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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 1424792'
_audit_update_record             
;
2016-02-26 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H68 Cu6 N8 O16, 4(Cl O4), H2 O'
_chemical_formula_sum            'C42 H70 Cl4 Cu6 N8 O33'
_chemical_formula_weight         1738.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.1433(16)
_cell_length_b                   12.7099(19)
_cell_length_c                   14.230(2)
_cell_angle_alpha                115.462(4)
_cell_angle_beta                 96.643(5)
_cell_angle_gamma                104.762(4)
_cell_volume                     1547.5(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    19239
_cell_measurement_theta_min      1.64
_cell_measurement_theta_max      25.92

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    2.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19239
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.92
_reflns_number_total             5892
_reflns_number_gt                4606
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Brucker SMART'
_computing_cell_refinement       'Brucker SMART'
_computing_data_reduction        'Brucker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PLATON (Spek, 2009)'

_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)+(0.0558P)²+2.5617P] 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         5892
_refine_ls_number_parameters     420
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1213
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.086
_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 0.77668(6) 0.23091(5) 0.30931(4) 0.01752(15) Uani 1 1 d . C .
Cu2 Cu 0.80377(5) -0.01919(5) 0.22993(4) 0.01777(15) Uani 1 1 d . C .
Cu3 Cu 0.62237(5) 0.03813(5) 0.06257(4) 0.01768(15) Uani 1 1 d . . .
O1 O 0.7373(3) 0.0930(3) 0.3415(2) 0.0173(6) Uani 1 1 d . . .
C1 C 0.7099(4) 0.0924(4) 0.4308(3) 0.0178(9) Uani 1 1 d . . .
C2 C 0.7098(5) -0.0089(4) 0.4484(4) 0.0201(10) Uani 1 1 d . . .
C3 C 0.6865(5) -0.0046(4) 0.5454(4) 0.0221(10) Uani 1 1 d . . .
H3 H 0.6891 -0.0706 0.5572 0.027 Uiso 1 1 calc R . .
C4 C 0.6601(5) 0.0931(4) 0.6238(4) 0.0244(10) Uani 1 1 d . . .
C5 C 0.6550(5) 0.1892(4) 0.6030(4) 0.0239(10) Uani 1 1 d . . .
H5 H 0.6341 0.2547 0.6535 0.029 Uiso 1 1 calc R . .
C6 C 0.6802(4) 0.1916(4) 0.5089(3) 0.0192(9) Uani 1 1 d . . .
C7 C 0.6383(6) 0.0972(5) 0.7288(4) 0.0342(12) Uani 1 1 d . . .
H7A H 0.5554 0.1186 0.7423 0.050 Uiso 1 1 d . . .
H7B H 0.7188 0.1585 0.7867 0.050 Uiso 1 1 d . . .
H7C H 0.6263 0.0176 0.7240 0.050 Uiso 1 1 d . . .
C8 C 0.6740(5) 0.3003(4) 0.5000(4) 0.0216(10) Uani 1 1 d . . .
H8 H 0.6419 0.3552 0.5517 0.026 Uiso 1 1 calc R . .
N1 N 0.7090(4) 0.3264(3) 0.4272(3) 0.0196(8) Uani 1 1 d . . .
C9 C 0.7041(5) 0.4430(4) 0.4300(4) 0.0241(10) Uani 1 1 d . . .
H9A H 0.7857 0.5121 0.4830 0.029 Uiso 1 1 calc R . .
H9B H 0.6197 0.4583 0.4493 0.029 Uiso 1 1 calc R . .
C10 C 0.7037(5) 0.4296(5) 0.3185(4) 0.0278(11) Uani 1 1 d . . .
H10A H 0.6105 0.3784 0.2702 0.033 Uiso 1 1 calc R . .
H10B H 0.7261 0.5104 0.3223 0.033 Uiso 1 1 calc R . .
N2 N 0.8088(4) 0.3723(3) 0.2761(3) 0.0212(8) Uani 1 1 d . . .
H2 H 0.7843 0.3396 0.2032 0.025 Uiso 1 1 calc R . .
C11 C 0.9569(5) 0.4588(4) 0.3166(4) 0.0292(11) Uani 1 1 d . B .
H11A H 1.0192 0.4114 0.2939 0.035 Uiso 1 1 calc R . .
H11B H 0.9817 0.5019 0.3948 0.035 Uiso 1 1 calc R . .
C12 C 0.9802(6) 0.5540(5) 0.2763(4) 0.0311(11) Uani 1 1 d D . .
