# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1486103'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H88 N8 Ni8 O40, 7(C H4 O), 12(O H2)'
_chemical_formula_sum            'C83 H140 N8 Ni8 O59'
_chemical_formula_weight         2663.70

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   29.3530(6)
_cell_length_b                   29.3530(6)
_cell_length_c                   16.1124(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13882.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9133
_cell_measurement_theta_min      2.435
_cell_measurement_theta_max      19.66

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             5560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.143
_shelx_estimated_absorpt_T_min   0.779
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7892
_exptl_absorpt_correction_T_max  0.8721

_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker, 2014)'

_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 Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            82208
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.387
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             6154
_reflns_number_gt                3072
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        ?
_computing_structure_solution    'SIR-2008 (Burla, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00075(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6154
_refine_ls_number_parameters     420
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.0940
_refine_ls_wR_factor_ref         0.3578
_refine_ls_wR_factor_gt          0.2893
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_restrained_S_all      1.196
_refine_ls_shift/su_max          0.002
_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 0.12411(4) 0.08548(4) 0.90487(10) 0.0745(6) Uani 1 1 d . . . . .
Ni2 Ni 0.09779(4) 0.12361(4) 1.07984(9) 0.0677(6) Uani 1 1 d . . . . .
N1 N 0.1786(3) 0.0977(2) 0.8332(6) 0.086(3) Uani 1 1 d . . . . .
N2 N 0.0990(3) 0.0339(2) 0.8358(6) 0.080(3) Uani 1 1 d . . . . .
O1 O 0.07233(18) 0.08291(18) 0.9860(4) 0.0688(18) Uani 1 1 d . . . . .
O2 O 0.14231(18) 0.13678(18) 0.9818(4) 0.0714(18) Uani 1 1 d . . . . .
O10W O 0.0857(3) 0.1322(2) 0.8306(5) 0.097(2) Uani 1 1 d . . . . .
O11W O 0.16022(19) 0.03394(19) 0.9726(5) 0.082(2) Uani 1 1 d . . . . .
O20W O 0.0559(2) 0.1775(2) 1.0453(5) 0.087(2) Uani 1 1 d . . . . .
O21W O 0.13932(19) 0.06974(19) 1.1202(5) 0.0733(19) Uani 1 1 d . . . . .
O30 O 0.1402(2) 0.29996(19) 1.0812(4) 0.0687(18) Uani 1 1 d . . . . .
O31 O 0.1996(2) 0.33128(19) 1.0119(5) 0.083(2) Uani 1 1 d . . . . .
O40 O -0.08507(19) 0.11957(17) 1.0876(4) 0.0690(18) Uani 1 1 d . . . . .
O41 O -0.12578(19) 0.05742(18) 1.0501(5) 0.0734(19) Uani 1 1 d . . . . .
C1 C 0.1602(3) 0.1754(3) 0.9558(7) 0.070(3) Uani 1 1 d . . . . .
C2 C 0.1553(3) 0.2170(3) 0.9991(7) 0.070(3) Uani 1 1 d . . . . .
H2 H 0.1371 0.2179 1.0478 0.084 Uiso 1 1 calc R U . . .
C3 C 0.1763(3) 0.2566(3) 0.9724(8) 0.077(3) Uani 1 1 d . . . . .
C30 C 0.1716(3) 0.2992(3) 1.0257(7) 0.072(3) Uani 1 1 d . . . . .
C4 C 0.2029(4) 0.2573(3) 0.9020(8) 0.093(4) Uani 1 1 d . . . . .
H4 H 0.2165 0.2849 0.8837 0.111 Uiso 1 1 calc R U . . .
C5 C 0.2095(4) 0.2183(4) 0.8592(9) 0.109(4) Uani 1 1 d . . . . .
H5 H 0.2287 0.2184 0.8118 0.131 Uiso 1 1 calc R U . . .
C6 C 0.1878(4) 0.1766(3) 0.8845(9) 0.094(4) Uani 1 1 d . . . . .
C7 C 0.1983(4) 0.1365(4) 0.8288(8) 0.100(4) Uani 1 1 d . . . . .
H7 H 0.2212 0.1404 0.7877 0.120 Uiso 1 1 calc R U . . .
C8 C 0.1976(4) 0.0625(4) 0.7829(9) 0.105(4) Uani 1 1 d . . . . .
H8A H 0.2125 0.0394 0.8186 0.126 Uiso 1 1 calc R U . . .
H8B H 0.2209 0.0755 0.7454 0.126 Uiso 1 1 calc R U . . .
C9 C 0.1592(5) 0.0397(4) 0.7309(10) 0.115(5) Uani 1 1 d . . . . .
H9A H 0.1404 0.0638 0.7051 0.138 Uiso 1 1 calc R U . . .
H9B H 0.1732 0.0218 0.6857 0.138 Uiso 1 1 calc R U . . .
C10 C 0.1292(4) 0.0096(3) 0.7796(8) 0.089(3) Uani 1 1 d . . . . .
H10C H 0.1106 -0.0089 0.7409 0.107 Uiso 1 1 calc R U . . .
H10D H 0.1483 -0.0117 0.8123 0.107 Uiso 1 1 calc R U . . .
C11 C 0.0579(3) 0.0211(3) 0.8435(7) 0.080(3) Uani 1 1 d . . . . .
H11 H 0.0488 -0.0032 0.8083 0.096 Uiso 1 1 calc R U . . .
