# 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_918246
_database_code_depnum_ccdc_archive 'CCDC 918246'
_audit_update_record             
;
2015-01-06 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H20 Cl Cu N O4'
_chemical_formula_weight         353.29

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P na 2(1)'
_symmetry_space_group_name_Hall  'P 2c -2n'

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

_cell_length_a                   7.480(9)
_cell_length_b                   15.997(18)
_cell_length_c                   12.467(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1492(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2236
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      25.12

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  '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            6819
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_av_sigmaI/netI    0.1199
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2313
_reflns_number_gt                1649
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.1133P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_number_reflns         2313
_refine_ls_number_parameters     183
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.1968
_refine_ls_wR_factor_gt          0.1605
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.004

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
Cu1 Cu 0.63956(12) 0.70584(4) 0.25504(8) 0.0359(2) Uani 1 1 d . . .
N1 N 0.5397(8) 0.6240(3) 0.3554(5) 0.0310(14) Uani 1 1 d . . .
O1 O 0.7178(8) 0.6021(3) 0.1792(4) 0.0460(15) Uani 1 1 d . . .
H1A H 0.8048 0.5996 0.1393 0.055 Uiso 1 1 calc R . .
O2 O 0.5731(9) 0.8012(3) 0.3386(5) 0.0473(15) Uani 1 1 d . . .
O3 O 0.2154(8) 0.5367(3) 0.2932(4) 0.0449(16) Uani 1 1 d . . .
H3 H 0.2110 0.5851 0.3146 0.067 Uiso 1 1 calc R . .
O4 O 0.4919(7) 0.9032(3) 1.0495(5) 0.0482(15) Uani 1 1 d . . .
H4A H 0.5711 0.8744 1.0760 0.058 Uiso 1 1 calc R . .
Cl1 Cl 0.7972(3) 0.78310(10) 0.13526(17) 0.0391(4) Uani 1 1 d . . .
C1 C 0.4729(10) 0.6430(5) 0.4463(6) 0.039(2) Uani 1 1 d . . .
H1 H 0.4291 0.5991 0.4877 0.047 Uiso 1 1 calc R . .
C2 C 0.4586(10) 0.7267(4) 0.4917(6) 0.0353(19) Uani 1 1 d . . .
C3 C 0.3928(11) 0.7325(6) 0.5976(7) 0.048(2) Uani 1 1 d . . .
H3A H 0.3565 0.6840 0.6324 0.057 Uiso 1 1 calc R . .
C4 C 0.3805(11) 0.8065(5) 0.6504(8) 0.051(2) Uani 1 1 d . . .
H4 H 0.3369 0.8087 0.7202 0.061 Uiso 1 1 calc R . .
C5 C 0.4348(13) 0.8793(6) 0.5978(7) 0.050(2) Uani 1 1 d . . .
H5 H 0.4306 0.9303 0.6335 0.059 Uiso 1 1 calc R . .
C6 C 0.4952(10) 0.8759(5) 0.4918(7) 0.042(2) Uani 1 1 d . . .
H6 H 0.5256 0.9254 0.4572 0.051 Uiso 1 1 calc R . .
C7 C 0.5114(10) 0.8007(5) 0.4365(6) 0.0339(19) Uani 1 1 d . . .
C8 C 0.5446(11) 0.5356(4) 0.3155(6) 0.036(2) Uani 1 1 d . . .
C9 C 0.7159(10) 0.5302(4) 0.2484(8) 0.044(2) Uani 1 1 d . . .
H9A H 0.8201 0.5303 0.2947 0.053 Uiso 1 1 calc R . .
H9B H 0.7166 0.4792 0.2063 0.053 Uiso 1 1 calc R . .
C10 C 0.3808(10) 0.5226(4) 0.2425(7) 0.039(2) Uani 1 1 d . . .
H10A H 0.3906 0.5598 0.1814 0.047 Uiso 1 1 calc R . .
H10B H 0.3828 0.4657 0.2155 0.047 Uiso 1 1 calc R . .
C11 C 0.5455(13) 0.4715(5) 0.4076(7) 0.046(2) Uani 1 1 d . . .
H11A H 0.4342 0.4764 0.4471 0.055 Uiso 1 1 calc R . .
H11B H 0.6421 0.4852 0.4565 0.055 Uiso 1 1 calc R . .
C12 C 0.5681(14) 0.3792(5) 0.3706(8) 0.058(3) Uani 1 1 d . . .
H12A H 0.4755 0.3654 0.3202 0.087 Uiso 1 1 calc R . .
H12B H 0.5600 0.3428 0.4316 0.087 Uiso 1 1 calc R . .
H12C H 0.6827 0.3724 0.3370 0.087 Uiso 1 1 calc R . .
C13 C 0.4448(13) 0.8704(6) 0.9481(9) 0.058(3) Uani 1 1 d . . .
H13A H 0.4252 0.9156 0.8987 0.087 Uiso 1 1 calc R . .
H13B H 0.3373 0.8380 0.9546 0.087 Uiso 1 1 calc R . .
H13C H 0.5397 0.8355 0.9221 0.087 Uiso 1 1 calc R . .


_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 O2 1.912(6) . ?
Cu1 N1 1.959(6) . ?
Cu1 O1 1.997(5) . ?
Cu1 Cl1 2.269(3) . ?
N1 C1 1.276(10) . ?
N1 C8 1.499(9) . ?
O1 C9 1.439(9) . ?
O1 H1A 0.8200 . ?
O2 C7 1.305(10) . ?
O3 C10 1.408(10) . ?
O3 H3 0.8200 . ?
O4 C13 1.413(11) . ?
O4 H4A 0.8200 . ?
C1 C2 1.458(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.413(11) . ?
C2 C7 1.425(10) . ?
C3 C4 1.358(12) . ?
C3 H3A 0.9300 . ?
C4 C5 1.397(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(11) . ?
C6 H6 0.9300 . ?
C8 C9 1.532(12) . ?
C8 C11 1.540(10) . ?
C8 C10 1.540(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.556(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N1 95.0(3) . . ?
O2 Cu1 O1 175.1(3) . . ?
N1 Cu1 O1 81.9(2) . . ?
O2 Cu1 Cl1 93.4(2) . . ?
N1 Cu1 Cl1 169.28(18) . . ?
O1 Cu1 Cl1 89.34(18) . . ?
C1 N1 C8 121.9(6) . . ?
C1 N1 Cu1 123.9(5) . . ?
C8 N1 Cu1 114.2(4) . . ?
C9 O1 Cu1 112.2(5) . . ?
C9 O1 H1A 109.5 . . ?
Cu1 O1 H1A 124.1 . . ?
C7 O2 Cu1 126.6(5) . . ?
C10 O3 H3 109.5 . . ?
C13 O4 H4A 109.5 . . ?
N1 C1 C2 126.3(7) . . ?
N1 C1 H1 116.9 . . ?
C2 C1 H1 116.9 . . ?
C3 C2 C7 119.6(7) . . ?
C3 C2 C1 116.7(7) . . ?
C7 C2 C1 123.8(7) . . ?
C4 C3 C2 122.3(8) . . ?
C4 C3 H3A 118.8 . . ?
C2 C3 H3A 118.8 . . ?
C3 C4 C5 118.6(9) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C6 C5 C4 120.4(8) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C7 C6 C5 122.0(8) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
O2 C7 C6 119.3(7) . . ?
O2 C7 C2 123.7(7) . . ?
C6 C7 C2 117.0(7) . . ?
N1 C8 C9 104.8(6) . . ?
N1 C8 C11 112.4(6) . . ?
C9 C8 C11 111.4(7) . . ?
N1 C8 C10 107.7(6) . . ?
C9 C8 C10 109.6(6) . . ?
C11 C8 C10 110.7(6) . . ?
O1 C9 C8 106.9(5) . . ?
O1 C9 H9A 110.3 . . ?
C8 C9 H9A 110.3 . . ?
O1 C9 H9B 110.3 . . ?
C8 C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
O3 C10 C8 114.4(7) . . ?
O3 C10 H10A 108.7 . . ?
C8 C10 H10A 108.7 . . ?
O3 C10 H10B 108.7 . . ?
C8 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C8 C11 C12 114.3(7) . . ?
C8 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
C8 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4 C13 H13A 109.5 . . ?
O4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
O2 Cu1 N1 C1 -5.0(6) . . . . ?
O1 Cu1 N1 C1 171.2(6) . . . . ?
Cl1 Cu1 N1 C1 135.9(8) . . . . ?
O2 Cu1 N1 C8 173.8(5) . . . . ?
O1 Cu1 N1 C8 -9.9(5) . . . . ?
Cl1 Cu1 N1 C8 -45.2(12) . . . . ?
N1 Cu1 O1 C9 -18.7(5) . . . . ?
Cl1 Cu1 O1 C9 155.1(5) . . . . ?
N1 Cu1 O2 C7 10.0(7) . . . . ?
Cl1 Cu1 O2 C7 -163.3(7) . . . . ?
C8 N1 C1 C2 -178.8(7) . . . . ?
Cu1 N1 C1 C2 0.0(11) . . . . ?
N1 C1 C2 C3 -175.1(8) . . . . ?
N1 C1 C2 C7 3.2(12) . . . . ?
C7 C2 C3 C4 -1.2(12) . . . . ?
C1 C2 C3 C4 177.1(8) . . . . ?
C2 C3 C4 C5 0.1(13) . . . . ?
C3 C4 C5 C6 1.9(14) . . . . ?
C4 C5 C6 C7 -2.9(14) . . . . ?
Cu1 O2 C7 C6 170.2(6) . . . . ?
Cu1 O2 C7 C2 -9.7(11) . . . . ?
C5 C6 C7 O2 -178.2(8) . . . . ?
C5 C6 C7 C2 1.7(12) . . . . ?
C3 C2 C7 O2 -179.8(7) . . . . ?
C1 C2 C7 O2 2.0(12) . . . . ?
C3 C2 C7 C6 0.3(11) . . . . ?
C1 C2 C7 C6 -177.9(7) . . . . ?
C1 N1 C8 C9 -147.4(7) . . . . ?
Cu1 N1 C8 C9 33.7(7) . . . . ?
C1 N1 C8 C11 -26.2(10) . . . . ?
Cu1 N1 C8 C11 154.9(6) . . . . ?
C1 N1 C8 C10 96.0(8) . . . . ?
Cu1 N1 C8 C10 -82.9(6) . . . . ?
Cu1 O1 C9 C8 41.8(7) . . . . ?
N1 C8 C9 O1 -47.2(8) . . . . ?
C11 C8 C9 O1 -168.9(6) . . . . ?
C10 C8 C9 O1 68.2(7) . . . . ?
N1 C8 C10 O3 -58.9(7) . . . . ?
C9 C8 C10 O3 -172.4(5) . . . . ?
C11 C8 C10 O3 64.3(8) . . . . ?
N1 C8 C11 C12 -174.7(7) . . . . ?
C9 C8 C11 C12 -57.4(9) . . . . ?
C10 C8 C11 C12 64.8(9) . . . . ?

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
O3 H3 O2 0.82 2.11 2.860(8) 151.5 4_465

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_110520b
_database_code_depnum_ccdc_archive 'CCDC 918247'
_audit_update_record             
;
2015-01-06 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H50 N2 Ni2 O12'
_chemical_formula_weight         772.16

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2560(10)
_cell_length_b                   11.9039(12)
_cell_length_c                   15.3331(16)
_cell_angle_alpha                90.2240(10)
_cell_angle_beta                 97.4350(10)
_cell_angle_gamma                104.270(2)
_cell_volume                     1797.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2865
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      25.44