H12A H 0.9084 0.5927 0.2885 0.037 Uiso 1 1 calc R A 1
H12B H 1.0716 0.6181 0.3161 0.037 Uiso 1 1 calc R A 1
O2A O 0.9736(8) 0.4949(6) 0.1633(5) 0.0324(16) Uiso 0.50 1 d PD B 1
H2A H 1.0349 0.4629 0.1533 0.049 Uiso 0.50 1 calc PR B 1
O2B O 0.8987(9) 0.5043(7) 0.1687(6) 0.048(2) Uiso 0.50 1 d PD B 2
H2B H 0.9207 0.4464 0.1281 0.072 Uiso 0.50 1 calc PR B 2
C13 C 0.7362(5) -0.1180(4) 0.3741(4) 0.0241(10) Uani 1 1 d . C .
H13 H 0.7272 -0.1817 0.3914 0.029 Uiso 1 1 calc R . .
N3 N 0.7710(4) -0.1336(4) 0.2863(3) 0.0274(9) Uani 1 1 d . . .
C14A C 0.7601(16) -0.2643(14) 0.2047(12) 0.015(3) Uiso 0.30 1 d PD C 1
H14A H 0.7773 -0.3123 0.2394 0.019 Uiso 0.30 1 calc PR C 1
H14B H 0.6694 -0.3086 0.1518 0.019 Uiso 0.30 1 calc PR C 1
C14B C 0.8209(9) -0.2357(7) 0.2274(5) 0.0256(16) Uiso 0.70 1 d PD C 2
H14C H 0.7735 -0.3075 0.2346 0.031 Uiso 0.70 1 calc PR C 2
H14D H 0.9217 -0.2116 0.2558 0.031 Uiso 0.70 1 calc PR C 2
C15A C 0.8789(15) -0.2312(13) 0.1555(12) 0.023(3) Uiso 0.30 1 d PD C 1
H15A H 0.8839 -0.3062 0.0983 0.028 Uiso 0.30 1 calc PR C 1
H15B H 0.9681 -0.1896 0.2100 0.028 Uiso 0.30 1 calc PR C 1
C15B C 0.7878(8) -0.2659(6) 0.1104(6) 0.0333(17) Uiso 0.70 1 d PD C 2
H15C H 0.8277 -0.3274 0.0690 0.040 Uiso 0.70 1 calc PR C 2
H15D H 0.6866 -0.2978 0.0796 0.040 Uiso 0.70 1 calc PR C 2
N4 N 0.8537(5) -0.1457(4) 0.1099(4) 0.0363(11) Uani 1 1 d D . .
H4 H 0.7846 -0.1869 0.0471 0.044 Uiso 1 1 calc R C 1
C16 C 0.9921(5) -0.1094(5) 0.0945(4) 0.0394(13) Uani 1 1 d . C .
H16A H 1.0601 -0.0976 0.1551 0.047 Uiso 1 1 calc R . .
H16B H 1.0107 -0.0297 0.0962 0.047 Uiso 1 1 calc R . .
C17 C 1.0181(6) -0.1979(5) -0.0084(4) 0.0341(12) Uani 1 1 d . . .
H17A H 1.1191 -0.1801 0.0015 0.041 Uiso 1 1 calc R C .
H17B H 0.9769 -0.2817 -0.0201 0.041 Uiso 1 1 calc R . .
O3 O 0.9625(4) -0.1930(3) -0.1032(3) 0.0382(9) Uani 1 1 d . C .
H3O H 0.8764 -0.2119 -0.1145 0.057 Uiso 1 1 calc R . .
O4 O 0.8144(3) 0.1072(3) 0.1849(2) 0.0162(6) Uani 1 1 d . . .
H4O H 0.9018 0.1364 0.1666 0.024 Uiso 1 1 calc R C .
O5 O 0.5583(3) -0.1172(3) 0.0720(2) 0.0240(7) Uani 1 1 d . . .
O6 O 0.3465(3) -0.1843(3) -0.0403(2) 0.0233(7) Uani 1 1 d . . .
C37 C 0.4378(5) -0.1969(4) 0.0184(4) 0.0212(10) Uani 1 1 d . C .
C38 C 0.3992(5) -0.3179(5) 0.0210(4) 0.0324(12) Uani 1 1 d . . .
H38A H 0.4493 -0.3054 0.0885 0.039 Uiso 1 1 calc R C .
H38B H 0.4242 -0.3771 -0.0369 0.039 Uiso 1 1 calc R . .
H38C H 0.2995 -0.3483 0.0130 0.039 Uiso 1 1 calc R . .
O7 O 0.5294(3) 0.1170(3) 0.1752(2) 0.0207(7) Uani 1 1 d . . .
O8 O 0.3160(3) 0.0494(3) 0.0657(2) 0.0233(7) Uani 1 1 d . . .