C12 C 0.0226(3) 0.0386(3) 0.8992(7) 0.071(3) Uani 1 1 d . . . . .
C13 C 0.0303(3) 0.0681(3) 0.9666(7) 0.067(3) Uani 1 1 d . . . . .
C14 C -0.0072(3) 0.0822(3) 1.0131(6) 0.063(3) Uani 1 1 d . . . . .
H14 H -0.0027 0.1031 1.0573 0.076 Uiso 1 1 calc R U . . .
C15 C -0.0502(3) 0.0667(3) 0.9968(7) 0.064(3) Uani 1 1 d . . . . .
C150 C -0.0895(3) 0.0821(3) 1.0485(7) 0.067(3) Uani 1 1 d . . . . .
C16 C -0.0579(3) 0.0364(3) 0.9313(7) 0.070(3) Uani 1 1 d . . . . .
H16 H -0.0876 0.0250 0.9204 0.084 Uiso 1 1 calc R U . . .
C17 C -0.0215(3) 0.0235(3) 0.8829(8) 0.075(3) Uani 1 1 d . . . . .
H17 H -0.0266 0.0038 0.8371 0.090 Uiso 1 1 calc R U . . .
O1S O 0.0140(6) 0.1778(5) 0.8942(13) 0.112(6) Uani 0.5 1 d . . P A 1
C1S C -0.0244(11) 0.1601(10) 0.8780(17) 0.108(8) Uiso 0.5 1 d . . P A 1
O2S O -0.0670(10) 0.2633(18) 0.8780(18) 0.26(2) Uani 0.5 1 d . . P B 2
C2S C -0.0654(9) 0.2255(15) 0.864(5) 0.26(4) Uani 0.5 1 d . . P B 2
O3S O -0.0622(7) 0.1798(10) 0.874(2) 0.183(11) Uani 0.5 1 d . . P C 3
C3S C -0.1002(10) 0.1603(10) 0.8673(17) 0.109(8) Uiso 0.5 1 d . . P C 3
O4S O 0.3122(15) 0.0726(16) 0.675(3) 0.126(13) Uiso 0.25 1 d . . P D 4
C4S C 0.3369(17) 0.0811(17) 0.738(3) 0.095(14) Uiso 0.25 1 d . . P D 4
O1W O 0.1083(14) 0.1646(18) 0.6795(17) 0.22(2) Uani 0.4 1 d . . P E 5
O1W' O 0.1287(19) 0.1822(18) 0.662(4) 0.109(17) Uiso 0.2 1 d . . P F 6
O2W O 0.2994(15) 0.0501(16) 0.640(3) 0.104(13) Uiso 0.2 1 d . . P G 7
O3W O 0.1540(15) 0.2463(17) 0.637(3) 0.105(13) Uiso 0.2 1 d . . P H 8
O3W' O 0.160(3) 0.303(3) 0.665(5) 0.09(2) Uiso 0.1 1 d . . P I 9
O3W" O 0.161(2) 0.277(2) 0.612(4) 0.102(17) Uiso 0.15 1 d . . P J 10
03W3 O 0.166(2) 0.248(2) 0.570(4) 0.071(18) Uiso 0.1 1 d . . P K 11
O4W O 0.2353(17) 0.1403(10) 0.6107(19) 0.169(20) Uani 0.3 1 d . . P L 12
O4W' O 0.2873(16) 0.1209(16) 0.656(3) 0.112(14) Uiso 0.2 1 d . . P M 13
O4W" O 0.3032(19) 0.1321(19) 0.743(4) 0.106(16) Uiso 0.15 1 d . . P N 14
O5W O -0.0516(7) 0.2277(7) 1.0635(15) 0.141(7) Uani 0.5 1 d . . P O 15
O5W' O -0.0366(10) 0.1919(12) 1.048(2) 0.111(9) Uiso 0.3 1 d . . P P 16
O5W" O -0.0487(14) 0.2057(14) 0.974(3) 0.096(11) Uiso 0.2 1 d . . P Q 17


_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 N1 2.004(8) . ?
Ni1 O1 2.006(6) . ?
Ni1 N2 2.020(9) . ?
Ni1 O2 2.022(6) . ?
Ni1 O10W 2.140(7) . ?
Ni1 O11W 2.146(7) . ?
Ni2 O40 2.039(6) 16_557 ?
Ni2 O30 2.047(7) 15_557 ?
Ni2 O1 2.067(6) . ?
Ni2 O20W 2.078(6) . ?
Ni2 O2 2.086(6) . ?
Ni2 O21W 2.100(6) . ?
N1 C7 1.281(12) . ?
N1 C8 1.427(13) . ?
N2 C11 1.268(12) . ?
N2 C10 1.454(13) . ?
O1 C13 1.344(10) . ?
O2 C1 1.317(10) . ?
O30 C30 1.284(12) . ?
O30 Ni2 2.047(7) 16_557 ?
O31 C30 1.271(10) . ?
O40 C150 1.274(10) . ?
O40 Ni2 2.039(6) 15_557 ?
O41 C150 1.288(10) . ?
C1 C6 1.406(15) . ?
C1 C2 1.416(12) . ?
C2 C3 1.384(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(15) . ?
C3 C30 1.523(14) . ?
C4 C5 1.350(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.439(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.512(15) . ?
C7 H7 0.9500 . ?
C8 C9 1.557(18) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.473(15) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C11 C12 1.465(14) . ?
C11 H11 0.9500 . ?
C12 C17 1.395(12) . ?
C12 C13 1.406(13) . ?