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  '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            9307
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         25.02
_reflns_number_total             6244
_reflns_number_gt                4157
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0607P)²+1.2043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6244
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1313
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.014
_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
Ni1 Ni 0.09491(5) 0.97557(4) 0.08121(3) 0.03303(17) Uani 1 1 d . . .
Ni2 Ni 0.06153(5) 0.40125(4) 0.53822(3) 0.02944(16) Uani 1 1 d . . .
N1 N 0.2902(4) 1.0461(3) 0.1292(2) 0.0351(8) Uani 1 1 d . . .
N2 N 0.1928(3) 0.3177(3) 0.4976(2) 0.0314(8) Uani 1 1 d . . .
O1 O 0.1135(3) 0.8678(2) 0.18674(17) 0.0371(7) Uani 1 1 d . . .
H1 H 0.0900 0.9099 0.2208 0.045 Uiso 1 1 calc R . .
O2 O 0.3601(3) 1.0263(3) 0.36980(19) 0.0540(9) Uani 1 1 d . . .
H2 H 0.2940 0.9775 0.3822 0.081 Uiso 1 1 calc R . .
O3 O 0.1014(3) 1.0854(2) -0.01790(17) 0.0355(7) Uani 1 1 d . . .
O4 O 0.0120(3) 1.0827(2) 0.15220(18) 0.0408(7) Uani 1 1 d . . .
O5 O -0.0112(3) 0.9881(3) 0.2759(2) 0.0500(8) Uani 1 1 d . . .
O6 O 0.1448(3) 0.8566(3) -0.00838(19) 0.0459(8) Uani 1 1 d . . .
H6 H 0.1200 0.8795 -0.0566 0.069 Uiso 1 1 d R . .
O7 O 0.0800(3) 0.2989(2) 0.64670(17) 0.0326(6) Uani 1 1 d . . .
H7 H 0.0176 0.2443 0.6262 0.039 Uiso 1 1 calc R . .
O8 O 0.1615(3) 0.0266(3) 0.5860(2) 0.0515(9) Uani 1 1 d . . .
H8 H 0.1222 0.0312 0.6286 0.077 Uiso 1 1 calc R . .
O9 O 0.0647(3) 0.4959(2) 0.42994(17) 0.0316(6) Uani 1 1 d . . .
O10 O -0.1169(3) 0.2869(2) 0.48321(18) 0.0372(7) Uani 1 1 d . . .
O11 O -0.1539(3) 0.1586(3) 0.58708(19) 0.0422(7) Uani 1 1 d . . .
O12 O 0.2231(3) 0.5422(2) 0.59770(18) 0.0405(7) Uani 1 1 d . . .
H12 H 0.2113 0.5969 0.5680 0.061 Uiso 1 1 d R . .
C1 C 0.2551(5) 0.8722(4) 0.2110(3) 0.0402(11) Uani 1 1 d . . .
H1A H 0.2825 0.8223 0.1705 0.048 Uiso 1 1 calc R . .
H1B H 0.2682 0.8430 0.2695 0.048 Uiso 1 1 calc R . .
C2 C 0.3447(4) 0.9950(4) 0.2096(3) 0.0368(10) Uani 1 1 d . . .
C3 C 0.3275(5) 1.0702(4) 0.2870(3) 0.0406(11) Uani 1 1 d . . .
H3A H 0.3850 1.1478 0.2841 0.049 Uiso 1 1 calc R . .
H3B H 0.2341 1.0762 0.2811 0.049 Uiso 1 1 calc R . .
C4 C 0.4954(5) 0.9920(5) 0.2154(3) 0.0525(13) Uani 1 1 d . . .
H4A H 0.5504 1.0713 0.2215 0.063 Uiso 1 1 calc R . .
H4B H 0.5184 0.9535 0.2688 0.063 Uiso 1 1 calc R . .
C5 C 0.5353(6) 0.9328(6) 0.1395(4) 0.087(2) Uani 1 1 d . . .
H5A H 0.4926 0.8513 0.1380 0.131 Uiso 1 1 calc R . .
H5B H 0.6321 0.9441 0.1468 0.131 Uiso 1 1 calc R . .
H5C H 0.5066 0.9653 0.0853 0.131 Uiso 1 1 calc R . .
C6 C 0.3628(5) 1.1374(4) 0.1003(3) 0.0428(11) Uani 1 1 d . . .
H6A H 0.4498 1.1649 0.1304 0.051 Uiso 1 1 calc R . .
C7 C 0.3262(5) 1.2032(4) 0.0262(3) 0.0388(10) Uani 1 1 d . . .
C8 C 0.2015(4) 1.1751(4) -0.0301(3) 0.0359(10) Uani 1 1 d . . .
C9 C 0.1875(5) 1.2471(4) -0.1005(3) 0.0504(13) Uani 1 1 d . . .
H9 H 0.1069 1.2300 -0.1391 0.061 Uiso 1 1 calc R . .
C10 C 0.2877(6) 1.3416(4) -0.1148(3) 0.0599(15) Uani 1 1 d . . .
H10 H 0.2737 1.3875 -0.1623 0.072 Uiso 1 1 calc R . .
C11 C 0.4085(6) 1.3697(4) -0.0603(3) 0.0665(16) Uani 1 1 d . . .
H11 H 0.4766 1.4343 -0.0702 0.080 Uiso 1 1 calc R . .
C12 C 0.4269(5) 1.3016(4) 0.0083(3) 0.0586(14) Uani 1 1 d . . .
H12A H 0.5092 1.3204 0.0452 0.070 Uiso 1 1 calc R . .
C13 C -0.0297(4) 1.0676(4) 0.2263(3) 0.0387(10) Uani 1 1 d . . .
C14 C -0.1009(6) 1.1533(5) 0.2566(3) 0.0639(15) Uani 1 1 d . . .
H14A H -0.1952 1.1304 0.2326 0.096 Uiso 1 1 calc R . .
H14B H -0.0607 1.2288 0.2368 0.096 Uiso 1 1 calc R . .
H14C H -0.0925 1.1556 0.3197 0.096 Uiso 1 1 calc R . .
C15 C 0.0913(8) 0.7326(5) -0.0065(4) 0.083(2) Uani 1 1 d . . .
H15A H 0.0783 0.7121 0.0535 0.099 Uiso 1 1 calc R . .
H15B H 0.0031 0.7114 -0.0422 0.099 Uiso 1 1 calc R . .
C16 C 0.1765(9) 0.6668(6) -0.0376(5) 0.124(3) Uani 1 1 d . . .
H16A H 0.1863 0.6836 -0.0980 0.186 Uiso 1 1 calc R . .
H16B H 0.1361 0.5856 -0.0332 0.186 Uiso 1 1 calc R . .
H16C H 0.2641 0.6871 -0.0026 0.186 Uiso 1 1 calc R . .
C17 C 0.2065(4) 0.2669(4) 0.6498(3) 0.0375(10) Uani 1 1 d . . .
H17A H 0.2053 0.2021 0.6881 0.045 Uiso 1 1 calc R . .
H17B H 0.2796 0.3315 0.6750 0.045 Uiso 1 1 calc R . .
C18 C 0.2347(4) 0.2331(3) 0.5591(3) 0.0335(10) Uani 1 1 d . . .
C19 C 0.1433(4) 0.1135(3) 0.5274(3) 0.0383(10) Uani 1 1 d . . .
H19A H 0.0491 0.1171 0.5209 0.046 Uiso 1 1 calc R . .
H19B H 0.1635 0.0936 0.4701 0.046 Uiso 1 1 calc R . .
C20 C 0.3847(4) 0.2301(4) 0.5634(3) 0.0464(12) Uani 1 1 d . . .
H20A H 0.4033 0.1766 0.6081 0.056 Uiso 1 1 calc R . .
H20B H 0.3973 0.1989 0.5075 0.056 Uiso 1 1 calc R . .
C21 C 0.4892(5) 0.3451(5) 0.5834(4) 0.0733(17) Uani 1 1 d . . .
H21A H 0.4682 0.4012 0.5427 0.110 Uiso 1 1 calc R . .
H21B H 0.5779 0.3351 0.5778 0.110 Uiso 1 1 calc R . .
H21C H 0.4877 0.3718 0.6423 0.110 Uiso 1 1 calc R . .
C22 C 0.2303(4) 0.3244(4) 0.4212(3) 0.0392(11) Uani 1 1 d . . .
H22 H 0.2848 0.2761 0.4087 0.047 Uiso 1 1 calc R . .
C23 C 0.1972(4) 0.3990(4) 0.3520(3) 0.0365(10) Uani 1 1 d . . .
C24 C 0.1219(4) 0.4830(3) 0.3594(3) 0.0331(10) Uani 1 1 d . . .
C25 C 0.1093(5) 0.5523(4) 0.2871(3) 0.0477(12) Uani 1 1 d . . .
H25 H 0.0638 0.6104 0.2907 0.057 Uiso 1 1 calc R . .
C26 C 0.1614(6) 0.5379(4) 0.2109(3) 0.0591(15) Uani 1 1 d . . .
H26 H 0.1490 0.5853 0.1640 0.071 Uiso 1 1 calc R . .
C27 C 0.2317(6) 0.4544(5) 0.2028(3) 0.0644(16) Uani 1 1 d . . .
H27 H 0.2656 0.4437 0.1508 0.077 Uiso 1 1 calc R . .
C28 C 0.2500(5) 0.3879(4) 0.2732(3) 0.0526(13) Uani 1 1 d . . .
H28 H 0.2996 0.3328 0.2689 0.063 Uiso 1 1 calc R . .
C29 C -0.1914(4) 0.2007(3) 0.5166(3) 0.0327(9) Uani 1 1 d . . .
C30 C -0.3296(5) 0.1480(4) 0.4673(3) 0.0500(12) Uani 1 1 d . . .
H30A H -0.3233 0.0899 0.4255 0.075 Uiso 1 1 calc R . .
H30B H -0.3637 0.2073 0.4368 0.075 Uiso 1 1 calc R . .
H30C H -0.3900 0.1131 0.5080 0.075 Uiso 1 1 calc R . .
C31 C 0.2340(6) 0.5735(5) 0.6893(3) 0.0609(15) Uani 1 1 d . . .
H31A H 0.1935 0.5057 0.7205 0.073 Uiso 1 1 calc R . .
H31B H 0.1836 0.6314 0.6959 0.073 Uiso 1 1 calc R . .
C32 C 0.3746(7) 0.6193(6) 0.7284(4) 0.106(3) Uani 1 1 d . . .
H32A H 0.4270 0.5658 0.7164 0.160 Uiso 1 1 calc R . .
H32B H 0.3786 0.6298 0.7908 0.160 Uiso 1 1 calc R . .
H32C H 0.4110 0.6925 0.7036 0.160 Uiso 1 1 calc R . .