C35 C 0.4020(5) 0.1109(4) 0.1581(4) 0.0210(10) Uani 1 1 d . C .
C36 C 0.3482(5) 0.1794(4) 0.2511(4) 0.0232(10) Uani 1 1 d . . .
H36A H 0.4028 0.1890 0.3159 0.028 Uiso 1 1 calc R C .
H36B H 0.2510 0.1337 0.2390 0.028 Uiso 1 1 calc R . .
H36C H 0.3562 0.2596 0.2584 0.028 Uiso 1 1 calc R . .
Cl1 Cl 1.08836(11) 0.21104(10) 0.43606(9) 0.0213(2) Uani 1 1 d . . .
O9 O 1.0271(4) 0.2916(3) 0.4135(3) 0.0371(9) Uani 1 1 d . . .
O10 O 1.0522(3) 0.0955(3) 0.3380(3) 0.0285(8) Uani 1 1 d . . .
O11 O 1.0318(4) 0.1884(4) 0.5158(3) 0.0418(10) Uani 1 1 d . . .
O12 O 1.2395(3) 0.2682(3) 0.4737(3) 0.0262(7) Uani 1 1 d . . .
Cl2 Cl 0.36211(16) 0.47141(12) 0.19413(12) 0.0422(3) Uani 1 1 d D . .
O15A O 0.3887(15) 0.4937(13) 0.3030(7) 0.080(4) Uiso 0.40 1 d PD D 1
O15B O 0.2636(8) 0.4487(8) 0.2525(6) 0.067(2) Uiso 0.60 1 d PD D 2
O16A O 0.2587(7) 0.5076(7) 0.1469(6) 0.073(2) Uiso 0.70 1 d PD D 1
O16B O 0.361(2) 0.5401(15) 0.1387(13) 0.078(5) Uiso 0.30 1 d PD D 2
O14 O 0.3582(6) 0.3503(4) 0.1241(3) 0.0674(14) Uani 1 1 d D D .
O13A O 0.4902(7) 0.5464(7) 0.1922(7) 0.051(2) Uiso 0.50 1 d PD D 1
O13B O 0.4783(9) 0.5561(9) 0.2875(7) 0.078(3) Uiso 0.50 1 d PD D 2
O1W O 0.0810(12) 0.5291(14) 0.0474(10) 0.107(5) Uani 0.50 1 d P . 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 N1 1.924(4) . ?
Cu1 O1 1.954(3) . ?
Cu1 O4 1.955(3) . ?
Cu1 N2 2.007(3) . ?
Cu1 Cu2 2.9809(8) . ?
Cu2 N3 1.921(4) . ?
Cu2 O1 1.949(3) . ?
Cu2 O4 1.954(3) . ?
Cu2 N4 2.004(4) . ?
Cu3 O8 1.958(3) 2_655 ?
Cu3 O6 1.969(3) 2_655 ?
Cu3 O7 1.978(3) . ?
Cu3 O5 1.983(3) . ?
Cu3 O4 2.150(3) . ?
Cu3 Cu3 2.5574(11) 2_655 ?
O1 C1 1.334(5) . ?
C1 C6 1.407(6) . ?
C1 C2 1.414(6) . ?
C2 C3 1.408(6) . ?
C2 C13 1.451(6) . ?
C3 C4 1.380(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(6) . ?
C4 C7 1.515(6) . ?
C5 C6 1.404(6) . ?
C5 H5 0.9300 . ?
C6 C8 1.456(6) . ?
C7 H7A 0.963(5) . ?
C7 H7B 0.960(6) . ?
C7 H7C 0.959(5) . ?
C8 N1 1.276(6) . ?
C8 H8 0.9300 . ?
N1 C9 1.479(5) . ?
C9 C10 1.520(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.483(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C11 1.486(6) . ?
N2 H2 0.9100 . ?
C11 C12 1.527(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2B 1.427(8) . ?
C12 O2A 1.438(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
O2A H2A 0.8200 . ?
O2B H2B 0.8200 . ?
C13 N3 1.283(6) . ?
C13 H13 0.9300 . ?
N3 C14B 1.462(8) . ?
N3 C14A 1.529(15) . ?
C14A C15A 1.520(11) . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C14B C15B 1.514(8) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C15A N4 1.541(10) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C15B N4 1.506(7) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
N4 C16 1.436(6) . ?
N4 H4 0.9100 . ?
C16 C17 1.518(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 O3 1.434(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
O3 H3O 0.8200 . ?
O4 H4O 0.9800 . ?
O5 C37 1.261(5) . ?
O6 C37 1.263(5) . ?
O6 Cu3 1.969(3) 2_655 ?