C13 C14 1.395(13) . ?
C14 C15 1.368(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.398(13) . ?
C15 C150 1.493(13) . ?
C16 C17 1.375(13) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
O1S C1S 1.27(3) . ?
O2S C2S 1.13(6) . ?
O3S C3S 1.26(3) . ?
O4S C4S 1.27(5) . ?

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 Ni1 O1 170.5(3) . . ?
N1 Ni1 N2 96.2(3) . . ?
O1 Ni1 N2 93.1(3) . . ?
N1 Ni1 O2 90.5(3) . . ?
O1 Ni1 O2 80.1(2) . . ?
N2 Ni1 O2 173.2(3) . . ?
N1 Ni1 O10W 89.0(4) . . ?
O1 Ni1 O10W 89.4(3) . . ?
N2 Ni1 O10W 88.9(3) . . ?
O2 Ni1 O10W 90.3(3) . . ?
N1 Ni1 O11W 91.5(3) . . ?
O1 Ni1 O11W 90.9(3) . . ?
N2 Ni1 O11W 86.1(3) . . ?
O2 Ni1 O11W 94.8(3) . . ?
O10W Ni1 O11W 174.9(3) . . ?
O40 Ni2 O30 89.0(3) 16_557 15_557 ?
O40 Ni2 O1 172.2(2) 16_557 . ?
O30 Ni2 O1 98.6(2) 15_557 . ?
O40 Ni2 O20W 90.0(3) 16_557 . ?
O30 Ni2 O20W 86.1(3) 15_557 . ?
O1 Ni2 O20W 91.7(3) . . ?
O40 Ni2 O2 95.1(2) 16_557 . ?
O30 Ni2 O2 175.2(3) 15_557 . ?
O1 Ni2 O2 77.3(2) . . ?
O20W Ni2 O2 91.5(3) . . ?
O40 Ni2 O21W 88.5(2) 16_557 . ?
O30 Ni2 O21W 91.9(3) 15_557 . ?
O1 Ni2 O21W 90.1(2) . . ?
O20W Ni2 O21W 177.5(3) . . ?
O2 Ni2 O21W 90.6(2) . . ?
C7 N1 C8 115.8(9) . . ?
C7 N1 Ni1 123.5(8) . . ?
C8 N1 Ni1 120.7(6) . . ?
C11 N2 C10 119.7(9) . . ?
C11 N2 Ni1 121.0(7) . . ?
C10 N2 Ni1 119.3(7) . . ?
C13 O1 Ni1 123.7(6) . . ?
C13 O1 Ni2 133.6(6) . . ?
Ni1 O1 Ni2 100.4(2) . . ?
C1 O2 Ni1 123.4(7) . . ?
C1 O2 Ni2 130.5(6) . . ?
Ni1 O2 Ni2 99.3(2) . . ?
C30 O30 Ni2 129.9(6) . 16_557 ?
C150 O40 Ni2 131.9(6) . 15_557 ?
O2 C1 C6 120.8(8) . . ?
O2 C1 C2 123.1(9) . . ?
C6 C1 C2 116.0(8) . . ?
C3 C2 C1 121.8(10) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 121.4(9) . . ?
C4 C3 C30 120.3(9) . . ?
C2 C3 C30 118.2(10) . . ?
O31 C30 O30 125.1(9) . . ?
O31 C30 C3 116.7(10) . . ?
O30 C30 C3 118.2(8) . . ?
C5 C4 C3 119.2(10) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 121.0(12) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 120.6(10) . . ?
C1 C6 C7 125.6(9) . . ?
C5 C6 C7 113.8(11) . . ?
N1 C7 C6 124.5(10) . . ?
N1 C7 H7 117.7 . . ?
C6 C7 H7 117.7 . . ?
N1 C8 C9 109.4(9) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C10 C9 C8 113.9(13) . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N2 C10 C9 113.6(8) . . ?
N2 C10 H10C 108.8 . . ?
C9 C10 H10C 108.8 . . ?
N2 C10 H10D 108.8 . . ?
C9 C10 H10D 108.8 . . ?
H10C C10 H10D 107.7 . . ?
N2 C11 C12 128.9(10) . . ?
N2 C11 H11 115.5 . . ?
C12 C11 H11 115.5 . . ?
C17 C12 C13 119.4(9) . . ?
C17 C12 C11 115.5(9) . . ?
C13 C12 C11 125.1(8) . . ?
O1 C13 C14 120.2(9) . . ?
O1 C13 C12 121.8(8) . . ?
C14 C13 C12 118.0(8) . . ?
C15 C14 C13 121.8(9) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C14 C15 C16 120.3(9) . . ?
C14 C15 C150 120.3(9) . . ?
C16 C15 C150 119.3(8) . . ?
O40 C150 O41 124.1(8) . . ?
O40 C150 C15 117.3(8) . . ?
O41 C150 C15 118.6(8) . . ?
C17 C16 C15 118.5(8) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C12 121.8(10) . . ?
C16 C17 H17 119.1 . . ?
C12 C17 H17 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C1 C6 -31.5(12) . . . . ?
Ni2 O2 C1 C6 -176.4(8) . . . . ?
Ni1 O2 C1 C2 152.1(7) . . . . ?
Ni2 O2 C1 C2 7.2(14) . . . . ?
O2 C1 C2 C3 176.8(9) . . . . ?
C6 C1 C2 C3 0.3(15) . . . . ?
C1 C2 C3 C4 0.3(16) . . . . ?