_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 O3 2.005(3) . ?
Ni1 N1 2.011(4) . ?
Ni1 O3 2.071(3) 2_575 ?
Ni1 O4 2.073(3) . ?
Ni1 O1 2.087(3) . ?
Ni1 O6 2.163(3) . ?
Ni2 O9 2.009(3) . ?
Ni2 N2 2.015(3) . ?
Ni2 O10 2.068(3) . ?
Ni2 O7 2.082(3) . ?
Ni2 O9 2.087(3) 2_566 ?
Ni2 O12 2.149(3) . ?
N1 C6 1.273(5) . ?
N1 C2 1.481(5) . ?
N2 C22 1.276(5) . ?
N2 C18 1.485(5) . ?
O1 C1 1.439(5) . ?
O1 H1 0.8200 . ?
O2 C3 1.406(5) . ?
O2 H2 0.8200 . ?
O3 C8 1.320(5) . ?
O3 Ni1 2.071(3) 2_575 ?
O4 C13 1.264(5) . ?
O5 C13 1.251(5) . ?
O6 C15 1.444(6) . ?
O6 H6 0.8200 . ?
O7 C17 1.435(5) . ?
O7 H7 0.8200 . ?
O8 C19 1.404(5) . ?
O8 H8 0.8200 . ?
O9 C24 1.320(4) . ?
O9 Ni2 2.087(3) 2_566 ?
O10 C29 1.272(5) . ?
O11 C29 1.248(5) . ?
O12 C31 1.435(6) . ?
O12 H12 0.8201 . ?
C1 C2 1.525(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.539(6) . ?
C2 C4 1.545(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.510(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.445(6) . ?
C6 H6A 0.9300 . ?
C7 C12 1.412(6) . ?
C7 C8 1.413(6) . ?
C8 C9 1.396(6) . ?
C9 C10 1.364(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.353(7) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.497(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.431(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.529(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.537(6) . ?
C18 C20 1.541(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.518(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.447(6) . ?
C22 H22 0.9300 . ?
C23 C28 1.406(6) . ?
C23 C24 1.418(6) . ?
C24 C25 1.396(6) . ?
C25 C26 1.374(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.378(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.362(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.501(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.457(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 N1 92.26(12) . . ?
O3 Ni1 O3 80.75(12) . 2_575 ?
N1 Ni1 O3 172.86(12) . 2_575 ?
O3 Ni1 O4 89.53(11) . . ?
N1 Ni1 O4 96.79(13) . . ?
O3 Ni1 O4 84.71(12) 2_575 . ?
O3 Ni1 O1 173.13(12) . . ?
N1 Ni1 O1 81.07(12) . . ?
O3 Ni1 O1 105.87(11) 2_575 . ?
O4 Ni1 O1 92.88(11) . . ?
O3 Ni1 O6 86.82(11) . . ?
N1 Ni1 O6 93.52(13) . . ?
O3 Ni1 O6 84.66(12) 2_575 . ?
O4 Ni1 O6 169.19(12) . . ?
O1 Ni1 O6 91.92(11) . . ?
O9 Ni2 N2 91.70(12) . . ?
O9 Ni2 O10 90.94(11) . . ?
N2 Ni2 O10 98.13(12) . . ?
O9 Ni2 O7 173.02(11) . . ?
N2 Ni2 O7 81.65(12) . . ?
O10 Ni2 O7 92.10(11) . . ?
O9 Ni2 O9 81.75(11) . 2_566 ?
N2 Ni2 O9 172.88(12) . 2_566 ?
O10 Ni2 O9 84.82(11) . 2_566 ?
O7 Ni2 O9 104.79(10) . 2_566 ?
O9 Ni2 O12 85.81(11) . . ?
N2 Ni2 O12 92.31(12) . . ?
O10 Ni2 O12 169.15(11) . . ?
O7 Ni2 O12 92.31(11) . . ?
O9 Ni2 O12 84.48(11) 2_566 . ?
C6 N1 C2 119.3(4) . . ?
C6 N1 Ni1 123.9(3) . . ?
C2 N1 Ni1 116.4(3) . . ?
C22 N2 C18 119.0(3) . . ?
C22 N2 Ni2 124.8(3) . . ?
C18 N2 Ni2 115.9(2) . . ?
C1 O1 Ni1 108.6(2) . . ?
C1 O1 H1 109.5 . . ?
Ni1 O1 H1 93.2 . . ?
C3 O2 H2 109.5 . . ?
C8 O3 Ni1 127.5(3) . . ?
C8 O3 Ni1 133.0(3) . 2_575 ?
Ni1 O3 Ni1 99.25(12) . 2_575 ?
C13 O4 Ni1 129.0(3) . . ?
C15 O6 Ni1 122.0(3) . . ?
C15 O6 H6 109.6 . . ?
Ni1 O6 H6 102.3 . . ?
C17 O7 Ni2 107.9(2) . . ?
C17 O7 H7 109.5 . . ?
Ni2 O7 H7 94.5 . . ?
C19 O8 H8 109.5 . . ?
C24 O9 Ni2 127.5(2) . . ?
C24 O9 Ni2 134.0(2) . 2_566 ?
Ni2 O9 Ni2 98.25(11) . 2_566 ?
C29 O10 Ni2 129.7(3) . . ?
C31 O12 Ni2 120.6(3) . . ?
C31 O12 H12 109.5 . . ?
Ni2 O12 H12 102.2 . . ?
O1 C1 C2 112.1(3) . . ?
O1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
O1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C1 105.9(3) . . ?
N1 C2 C3 105.6(3) . . ?
C1 C2 C3 110.8(4) . . ?
N1 C2 C4 115.4(4) . . ?
C1 C2 C4 110.1(4) . . ?
C3 C2 C4 109.1(4) . . ?
O2 C3 C2 113.4(3) . . ?
O2 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
O2 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C5 C4 C2 116.8(4) . . ?
C5 C4 H4A 108.1 . . ?
C2 C4 H4A 108.1 . . ?
C5 C4 H4B 108.1 . . ?
C2 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 127.8(4) . . ?
N1 C6 H6A 116.1 . . ?
C7 C6 H6A 116.1 . . ?
C12 C7 C8 118.4(4) . . ?
C12 C7 C6 116.0(4) . . ?
C8 C7 C6 125.5(4) . . ?
O3 C8 C9 120.6(4) . . ?
O3 C8 C7 122.5(4) . . ?
C9 C8 C7 117.0(4) . . ?
C10 C9 C8 122.4(5) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C9 C10 C11 120.9(5) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 118.6(5) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 C7 122.6(5) . . ?
C11 C12 H12A 118.7 . . ?
C7 C12 H12A 118.7 . . ?
O5 C13 O4 123.8(4) . . ?
O5 C13 C14 119.1(4) . . ?
O4 C13 C14 117.0(4) . . ?
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 . . ?
C16 C15 O6 113.9(6) . . ?
C16 C15 H15A 108.8 . . ?
O6 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
O6 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 C17 C18 112.8(3) . . ?
O7 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
O7 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
N2 C18 C17 106.1(3) . . ?
N2 C18 C19 106.2(3) . . ?
C17 C18 C19 110.6(3) . . ?
N2 C18 C20 114.7(3) . . ?
C17 C18 C20 109.8(3) . . ?
C19 C18 C20 109.4(3) . . ?
O8 C19 C18 112.1(3) . . ?
O8 C19 H19A 109.2 . . ?
C18 C19 H19A 109.2 . . ?
O8 C19 H19B 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 C18 116.4(4) . . ?
C21 C20 H20A 108.2 . . ?
C18 C20 H20A 108.2 . . ?
C21 C20 H20B 108.2 . . ?
C18 C20 H20B 108.2 . . ?
H20A C20 H20B 107.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 C23 127.0(4) . . ?
N2 C22 H22 116.5 . . ?
C23 C22 H22 116.5 . . ?
C28 C23 C24 119.2(4) . . ?
C28 C23 C22 115.5(4) . . ?
C24 C23 C22 125.3(4) . . ?
O9 C24 C25 120.7(4) . . ?
O9 C24 C23 122.8(4) . . ?
C25 C24 C23 116.5(4) . . ?
C26 C25 C24 122.5(4) . . ?
C26 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
C25 C26 C27 121.0(4) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 118.0(4) . . ?
C28 C27 H27 121.0 . . ?
C26 C27 H27 121.0 . . ?
C27 C28 C23 122.7(4) . . ?
C27 C28 H28 118.6 . . ?
C23 C28 H28 118.6 . . ?
O11 C29 O10 123.0(4) . . ?
O11 C29 C30 119.6(4) . . ?
O10 C29 C30 117.4(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O12 C31 C32 112.0(5) . . ?
O12 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
O12 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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
O3 Ni1 N1 C6 7.2(4) . . . . ?
O4 Ni1 N1 C6 -82.6(4) . . . . ?
O1 Ni1 N1 C6 -174.5(4) . . . . ?
O6 Ni1 N1 C6 94.2(4) . . . . ?
O3 Ni1 N1 C2 179.7(3) . . . . ?
O4 Ni1 N1 C2 90.0(3) . . . . ?
O1 Ni1 N1 C2 -1.9(3) . . . . ?
O6 Ni1 N1 C2 -93.3(3) . . . . ?
O9 Ni2 N2 C22 -9.6(4) . . . . ?
O10 Ni2 N2 C22 81.6(4) . . . . ?
O7 Ni2 N2 C22 172.6(4) . . . . ?
O12 Ni2 N2 C22 -95.4(4) . . . . ?
O9 Ni2 N2 C18 177.6(3) . . . . ?
O10 Ni2 N2 C18 -91.3(3) . . . . ?
O7 Ni2 N2 C18 -0.3(3) . . . . ?
O12 Ni2 N2 C18 91.7(3) . . . . ?
N1 Ni1 O1 C1 -21.6(2) . . . . ?
O3 Ni1 O1 C1 156.7(2) 2_575 . . . ?
O4 Ni1 O1 C1 -118.0(2) . . . . ?
O6 Ni1 O1 C1 71.7(2) . . . . ?
N1 Ni1 O3 C8 -6.9(3) . . . . ?
O3 Ni1 O3 C8 174.6(4) 2_575 . . . ?
O4 Ni1 O3 C8 89.9(3) . . . . ?
O6 Ni1 O3 C8 -100.3(3) . . . . ?
N1 Ni1 O3 Ni1 178.50(13) . . . 2_575 ?
O3 Ni1 O3 Ni1 0.0 2_575 . . 2_575 ?
O4 Ni1 O3 Ni1 -84.72(13) . . . 2_575 ?
O6 Ni1 O3 Ni1 85.10(13) . . . 2_575 ?
O3 Ni1 O4 C13 176.0(4) . . . . ?
N1 Ni1 O4 C13 -91.8(4) . . . . ?
O3 Ni1 O4 C13 95.2(4) 2_575 . . . ?
O1 Ni1 O4 C13 -10.4(4) . . . . ?
O6 Ni1 O4 C13 105.8(6) . . . . ?
O3 Ni1 O6 C15 -145.1(4) . . . . ?
N1 Ni1 O6 C15 122.8(4) . . . . ?
O3 Ni1 O6 C15 -64.1(4) 2_575 . . . ?
O4 Ni1 O6 C15 -74.7(7) . . . . ?
O1 Ni1 O6 C15 41.6(4) . . . . ?
N2 Ni2 O7 C17 23.0(2) . . . . ?
O10 Ni2 O7 C17 120.9(2) . . . . ?
O9 Ni2 O7 C17 -153.9(2) 2_566 . . . ?
O12 Ni2 O7 C17 -69.0(2) . . . . ?
N2 Ni2 O9 C24 8.3(3) . . . . ?
O10 Ni2 O9 C24 -89.9(3) . . . . ?
O9 Ni2 O9 C24 -174.5(4) 2_566 . . . ?
O12 Ni2 O9 C24 100.5(3) . . . . ?
N2 Ni2 O9 Ni2 -177.21(13) . . . 2_566 ?
O10 Ni2 O9 Ni2 84.62(12) . . . 2_566 ?
O9 Ni2 O9 Ni2 0.0 2_566 . . 2_566 ?
O12 Ni2 O9 Ni2 -85.02(12) . . . 2_566 ?
O9 Ni2 O10 C29 -175.4(3) . . . . ?
N2 Ni2 O10 C29 92.7(3) . . . . ?
O7 Ni2 O10 C29 10.9(3) . . . . ?
O9 Ni2 O10 C29 -93.8(3) 2_566 . . . ?
O12 Ni2 O10 C29 -103.0(6) . . . . ?
O9 Ni2 O12 C31 145.3(3) . . . . ?
N2 Ni2 O12 C31 -123.1(3) . . . . ?
O10 Ni2 O12 C31 72.5(7) . . . . ?
O7 Ni2 O12 C31 -41.4(3) . . . . ?
O9 Ni2 O12 C31 63.2(3) 2_566 . . . ?
Ni1 O1 C1 C2 41.5(4) . . . . ?
C6 N1 C2 C1 -163.9(4) . . . . ?
Ni1 N1 C2 C1 23.2(4) . . . . ?
C6 N1 C2 C3 78.6(5) . . . . ?
Ni1 N1 C2 C3 -94.3(3) . . . . ?
C6 N1 C2 C4 -41.9(6) . . . . ?
Ni1 N1 C2 C4 145.2(3) . . . . ?
O1 C1 C2 N1 -42.1(4) . . . . ?
O1 C1 C2 C3 71.8(4) . . . . ?
O1 C1 C2 C4 -167.5(3) . . . . ?
N1 C2 C3 O2 173.2(3) . . . . ?
C1 C2 C3 O2 59.0(5) . . . . ?
C4 C2 C3 O2 -62.3(5) . . . . ?
N1 C2 C4 C5 -55.1(6) . . . . ?
C1 C2 C4 C5 64.6(6) . . . . ?
C3 C2 C4 C5 -173.6(4) . . . . ?
C2 N1 C6 C7 -176.8(4) . . . . ?
Ni1 N1 C6 C7 -4.4(7) . . . . ?
N1 C6 C7 C12 -180.0(5) . . . . ?
N1 C6 C7 C8 -2.0(8) . . . . ?
Ni1 O3 C8 C9 -176.7(3) . . . . ?
Ni1 O3 C8 C9 -4.0(6) 2_575 . . . ?
Ni1 O3 C8 C7 3.3(6) . . . . ?
Ni1 O3 C8 C7 176.0(3) 2_575 . . . ?
C12 C7 C8 O3 -179.4(4) . . . . ?
C6 C7 C8 O3 2.6(7) . . . . ?
C12 C7 C8 C9 0.6(7) . . . . ?
C6 C7 C8 C9 -177.4(4) . . . . ?
O3 C8 C9 C10 179.1(5) . . . . ?
C7 C8 C9 C10 -0.9(7) . . . . ?
C8 C9 C10 C11 0.5(9) . . . . ?
C9 C10 C11 C12 0.1(9) . . . . ?
C10 C11 C12 C7 -0.4(9) . . . . ?
C8 C7 C12 C11 0.0(8) . . . . ?
C6 C7 C12 C11 178.2(5) . . . . ?
Ni1 O4 C13 O5 9.6(7) . . . . ?
Ni1 O4 C13 C14 -172.5(3) . . . . ?
Ni1 O6 C15 C16 -152.7(5) . . . . ?
Ni2 O7 C17 C18 -42.1(4) . . . . ?
C22 N2 C18 C17 166.0(4) . . . . ?
Ni2 N2 C18 C17 -20.7(4) . . . . ?
C22 N2 C18 C19 -76.3(5) . . . . ?
Ni2 N2 C18 C19 97.0(3) . . . . ?
C22 N2 C18 C20 44.6(5) . . . . ?
Ni2 N2 C18 C20 -142.0(3) . . . . ?
O7 C17 C18 N2 41.3(4) . . . . ?
O7 C17 C18 C19 -73.4(4) . . . . ?
O7 C17 C18 C20 165.7(3) . . . . ?
N2 C18 C19 O8 -173.1(3) . . . . ?
C17 C18 C19 O8 -58.4(4) . . . . ?
C20 C18 C19 O8 62.7(4) . . . . ?
N2 C18 C20 C21 54.0(6) . . . . ?
C17 C18 C20 C21 -65.3(5) . . . . ?
C19 C18 C20 C21 173.1(4) . . . . ?
C18 N2 C22 C23 178.5(4) . . . . ?
Ni2 N2 C22 C23 5.8(7) . . . . ?
N2 C22 C23 C28 -179.0(5) . . . . ?
N2 C22 C23 C24 3.5(8) . . . . ?
Ni2 O9 C24 C25 176.6(3) . . . . ?
Ni2 O9 C24 C25 4.2(6) 2_566 . . . ?
Ni2 O9 C24 C23 -2.7(6) . . . . ?
Ni2 O9 C24 C23 -175.2(3) 2_566 . . . ?
C28 C23 C24 O9 177.4(4) . . . . ?
C22 C23 C24 O9 -5.2(7) . . . . ?
C28 C23 C24 C25 -1.9(7) . . . . ?
C22 C23 C24 C25 175.4(4) . . . . ?
O9 C24 C25 C26 -176.7(5) . . . . ?
C23 C24 C25 C26 2.7(7) . . . . ?
C24 C25 C26 C27 -1.2(9) . . . . ?
C25 C26 C27 C28 -1.1(9) . . . . ?
C26 C27 C28 C23 1.8(9) . . . . ?
C24 C23 C28 C27 -0.3(8) . . . . ?
C22 C23 C28 C27 -177.9(5) . . . . ?
Ni2 O10 C29 O11 -12.8(6) . . . . ?
Ni2 O10 C29 C30 167.9(3) . . . . ?
Ni2 O12 C31 C32 148.5(4) . . . . ?

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
O2 H2 O11 0.82 1.99 2.799(4) 170.5 2_566
O8 H8 O5 0.82 1.95 2.759(4) 169.2 2_566
C30 H30A O8 0.96 2.43 3.174(6) 133.9 2_556

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_110827d
_database_code_depnum_ccdc_archive 'CCDC 918248'
_audit_update_record             
;
2015-01-06 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H72 N3 Ni4 O25'
_chemical_formula_weight         1217.84

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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'P -4 3 n'
_symmetry_space_group_name_Hall  'P -4n 2 3'

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

_cell_length_a                   23.4500(17)
_cell_length_b                   23.4500(17)
_cell_length_c                   23.4500(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12895.2(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    903
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      16.36

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5112
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_T_max  0.8675
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3806
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1352
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3806
_reflns_number_gt                1412
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0752P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_number_reflns         3806
_refine_ls_number_parameters     216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.2037
_refine_ls_wR_factor_gt          0.1873
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_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
Ni1 Ni 0.24351(7) 0.32250(7) 0.78018(6) 0.0883(6) Uani 1 1 d . . .
Ni2 Ni 0.20101(7) 0.20101(7) 0.79899(7) 0.0943(9) Uani 1 3 d S . .
O1 O 0.2115(4) 0.3902(4) 0.7413(4) 0.100(2) Uani 1 1 d . . .
O2 O 0.1722(4) 0.4681(4) 0.6763(5) 0.122(3) Uani 1 1 d . . .
O3 O 0.2686(3) 0.2511(3) 0.8216(3) 0.082(2) Uani 1 1 d . . .
O4 O 0.2303(4) 0.1310(4) 0.8463(3) 0.111(3) Uani 1 1 d . . .
H4 H 0.2157 0.1248 0.8774 0.134 Uiso 1 1 d R . .
O5 O 0.2871(4) 0.2871(4) 0.7129(4) 0.101(4) Uani 1 3 d S . .
O6 O 0.3252(3) 0.3590(4) 0.8045(3) 0.118(3) Uani 1 1 d . . .
H6E H 0.3324 0.3871 0.7827 0.141 Uiso 1 1 d R . .
H6F H 0.3511 0.3342 0.7998 0.141 Uiso 1 1 d R . .
O7 O 0.2953(5) 0.4568(5) 0.6729(6) 0.196(5) Uani 1 1 d . . .
H7C H 0.2783 0.4257 0.6803 0.236 Uiso 1 1 d R . .
H7D H 0.2679 0.4792 0.6805 0.236 Uiso 1 1 d R . .
O8 O 0.1921(6) 0.1021(6) 0.9502(5) 0.212(5) Uani 1 1 d . . .
H8D H 0.1698 0.1280 0.9622 0.255 Uiso 1 1 d R . .
H8E H 0.2197 0.1027 0.9736 0.255 Uiso 1 1 d R . .
O9 O 0.3908(9) 0.4419(8) 0.7357(9) 0.315(10) Uani 1 1 d . . .
H9C H 0.4072 0.4108 0.7273 0.377 Uiso 1 1 d R . .
H9D H 0.3605 0.4447 0.7159 0.377 Uiso 1 1 d R . .
N1 N 0.2057(5) 0.3420(5) 0.8520(4) 0.098(3) Uani 1 1 d . . .
C1 C 0.1701(6) 0.3831(6) 0.8587(6) 0.100(4) Uani 1 1 d . . .
H1 H 0.1544 0.3873 0.8949 0.120 Uiso 1 1 calc R . .
C2 C 0.1525(6) 0.4216(6) 0.8181(7) 0.091(4) Uani 1 1 d . . .
C3 C 0.1170(5) 0.4615(6) 0.8384(6) 0.100(4) Uani 1 1 d . . .
H3 H 0.1062 0.4619 0.8766 0.119 Uiso 1 1 calc R . .
C4 C 0.0971(6) 0.5021(6) 0.8007(8) 0.111(4) Uani 1 1 d . . .
H4A H 0.0702 0.5283 0.8134 0.133 Uiso 1 1 calc R . .
C5 C 0.1147(6) 0.5054(7) 0.7466(8) 0.108(4) Uani 1 1 d . . .
H5 H 0.1020 0.5339 0.7222 0.130 Uiso 1 1 calc R . .
C6 C 0.1504(6) 0.4669(7) 0.7299(7) 0.101(4) Uani 1 1 d . . .
C7 C 0.1721(6) 0.4245(6) 0.7641(8) 0.099(4) Uani 1 1 d . . .
C8 C 0.1526(6) 0.5061(7) 0.6318(7) 0.151(6) Uani 1 1 d . . .
H8A H 0.1173 0.4921 0.6164 0.226 Uiso 1 1 calc R . .
H8B H 0.1806 0.5078 0.6020 0.226 Uiso 1 1 calc R . .
H8C H 0.1468 0.5435 0.6473 0.226 Uiso 1 1 calc R . .
C9 C 0.2221(7) 0.2992(6) 0.9030(5) 0.104(4) Uani 1 1 d . . .
C11 C 0.2760(5) 0.2645(6) 0.8808(5) 0.106(4) Uani 1 1 d . . .
H11A H 0.3102 0.2871 0.8859 0.127 Uiso 1 1 calc R . .
H11B H 0.2801 0.2296 0.9027 0.127 Uiso 1 1 calc R . .
C12 C 0.2406(6) 0.3306(6) 0.9539(6) 0.115(4) Uani 1 1 d . . .
H12A H 0.2613 0.3042 0.9780 0.138 Uiso 1 1 calc R . .
H12B H 0.2066 0.3419 0.9746 0.138 Uiso 1 1 calc R . .
C13 C 0.2815(7) 0.3893(7) 0.9459(7) 0.155(6) Uani 1 1 d . . .
H13A H 0.3044 0.3855 0.9122 0.232 Uiso 1 1 calc R . .
H13B H 0.3059 0.3935 0.9785 0.232 Uiso 1 1 calc R . .
H13C H 0.2575 0.4223 0.9425 0.232 Uiso 1 1 calc R . .
C23 C 0.2624(8) 0.0844(6) 0.8295(6) 0.132(5) Uani 1 1 d . . .
H23A H 0.2370 0.0530 0.8207 0.158 Uiso 1 1 calc R . .
H23B H 0.2867 0.0727 0.8609 0.158 Uiso 1 1 calc R . .


