5 Cl2A O8A 90.8(6) . . ?
O6 Cl2A O7A 111.7(5) . . ?
O5 Cl2A O7A 109.6(6) . . ?
O8A Cl2A O7A 121.4(6) . . ?
Cl2A O8A O6 46.6(3) . . ?
O7B Cl2B O5 108.5(6) . . ?
O7B Cl2B O8B 106.7(6) . . ?
O5 Cl2B O8B 110.8(6) . . ?
O7B Cl2B O6 108.5(5) . . ?
O5 Cl2B O6 119.1(5) . . ?
O8B Cl2B O6 102.5(5) . . ?
Cl2A O6 O8A 49.5(4) . . ?
O12 O10 O12 179.8(16) . 2 ?
O12 O11 O12 180.0(14) 6_565 2 ?
O11 O12 O10 179.1(14) 2 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10A S1A C1A C2A 152.6(4) . . . . ?
Ni1 S1A C1A C2A 42.6(4) . . . . ?
C3A N1A C2A C1A 178.4(5) . . . . ?
Ni1 N1A C2A C1A 49.8(5) . . . . ?
S1A C1A C2A N1A -62.7(5) . . . . ?
C2A N1A C3A C4A 172.4(6) . . . . ?
Ni1 N1A C3A C4A -60.6(6) . . . . ?
N1A C3A C4A C5A 77.0(7) . . . . ?
C3A C4A C5A S2A -65.1(7) . . . . ?
C6A S2A C5A C4A -59.9(5) . . . . ?
Ni1 S2A C5A C4A 43.0(5) . . . . ?
C5A S2A C6A C7A 155.0(4) . . . . ?
Ni1 S2A C6A C7A 43.0(4) . . . . ?
S2A C6A C7A N2A -66.5(5) . . . . ?
C8A N2A C7A C6A 178.9(5) . . . . ?
Ni1 N2A C7A C6A 54.4(5) . . . . ?
C7A N2A C8A C9A 170.0(5) . . . . ?
Ni1 N2A C8A C9A -69.0(6) . . . . ?
N2A C8A C9A C10A 82.1(7) . . . . ?
C8A C9A C10A S1A -66.0(7) . . . . ?
C1A S1A C10A C9A -59.4(5) . . . . ?
Ni1 S1A C10A C9A 42.1(5) . . . . ?
C10B S1B C1B C2B 56.1(10) . . . . ?
Ni1 S1B C1B C2B -40.2(9) . . . . ?
S1B C1B C2B C3B 59.7(13) . . . . ?
C6B S2B C5B C4B -150.1(7) . . . . ?
Ni1 S2B C5B C4B -39.0(7) . . . . ?
C5B S2B C6B C7B 60.2(9) . . . . ?
Ni1 S2B C6B C7B -41.7(9) . . . . ?
S2B C6B C7B C8B 47.2(14) . . . . ?
C1B S1B C10B C9B -155.8(8) . . . . ?
Ni1 S1B C10B C9B -50.0(8) . . . . ?
O5 Cl2A O8A O6 134.6(5) . . . . ?
O7A Cl2A O8A O6 -111.8(6) . . . . ?
O6 Cl2A O5 Cl2B -64.4(7) . . . . ?
O8A Cl2A O5 Cl2B -146.6(5) . . . . ?
O7A Cl2A O5 Cl2B 89.4(6) . . . . ?
O7B Cl2B O5 Cl2A 165.6(5) . . . . ?
O8B Cl2B O5 Cl2A -77.6(5) . . . . ?
O6 Cl2B O5 Cl2A 40.9(5) . . . . ?
O5 Cl2A O6 Cl2B 60.4(7) . . . . ?
O8A Cl2A O6 Cl2B 145.5(5) . . . . ?
O7A Cl2A O6 Cl2B -93.0(5) . . . . ?
O5 Cl2A O6 O8A -85.1(8) . . . . ?
O7A Cl2A O6 O8A 121.5(7) . . . . ?
O7B Cl2B O6 Cl2A -169.3(5) . . . . ?
O5 Cl2B O6 Cl2A -44.6(6) . . . . ?
O8B Cl2B O6 Cl2A 78.1(5) . . . . ?
O7B Cl2B O6 O8A -143.3(5) . . . . ?
O5 Cl2B O6 O8A -18.6(7) . . . . ?
O8B Cl2B O6 O8A 104.1(6) . . . . ?
Cl2A O8A O6 Cl2B -18.7(3) . . . . ?

_refine_diff_density_max         1.851
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.139

# start Validation Reply Form

_vrf_PLAT201_I                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         15 Report
RESPONSE: The strcture is a pseudo-merohedral twin in space group I2/a.
One perchlorate is disordered and it was treated as edge-sharing
alternative tetrahedra.
Residual electron density along a line (water) was treated as three
alternative sites from one water oxygen with SUMP
The macrocyclic ligand is disordered with propylene versus ethylene bridges. 
;
# end Validation Reply Form


_shelxl_version_number           2013-4