C1 C2 C3 C30 -176.3(8) . . . . ?
Ni2 O30 C30 O31 -4.9(14) 16_557 . . . ?
Ni2 O30 C30 C3 174.3(6) 16_557 . . . ?
C4 C3 C30 O31 -13.7(14) . . . . ?
C2 C3 C30 O31 163.0(9) . . . . ?
C4 C3 C30 O30 167.0(9) . . . . ?
C2 C3 C30 O30 -16.3(13) . . . . ?
C2 C3 C4 C5 -1.6(18) . . . . ?
C30 C3 C4 C5 175.0(11) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
O2 C1 C6 C5 -176.3(11) . . . . ?
C2 C1 C6 C5 0.3(17) . . . . ?
O2 C1 C6 C7 2.9(18) . . . . ?
C2 C1 C6 C7 179.5(11) . . . . ?
C4 C5 C6 C1 -2(2) . . . . ?
C4 C5 C6 C7 179.1(13) . . . . ?
C8 N1 C7 C6 -171.7(12) . . . . ?
Ni1 N1 C7 C6 8.5(19) . . . . ?
C1 C6 C7 N1 10(2) . . . . ?
C5 C6 C7 N1 -171.0(13) . . . . ?
C7 N1 C8 C9 -129.2(13) . . . . ?
Ni1 N1 C8 C9 50.6(14) . . . . ?
N1 C8 C9 C10 -74.1(13) . . . . ?
C11 N2 C10 C9 138.7(12) . . . . ?
Ni1 N2 C10 C9 -44.4(14) . . . . ?
C8 C9 C10 N2 71.5(14) . . . . ?
C10 N2 C11 C12 176.2(10) . . . . ?
Ni1 N2 C11 C12 -0.6(16) . . . . ?
N2 C11 C12 C17 168.5(11) . . . . ?
N2 C11 C12 C13 -12.7(18) . . . . ?
Ni1 O1 C13 C14 -156.2(7) . . . . ?
Ni2 O1 C13 C14 3.1(13) . . . . ?
Ni1 O1 C13 C12 23.0(11) . . . . ?
Ni2 O1 C13 C12 -177.7(6) . . . . ?
C17 C12 C13 O1 178.7(8) . . . . ?
C11 C12 C13 O1 -0.1(15) . . . . ?
C17 C12 C13 C14 -2.1(13) . . . . ?
C11 C12 C13 C14 179.2(9) . . . . ?
O1 C13 C14 C15 -178.0(8) . . . . ?
C12 C13 C14 C15 2.8(14) . . . . ?
C13 C14 C15 C16 -1.0(14) . . . . ?
C13 C14 C15 C150 179.3(8) . . . . ?
Ni2 O40 C150 O41 5.4(15) 15_557 . . . ?
Ni2 O40 C150 C15 -175.6(6) 15_557 . . . ?
C14 C15 C150 O40 22.5(13) . . . . ?
C16 C15 C150 O40 -157.2(8) . . . . ?
C14 C15 C150 O41 -158.4(9) . . . . ?
C16 C15 C150 O41 21.9(13) . . . . ?
C14 C15 C16 C17 -1.5(14) . . . . ?
C150 C15 C16 C17 178.2(9) . . . . ?
C15 C16 C17 C12 2.1(15) . . . . ?
C13 C12 C17 C16 -0.3(15) . . . . ?
C11 C12 C17 C16 178.5(9) . . . . ?

_refine_diff_density_max         0.978
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.167

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1486104'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT214_2                   
;
PROBLEM: Atom O60     (Anion/Solvent) ADP max/min Ratio          6.6 prolat
RESPONSE: It is due to the disorder of the perchlorate anion
;
_vrf_PLAT355_2                   
;
PROBLEM: Long    O-H (X0.82,N0.98A)  O2S    -   H2S    ..       1.11 Ang.
RESPONSE: This H atom was found in the map
;
# Added during the CSD deposition process: Wednesday 13 July 2016 05:00 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H48 Cu4 N4 O18, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C43 H56 Cl2 Cu4 N4 O28'
_chemical_formula_weight         1401.97

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'
Cu Cu 0.3201 1.2651 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, 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                   19.0860(16)
_cell_length_b                   18.0840(17)
_cell_length_c                   15.8470(15)
_cell_angle_alpha                90
_cell_angle_beta                 107.522(4)
_cell_angle_gamma                90
_cell_volume                     5215.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2898
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      22.71

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_F_000             2864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.809
_shelx_estimated_absorpt_T_min   0.641
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.7586
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS 2014/2 (Bruker,2014)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25693
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.587
_diffrn_reflns_theta_max         24.405
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.898
_reflns_number_total             4231
_reflns_number_gt                2858
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        ?
_computing_structure_solution    'SIR-2008 (Burla, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0765P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4231
_refine_ls_number_parameters     420
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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_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
Cu1 Cu 0.62740(4) 0.21949(4) 0.59237(4) 0.0208(2) Uani 1 1 d . . . . .
N1 N 0.6932(2) 0.2345(2) 0.7135(3) 0.0216(11) Uani 1 1 d . . . . .
N2 N 0.6436(2) 0.1129(2) 0.5819(3) 0.0193(11) Uani 1 1 d . . . . .
O1 O 0.6050(2) 0.3247(2) 0.5796(2) 0.0303(11) Uani 1 1 d . . . . .
O2 O 0.5555(2) 0.22091(19) 0.4729(2) 0.0188(9) Uani 1 1 d . . . . .