_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 1.957(11) . ?
Ni1 O1 1.977(8) . ?
Ni1 O3 2.023(8) . ?
Ni1 O5 2.056(8) . ?
Ni1 O3 2.115(7) 8_656 ?
Ni1 O6 2.174(8) . ?
Ni2 O3 2.043(8) . ?
Ni2 O3 2.043(8) 8_656 ?
Ni2 O3 2.043(8) 11_566 ?
Ni2 O4 2.096(8) 11_566 ?
Ni2 O4 2.096(8) 8_656 ?
Ni2 O4 2.096(8) . ?
O1 C7 1.338(16) . ?
O2 C6 1.357(16) . ?
O2 C8 1.446(14) . ?
O3 C11 1.434(12) . ?
O3 Ni1 2.115(7) 11_566 ?
O4 C23 1.384(14) . ?
O5 Ni1 2.056(8) 8_656 ?
O5 Ni1 2.056(8) 11_566 ?
N1 C1 1.287(14) . ?
N1 C9 1.607(16) . ?
C1 C2 1.375(18) . ?
C2 C3 1.340(16) . ?
C2 C7 1.349(17) . ?
C3 C4 1.381(17) . ?
C4 C5 1.337(18) . ?
C5 C6 1.290(17) . ?
C6 C7 1.375(18) . ?
C9 C12 1.467(16) . ?
C9 C23 1.515(18) 8_656 ?
C9 C11 1.591(16) . ?
C12 C13 1.689(19) . ?
C23 C9 1.515(18) 11_566 ?

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 92.1(4) . . ?
N1 Ni1 O3 84.9(4) . . ?
O1 Ni1 O3 174.6(3) . . ?
N1 Ni1 O5 168.6(5) . . ?
O1 Ni1 O5 99.1(4) . . ?
O3 Ni1 O5 83.7(3) . . ?
N1 Ni1 O3 96.4(4) . 8_656 ?
O1 Ni1 O3 92.6(3) . 8_656 ?
O3 Ni1 O3 83.2(4) . 8_656 ?
O5 Ni1 O3 81.5(3) . 8_656 ?
N1 Ni1 O6 94.6(4) . . ?
O1 Ni1 O6 98.0(3) . . ?
O3 Ni1 O6 86.8(3) . . ?
O5 Ni1 O6 85.5(3) . . ?
O3 Ni1 O6 164.4(3) 8_656 . ?
O3 Ni2 O3 84.6(3) . 8_656 ?
O3 Ni2 O3 84.6(3) . 11_566 ?
O3 Ni2 O3 84.6(3) 8_656 11_566 ?
O3 Ni2 O4 175.3(4) . 11_566 ?
O3 Ni2 O4 91.0(3) 8_656 11_566 ?
O3 Ni2 O4 93.3(3) 11_566 11_566 ?
O3 Ni2 O4 91.0(3) . 8_656 ?
O3 Ni2 O4 93.3(3) 8_656 8_656 ?
O3 Ni2 O4 175.3(4) 11_566 8_656 ?
O4 Ni2 O4 90.9(4) 11_566 8_656 ?
O3 Ni2 O4 93.3(3) . . ?
O3 Ni2 O4 175.3(4) 8_656 . ?
O3 Ni2 O4 91.0(3) 11_566 . ?
O4 Ni2 O4 90.9(4) 11_566 . ?
O4 Ni2 O4 90.9(4) 8_656 . ?
C7 O1 Ni1 124.2(9) . . ?
C6 O2 C8 124.1(12) . . ?
C11 O3 Ni1 108.6(7) . . ?
C11 O3 Ni2 118.1(8) . . ?
Ni1 O3 Ni2 97.2(3) . . ?
C11 O3 Ni1 134.7(7) . 11_566 ?
Ni1 O3 Ni1 96.5(3) . 11_566 ?
Ni2 O3 Ni1 94.4(3) . 11_566 ?
C23 O4 Ni2 130.3(8) . . ?
Ni1 O5 Ni1 97.4(5) 8_656 . ?
Ni1 O5 Ni1 97.4(5) 8_656 11_566 ?
Ni1 O5 Ni1 97.4(5) . 11_566 ?
C1 N1 C9 122.2(11) . . ?
C1 N1 Ni1 125.0(10) . . ?
C9 N1 Ni1 112.8(8) . . ?
N1 C1 C2 127.1(14) . . ?
C3 C2 C7 120.7(15) . . ?
C3 C2 C1 113.5(16) . . ?
C7 C2 C1 125.5(15) . . ?
C2 C3 C4 117.6(14) . . ?
C5 C4 C3 122.9(15) . . ?
C6 C5 C4 116.7(17) . . ?
C5 C6 O2 120.7(17) . . ?
C5 C6 C7 124.6(17) . . ?
O2 C6 C7 114.5(16) . . ?
O1 C7 C2 125.4(15) . . ?
O1 C7 C6 117.4(16) . . ?
C2 C7 C6 117.3(15) . . ?
C12 C9 C23 111.4(12) . 8_656 ?
C12 C9 C11 106.7(11) . . ?
C23 C9 C11 114.0(11) 8_656 . ?
C12 C9 N1 111.2(10) . . ?
C23 C9 N1 108.0(10) 8_656 . ?
C11 C9 N1 105.3(10) . . ?
O3 C11 C9 109.5(9) . . ?
C9 C12 C13 119.2(12) . . ?
O4 C23 C9 112.5(12) . 11_566 ?

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
N1 Ni1 O1 C7 -8.4(9) . . . . ?
O5 Ni1 O1 C7 169.9(9) . . . . ?
O3 Ni1 O1 C7 88.1(9) 8_656 . . . ?
O6 Ni1 O1 C7 -103.3(9) . . . . ?
N1 Ni1 O3 C11 -31.9(7) . . . . ?
O5 Ni1 O3 C11 148.9(7) . . . . ?
O3 Ni1 O3 C11 -129.0(7) 8_656 . . . ?
O6 Ni1 O3 C11 63.0(7) . . . . ?
N1 Ni1 O3 Ni2 91.1(3) . . . . ?
O5 Ni1 O3 Ni2 -88.1(4) . . . . ?
O3 Ni1 O3 Ni2 -6.0(3) 8_656 . . . ?
O6 Ni1 O3 Ni2 -174.0(3) . . . . ?
N1 Ni1 O3 Ni1 -173.7(4) . . . 11_566 ?
O5 Ni1 O3 Ni1 7.1(3) . . . 11_566 ?
O3 Ni1 O3 Ni1 89.3(3) 8_656 . . 11_566 ?
O6 Ni1 O3 Ni1 -78.7(3) . . . 11_566 ?
O3 Ni2 O3 C11 121.8(9) 8_656 . . . ?
O3 Ni2 O3 C11 -153.2(8) 11_566 . . . ?
O4 Ni2 O3 C11 28.5(8) 8_656 . . . ?
O4 Ni2 O3 C11 -62.4(7) . . . . ?
O3 Ni2 O3 Ni1 6.2(3) 8_656 . . . ?
O3 Ni2 O3 Ni1 91.25(8) 11_566 . . . ?
O4 Ni2 O3 Ni1 -87.1(3) 8_656 . . . ?
O4 Ni2 O3 Ni1 -178.0(3) . . . . ?
O3 Ni2 O3 Ni1 -90.95(7) 8_656 . . 11_566 ?
O3 Ni2 O3 Ni1 -5.9(3) 11_566 . . 11_566 ?
O4 Ni2 O3 Ni1 175.8(3) 8_656 . . 11_566 ?
O4 Ni2 O3 Ni1 84.8(3) . . . 11_566 ?
O3 Ni2 O4 C23 -95.1(11) . . . . ?
O3 Ni2 O4 C23 -10.5(11) 11_566 . . . ?
O4 Ni2 O4 C23 82.8(13) 11_566 . . . ?
O4 Ni2 O4 C23 173.8(11) 8_656 . . . ?
N1 Ni1 O5 Ni1 87.0(17) . . . 8_656 ?
O1 Ni1 O5 Ni1 -84.2(5) . . . 8_656 ?
O3 Ni1 O5 Ni1 91.1(4) . . . 8_656 ?
O3 Ni1 O5 Ni1 7.1(4) 8_656 . . 8_656 ?
O6 Ni1 O5 Ni1 178.4(4) . . . 8_656 ?
N1 Ni1 O5 Ni1 -11(2) . . . 11_566 ?
O1 Ni1 O5 Ni1 177.3(4) . . . 11_566 ?
O3 Ni1 O5 Ni1 -7.4(4) . . . 11_566 ?
O3 Ni1 O5 Ni1 -91.4(4) 8_656 . . 11_566 ?
O6 Ni1 O5 Ni1 79.9(4) . . . 11_566 ?
O1 Ni1 N1 C1 5.9(10) . . . . ?
O3 Ni1 N1 C1 -169.5(10) . . . . ?
O5 Ni1 N1 C1 -165.4(15) . . . . ?
O3 Ni1 N1 C1 -86.9(10) 8_656 . . . ?
O6 Ni1 N1 C1 104.1(10) . . . . ?
O1 Ni1 N1 C9 -176.2(8) . . . . ?
O3 Ni1 N1 C9 8.3(8) . . . . ?
O5 Ni1 N1 C9 12(2) . . . . ?
O3 Ni1 N1 C9 90.9(8) 8_656 . . . ?
O6 Ni1 N1 C9 -78.0(8) . . . . ?
C9 N1 C1 C2 -179.1(12) . . . . ?
Ni1 N1 C1 C2 -1.4(18) . . . . ?
N1 C1 C2 C3 -176.8(12) . . . . ?
N1 C1 C2 C7 -3(2) . . . . ?
C7 C2 C3 C4 6.3(19) . . . . ?
C1 C2 C3 C4 180.0(11) . . . . ?
C2 C3 C4 C5 -5(2) . . . . ?
C3 C4 C5 C6 3(2) . . . . ?
C4 C5 C6 O2 -177.6(13) . . . . ?
C4 C5 C6 C7 -2(2) . . . . ?
C8 O2 C6 C5 -8.8(19) . . . . ?
C8 O2 C6 C7 175.1(11) . . . . ?
Ni1 O1 C7 C2 6.7(18) . . . . ?
Ni1 O1 C7 C6 -174.4(9) . . . . ?
C3 C2 C7 O1 173.4(11) . . . . ?
C1 C2 C7 O1 0(2) . . . . ?
C3 C2 C7 C6 -6(2) . . . . ?
C1 C2 C7 C6 -178.4(12) . . . . ?
C5 C6 C7 O1 -175.7(12) . . . . ?
O2 C6 C7 O1 0.3(17) . . . . ?
C5 C6 C7 C2 3(2) . . . . ?
O2 C6 C7 C2 179.3(11) . . . . ?
C1 N1 C9 C12 -53.0(16) . . . . ?
Ni1 N1 C9 C12 129.1(10) . . . . ?
C1 N1 C9 C23 69.6(14) . . . 8_656 ?
Ni1 N1 C9 C23 -108.3(10) . . . 8_656 ?
C1 N1 C9 C11 -168.2(11) . . . . ?
Ni1 N1 C9 C11 13.9(12) . . . . ?
Ni1 O3 C11 C9 47.6(12) . . . . ?
Ni2 O3 C11 C9 -61.7(12) . . . . ?
Ni1 O3 C11 C9 167.7(8) 11_566 . . . ?
C12 C9 C11 O3 -157.9(11) . . . . ?
C23 C9 C11 O3 78.7(14) 8_656 . . . ?
N1 C9 C11 O3 -39.6(13) . . . . ?
C23 C9 C12 C13 -159.6(11) 8_656 . . . ?
C11 C9 C12 C13 75.3(14) . . . . ?
N1 C9 C12 C13 -39.0(15) . . . . ?
Ni2 O4 C23 C9 25.6(17) . . . 11_566 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.092

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 0.000 0.000 0.000 445 66 ' '
2 0.000 0.000 0.500 360 58 ' '
3 0.000 0.500 0.000 361 58 ' '
4 0.000 0.500 0.500 359 58 ' '
5 0.500 0.000 0.000 360 58 ' '
6 0.500 0.500 0.000 359 58 ' '
7 0.500 0.500 0.500 445 66 ' '
8 0.500 0.000 0.500 359 58 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_110927d
_database_code_depnum_ccdc_archive 'CCDC 918249'
_audit_update_record             
;
2015-01-06 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H88 Cl2 Cu4 N4 O28'
_chemical_formula_weight         1614.38

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.6420(12)
_cell_length_b                   13.8856(14)
_cell_length_c                   21.048(2)
_cell_angle_alpha                89.928(2)
_cell_angle_beta                 81.7480(10)
_cell_angle_gamma                62.5610(10)
_cell_volume                     3492.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    948
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      26.18