C37 C38 1.505(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
O7 C35 1.263(5) . ?
O8 C35 1.266(5) . ?
O8 Cu3 1.958(3) 2_655 ?
C35 C36 1.493(6) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
Cl1 O11 1.430(4) . ?
Cl1 O12 1.439(3) . ?
Cl1 O10 1.443(3) . ?
Cl1 O9 1.449(3) . ?
Cl2 O16B 1.408(8) . ?
Cl2 O13A 1.413(6) . ?
Cl2 O14 1.416(4) . ?
Cl2 O15B 1.422(6) . ?
Cl2 O15A 1.429(7) . ?
Cl2 O13B 1.440(7) . ?
Cl2 O16A 1.453(6) . ?
O1W O1W 1.76(2) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 O1 91.96(13) . . ?
N1 Cu1 O4 169.01(14) . . ?
O1 Cu1 O4 79.81(12) . . ?
N1 Cu1 N2 86.62(15) . . ?
O1 Cu1 N2 177.63(13) . . ?
O4 Cu1 N2 101.36(13) . . ?
N1 Cu1 Cu2 132.10(11) . . ?
O1 Cu1 Cu2 40.15(8) . . ?
O4 Cu1 Cu2 40.29(8) . . ?
N2 Cu1 Cu2 141.27(11) . . ?
N3 Cu2 O1 91.24(14) . . ?
N3 Cu2 O4 170.48(14) . . ?
O1 Cu2 O4 79.95(11) . . ?
N3 Cu2 N4 86.65(16) . . ?
O1 Cu2 N4 174.67(16) . . ?
O4 Cu2 N4 101.82(14) . . ?
N3 Cu2 Cu1 131.32(12) . . ?
O1 Cu2 Cu1 40.26(8) . . ?
O4 Cu2 Cu1 40.32(8) . . ?
N4 Cu2 Cu1 142.03(12) . . ?
O8 Cu3 O6 91.50(13) 2_655 2_655 ?
O8 Cu3 O7 170.45(12) 2_655 . ?
O6 Cu3 O7 87.25(12) 2_655 . ?
O8 Cu3 O5 89.36(13) 2_655 . ?
O6 Cu3 O5 170.57(13) 2_655 . ?
O7 Cu3 O5 90.36(13) . . ?
O8 Cu3 O4 99.83(11) 2_655 . ?
O6 Cu3 O4 97.59(12) 2_655 . ?
O7 Cu3 O4 89.73(11) . . ?
O5 Cu3 O4 91.52(12) . . ?
O8 Cu3 Cu3 87.47(9) 2_655 2_655 ?
O6 Cu3 Cu3 84.36(9) 2_655 2_655 ?
O7 Cu3 Cu3 82.98(9) . 2_655 ?
O5 Cu3 Cu3 86.30(9) . 2_655 ?
O4 Cu3 Cu3 172.37(8) . 2_655 ?
C1 O1 Cu2 130.0(3) . . ?
C1 O1 Cu1 128.2(3) . . ?
Cu2 O1 Cu1 99.58(12) . . ?
O1 C1 C6 121.1(4) . . ?
O1 C1 C2 120.2(4) . . ?
C6 C1 C2 118.7(4) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 C13 116.5(4) . . ?
C1 C2 C13 124.6(4) . . ?
C4 C3 C2 123.1(4) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C3 C4 C5 117.0(4) . . ?
C3 C4 C7 122.3(4) . . ?
C5 C4 C7 120.7(4) . . ?
C4 C5 C6 122.6(4) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C1 119.6(4) . . ?
C5 C6 C8 116.0(4) . . ?
C1 C6 C8 124.4(4) . . ?
C4 C7 H7A 109.4(4) . . ?
C4 C7 H7B 109.6(4) . . ?
H7A C7 H7B 109.3(5) . . ?
C4 C7 H7C 109.6(4) . . ?
H7A C7 H7C 109.4(5) . . ?
H7B C7 H7C 109.6(5) . . ?
N1 C8 C6 125.5(4) . . ?
N1 C8 H8 117.3 . . ?
C6 C8 H8 117.3 . . ?
C8 N1 C9 120.3(4) . . ?
C8 N1 Cu1 127.1(3) . . ?
C9 N1 Cu1 112.6(3) . . ?
N1 C9 C10 107.9(3) . . ?
N1 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
N1 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C9 110.2(4) . . ?
N2 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C10 N2 C11 115.0(4) . . ?
C10 N2 Cu1 103.7(3) . . ?
C11 N2 Cu1 114.8(3) . . ?
C10 N2 H2 107.6 . . ?
C11 N2 H2 107.6 . . ?