O1W O 0.7283(4) 0.2430(4) 0.5346(5) 0.026(2) Uani 0.5 1 d . . P A 1
H1W1 H 0.7323 0.2089 0.4989 0.031 Uiso 0.5 1 d R U P A 1
H1W2 H 0.7647 0.2658 0.5632 0.031 Uiso 0.5 1 d R U P A 1
O1S O 0.5334(15) 0.184(2) 0.6605(18) 0.015(11) Uiso 0.18(3) 1 d . . P A 2
H1S H 0.4973 0.1827 0.6090 0.018 Uiso 0.5 1 d R U P A 2
C1S C 0.5196(9) 0.2065(10) 0.7337(12) 0.074(6) Uani 0.5 1 d . . P A 2
H1S1 H 0.5225 0.1642 0.7732 0.110 Uiso 0.5 1 calc R U P A 2
H1S2 H 0.4703 0.2281 0.7183 0.110 Uiso 0.5 1 calc R U P A 2
H1S3 H 0.5559 0.2438 0.7634 0.110 Uiso 0.5 1 calc R U P A 2
O1S' O 0.5209(9) 0.2154(17) 0.6457(11) 0.031(6) Uiso 0.32(3) 1 d . . P A 3
Cu2 Cu 0.52711(4) 0.32290(4) 0.44251(4) 0.0194(2) Uani 1 1 d . . . . .
O2W O 0.6001(2) 0.3261(2) 0.3760(2) 0.0210(9) Uani 1 1 d . . . . .
H2W2 H 0.5852 0.3549 0.3211 0.025 Uiso 1 1 d R U . . .
H2W1 H 0.6113 0.2784 0.3642 0.025 Uiso 1 1 d R U . . .
O2S O 0.4369(3) 0.3055(2) 0.4780(3) 0.0440(13) Uani 1 1 d . . . . .
H2S H 0.4387 0.2479 0.5025 0.053 Uiso 1 1 d R U . . .
C2S C 0.3950(4) 0.3558(4) 0.5087(6) 0.061(2) Uani 1 1 d . . . . .
H2S1 H 0.4226 0.3717 0.5687 0.091 Uiso 1 1 calc R U . . .
H2S2 H 0.3490 0.3323 0.5098 0.091 Uiso 1 1 calc R U . . .
H2S3 H 0.3839 0.3989 0.4694 0.091 Uiso 1 1 calc R U . . .
C1 C 0.6075(3) 0.3731(3) 0.6437(3) 0.0184(13) Uani 1 1 d . . . . .
C2 C 0.5725(3) 0.4407(3) 0.6236(4) 0.0213(14) Uani 1 1 d . . . . .
H2 H 0.5441 0.4507 0.5643 0.026 Uiso 1 1 calc R U . . .
C3 C 0.5779(3) 0.4940(3) 0.6878(4) 0.0172(13) Uani 1 1 d . . . . .
C30 C 0.5457(3) 0.5694(3) 0.6622(4) 0.0191(13) Uani 1 1 d . . . . .
O31 O 0.4981(2) 0.5756(2) 0.5855(2) 0.0213(9) Uani 1 1 d . . . . .
O32 O 0.56615(19) 0.6226(2) 0.7126(2) 0.0205(9) Uani 1 1 d . . . . .
C4 C 0.6192(3) 0.4800(3) 0.7750(4) 0.0200(13) Uani 1 1 d . . . . .
H4 H 0.6232 0.5165 0.8194 0.024 Uiso 1 1 calc R U . . .
C5 C 0.6537(3) 0.4141(3) 0.7961(4) 0.0204(13) Uani 1 1 d . . . . .
H5 H 0.6817 0.4048 0.8557 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6491(3) 0.3588(3) 0.7318(4) 0.0185(13) Uani 1 1 d . . . . .
C7 C 0.6917(3) 0.2928(3) 0.7597(4) 0.0204(14) Uani 1 1 d . . . . .
H7 H 0.7224 0.2920 0.8193 0.024 Uiso 1 1 calc R U . . .
C8 C 0.7476(3) 0.1766(3) 0.7593(4) 0.0279(15) Uani 1 1 d . . . . .
H8A H 0.7922 0.1810 0.7400 0.033 Uiso 1 1 calc R U . . .
H8B H 0.7622 0.1853 0.8240 0.033 Uiso 1 1 calc R U . . .
C9 C 0.7175(3) 0.1005(3) 0.7403(4) 0.0283(15) Uani 1 1 d . . . . .
H9A H 0.6698 0.0982 0.7531 0.034 Uiso 1 1 calc R U . . .
H9B H 0.7514 0.0655 0.7806 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7061(3) 0.0761(3) 0.6472(4) 0.0292(15) Uani 1 1 d . . . . .
H10A H 0.7515 0.0861 0.6311 0.035 Uiso 1 1 calc R U . . .
H10B H 0.6978 0.0220 0.6436 0.035 Uiso 1 1 calc R U . . .
C11 C 0.6050(3) 0.0702(3) 0.5203(4) 0.0240(14) Uani 1 1 d . . . . .
H11 H 0.6182 0.0194 0.5245 0.029 Uiso 1 1 calc R U . . .
C12 C 0.5434(3) 0.0914(3) 0.4452(4) 0.0203(13) Uani 1 1 d . . . . .
C13 C 0.5217(3) 0.1649(3) 0.4218(4) 0.0193(14) Uani 1 1 d . . . . .