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1676
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_T_max  0.8988
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17821
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         25.02
_reflns_number_total             12122
_reflns_number_gt                7131
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0885P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12122
_refine_ls_number_parameters     942
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1868
_refine_ls_wR_factor_gt          0.1659
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_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
Cu1 Cu 0.65976(6) 0.64779(6) 0.14872(4) 0.0320(2) Uani 1 1 d . . .
Cu2 Cu 0.75898(6) 0.45984(6) 0.25553(4) 0.0341(2) Uani 1 1 d . . .
Cu3 Cu 0.57347(6) 0.70858(6) 0.30665(4) 0.0342(2) Uani 1 1 d . . .
Cu4 Cu 0.80981(6) 0.70258(6) 0.23549(4) 0.0323(2) Uani 1 1 d . . .
Cl1 Cl 0.15845(17) 0.16614(16) 0.44315(11) 0.0581(5) Uani 1 1 d . . .
Cl2 Cl 0.7512(3) 0.1141(3) 0.16396(19) 0.0915(9) Uani 1 1 d . . .
N1 N 0.5280(4) 0.6529(4) 0.1200(3) 0.0392(14) Uani 1 1 d . . .
N2 N 0.8972(4) 0.3660(4) 0.2868(3) 0.0392(14) Uani 1 1 d . . .
N3 N 0.4409(4) 0.8467(4) 0.3048(3) 0.0398(14) Uani 1 1 d . . .
N4 N 0.9728(4) 0.6283(4) 0.2325(3) 0.0347(13) Uani 1 1 d . . .
O1 O 0.6666(3) 0.7560(3) 0.0953(2) 0.0381(11) Uani 1 1 d . . .
O2 O 0.7224(4) 0.8783(4) 0.0214(2) 0.0476(13) Uani 1 1 d . . .
O3 O 0.6376(3) 0.5549(3) 0.2124(2) 0.0355(11) Uani 1 1 d . . .
O4 O 0.3017(4) 0.7614(4) 0.1848(3) 0.0518(14) Uani 1 1 d . . .
H4 H 0.2467 0.7518 0.1851 0.078 Uiso 1 1 calc R . .
O5 O 0.7268(3) 0.5832(3) 0.3140(2) 0.0362(11) Uani 1 1 d . . .
O6 O 0.6232(4) 0.7570(4) 0.3998(2) 0.0460(12) Uani 1 1 d . . .
O7 O 0.8162(4) 0.3331(4) 0.1893(3) 0.0518(13) Uani 1 1 d . . .
O8 O 1.1594(4) 0.1650(4) 0.1862(3) 0.0660(16) Uani 1 1 d . . .
H8 H 1.2001 0.1042 0.1967 0.099 Uiso 1 1 calc R . .
O9 O 0.4966(4) 0.6434(4) 0.3571(3) 0.0524(14) Uani 1 1 d . . .
O10 O 0.4294(5) 0.5347(5) 0.4356(3) 0.088(2) Uani 1 1 d . . .
O11 O 0.3108(4) 0.9545(4) 0.2018(3) 0.0555(14) Uani 1 1 d . . .
H11 H 0.2949 0.9113 0.2215 0.083 Uiso 1 1 calc R . .
O12 O 0.6483(3) 0.7690(3) 0.2451(2) 0.0358(11) Uani 1 1 d . . .
O13 O 0.8154(3) 0.6017(3) 0.1692(2) 0.0352(11) Uani 1 1 d . . .
O14 O 0.7851(4) 0.5065(4) 0.0700(2) 0.0442(12) Uani 1 1 d . . .
O15 O 0.8163(4) 0.7857(4) 0.3111(2) 0.0458(12) Uani 1 1 d . . .
O16 O 1.1254(4) 0.7184(4) 0.1917(3) 0.0536(14) Uani 1 1 d . . .
H16 H 1.1004 0.7446 0.1591 0.080 Uiso 1 1 calc R . .
O17 O 0.8144(3) 0.8146(4) 0.1448(2) 0.0449(12) Uani 1 1 d . . .
H17A H 0.7899 0.8808 0.1579 0.054 Uiso 1 1 d R . .
H17B H 0.7962 0.8136 0.1079 0.054 Uiso 1 1 d R . .
O18 O 0.6400(4) 0.4220(4) 0.3269(3) 0.0611(15) Uani 1 1 d U . .
H18 H 0.5843 0.4807 0.3373 0.092 Uiso 1 1 d R . .
O19 O 0.1762(5) 0.2436(5) 0.4048(3) 0.0767(18) Uani 1 1 d . . .
O20 O 0.2637(5) 0.0876(5) 0.4590(3) 0.087(2) Uani 1 1 d . . .
O21 O 0.1149(6) 0.1132(5) 0.4071(3) 0.089(2) Uani 1 1 d . . .
O22 O 0.0844(5) 0.2206(5) 0.5001(3) 0.0830(19) Uani 1 1 d . . .
O23 O 0.7361(13) 0.1783(13) 0.2202(9) 0.094(6) Uani 0.520(18) 1 d P A 1
O24 O 0.8677(14) 0.0398(15) 0.1542(10) 0.110(7) Uani 0.520(18) 1 d P A 1
O25 O 0.7283(14) 0.1851(14) 0.1153(9) 0.116(7) Uani 0.520(18) 1 d P A 1
O26 O 0.6900(16) 0.0587(15) 0.1736(12) 0.102(6) Uani 0.520(18) 1 d P A 1
O27 O 0.7164(9) -0.0574(9) 0.4052(6) 0.098(5) Uani 0.652(16) 1 d P B 1
H27 H 0.7228 -0.0742 0.4423 0.147 Uiso 0.652(16) 1 calc PR B 1
O23' O 0.7910(16) 0.0457(14) 0.2131(10) 0.115(8) Uani 0.480(18) 1 d P A 2
O24' O 0.6862(16) 0.2188(15) 0.1822(11) 0.107(7) Uani 0.480(18) 1 d P A 2
O25' O 0.7128(17) 0.0623(15) 0.1259(12) 0.096(7) Uani 0.480(18) 1 d P A 2
O26' O 0.8480(16) 0.1070(15) 0.1221(10) 0.102(7) Uani 0.480(18) 1 d P A 2
O27' O 0.7473(19) -0.0054(17) 0.3274(13) 0.106(10) Uani 0.348(16) 1 d P B 2
H27' H 0.7633 0.0119 0.2916 0.160 Uiso 0.348(16) 1 calc PR B 2
O28 O 0.0317(4) 0.7634(4) 0.0859(3) 0.0633(15) Uani 1 1 d . . .
H28 H -0.0335 0.7747 0.0928 0.095 Uiso 1 1 calc R . .
C1 C 0.4893(6) 0.7016(6) 0.0701(4) 0.0443(18) Uani 1 1 d . . .
H1 H 0.4287 0.6959 0.0586 0.053 Uiso 1 1 calc R . .
C2 C 0.5305(6) 0.7631(6) 0.0308(4) 0.0445(18) Uani 1 1 d . . .
C3 C 0.6147(5) 0.7882(6) 0.0445(4) 0.0406(17) Uani 1 1 d . . .
C4 C 0.6451(6) 0.8537(6) 0.0030(4) 0.0436(18) Uani 1 1 d . . .
C5 C 0.5996(6) 0.8848(6) -0.0528(4) 0.056(2) Uani 1 1 d . . .
H5 H 0.6237 0.9239 -0.0811 0.067 Uiso 1 1 calc R . .
C6 C 0.5180(7) 0.8582(7) -0.0672(4) 0.060(2) Uani 1 1 d . . .
H6 H 0.4877 0.8798 -0.1048 0.072 Uiso 1 1 calc R . .
C7 C 0.4825(6) 0.8005(6) -0.0262(4) 0.052(2) Uani 1 1 d . . .
H7 H 0.4262 0.7852 -0.0353 0.062 Uiso 1 1 calc R . .
C8 C 0.7645(6) 0.9347(6) -0.0206(4) 0.058(2) Uani 1 1 d . . .
H8A H 0.7968 0.8938 -0.0616 0.087 Uiso 1 1 calc R . .
H8B H 0.8208 0.9440 -0.0027 0.087 Uiso 1 1 calc R . .
H8C H 0.7047 1.0048 -0.0262 0.087 Uiso 1 1 calc R . .
C9 C 0.4790(5) 0.5908(5) 0.1574(4) 0.0405(17) Uani 1 1 d . . .
C10 C 0.5738(5) 0.5079(5) 0.1893(4) 0.0427(18) Uani 1 1 d . . .
H10A H 0.5428 0.4808 0.2250 0.051 Uiso 1 1 calc R . .
H10B H 0.6228 0.4469 0.1585 0.051 Uiso 1 1 calc R . .
C11 C 0.4346(6) 0.5332(6) 0.1155(4) 0.049(2) Uani 1 1 d . . .
H11A H 0.3684 0.5883 0.1007 0.059 Uiso 1 1 calc R . .
H11B H 0.4907 0.4971 0.0777 0.059 Uiso 1 1 calc R . .
C12 C 0.4056(7) 0.4511(6) 0.1474(4) 0.061(2) Uani 1 1 d . . .
H12A H 0.4718 0.3925 0.1589 0.092 Uiso 1 1 calc R . .
H12B H 0.3751 0.4232 0.1183 0.092 Uiso 1 1 calc R . .
H12C H 0.3513 0.4851 0.1855 0.092 Uiso 1 1 calc R . .
C13 C 0.3871(5) 0.6701(5) 0.2105(4) 0.0434(18) Uani 1 1 d . . .
H13A H 0.3530 0.6316 0.2357 0.052 Uiso 1 1 calc R . .
H13B H 0.4207 0.6966 0.2391 0.052 Uiso 1 1 calc R . .
C14 C 0.9191(6) 0.3848(6) 0.3412(4) 0.0427(18) Uani 1 1 d . . .
H14 H 0.9816 0.3293 0.3546 0.051 Uiso 1 1 calc R . .
C15 C 0.8581(5) 0.4821(5) 0.3840(4) 0.0406(17) Uani 1 1 d . . .
C16 C 0.7646(5) 0.5758(5) 0.3699(3) 0.0361(16) Uani 1 1 d . . .
C17 C 0.7122(5) 0.6661(5) 0.4167(4) 0.0395(17) Uani 1 1 d . . .
C18 C 0.7540(6) 0.6617(6) 0.4737(4) 0.0437(18) Uani 1 1 d . . .
H18A H 0.7197 0.7212 0.5039 0.052 Uiso 1 1 calc R . .
C19 C 0.8467(6) 0.5686(6) 0.4858(4) 0.0468(18) Uani 1 1 d . . .
H19 H 0.8747 0.5668 0.5237 0.056 Uiso 1 1 calc R . .
C20 C 0.8968(6) 0.4809(6) 0.4435(4) 0.0444(18) Uani 1 1 d . . .
H20 H 0.9575 0.4186 0.4532 0.053 Uiso 1 1 calc R . .
C21 C 0.5474(7) 0.8346(6) 0.4505(4) 0.067(2) Uani 1 1 d . . .
H21A H 0.5276 0.7977 0.4846 0.100 Uiso 1 1 calc R . .
H21B H 0.4813 0.8846 0.4344 0.100 Uiso 1 1 calc R . .
H21C H 0.5824 0.8737 0.4666 0.100 Uiso 1 1 calc R . .
C22 C 0.9711(5) 0.2579(5) 0.2508(4) 0.0410(17) Uani 1 1 d . . .
C23 C 0.9371(6) 0.2696(6) 0.1839(4) 0.053(2) Uani 1 1 d . . .
H23A H 0.9731 0.3054 0.1576 0.064 Uiso 1 1 calc R . .
H23B H 0.9615 0.1982 0.1632 0.064 Uiso 1 1 calc R . .
C24 C 0.9492(6) 0.1718(5) 0.2871(4) 0.050(2) Uani 1 1 d . . .
H24A H 0.9580 0.1783 0.3316 0.060 Uiso 1 1 calc R . .
H24B H 0.8719 0.1887 0.2870 0.060 Uiso 1 1 calc R . .
C25 C 1.0230(7) 0.0546(6) 0.2612(5) 0.071(3) Uani 1 1 d . . .
H25A H 1.0278 0.0495 0.2153 0.106 Uiso 1 1 calc R . .
H25B H 0.9914 0.0100 0.2800 0.106 Uiso 1 1 calc R . .
H25C H 1.0965 0.0301 0.2719 0.106 Uiso 1 1 calc R . .
C26 C 1.0949(6) 0.2342(6) 0.2421(4) 0.0490(19) Uani 1 1 d . . .
H26A H 1.0984 0.3023 0.2393 0.059 Uiso 1 1 calc R . .
H26B H 1.1267 0.2003 0.2796 0.059 Uiso 1 1 calc R . .
C27 C 0.3430(6) 0.8711(6) 0.3353(4) 0.049(2) Uani 1 1 d . . .
H27A H 0.2861 0.9412 0.3331 0.059 Uiso 1 1 calc R . .
C28 C 0.3150(6) 0.7980(6) 0.3728(4) 0.061(2) Uani 1 1 d . . .
C29 C 0.1994(7) 0.8418(7) 0.4021(5) 0.075(3) Uani 1 1 d . . .
H29 H 0.1490 0.9124 0.3950 0.090 Uiso 1 1 calc R . .
C30 C 0.1634(8) 0.7825(8) 0.4395(5) 0.087(3) Uani 1 1 d . . .
H30 H 0.0882 0.8115 0.4574 0.105 Uiso 1 1 calc R . .
C31 C 0.2378(8) 0.6789(8) 0.4512(5) 0.087(3) Uani 1 1 d . . .
H31 H 0.2127 0.6386 0.4778 0.104 Uiso 1 1 calc R . .
C32 C 0.3491(8) 0.6340(8) 0.4241(5) 0.079(3) Uani 1 1 d . . .
C33 C 0.3902(7) 0.6924(7) 0.3836(4) 0.062(2) Uani 1 1 d . . .
C34 C 0.3930(9) 0.4751(8) 0.4810(6) 0.102(4) Uani 1 1 d . . .
H34A H 0.3381 0.5246 0.5151 0.152 Uiso 1 1 calc R . .
H34B H 0.4560 0.4224 0.4986 0.152 Uiso 1 1 calc R . .
H34C H 0.3607 0.4385 0.4595 0.152 Uiso 1 1 calc R . .
C35 C 0.4613(5) 0.9253(5) 0.2645(4) 0.0394(17) Uani 1 1 d . . .
C36 C 0.3990(6) 1.0415(5) 0.2980(4) 0.049(2) Uani 1 1 d . . .
H36A H 0.3192 1.0649 0.3038 0.059 Uiso 1 1 calc R . .
H36B H 0.4197 1.0387 0.3404 0.059 Uiso 1 1 calc R . .
C37 C 0.4209(7) 1.1257(6) 0.2633(4) 0.064(2) Uani 1 1 d . . .
H37A H 0.4986 1.1069 0.2603 0.096 Uiso 1 1 calc R . .
H37B H 0.3759 1.1954 0.2866 0.096 Uiso 1 1 calc R . .
H37C H 0.4022 1.1286 0.2208 0.096 Uiso 1 1 calc R . .
C38 C 0.4281(5) 0.9207(6) 0.1984(4) 0.0452(18) Uani 1 1 d . . .
H38A H 0.4479 0.9671 0.1708 0.054 Uiso 1 1 calc R . .
H38B H 0.4704 0.8468 0.1790 0.054 Uiso 1 1 calc R . .
C39 C 0.5873(5) 0.8855(5) 0.2551(4) 0.0420(18) Uani 1 1 d . . .
H39A H 0.6088 0.9176 0.2182 0.050 Uiso 1 1 calc R . .
H39B H 0.6063 0.9090 0.2927 0.050 Uiso 1 1 calc R . .
C40 C 1.0409(6) 0.5524(6) 0.1905(4) 0.0414(17) Uani 1 1 d . . .
H40 H 1.1165 0.5259 0.1927 0.050 Uiso 1 1 calc R . .
C41 C 1.0148(5) 0.5026(5) 0.1400(3) 0.0370(16) Uani 1 1 d . . .
C42 C 0.9073(5) 0.5287(5) 0.1299(3) 0.0356(16) Uani 1 1 d . . .
C43 C 0.8942(5) 0.4751(5) 0.0769(4) 0.0385(17) Uani 1 1 d . . .
C44 C 0.9854(6) 0.3965(5) 0.0373(4) 0.0444(18) Uani 1 1 d . . .
H44 H 0.9753 0.3614 0.0032 0.053 Uiso 1 1 calc R . .
C45 C 1.0927(6) 0.3696(6) 0.0483(4) 0.0482(19) Uani 1 1 d . . .
H45 H 1.1542 0.3166 0.0212 0.058 Uiso 1 1 calc R . .
C46 C 1.1085(5) 0.4197(5) 0.0977(4) 0.0439(18) Uani 1 1 d . . .
H46 H 1.1809 0.4004 0.1046 0.053 Uiso 1 1 calc R . .
C47 C 1.0158(5) 0.6748(6) 0.2790(4) 0.0426(18) Uani 1 1 d . . .
C48 C 1.1223(6) 0.5931(6) 0.3018(4) 0.054(2) Uani 1 1 d . . .
H48A H 1.1826 0.5701 0.2655 0.064 Uiso 1 1 calc R . .
H48B H 1.1391 0.6312 0.3338 0.064 Uiso 1 1 calc R . .
C49 C 1.1261(7) 0.4949(7) 0.3294(5) 0.072(3) Uani 1 1 d . . .
H49A H 1.0805 0.5139 0.3711 0.109 Uiso 1 1 calc R . .
H49B H 1.2019 0.4448 0.3332 0.109 Uiso 1 1 calc R . .
H49C H 1.0983 0.4615 0.3018 0.109 Uiso 1 1 calc R . .
C50 C 0.9203(5) 0.7286(6) 0.3352(4) 0.0473(19) Uani 1 1 d . . .
H50A H 0.9173 0.6738 0.3629 0.057 Uiso 1 1 calc R . .
H50B H 0.9328 0.7792 0.3604 0.057 Uiso 1 1 calc R . .
C51 C 0.7658(6) 0.4484(6) 0.0229(4) 0.055(2) Uani 1 1 d . . .
H51A H 0.8078 0.4477 -0.0179 0.083 Uiso 1 1 calc R . .
H51B H 0.6875 0.4827 0.0200 0.083 Uiso 1 1 calc R . .
H51C H 0.7890 0.3750 0.0345 0.083 Uiso 1 1 calc R . .
C52 C 1.0384(6) 0.7632(6) 0.2460(4) 0.0481(19) Uani 1 1 d . . .
H52A H 0.9704 0.8170 0.2322 0.058 Uiso 1 1 calc R . .
H52B H 1.0594 0.7995 0.2767 0.058 Uiso 1 1 calc R . .
C53 C 0.6171(8) 0.3378(7) 0.3528(5) 0.087(3) Uani 1 1 d U . .
H53A H 0.6014 0.3492 0.3994 0.104 Uiso 1 1 calc R . .
H53B H 0.6834 0.2684 0.3415 0.104 Uiso 1 1 calc R . .
C54 C 0.5177(9) 0.3323(9) 0.3290(6) 0.108(4) Uani 1 1 d . . .
H54A H 0.4538 0.4032 0.3352 0.162 Uiso 1 1 calc R . .
H54B H 0.4999 0.2820 0.3529 0.162 Uiso 1 1 calc R . .
H54C H 0.5376 0.3084 0.2841 0.162 Uiso 1 1 calc R . .
C55 C 0.1410(8) 0.8487(8) 0.0508(5) 0.091(3) Uani 1 1 d . . .
H55A H 0.1356 0.8821 0.0920 0.137 Uiso 1 1 calc R . .
H55B H 0.1529 0.8911 0.0174 0.137 Uiso 1 1 calc R . .
H55C H 0.2027 0.7765 0.0454 0.137 Uiso 1 1 calc R . .
C56 C 0.0399(8) 0.8436(8) 0.0474(5) 0.086(3) Uani 1 1 d . . .
H56A H -0.0236 0.9139 0.0619 0.103 Uiso 1 1 calc R . .
H56B H 0.0376 0.8270 0.0031 0.103 Uiso 1 1 calc R . .
C57 C 0.713(3) 0.045(2) 0.3987(18) 0.106(8) Uani 0.652(16) 1 d P B 1
H57A H 0.6439 0.0999 0.4237 0.128 Uiso 0.652(16) 1 calc PR B 1
H57B H 0.7117 0.0612 0.3539 0.128 Uiso 0.652(16) 1 calc PR B 1
C58 C 0.812(3) 0.052(2) 0.4209(18) 0.122(9) Uani 0.652(16) 1 d P B 1
H58A H 0.7848 0.1177 0.4482 0.183 Uiso 0.652(16) 1 calc PR B 1
H58B H 0.8618 0.0534 0.3839 0.183 Uiso 0.652(16) 1 calc PR B 1
H58C H 0.8517 -0.0096 0.4443 0.183 Uiso 0.652(16) 1 calc PR B 1
C57' C 0.804(5) 0.019(3) 0.372(3) 0.106(13) Uani 0.348(16) 1 d P B 2
H57C H 0.8399 0.0596 0.3511 0.127 Uiso 0.348(16) 1 calc PR B 2
H57D H 0.8626 -0.0486 0.3836 0.127 Uiso 0.348(16) 1 calc PR B 2
C58' C 0.728(5) 0.085(4) 0.434(3) 0.112(16) Uani 0.348(16) 1 d P B 2
H58D H 0.6728 0.1539 0.4237 0.167 Uiso 0.348(16) 1 calc PR B 2
H58E H 0.7727 0.0961 0.4620 0.167 Uiso 0.348(16) 1 calc PR B 2
H58F H 0.6925 0.0456 0.4554 0.167 Uiso 0.348(16) 1 calc PR B 2