Cu1 N2 H2 107.6 . . ?
N2 C11 C12 112.8(4) . . ?
N2 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N2 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O2B C12 O2A 32.7(4) . . ?
O2B C12 C11 112.6(5) . . ?
O2A C12 C11 110.1(5) . . ?
O2B C12 H12A 78.7 . . ?
O2A C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
O2B C12 H12B 131.5 . . ?
O2A C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.2 . . ?
C12 O2A H2A 109.5 . . ?
C12 O2B H2B 109.5 . . ?
N3 C13 C2 125.3(4) . . ?
N3 C13 H13 117.4 . . ?
C2 C13 H13 117.4 . . ?
C13 N3 C14B 120.9(4) . . ?
C13 N3 C14A 118.2(6) . . ?
C14B N3 C14A 22.9(5) . . ?
C13 N3 Cu2 127.7(3) . . ?
C14B N3 Cu2 110.2(3) . . ?
C14A N3 Cu2 113.0(5) . . ?
C15A C14A N3 99.1(10) . . ?
C15A C14A H14A 112.0 . . ?
N3 C14A H14A 112.0 . . ?
C15A C14A H14B 112.0 . . ?
N3 C14A H14B 112.0 . . ?
H14A C14A H14B 109.6 . . ?
N3 C14B C15B 107.4(5) . . ?
N3 C14B H14C 110.2 . . ?
C15B C14B H14C 110.2 . . ?
N3 C14B H14D 110.2 . . ?
C15B C14B H14D 110.2 . . ?
H14C C14B H14D 108.5 . . ?
C14A C15A N4 110.3(9) . . ?
C14A C15A H15A 109.6 . . ?
N4 C15A H15A 109.6 . . ?
C14A C15A H15B 109.6 . . ?
N4 C15A H15B 109.6 . . ?
H15A C15A H15B 108.1 . . ?
N4 C15B C14B 105.8(5) . . ?
N4 C15B H15C 110.6 . . ?
C14B C15B H15C 110.6 . . ?
N4 C15B H15D 110.6 . . ?
C14B C15B H15D 110.6 . . ?
H15C C15B H15D 108.7 . . ?
C16 N4 C15B 123.2(5) . . ?
C16 N4 C15A 96.6(6) . . ?
C15B N4 C15A 35.7(6) . . ?
C16 N4 Cu2 117.7(3) . . ?
C15B N4 Cu2 105.0(3) . . ?
C15A N4 Cu2 102.6(6) . . ?
C16 N4 H4 112.7 . . ?
C15B N4 H4 79.7 . . ?
C15A N4 H4 112.7 . . ?
Cu2 N4 H4 112.7 . . ?
N4 C16 C17 116.5(5) . . ?
N4 C16 H16A 108.2 . . ?
C17 C16 H16A 108.2 . . ?
N4 C16 H16B 108.2 . . ?
C17 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
O3 C17 C16 115.0(4) . . ?
O3 C17 H17A 108.5 . . ?
C16 C17 H17A 108.5 . . ?
O3 C17 H17B 108.5 . . ?
C16 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 O3 H3O 109.5 . . ?
Cu2 O4 Cu1 99.40(12) . . ?
Cu2 O4 Cu3 105.95(13) . . ?
Cu1 O4 Cu3 101.76(12) . . ?
Cu2 O4 H4O 115.8 . . ?
Cu1 O4 H4O 115.8 . . ?
Cu3 O4 H4O 115.8 . . ?
C37 O5 Cu3 120.8(3) . . ?
C37 O6 Cu3 123.7(3) . 2_655 ?
O5 C37 O6 124.8(4) . . ?
O5 C37 C38 118.6(4) . . ?
O6 C37 C38 116.6(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 O7 Cu3 125.0(3) . . ?
C35 O8 Cu3 120.8(3) . 2_655 ?
O7 C35 O8 123.7(4) . . ?
O7 C35 C36 118.8(4) . . ?
O8 C35 C36 117.5(4) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O11 Cl1 O12 110.4(2) . . ?
O11 Cl1 O10 109.6(2) . . ?
O12 Cl1 O10 109.43(19) . . ?
O11 Cl1 O9 109.1(2) . . ?
O12 Cl1 O9 109.8(2) . . ?
O10 Cl1 O9 108.6(2) . . ?
O16B Cl2 O13A 59.6(8) . . ?
O16B Cl2 O14 110.8(8) . . ?
O13A Cl2 O14 102.5(4) . . ?
O16B Cl2 O15B 125.9(8) . . ?
O13A Cl2 O15B 149.4(5) . . ?
O14 Cl2 O15B 102.1(4) . . ?