C14 C 0.4633(3) 0.1781(3) 0.3461(3) 0.0161(12) Uani 1 1 d . . . . .
H14 H 0.4486 0.2275 0.3293 0.019 Uiso 1 1 calc R U . . .
C15 C 0.4263(3) 0.1202(3) 0.2952(4) 0.0190(13) Uani 1 1 d . . . . .
C150 C 0.3638(3) 0.1373(3) 0.2144(4) 0.0198(13) Uani 1 1 d . . . . .
O151 O 0.3516(2) 0.1985(2) 0.1815(3) 0.0253(10) Uani 1 1 d . . . . .
O152 O 0.3234(2) 0.0791(2) 0.1822(3) 0.0335(11) Uani 1 1 d . . . . .
H152 H 0.2864 0.0831 0.1243 0.050 Uiso 1 1 d R U . . .
C16 C 0.4468(3) 0.0476(3) 0.3183(4) 0.0256(14) Uani 1 1 d . . . . .
H16 H 0.4204 0.0080 0.2837 0.031 Uiso 1 1 calc R U . . .
C17 C 0.5055(3) 0.0335(3) 0.3915(4) 0.0237(14) Uani 1 1 d . . . . .
H17 H 0.5207 -0.0161 0.4060 0.028 Uiso 1 1 calc R U . . .
Cl1 Cl 0.34526(10) 0.14544(11) 0.53149(13) 0.0474(5) Uani 1 1 d . . . . .
O60 O 0.3129(14) 0.1977(13) 0.5615(16) 0.116(10) Uani 0.622(10) 1 d . . P B 2
O61 O 0.4208(6) 0.1664(6) 0.5448(8) 0.052(3) Uani 0.622(10) 1 d . . P B 2
O62 O 0.3514(4) 0.0787(4) 0.5941(5) 0.045(3) Uani 0.622(10) 1 d . . P B 2
O63 O 0.3166(6) 0.1194(5) 0.4478(5) 0.067(3) Uani 0.622(10) 1 d . . P B 2
O60' O 0.4145(10) 0.1201(11) 0.5357(12) 0.056(5) Uani 0.378(10) 1 d . . P B 3
O61' O 0.2850(9) 0.1029(10) 0.5078(14) 0.095(7) Uani 0.378(10) 1 d . . P B 3
O62' O 0.3319(8) 0.1972(10) 0.4395(9) 0.072(6) Uani 0.378(10) 1 d . . P B 3
O63' O 0.333(2) 0.2062(18) 0.5852(18) 0.084(12) Uani 0.378(10) 1 d . . P B 3
O3S O 0.2252(2) 0.1005(2) 0.0326(3) 0.0345(11) Uani 1 1 d . . . C 3
H3S H 0.1916 0.1311 0.0302 0.052 Uiso 1 1 calc R U . C 3
C3S C 0.1943(4) 0.0294(4) 0.0111(4) 0.0452(19) Uani 1 1 d . . . C 3
H3S1 H 0.1992 0.0015 0.0656 0.068 Uiso 1 1 calc R U . C 3
H3S2 H 0.2202 0.0033 -0.0249 0.068 Uiso 1 1 calc R U . C 3
H3S3 H 0.1422 0.0341 -0.0224 0.068 Uiso 1 1 calc R U . C 3


_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
Cu1 O1 1.948(4) . ?
Cu1 N2 1.968(5) . ?
Cu1 N1 1.971(5) . ?
Cu1 O2 1.976(4) . ?
Cu1 O1W 2.405(7) . ?
Cu1 O1S' 2.427(14) . ?
N1 C7 1.289(7) . ?
N1 C8 1.500(7) . ?
N2 C11 1.288(7) . ?
N2 C10 1.481(7) . ?
O1 C1 1.331(6) . ?
O1 Cu2 2.233(4) . ?
O2 C13 1.335(6) . ?
O2 Cu2 1.942(4) . ?
O1W H1W1 0.8553 . ?
O1W H1W2 0.8175 . ?
O1S C1S 1.33(2) . ?
O1S H1S 0.8962 . ?
C1S O1S' 1.41(2) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O1S' H1S 0.8569 . ?
Cu2 O31 1.915(4) 5_666 ?
Cu2 O2W 1.985(4) . ?
Cu2 O2S 1.992(4) . ?
O2W H2W2 0.9807 . ?
O2W H2W1 0.9207 . ?
O2S C2S 1.392(7) . ?
O2S H2S 1.1083 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C1 C2 1.383(7) . ?
C1 C6 1.406(7) . ?
C2 C3 1.383(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(7) . ?
C3 C30 1.499(7) . ?
C30 O32 1.236(6) . ?
C30 O31 1.285(6) . ?
O31 Cu2 1.915(4) 5_666 ?
C4 C5 1.354(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.411(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.438(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.487(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.492(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.449(8) . ?
C11 H11 0.9500 . ?
C12 C17 1.405(8) . ?
C12 C13 1.409(8) . ?
C13 C14 1.391(8) . ?
C14 C15 1.379(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(8) . ?
C15 C150 1.495(8) . ?
C150 O151 1.217(6) . ?
C150 O152 1.314(6) . ?
O152 H152 0.9773 . ?
C16 C17 1.372(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
Cl1 O60 1.296(16) . ?
Cl1 O61' 1.340(15) . ?
Cl1 O63 1.358(8) . ?
Cl1 O60' 1.380(16) . ?
Cl1 O61 1.444(10) . ?