_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 1.905(4) . ?
Cu1 O3 1.946(4) . ?
Cu1 N1 1.947(5) . ?
Cu1 O13 2.029(4) . ?
Cu1 O14 2.370(4) . ?
Cu1 O12 2.578(4) . ?
Cu2 O3 1.930(4) . ?
Cu2 N2 1.943(5) . ?
Cu2 O5 1.949(4) . ?
Cu2 O7 2.019(5) . ?
Cu2 O18 2.292(5) . ?
Cu3 O9 1.898(4) . ?
Cu3 N3 1.943(5) . ?
Cu3 O12 1.958(4) . ?
Cu3 O5 2.041(4) . ?
Cu3 O6 2.359(5) . ?
Cu3 O3 2.654(4) . ?
Cu4 O12 1.936(4) . ?
Cu4 O13 1.947(4) . ?
Cu4 N4 1.964(5) . ?
Cu4 O15 2.002(5) . ?
Cu4 O17 2.473(5) . ?
Cl1 O22 1.408(6) . ?
Cl1 O21 1.414(7) . ?
Cl1 O19 1.431(6) . ?
Cl1 O20 1.434(6) . ?
Cl2 O24' 1.328(18) . ?
Cl2 O26 1.369(19) . ?
Cl2 O25' 1.380(18) . ?
Cl2 O25 1.386(18) . ?
Cl2 O23' 1.397(19) . ?
Cl2 O23 1.414(17) . ?
Cl2 O24 1.424(17) . ?
Cl2 O26' 1.440(19) . ?
N1 C1 1.292(9) . ?
N1 C9 1.480(8) . ?
N2 C14 1.280(9) . ?
N2 C22 1.495(8) . ?
N3 C27 1.284(8) . ?
N3 C35 1.482(8) . ?
N4 C40 1.272(8) . ?
N4 C47 1.495(9) . ?
O1 C3 1.329(8) . ?
O2 C4 1.352(8) . ?
O2 C8 1.412(8) . ?
O3 C10 1.438(7) . ?
O4 C13 1.441(8) . ?
O5 C16 1.337(8) . ?
O6 C17 1.379(8) . ?
O6 C21 1.423(8) . ?
O7 C23 1.456(8) . ?
O8 C26 1.417(9) . ?
O9 C33 1.318(8) . ?
O10 C32 1.357(10) . ?
O10 C34 1.445(10) . ?
O11 C38 1.436(8) . ?
O12 C39 1.436(7) . ?
O13 C42 1.347(7) . ?
O14 C43 1.375(7) . ?
O14 C51 1.405(8) . ?
O15 C50 1.439(8) . ?
O16 C52 1.426(8) . ?
O18 C53 1.431(9) . ?
O27 C57 1.41(2) . ?
O27' C57' 1.44(7) . ?
O28 C56 1.412(10) . ?
C1 C2 1.428(10) . ?
C2 C3 1.409(9) . ?
C2 C7 1.431(10) . ?
C3 C4 1.415(9) . ?
C4 C5 1.384(10) . ?
C5 C6 1.394(11) . ?
C6 C7 1.362(10) . ?
C9 C10 1.523(9) . ?
C9 C13 1.537(9) . ?
C9 C11 1.545(9) . ?
C11 C12 1.499(10) . ?
C14 C15 1.444(9) . ?
C15 C16 1.410(9) . ?
C15 C20 1.423(10) . ?
C16 C17 1.424(9) . ?
C17 C18 1.390(10) . ?
C18 C19 1.385(10) . ?
C19 C20 1.342(9) . ?
C22 C23 1.528(10) . ?
C22 C24 1.538(9) . ?
C22 C26 1.547(9) . ?
C24 C25 1.514(10) . ?
C27 C28 1.439(10) . ?
C28 C33 1.390(11) . ?
C28 C29 1.440(10) . ?
C29 C30 1.341(11) . ?
C30 C31 1.373(12) . ?
C31 C32 1.378(11) . ?
C32 C33 1.408(11) . ?
C35 C39 1.525(8) . ?
C35 C38 1.532(10) . ?
C35 C36 1.547(9) . ?
C36 C37 1.498(10) . ?
C40 C41 1.439(10) . ?
C41 C42 1.388(9) . ?
C41 C46 1.440(9) . ?
C42 C43 1.420(9) . ?
C43 C44 1.372(9) . ?
C44 C45 1.389(10) . ?
C45 C46 1.348(10) . ?
C47 C48 1.520(10) . ?
C47 C50 1.522(10) . ?
C47 C52 1.539(9) . ?
C48 C49 1.463(10) . ?
C53 C54 1.545(14) . ?
C55 C56 1.426(12) . ?
C57 C58 1.54(5) . ?
C57' C58' 1.53(8) . ?