O16B Cl2 O15A 138.1(9) . . ?
O13A Cl2 O15A 102.8(7) . . ?
O14 Cl2 O15A 110.1(6) . . ?
O15B Cl2 O15A 51.2(6) . . ?
O16B Cl2 O13B 101.5(9) . . ?
O13A Cl2 O13B 55.6(5) . . ?
O14 Cl2 O13B 121.7(5) . . ?
O15B Cl2 O13B 95.7(6) . . ?
O15A Cl2 O13B 47.5(6) . . ?
O16B Cl2 O16A 43.2(7) . . ?
O13A Cl2 O16A 101.9(4) . . ?
O14 Cl2 O16A 112.1(4) . . ?
O15B Cl2 O16A 85.2(5) . . ?
O15A Cl2 O16A 124.1(6) . . ?
O13B Cl2 O16A 124.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.92
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.120
####################################################################### 
# 
# 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_complex_2
_database_code_depnum_ccdc_archive 'CCDC 1424793'
_audit_update_record             
;
2016-02-26 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H76 Cu6 N8 O16, 4(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C46 H80 Cl4 Cu6 N8 O34'
_chemical_formula_weight         1812.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.6038(9)
_cell_length_b                   12.1267(5)
_cell_length_c                   26.1807(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.4240(10)
_cell_angle_gamma                90.00
_cell_volume                     7079.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    295
_cell_measurement_reflns_used    43821
_cell_measurement_theta_min      1.58
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3704
_exptl_absorpt_coefficient_mu    2.013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43821
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6924
_reflns_number_gt                4294
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Brucker SMART'
_computing_cell_refinement       'Brucker SMART'
_computing_data_reduction        'Brucker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PLATON (Spek, 2009)'


_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)+(0.0757P)²+45.2446P] 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         6924
_refine_ls_number_parameters     439
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1731
_refine_ls_wR_factor_gt          0.1390
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.12625(3) 0.38631(6) 0.37824(3) 0.0395(2) Uani 1 1 d . A .
Cu2 Cu 0.25097(3) 0.38799(6) 0.35311(3) 0.0366(2) Uani 1 1 d . A .
Cu3 Cu 0.22902(3) 0.24728(6) 0.45195(3) 0.0340(2) Uani 1 1 d . . .
O1 O 0.18759(17) 0.4906(3) 0.36418(16) 0.0392(10) Uani 1 1 d . . .
C1 C 0.1849(3) 0.5990(5) 0.3592(2) 0.0363(14) Uani 1 1 d . . .
C2 C 0.2344(3) 0.6584(5) 0.3468(2) 0.0378(14) Uani 1 1 d . . .
C3 C 0.2301(3) 0.7743(5) 0.3428(3) 0.0495(17) Uani 1 1 d . . .
H3 H 0.2631 0.8136 0.3356 0.059 Uiso 1 1 calc R . .
C4 C 0.1794(3) 0.8319(6) 0.3492(3) 0.0533(18) Uani 1 1 d . . .
C5 C 0.1320(3) 0.7727(5) 0.3603(3) 0.0489(17) Uani 1 1 d . . .
H5 H 0.0975 0.8106 0.3652 0.059 Uiso 1 1 calc R . .
C6 C 0.1324(3) 0.6573(6) 0.3648(2) 0.0411(15) Uani 1 1 d . . .
C7 C 0.1775(4) 0.9578(6) 0.3447(4) 0.078(3) Uani 1 1 d . . .
H7A H 0.2034 0.9814 0.3212 0.117 Uiso 1 1 calc R . .
H7B H 0.1906 0.9899 0.3782 0.117 Uiso 1 1 calc R . .
H7C H 0.1371 0.9811 0.3320 0.117 Uiso 1 1 calc R . .
C8 C 0.0782(3) 0.6052(6) 0.3751(3) 0.0523(18) Uani 1 1 d . A .
H8 H 0.0461 0.6517 0.3774 0.063 Uiso 1 1 calc R . .
N1 N 0.0695(2) 0.5034(5) 0.3812(3) 0.0535(15) Uani 1 1 d . . .