Cl1 O63' 1.45(3) . ?
Cl1 O62 1.544(7) . ?
Cl1 O62' 1.685(15) . ?
O3S C3S 1.412(7) . ?
O3S H3S 0.8400 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N2 169.71(18) . . ?
O1 Cu1 N1 91.29(17) . . ?
N2 Cu1 N1 98.42(18) . . ?
O1 Cu1 O2 79.64(15) . . ?
N2 Cu1 O2 90.78(17) . . ?
N1 Cu1 O2 170.61(17) . . ?
O1 Cu1 O1W 87.9(2) . . ?
N2 Cu1 O1W 88.7(2) . . ?
N1 Cu1 O1W 89.9(2) . . ?
O2 Cu1 O1W 92.2(2) . . ?
O1 Cu1 O1S' 83.4(8) . . ?
N2 Cu1 O1S' 99.7(7) . . ?
N1 Cu1 O1S' 91.1(4) . . ?
O2 Cu1 O1S' 85.5(4) . . ?
C7 N1 C8 115.3(5) . . ?
C7 N1 Cu1 123.3(4) . . ?
C8 N1 Cu1 121.4(4) . . ?
C11 N2 C10 114.7(5) . . ?
C11 N2 Cu1 125.6(4) . . ?
C10 N2 Cu1 119.7(4) . . ?
C1 O1 Cu1 127.4(3) . . ?
C1 O1 Cu2 127.8(3) . . ?
Cu1 O1 Cu2 98.49(16) . . ?
C13 O2 Cu2 121.5(3) . . ?
C13 O2 Cu1 129.9(3) . . ?
Cu2 O2 Cu1 108.15(17) . . ?
Cu1 O1W H1W1 111.5 . . ?
Cu1 O1W H1W2 121.5 . . ?
H1W1 O1W H1W2 120.0 . . ?
C1S O1S H1S 120.3 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
H1S O1S' C1S 115.6 . . ?
H1S O1S' Cu1 96.2 . . ?
C1S O1S' Cu1 127.8(13) . . ?
O31 Cu2 O2 178.34(16) 5_666 . ?
O31 Cu2 O2W 90.93(15) 5_666 . ?
O2 Cu2 O2W 88.36(15) . . ?
O31 Cu2 O2S 92.24(17) 5_666 . ?
O2 Cu2 O2S 88.85(17) . . ?
O2W Cu2 O2S 163.70(18) . . ?
O31 Cu2 O1 104.98(15) 5_666 . ?
O2 Cu2 O1 73.64(14) . . ?
O2W Cu2 O1 98.51(15) . . ?
O2S Cu2 O1 96.09(18) . . ?
Cu2 O2W H2W2 115.1 . . ?
Cu2 O2W H2W1 108.9 . . ?
H2W2 O2W H2W1 109.9 . . ?
C2S O2S Cu2 129.2(5) . . ?
C2S O2S H2S 117.0 . . ?
Cu2 O2S H2S 107.9 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
O1 C1 C2 120.0(5) . . ?
O1 C1 C6 121.1(5) . . ?
C2 C1 C6 118.8(5) . . ?
C1 C2 C3 121.5(5) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 C30 120.1(5) . . ?
C4 C3 C30 119.8(5) . . ?
O32 C30 O31 122.6(5) . . ?
O32 C30 C3 120.6(5) . . ?
O31 C30 C3 116.8(5) . . ?
C30 O31 Cu2 111.1(3) . 5_666 ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.8(5) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 118.6(5) . . ?
C1 C6 C7 123.8(5) . . ?
C5 C6 C7 117.4(5) . . ?
N1 C7 C6 127.7(5) . . ?
N1 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
C9 C8 N1 112.2(5) . . ?
C9 C8 H8A 109.2 . . ?
N1 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
N1 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 C10 114.0(5) . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.6 . . ?
N2 C10 C9 113.8(5) . . ?
N2 C10 H10A 108.8 . . ?
C9 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 C12 127.0(5) . . ?
N2 C11 H11 116.5 . . ?
C12 C11 H11 116.5 . . ?
C17 C12 C13 119.2(5) . . ?
C17 C12 C11 116.3(5) . . ?
C13 C12 C11 124.5(5) . . ?
O2 C13 C14 120.6(5) . . ?
O2 C13 C12 120.4(5) . . ?
C14 C13 C12 119.0(5) . . ?
C15 C14 C13 120.8(5) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.6(5) . . ?
C14 C15 C150 118.7(5) . . ?
C16 C15 C150 120.7(5) . . ?
O151 C150 O152 123.2(5) . . ?
O151 C150 C15 123.8(5) . . ?
O152 C150 C15 113.0(5) . . ?
C150 O152 H152 118.6 . . ?
C17 C16 C15 119.6(6) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C12 120.9(5) . . ?
C16 C17 H17 119.6 . . ?
C12 C17 H17 119.6 . . ?
O60 Cl1 O63 121.0(13) . . ?
O61' Cl1 O60' 123.4(12) . . ?
O60 Cl1 O61 108.7(13) . . ?
O63 Cl1 O61 109.0(7) . . ?
O61' Cl1 O63' 108.8(19) . . ?
O60' Cl1 O63' 123.0(19) . . ?
O60 Cl1 O62 106.7(11) . . ?
O63 Cl1 O62 106.7(5) . . ?
O61 Cl1 O62 103.4(5) . . ?
O61' Cl1 O62' 100.5(11) . . ?
O60' Cl1 O62' 96.9(10) . . ?