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 O3 171.59(18) . . ?
O1 Cu1 N1 95.3(2) . . ?
O3 Cu1 N1 84.2(2) . . ?
O1 Cu1 O13 92.08(17) . . ?
O3 Cu1 O13 90.34(17) . . ?
N1 Cu1 O13 165.1(2) . . ?
O1 Cu1 O14 91.57(18) . . ?
O3 Cu1 O14 96.84(17) . . ?
N1 Cu1 O14 93.1(2) . . ?
O13 Cu1 O14 73.70(16) . . ?
O1 Cu1 O12 87.06(17) . . ?
O3 Cu1 O12 86.17(16) . . ?
N1 Cu1 O12 122.98(19) . . ?
O13 Cu1 O12 70.26(15) . . ?
O14 Cu1 O12 143.86(14) . . ?
O3 Cu2 N2 170.5(2) . . ?
O3 Cu2 O5 89.05(18) . . ?
N2 Cu2 O5 93.1(2) . . ?
O3 Cu2 O7 94.45(19) . . ?
N2 Cu2 O7 82.0(2) . . ?
O5 Cu2 O7 170.45(19) . . ?
O3 Cu2 O18 91.31(18) . . ?
N2 Cu2 O18 98.0(2) . . ?
O5 Cu2 O18 88.60(19) . . ?
O7 Cu2 O18 100.2(2) . . ?
O9 Cu3 N3 95.0(2) . . ?
O9 Cu3 O12 172.7(2) . . ?
N3 Cu3 O12 84.79(19) . . ?
O9 Cu3 O5 92.81(19) . . ?
N3 Cu3 O5 168.1(2) . . ?
O12 Cu3 O5 88.59(17) . . ?
O9 Cu3 O6 90.5(2) . . ?
N3 Cu3 O6 96.1(2) . . ?
O12 Cu3 O6 96.79(18) . . ?
O5 Cu3 O6 74.88(17) . . ?
O9 Cu3 O3 89.97(18) . . ?
N3 Cu3 O3 119.5(2) . . ?
O12 Cu3 O3 83.83(15) . . ?
O5 Cu3 O3 69.39(16) . . ?
O6 Cu3 O3 144.24(14) . . ?
O12 Cu4 O13 87.66(17) . . ?
O12 Cu4 N4 175.0(2) . . ?
O13 Cu4 N4 93.2(2) . . ?
O12 Cu4 O15 96.54(18) . . ?
O13 Cu4 O15 171.06(19) . . ?
N4 Cu4 O15 82.0(2) . . ?
O12 Cu4 O17 90.44(16) . . ?
O13 Cu4 O17 84.39(17) . . ?
N4 Cu4 O17 94.58(18) . . ?
O15 Cu4 O17 103.41(18) . . ?
O22 Cl1 O21 111.3(4) . . ?
O22 Cl1 O19 109.0(4) . . ?
O21 Cl1 O19 108.9(4) . . ?
O22 Cl1 O20 109.4(4) . . ?
O21 Cl1 O20 109.5(4) . . ?
O19 Cl1 O20 108.7(4) . . ?
O24' Cl2 O26 109.9(12) . . ?
O24' Cl2 O25' 118.6(13) . . ?
O24' Cl2 O25 63.7(11) . . ?
O26 Cl2 O25 116.9(12) . . ?
O25' Cl2 O25 82.4(12) . . ?
O24' Cl2 O23' 116.0(13) . . ?
O26 Cl2 O23' 73.2(12) . . ?
O25' Cl2 O23' 105.7(12) . . ?
O25 Cl2 O23' 169.7(11) . . ?
O24' Cl2 O23 47.4(9) . . ?
O26 Cl2 O23 110.9(13) . . ?
O25' Cl2 O23 150.3(12) . . ?
O25 Cl2 O23 105.2(10) . . ?
O23' Cl2 O23 71.1(10) . . ?
O24' Cl2 O24 137.3(12) . . ?
O26 Cl2 O24 110.1(12) . . ?
O25' Cl2 O24 100.8(11) . . ?
O25 Cl2 O24 109.4(12) . . ?
O23' Cl2 O24 63.3(10) . . ?
O23 Cl2 O24 103.3(10) . . ?
O24' Cl2 O26' 106.6(11) . . ?
O26 Cl2 O26' 139.1(11) . . ?
O25' Cl2 O26' 102.0(13) . . ?
O25 Cl2 O26' 64.8(10) . . ?
O23' Cl2 O26' 106.6(12) . . ?
O23 Cl2 O26' 107.2(10) . . ?
O24 Cl2 O26' 45.3(8) . . ?
C1 N1 C9 121.9(6) . . ?
C1 N1 Cu1 123.1(5) . . ?
C9 N1 Cu1 114.9(4) . . ?
C14 N2 C22 118.5(6) . . ?
C14 N2 Cu2 123.2(5) . . ?
C22 N2 Cu2 117.4(5) . . ?
C27 N3 C35 121.2(6) . . ?
C27 N3 Cu3 124.7(5) . . ?
C35 N3 Cu3 114.1(4) . . ?
C40 N4 C47 120.2(5) . . ?
C40 N4 Cu4 124.0(5) . . ?
C47 N4 Cu4 115.5(4) . . ?
C3 O1 Cu1 124.5(4) . . ?
C4 O2 C8 118.2(6) . . ?
C10 O3 Cu2 116.0(4) . . ?
C10 O3 Cu1 109.1(4) . . ?
Cu2 O3 Cu1 120.3(2) . . ?
C10 O3 Cu3 128.5(4) . . ?
Cu2 O3 Cu3 89.41(17) . . ?
Cu1 O3 Cu3 91.58(15) . . ?
C16 O5 Cu2 125.0(4) . . ?
C16 O5 Cu3 118.2(4) . . ?
Cu2 O5 Cu3 109.8(2) . . ?
C17 O6 C21 117.3(6) . . ?
C17 O6 Cu3 108.4(4) . . ?
C21 O6 Cu3 125.4(4) . . ?
C23 O7 Cu2 109.9(4) . . ?
C33 O9 Cu3 125.9(5) . . ?
C32 O10 C34 115.9(7) . . ?
C39 O12 Cu4 117.5(3) . . ?
C39 O12 Cu3 107.7(4) . . ?
Cu4 O12 Cu3 116.9(2) . . ?
C39 O12 Cu1 127.9(4) . . ?
Cu4 O12 Cu1 91.29(16) . . ?
Cu3 O12 Cu1 93.62(16) . . ?
C42 O13 Cu4 126.7(4) . . ?
C42 O13 Cu1 121.3(4) . . ?
Cu4 O13 Cu1 110.08(19) . . ?
C43 O14 C51 117.7(5) . . ?
C43 O14 Cu1 110.8(4) . . ?
C51 O14 Cu1 131.4(4) . . ?
C50 O15 Cu4 111.8(4) . . ?
C53 O18 Cu2 145.2(5) . . ?
N1 C1 C2 126.3(7) . . ?
C3 C2 C1 124.3(7) . . ?
C3 C2 C7 118.8(7) . . ?
C1 C2 C7 116.8(7) . . ?
O1 C3 C2 124.1(6) . . ?
O1 C3 C4 117.1(6) . . ?
C2 C3 C4 118.8(7) . . ?
O2 C4 C5 124.6(7) . . ?
O2 C4 C3 115.0(6) . . ?
C5 C4 C3 120.3(7) . . ?
C4 C5 C6 120.8(8) . . ?
C7 C6 C5 120.0(8) . . ?
C6 C7 C2 121.0(7) . . ?
N1 C9 C10 104.8(5) . . ?
N1 C9 C13 107.3(5) . . ?
C10 C9 C13 108.2(6) . . ?
N1 C9 C11 113.3(6) . . ?
C10 C9 C11 110.7(5) . . ?
C13 C9 C11 112.1(5) . . ?
O3 C10 C9 111.5(5) . . ?
C12 C11 C9 116.0(7) . . ?
O4 C13 C9 112.3(6) . . ?
N2 C14 C15 127.6(7) . . ?
C16 C15 C20 119.5(6) . . ?
C16 C15 C14 123.7(7) . . ?
C20 C15 C14 116.7(6) . . ?
O5 C16 C15 122.3(6) . . ?
O5 C16 C17 119.9(6) . . ?
C15 C16 C17 117.8(7) . . ?
O6 C17 C18 123.8(6) . . ?
O6 C17 C16 115.6(6) . . ?
C18 C17 C16 120.5(6) . . ?
C19 C18 C17 120.1(7) . . ?
C20 C19 C18 121.1(7) . . ?
C19 C20 C15 120.9(7) . . ?
N2 C22 C23 105.2(5) . . ?
N2 C22 C24 107.9(6) . . ?
C23 C22 C24 112.2(6) . . ?
N2 C22 C26 110.4(5) . . ?
C23 C22 C26 107.6(6) . . ?
C24 C22 C26 113.3(6) . . ?
O7 C23 C22 110.0(6) . . ?
C25 C24 C22 116.2(6) . . ?
O8 C26 C22 112.2(6) . . ?
N3 C27 C28 124.7(7) . . ?
C33 C28 C27 125.3(7) . . ?
C33 C28 C29 119.3(7) . . ?
C27 C28 C29 115.4(7) . . ?
C30 C29 C28 121.1(8) . . ?
C29 C30 C31 119.8(8) . . ?
C30 C31 C32 120.9(8) . . ?
O10 C32 C31 125.0(8) . . ?
O10 C32 C33 113.7(7) . . ?
C31 C32 C33 121.2(9) . . ?
O9 C33 C28 124.0(7) . . ?
O9 C33 C32 118.3(7) . . ?
C28 C33 C32 117.6(7) . . ?
N3 C35 C39 105.9(5) . . ?
N3 C35 C38 109.2(5) . . ?
C39 C35 C38 108.3(6) . . ?
N3 C35 C36 111.4(6) . . ?
C39 C35 C36 109.8(5) . . ?
C38 C35 C36 112.0(6) . . ?
C37 C36 C35 115.6(6) . . ?
O11 C38 C35 113.0(6) . . ?
O12 C39 C35 111.4(5) . . ?
N4 C40 C41 127.7(6) . . ?
C42 C41 C40 124.8(6) . . ?
C42 C41 C46 118.9(6) . . ?
C40 C41 C46 116.4(6) . . ?
O13 C42 C41 122.3(6) . . ?
O13 C42 C43 119.1(6) . . ?
C41 C42 C43 118.5(6) . . ?
C44 C43 O14 124.1(7) . . ?
C44 C43 C42 121.1(6) . . ?
O14 C43 C42 114.7(6) . . ?
C43 C44 C45 120.0(7) . . ?
C46 C45 C44 120.6(7) . . ?
C45 C46 C41 120.8(6) . . ?
N4 C47 C48 114.9(6) . . ?
N4 C47 C50 105.6(5) . . ?
C48 C47 C50 111.2(6) . . ?
N4 C47 C52 107.8(6) . . ?
C48 C47 C52 108.4(6) . . ?
C50 C47 C52 108.8(6) . . ?
C49 C48 C47 119.2(7) . . ?
O15 C50 C47 109.5(6) . . ?
O16 C52 C47 111.7(6) . . ?
O18 C53 C54 114.0(9) . . ?
O28 C56 C55 111.2(8) . . ?
O27 C57 C58 114(2) . . ?
O27' C57' C58' 114(6) . . ?