C9A C 0.0153(6) 0.4644(11) 0.4019(6) 0.037(3) Uiso 0.50 1 d P A 1
H9A1 H -0.0186 0.5130 0.3916 0.044 Uiso 0.50 1 calc PR A 1
H9A2 H 0.0231 0.4581 0.4393 0.044 Uiso 0.50 1 calc PR A 1
C10A C 0.0050(6) 0.3487(12) 0.3753(6) 0.043(3) Uiso 0.50 1 d P A 1
H10A H -0.0294 0.3122 0.3856 0.051 Uiso 0.50 1 calc PR A 1
H10B H -0.0018 0.3561 0.3379 0.051 Uiso 0.50 1 calc PR A 1
C9B C 0.0072(7) 0.4587(14) 0.3771(7) 0.061(5) Uiso 0.50 1 d P A 2
H9B1 H -0.0172 0.5084 0.3940 0.073 Uiso 0.50 1 calc PR A 2
H9B2 H -0.0109 0.4520 0.3410 0.073 Uiso 0.50 1 calc PR A 2
C10B C 0.0102(7) 0.3536(14) 0.4014(7) 0.060(4) Uiso 0.50 1 d P A 2
H10C H -0.0265 0.3138 0.3886 0.071 Uiso 0.50 1 calc PR A 2
H10D H 0.0117 0.3643 0.4383 0.071 Uiso 0.50 1 calc PR A 2
N2 N 0.0614(2) 0.2847(5) 0.3935(2) 0.0516(15) Uani 1 1 d . . .
H2A H 0.0708 0.2717 0.4281 0.062 Uiso 1 1 d R A .
C11 C 0.0555(5) 0.1761(7) 0.3710(4) 0.091(3) Uani 1 1 d . A .
H11A H 0.0944 0.1403 0.3786 0.109 Uiso 1 1 calc R . .
H11B H 0.0462 0.1846 0.3337 0.109 Uiso 1 1 calc R . .
C12 C 0.0109(5) 0.1015(7) 0.3869(5) 0.094(3) Uani 1 1 d . . .
H12A H 0.0164 0.0980 0.4244 0.113 Uiso 1 1 calc R A .
H12B H -0.0290 0.1296 0.3746 0.113 Uiso 1 1 calc R . .
O2 O 0.0166(4) -0.0033(7) 0.3670(4) 0.151(4) Uani 1 1 d . A .
H2 H 0.0114 0.0015 0.3354 0.227 Uiso 1 1 d R . .
C13 C 0.2895(3) 0.6104(6) 0.3368(2) 0.0438(16) Uani 1 1 d . . .
H13 H 0.3191 0.6583 0.3294 0.053 Uiso 1 1 calc R . .
N3 N 0.3011(2) 0.5066(5) 0.3371(2) 0.0425(13) Uani 1 1 d . . .
C14 C 0.3591(3) 0.4683(6) 0.3259(3) 0.0566(19) Uani 1 1 d . . .
H14A H 0.3885 0.4675 0.3573 0.068 Uiso 1 1 calc R . .
H14B H 0.3732 0.5170 0.3011 0.068 Uiso 1 1 calc R . .
C15 C 0.3500(4) 0.3537(7) 0.3040(3) 0.064(2) Uani 1 1 d . . .
H15A H 0.3274 0.3569 0.2692 0.077 Uiso 1 1 calc R . .
H15B H 0.3886 0.3199 0.3024 0.077 Uiso 1 1 calc R . .
N4 N 0.3171(2) 0.2876(4) 0.3374(2) 0.0438(13) Uani 1 1 d . A .
H4A H 0.3420 0.2749 0.3678 0.053 Uiso 1 1 d R . .
C16 C 0.2981(4) 0.1799(7) 0.3138(4) 0.069(2) Uani 1 1 d D . .
H16A H 0.2835 0.1359 0.3401 0.082 Uiso 1 1 calc R B 1
H16B H 0.2641 0.1933 0.2867 0.082 Uiso 1 1 calc R B 1
C17A C 0.3413(6) 0.1117(15) 0.2913(7) 0.074(4) Uiso 0.60 1 d PD C 1
H17A H 0.3236 0.0410 0.2801 0.089 Uiso 0.60 1 calc PR C 1
H17B H 0.3533 0.1485 0.2618 0.089 Uiso 0.60 1 calc PR C 1
O3A O 0.3904(7) 0.0974(12) 0.3306(5) 0.129(5) Uiso 0.60 1 d PD C 1
H3A H 0.4047 0.1577 0.3397 0.193 Uiso 0.60 1 calc PR C 1
C17B C 0.3471(9) 0.0975(17) 0.3146(10) 0.072(7) Uiso 0.40 1 d PD C 2
H17C H 0.3768 0.1054 0.3456 0.087 Uiso 0.40 1 calc PR C 2
H17D H 0.3313 0.0230 0.3131 0.087 Uiso 0.40 1 calc PR C 2
O3B O 0.3721(12) 0.122(2) 0.2703(8) 0.144(8) Uiso 0.40 1 d PD C 2
H3B H 0.3999 0.0791 0.2685 0.216 Uiso 0.40 1 calc PR C 2
O4 O 0.19195(16) 0.2835(3) 0.37266(14) 0.0321(9) Uani 1 1 d . . .