O63' Cl1 O62' 94.4(12) . . ?
C3S O3S H3S 109.5 . . ?
O3S C3S H3S1 109.5 . . ?
O3S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
O3S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1S C1S O1S' H1S 57.3 . . . . ?
O1S C1S O1S' Cu1 -64(3) . . . . ?
Cu1 O1 C1 C2 -163.4(4) . . . . ?
Cu2 O1 C1 C2 -17.5(7) . . . . ?
Cu1 O1 C1 C6 20.6(7) . . . . ?
Cu2 O1 C1 C6 166.5(4) . . . . ?
O1 C1 C2 C3 -175.9(5) . . . . ?
C6 C1 C2 C3 0.2(8) . . . . ?
C1 C2 C3 C4 -0.1(8) . . . . ?
C1 C2 C3 C30 173.8(5) . . . . ?
C2 C3 C30 O32 -160.4(5) . . . . ?
C4 C3 C30 O32 13.5(8) . . . . ?
C2 C3 C30 O31 17.8(7) . . . . ?
C4 C3 C30 O31 -168.3(5) . . . . ?
O32 C30 O31 Cu2 6.0(7) . . . 5_666 ?
C3 C30 O31 Cu2 -172.1(4) . . . 5_666 ?
C2 C3 C4 C5 -0.1(8) . . . . ?
C30 C3 C4 C5 -174.0(5) . . . . ?
C3 C4 C5 C6 0.1(8) . . . . ?
O1 C1 C6 C5 175.9(5) . . . . ?
C2 C1 C6 C5 -0.1(8) . . . . ?
O1 C1 C6 C7 0.2(8) . . . . ?
C2 C1 C6 C7 -175.8(5) . . . . ?
C4 C5 C6 C1 0.0(8) . . . . ?
C4 C5 C6 C7 175.9(5) . . . . ?
C8 N1 C7 C6 175.6(5) . . . . ?
Cu1 N1 C7 C6 -6.1(8) . . . . ?
C1 C6 C7 N1 -7.6(9) . . . . ?
C5 C6 C7 N1 176.6(5) . . . . ?
C7 N1 C8 C9 139.6(5) . . . . ?
Cu1 N1 C8 C9 -38.7(6) . . . . ?
N1 C8 C9 C10 69.3(7) . . . . ?
C11 N2 C10 C9 -140.1(5) . . . . ?
Cu1 N2 C10 C9 41.7(6) . . . . ?
C8 C9 C10 N2 -72.1(7) . . . . ?
C10 N2 C11 C12 -176.4(5) . . . . ?
Cu1 N2 C11 C12 1.7(8) . . . . ?
N2 C11 C12 C17 -174.1(6) . . . . ?
N2 C11 C12 C13 8.4(9) . . . . ?
Cu2 O2 C13 C14 -2.0(7) . . . . ?
Cu1 O2 C13 C14 168.7(4) . . . . ?
Cu2 O2 C13 C12 179.9(4) . . . . ?
Cu1 O2 C13 C12 -9.4(7) . . . . ?
C17 C12 C13 O2 178.3(5) . . . . ?
C11 C12 C13 O2 -4.3(8) . . . . ?
C17 C12 C13 C14 0.1(8) . . . . ?
C11 C12 C13 C14 177.6(5) . . . . ?
O2 C13 C14 C15 -177.3(5) . . . . ?
C12 C13 C14 C15 0.9(8) . . . . ?
C13 C14 C15 C16 -0.2(8) . . . . ?
C13 C14 C15 C150 -180.0(5) . . . . ?
C14 C15 C150 O151 13.8(8) . . . . ?
C16 C15 C150 O151 -166.0(5) . . . . ?
C14 C15 C150 O152 -166.4(5) . . . . ?
C16 C15 C150 O152 13.8(7) . . . . ?
C14 C15 C16 C17 -1.5(8) . . . . ?
C150 C15 C16 C17 178.3(5) . . . . ?
C15 C16 C17 C12 2.5(8) . . . . ?
C13 C12 C17 C16 -1.8(8) . . . . ?
C11 C12 C17 C16 -179.4(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W2 O151 0.82 2.19 2.962(8) 156.8 8_556
O1S H1S Cl1 0.90 2.87 3.62(2) 142.8 .
O1S H1S O61 0.90 1.53 2.39(3) 157.7 .
O2W H2W2 O32 0.98 1.70 2.642(5) 160.7 6_565
O2W H2W1 O151 0.92 1.85 2.739(5) 161.8 2_655
O2S H2S O1S' 1.11 2.41 3.12(3) 120.1 .
O2S H2S Cl1 1.11 2.71 3.612(5) 138.6 .
O2S H2S O61 1.11 1.70 2.781(11) 165.0 .
O2S H2S O60' 1.11 2.45 3.54(2) 167.2 .
C2S H2S2 O63' 0.98 2.63 3.33(3) 127.6 .
C2 H2 O31 0.95 2.32 3.193(6) 153.3 5_666
C7 H7 O62' 0.95 2.37 3.274(15) 157.9 8_556
C7 H7 O63' 0.95 2.60 3.07(3) 110.5 2_656
C8 H8B O60 0.99 2.64 3.39(2) 133.1 2_656
C9 H9A O62 0.99 2.60 3.294(9) 127.4 2_656
O152 H152 O3S 0.98 1.60 2.571(6) 172.8 .

_refine_diff_density_max         0.953
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.128

_shelxl_version_number           2013-4