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
O1 Cu1 N1 C1 12.7(6) . . . . ?
O3 Cu1 N1 C1 -175.7(6) . . . . ?
O13 Cu1 N1 C1 -106.6(9) . . . . ?
O14 Cu1 N1 C1 -79.1(6) . . . . ?
O12 Cu1 N1 C1 102.7(6) . . . . ?
O1 Cu1 N1 C9 -171.0(4) . . . . ?
O3 Cu1 N1 C9 0.6(4) . . . . ?
O13 Cu1 N1 C9 69.7(10) . . . . ?
O14 Cu1 N1 C9 97.2(4) . . . . ?
O12 Cu1 N1 C9 -81.0(5) . . . . ?
O5 Cu2 N2 C14 19.4(6) . . . . ?
O7 Cu2 N2 C14 -168.8(6) . . . . ?
O18 Cu2 N2 C14 -69.6(6) . . . . ?
O5 Cu2 N2 C22 -171.4(4) . . . . ?
O7 Cu2 N2 C22 0.3(4) . . . . ?
O18 Cu2 N2 C22 99.5(5) . . . . ?
O9 Cu3 N3 C27 4.4(7) . . . . ?
O12 Cu3 N3 C27 177.1(7) . . . . ?
O5 Cu3 N3 C27 -126.5(10) . . . . ?
O6 Cu3 N3 C27 -86.6(6) . . . . ?
O3 Cu3 N3 C27 97.2(7) . . . . ?
O9 Cu3 N3 C35 -176.0(5) . . . . ?
O12 Cu3 N3 C35 -3.3(5) . . . . ?
O5 Cu3 N3 C35 53.1(13) . . . . ?
O6 Cu3 N3 C35 93.0(5) . . . . ?
O3 Cu3 N3 C35 -83.2(5) . . . . ?
O13 Cu4 N4 C40 8.4(6) . . . . ?
O15 Cu4 N4 C40 -179.2(6) . . . . ?
O17 Cu4 N4 C40 -76.2(6) . . . . ?
O13 Cu4 N4 C47 -178.2(4) . . . . ?
O15 Cu4 N4 C47 -5.8(4) . . . . ?
O17 Cu4 N4 C47 97.1(4) . . . . ?
N1 Cu1 O1 C3 -17.3(5) . . . . ?
O13 Cu1 O1 C3 149.7(5) . . . . ?
O14 Cu1 O1 C3 76.0(5) . . . . ?
O12 Cu1 O1 C3 -140.2(5) . . . . ?
O5 Cu2 O3 C10 -143.9(4) . . . . ?
O7 Cu2 O3 C10 45.0(4) . . . . ?
O18 Cu2 O3 C10 -55.3(4) . . . . ?
O5 Cu2 O3 Cu1 81.1(3) . . . . ?
O7 Cu2 O3 Cu1 -90.0(3) . . . . ?
O18 Cu2 O3 Cu1 169.6(3) . . . . ?
O5 Cu2 O3 Cu3 -10.41(15) . . . . ?
O7 Cu2 O3 Cu3 178.48(16) . . . . ?
O18 Cu2 O3 Cu3 78.16(16) . . . . ?
N1 Cu1 O3 C10 22.4(4) . . . . ?
O13 Cu1 O3 C10 -143.6(4) . . . . ?
O14 Cu1 O3 C10 -70.0(4) . . . . ?
O12 Cu1 O3 C10 146.2(4) . . . . ?
N1 Cu1 O3 Cu2 160.2(3) . . . . ?
O13 Cu1 O3 Cu2 -5.9(3) . . . . ?
O14 Cu1 O3 Cu2 67.8(3) . . . . ?
O12 Cu1 O3 Cu2 -76.1(2) . . . . ?
N1 Cu1 O3 Cu3 -109.54(18) . . . . ?
O13 Cu1 O3 Cu3 84.37(15) . . . . ?
O14 Cu1 O3 Cu3 157.99(14) . . . . ?
O12 Cu1 O3 Cu3 14.18(12) . . . . ?
O9 Cu3 O3 C10 41.2(5) . . . . ?
N3 Cu3 O3 C10 -54.5(5) . . . . ?
O12 Cu3 O3 C10 -135.0(5) . . . . ?
O5 Cu3 O3 C10 134.2(5) . . . . ?
O6 Cu3 O3 C10 132.0(5) . . . . ?
O9 Cu3 O3 Cu2 -82.39(19) . . . . ?
N3 Cu3 O3 Cu2 -178.13(19) . . . . ?
O12 Cu3 O3 Cu2 101.43(17) . . . . ?
O5 Cu3 O3 Cu2 10.62(15) . . . . ?
O6 Cu3 O3 Cu2 8.4(3) . . . . ?
O9 Cu3 O3 Cu1 157.3(2) . . . . ?
N3 Cu3 O3 Cu1 61.6(2) . . . . ?
O12 Cu3 O3 Cu1 -18.88(17) . . . . ?
O5 Cu3 O3 Cu1 -109.69(19) . . . . ?
O6 Cu3 O3 Cu1 -111.9(2) . . . . ?
O3 Cu2 O5 C16 164.4(5) . . . . ?
N2 Cu2 O5 C16 -24.8(5) . . . . ?
O18 Cu2 O5 C16 73.1(5) . . . . ?
O3 Cu2 O5 Cu3 14.5(2) . . . . ?
N2 Cu2 O5 Cu3 -174.8(2) . . . . ?
O18 Cu2 O5 Cu3 -76.9(2) . . . . ?
O9 Cu3 O5 C16 -74.6(4) . . . . ?
N3 Cu3 O5 C16 56.5(12) . . . . ?
O12 Cu3 O5 C16 112.6(4) . . . . ?
O6 Cu3 O5 C16 15.2(4) . . . . ?
O3 Cu3 O5 C16 -163.5(5) . . . . ?
O9 Cu3 O5 Cu2 77.7(2) . . . . ?
N3 Cu3 O5 Cu2 -151.2(10) . . . . ?
O12 Cu3 O5 Cu2 -95.1(2) . . . . ?
O6 Cu3 O5 Cu2 167.4(2) . . . . ?
O3 Cu3 O5 Cu2 -11.19(16) . . . . ?
O9 Cu3 O6 C17 78.7(4) . . . . ?
N3 Cu3 O6 C17 173.8(4) . . . . ?
O12 Cu3 O6 C17 -100.7(4) . . . . ?
O5 Cu3 O6 C17 -14.1(4) . . . . ?
O3 Cu3 O6 C17 -11.9(5) . . . . ?
O9 Cu3 O6 C21 -67.4(6) . . . . ?
N3 Cu3 O6 C21 27.7(6) . . . . ?
O12 Cu3 O6 C21 113.1(6) . . . . ?
O5 Cu3 O6 C21 -160.2(6) . . . . ?
O3 Cu3 O6 C21 -158.0(5) . . . . ?
O3 Cu2 O7 C23 147.9(4) . . . . ?
N2 Cu2 O7 C23 -23.3(5) . . . . ?
O18 Cu2 O7 C23 -120.0(5) . . . . ?
N3 Cu3 O9 C33 -5.9(7) . . . . ?
O5 Cu3 O9 C33 165.1(7) . . . . ?
O6 Cu3 O9 C33 90.2(7) . . . . ?
O3 Cu3 O9 C33 -125.6(7) . . . . ?
O13 Cu4 O12 C39 -140.6(5) . . . . ?
O15 Cu4 O12 C39 47.3(5) . . . . ?
O17 Cu4 O12 C39 -56.2(5) . . . . ?
O13 Cu4 O12 Cu3 88.9(2) . . . . ?
O15 Cu4 O12 Cu3 -83.2(3) . . . . ?
O17 Cu4 O12 Cu3 173.3(2) . . . . ?
O13 Cu4 O12 Cu1 -5.82(16) . . . . ?
O15 Cu4 O12 Cu1 -177.90(16) . . . . ?
O17 Cu4 O12 Cu1 78.55(15) . . . . ?
N3 Cu3 O12 C39 25.5(4) . . . . ?
O5 Cu3 O12 C39 -144.6(4) . . . . ?
O6 Cu3 O12 C39 -70.0(4) . . . . ?
O3 Cu3 O12 C39 146.0(4) . . . . ?
N3 Cu3 O12 Cu4 160.4(3) . . . . ?
O5 Cu3 O12 Cu4 -9.7(2) . . . . ?
O6 Cu3 O12 Cu4 64.9(2) . . . . ?
O3 Cu3 O12 Cu4 -79.1(2) . . . . ?
N3 Cu3 O12 Cu1 -106.3(2) . . . . ?
O5 Cu3 O12 Cu1 83.58(16) . . . . ?
O6 Cu3 O12 Cu1 158.17(14) . . . . ?
O3 Cu3 O12 Cu1 14.16(12) . . . . ?
O1 Cu1 O12 C39 39.7(4) . . . . ?
O3 Cu1 O12 C39 -135.3(4) . . . . ?
N1 Cu1 O12 C39 -54.7(5) . . . . ?
O13 Cu1 O12 C39 133.0(4) . . . . ?
O14 Cu1 O12 C39 128.4(4) . . . . ?
O1 Cu1 O12 Cu4 -87.34(18) . . . . ?
O3 Cu1 O12 Cu4 97.66(17) . . . . ?
N1 Cu1 O12 Cu4 178.3(2) . . . . ?
O13 Cu1 O12 Cu4 5.93(16) . . . . ?
O14 Cu1 O12 Cu4 1.3(3) . . . . ?
O1 Cu1 O12 Cu3 155.57(18) . . . . ?
O3 Cu1 O12 Cu3 -19.43(17) . . . . ?
N1 Cu1 O12 Cu3 61.2(3) . . . . ?
O13 Cu1 O12 Cu3 -111.16(19) . . . . ?
O14 Cu1 O12 Cu3 -115.8(2) . . . . ?
O12 Cu4 O13 C42 172.0(5) . . . . ?
N4 Cu4 O13 C42 -13.0(5) . . . . ?
O17 Cu4 O13 C42 81.3(5) . . . . ?
O12 Cu4 O13 Cu1 7.9(2) . . . . ?
N4 Cu4 O13 Cu1 -177.1(2) . . . . ?
O17 Cu4 O13 Cu1 -82.8(2) . . . . ?
O1 Cu1 O13 C42 -85.2(5) . . . . ?
O3 Cu1 O13 C42 102.8(5) . . . . ?
N1 Cu1 O13 C42 34.4(11) . . . . ?
O14 Cu1 O13 C42 5.8(4) . . . . ?
O12 Cu1 O13 C42 -171.4(5) . . . . ?
O1 Cu1 O13 Cu4 79.9(2) . . . . ?
O3 Cu1 O13 Cu4 -92.1(2) . . . . ?
N1 Cu1 O13 Cu4 -160.5(8) . . . . ?
O14 Cu1 O13 Cu4 170.9(2) . . . . ?
O12 Cu1 O13 Cu4 -6.28(17) . . . . ?
O1 Cu1 O14 C43 87.2(4) . . . . ?
O3 Cu1 O14 C43 -92.9(4) . . . . ?
N1 Cu1 O14 C43 -177.4(4) . . . . ?
O13 Cu1 O14 C43 -4.5(4) . . . . ?
O12 Cu1 O14 C43 0.0(5) . . . . ?
O1 Cu1 O14 C51 -97.5(6) . . . . ?
O3 Cu1 O14 C51 82.4(6) . . . . ?
N1 Cu1 O14 C51 -2.1(6) . . . . ?
O13 Cu1 O14 C51 170.8(6) . . . . ?
O12 Cu1 O14 C51 175.3(5) . . . . ?
O12 Cu4 O15 C50 156.2(4) . . . . ?
N4 Cu4 O15 C50 -19.0(4) . . . . ?
O17 Cu4 O15 C50 -111.8(4) . . . . ?
O3 Cu2 O18 C53 122.9(11) . . . . ?
N2 Cu2 O18 C53 -55.1(11) . . . . ?
O5 Cu2 O18 C53 -148.1(11) . . . . ?
O7 Cu2 O18 C53 28.1(11) . . . . ?
C9 N1 C1 C2 -179.8(6) . . . . ?
Cu1 N1 C1 C2 -3.8(10) . . . . ?
N1 C1 C2 C3 -6.0(12) . . . . ?
N1 C1 C2 C7 173.6(7) . . . . ?
Cu1 O1 C3 C2 13.1(9) . . . . ?
Cu1 O1 C3 C4 -168.3(4) . . . . ?
C1 C2 C3 O1 1.0(11) . . . . ?
C7 C2 C3 O1 -178.6(6) . . . . ?
C1 C2 C3 C4 -177.5(7) . . . . ?
C7 C2 C3 C4 2.8(10) . . . . ?
C8 O2 C4 C5 -3.6(10) . . . . ?
C8 O2 C4 C3 174.2(6) . . . . ?
O1 C3 C4 O2 -1.8(9) . . . . ?
C2 C3 C4 O2 176.8(6) . . . . ?
O1 C3 C4 C5 176.1(6) . . . . ?
C2 C3 C4 C5 -5.3(10) . . . . ?
O2 C4 C5 C6 -178.3(7) . . . . ?
C3 C4 C5 C6 4.0(11) . . . . ?
C4 C5 C6 C7 -0.3(12) . . . . ?
C5 C6 C7 C2 -2.2(12) . . . . ?
C3 C2 C7 C6 0.9(11) . . . . ?
C1 C2 C7 C6 -178.8(7) . . . . ?
C1 N1 C9 C10 154.7(6) . . . . ?
Cu1 N1 C9 C10 -21.6(6) . . . . ?
C1 N1 C9 C13 -90.4(8) . . . . ?
Cu1 N1 C9 C13 93.3(5) . . . . ?
C1 N1 C9 C11 33.9(9) . . . . ?
Cu1 N1 C9 C11 -142.4(5) . . . . ?
Cu2 O3 C10 C9 178.8(4) . . . . ?
Cu1 O3 C10 C9 -41.4(6) . . . . ?
Cu3 O3 C10 C9 66.8(7) . . . . ?
N1 C9 C10 O3 40.4(7) . . . . ?
C13 C9 C10 O3 -73.9(7) . . . . ?
C11 C9 C10 O3 162.9(6) . . . . ?
N1 C9 C11 C12 168.0(6) . . . . ?
C10 C9 C11 C12 50.6(8) . . . . ?
C13 C9 C11 C12 -70.4(8) . . . . ?
N1 C9 C13 O4 58.4(7) . . . . ?
C10 C9 C13 O4 171.0(5) . . . . ?
C11 C9 C13 O4 -66.6(7) . . . . ?
C22 N2 C14 C15 -178.9(6) . . . . ?
Cu2 N2 C14 C15 -9.9(10) . . . . ?
N2 C14 C15 C16 -3.0(12) . . . . ?
N2 C14 C15 C20 177.1(7) . . . . ?
Cu2 O5 C16 C15 19.8(8) . . . . ?
Cu3 O5 C16 C15 167.5(5) . . . . ?
Cu2 O5 C16 C17 -162.4(4) . . . . ?
Cu3 O5 C16 C17 -14.7(8) . . . . ?
C20 C15 C16 O5 177.6(6) . . . . ?
C14 C15 C16 O5 -2.2(10) . . . . ?
C20 C15 C16 C17 -0.2(9) . . . . ?
C14 C15 C16 C17 179.9(6) . . . . ?
C21 O6 C17 C18 -22.4(10) . . . . ?
Cu3 O6 C17 C18 -171.6(6) . . . . ?
C21 O6 C17 C16 160.7(6) . . . . ?
Cu3 O6 C17 C16 11.5(6) . . . . ?
O5 C16 C17 O6 0.2(9) . . . . ?
C15 C16 C17 O6 178.1(6) . . . . ?
O5 C16 C17 C18 -176.8(6) . . . . ?
C15 C16 C17 C18 1.1(10) . . . . ?
O6 C17 C18 C19 -177.3(6) . . . . ?
C16 C17 C18 C19 -0.6(10) . . . . ?
C17 C18 C19 C20 -1.0(11) . . . . ?
C18 C19 C20 C15 1.9(11) . . . . ?
C16 C15 C20 C19 -1.3(10) . . . . ?
C14 C15 C20 C19 178.6(6) . . . . ?
C14 N2 C22 C23 -169.4(6) . . . . ?
Cu2 N2 C22 C23 21.0(7) . . . . ?
C14 N2 C22 C24 70.7(8) . . . . ?
Cu2 N2 C22 C24 -99.0(6) . . . . ?
C14 N2 C22 C26 -53.6(8) . . . . ?
Cu2 N2 C22 C26 136.7(5) . . . . ?
Cu2 O7 C23 C22 41.4(7) . . . . ?
N2 C22 C23 O7 -39.4(7) . . . . ?
C24 C22 C23 O7 77.6(7) . . . . ?
C26 C22 C23 O7 -157.1(5) . . . . ?
N2 C22 C24 C25 -175.3(7) . . . . ?
C23 C22 C24 C25 69.3(8) . . . . ?
C26 C22 C24 C25 -52.8(9) . . . . ?
N2 C22 C26 O8 -152.1(6) . . . . ?
C23 C22 C26 O8 -37.8(8) . . . . ?
C24 C22 C26 O8 86.8(8) . . . . ?
C35 N3 C27 C28 176.8(7) . . . . ?
Cu3 N3 C27 C28 -3.6(12) . . . . ?
N3 C27 C28 C33 2.8(15) . . . . ?
N3 C27 C28 C29 -178.8(8) . . . . ?
C33 C28 C29 C30 0.0(16) . . . . ?
C27 C28 C29 C30 -178.4(9) . . . . ?
C28 C29 C30 C31 1.2(17) . . . . ?
C29 C30 C31 C32 -1.2(18) . . . . ?
C34 O10 C32 C31 -1.5(16) . . . . ?
C34 O10 C32 C33 175.2(9) . . . . ?
C30 C31 C32 O10 176.5(11) . . . . ?
C30 C31 C32 C33 -0.1(18) . . . . ?
Cu3 O9 C33 C28 6.7(13) . . . . ?
Cu3 O9 C33 C32 -174.7(7) . . . . ?
C27 C28 C33 O9 -4.4(16) . . . . ?
C29 C28 C33 O9 177.3(9) . . . . ?
C27 C28 C33 C32 177.0(9) . . . . ?
C29 C28 C33 C32 -1.3(14) . . . . ?
O10 C32 C33 O9 5.7(14) . . . . ?
C31 C32 C33 O9 -177.4(10) . . . . ?
O10 C32 C33 C28 -175.6(9) . . . . ?
C31 C32 C33 C28 1.3(16) . . . . ?
C27 N3 C35 C39 161.4(7) . . . . ?
Cu3 N3 C35 C39 -18.2(7) . . . . ?
C27 N3 C35 C38 -82.2(8) . . . . ?
Cu3 N3 C35 C38 98.2(5) . . . . ?
C27 N3 C35 C36 42.1(9) . . . . ?
Cu3 N3 C35 C36 -137.5(5) . . . . ?
N3 C35 C36 C37 175.7(6) . . . . ?
C39 C35 C36 C37 58.7(9) . . . . ?
C38 C35 C36 C37 -61.7(8) . . . . ?
N3 C35 C38 O11 63.9(7) . . . . ?
C39 C35 C38 O11 178.8(5) . . . . ?
C36 C35 C38 O11 -60.0(7) . . . . ?
Cu4 O12 C39 C35 -177.7(4) . . . . ?
Cu3 O12 C39 C35 -43.1(7) . . . . ?
Cu1 O12 C39 C35 66.4(7) . . . . ?
N3 C35 C39 O12 39.8(8) . . . . ?
C38 C35 C39 O12 -77.1(7) . . . . ?
C36 C35 C39 O12 160.2(6) . . . . ?
C47 N4 C40 C41 -176.1(6) . . . . ?
Cu4 N4 C40 C41 -3.1(10) . . . . ?
N4 C40 C41 C42 -1.9(12) . . . . ?
N4 C40 C41 C46 178.4(7) . . . . ?
Cu4 O13 C42 C41 12.1(9) . . . . ?
Cu1 O13 C42 C41 174.5(5) . . . . ?
Cu4 O13 C42 C43 -168.9(4) . . . . ?
Cu1 O13 C42 C43 -6.5(8) . . . . ?
C40 C41 C42 O13 -2.8(10) . . . . ?
C46 C41 C42 O13 176.9(6) . . . . ?
C40 C41 C42 C43 178.1(6) . . . . ?
C46 C41 C42 C43 -2.2(10) . . . . ?
C51 O14 C43 C44 5.4(10) . . . . ?
Cu1 O14 C43 C44 -178.5(6) . . . . ?
C51 O14 C43 C42 -173.1(6) . . . . ?
Cu1 O14 C43 C42 2.9(7) . . . . ?
O13 C42 C43 C44 -177.0(6) . . . . ?
C41 C42 C43 C44 2.1(10) . . . . ?
O13 C42 C43 O14 1.6(9) . . . . ?
C41 C42 C43 O14 -179.3(6) . . . . ?
O14 C43 C44 C45 -179.5(6) . . . . ?
C42 C43 C44 C45 -1.1(11) . . . . ?
C43 C44 C45 C46 0.3(11) . . . . ?
C44 C45 C46 C41 -0.5(11) . . . . ?
C42 C41 C46 C45 1.4(10) . . . . ?
C40 C41 C46 C45 -178.8(6) . . . . ?
C40 N4 C47 C48 -36.3(9) . . . . ?
Cu4 N4 C47 C48 150.0(5) . . . . ?
C40 N4 C47 C50 -159.3(6) . . . . ?
Cu4 N4 C47 C50 27.1(6) . . . . ?
C40 N4 C47 C52 84.6(7) . . . . ?
Cu4 N4 C47 C52 -89.0(5) . . . . ?
N4 C47 C48 C49 -53.5(10) . . . . ?
C50 C47 C48 C49 66.4(9) . . . . ?
C52 C47 C48 C49 -174.1(7) . . . . ?
Cu4 O15 C50 C47 39.2(6) . . . . ?
N4 C47 C50 O15 -41.6(7) . . . . ?
C48 C47 C50 O15 -166.9(6) . . . . ?
C52 C47 C50 O15 73.8(7) . . . . ?
N4 C47 C52 O16 -64.5(7) . . . . ?
C48 C47 C52 O16 60.5(8) . . . . ?
C50 C47 C52 O16 -178.5(6) . . . . ?
Cu2 O18 C53 C54 -106.2(10) . . . . ?

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
O4 H4 O16 0.82 1.90 2.717(6) 174.1 1_455
C29 H29 O21 0.93 2.61 3.392(11) 141.6 1_565
C54 H54C O24' 0.96 2.59 3.46(2) 150.8 .

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.910
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.114