H4 H 0.1820 0.2200 0.3497 0.048 Uiso 1 1 d R A .
O6 O 0.28712(19) 0.3686(4) 0.44745(16) 0.0434(11) Uani 1 1 d . . .
O8 O 0.3228(2) 0.3714(4) 0.53204(17) 0.0465(11) Uani 1 1 d . . .
C18 C 0.3197(3) 0.4089(5) 0.4871(3) 0.0408(15) Uani 1 1 d . A .
C19 C 0.3547(4) 0.5105(6) 0.4800(3) 0.064(2) Uani 1 1 d . . .
H19A H 0.3943 0.5049 0.5008 0.076 Uiso 1 1 calc R A .
H19B H 0.3596 0.5168 0.4440 0.076 Uiso 1 1 calc R . .
C20 C 0.3243(7) 0.6105(8) 0.4954(6) 0.145(6) Uani 1 1 d . A .
H20A H 0.3470 0.6747 0.4891 0.218 Uiso 1 1 calc R . .
H20B H 0.3216 0.6065 0.5315 0.218 Uiso 1 1 calc R . .
H20C H 0.2848 0.6152 0.4755 0.218 Uiso 1 1 calc R . .
O5 O 0.17318(19) 0.3602(4) 0.47138(17) 0.0447(11) Uani 1 1 d . . .
O7 O 0.2100(2) 0.3625(4) 0.55539(18) 0.0488(12) Uani 1 1 d . . .
C21 C 0.1752(3) 0.3973(5) 0.5169(3) 0.0427(15) Uani 1 1 d . A .
C22 C 0.1326(4) 0.4885(7) 0.5249(3) 0.073(2) Uani 1 1 d D . .
H22A H 0.1214 0.5266 0.4922 0.087 Uiso 1 1 calc R A 1
H22B H 0.0965 0.4550 0.5334 0.087 Uiso 1 1 calc R A 1
C23A C 0.1531(6) 0.5705(11) 0.5643(5) 0.082(4) Uiso 0.70 1 d PD A 1
H23A H 0.1549 0.5383 0.5980 0.123 Uiso 0.70 1 calc PR A 1
H23B H 0.1257 0.6316 0.5607 0.123 Uiso 0.70 1 calc PR A 1
H23C H 0.1922 0.5960 0.5602 0.123 Uiso 0.70 1 calc PR A 1
C23B C 0.1601(15) 0.5961(17) 0.5256(15) 0.095(11) Uiso 0.30 1 d PD A 2
H23D H 0.1895 0.6035 0.5563 0.143 Uiso 0.30 1 calc PR A 2
H23E H 0.1299 0.6518 0.5253 0.143 Uiso 0.30 1 calc PR A 2
H23F H 0.1790 0.6043 0.4956 0.143 Uiso 0.30 1 calc PR A 2
Cl1 Cl 0.13199(10) 0.3030(2) 0.24799(7) 0.0710(6) Uani 1 1 d . . .
O9 O 0.1410(3) 0.1929(5) 0.2687(2) 0.0785(17) Uani 1 1 d . . .
O10 O 0.1119(3) 0.3026(6) 0.1945(2) 0.101(2) Uani 1 1 d . . .
O11 O 0.0937(3) 0.3628(5) 0.2757(2) 0.0789(18) Uani 1 1 d . . .
O12 O 0.1918(3) 0.3586(6) 0.2571(2) 0.0845(19) Uani 1 1 d . . .
Cl2 Cl -0.02269(11) -0.2247(2) 0.45546(11) 0.0836(7) Uani 1 1 d D . .
O13A O -0.0507(9) -0.2516(17) 0.4047(4) 0.142(7) Uiso 0.50 1 d PD D 1
O13B O -0.0233(8) -0.2017(15) 0.4019(4) 0.114(5) Uiso 0.50 1 d PD D 2
O14A O 0.0257(13) -0.161(3) 0.4440(17) 0.182(15) Uiso 0.30 1 d PD D 1
O14B O -0.0003(6) -0.1197(8) 0.4727(5) 0.143(5) Uiso 0.70 1 d PD D 2
O15 O 0.0133(4) -0.3157(8) 0.4717(4) 0.164(4) Uani 1 1 d D D .
O16A O -0.0862(4) -0.2277(18) 0.4479(9) 0.088(6) Uiso 0.30 1 d PD D 1
O16B O -0.0685(5) -0.2289(9) 0.4862(4) 0.114(4) Uiso 0.70 1 d PD D 2
O1W O 0.5000 0.155(3) 0.2500 0.334(15) Uani 1 2 d S . .
O2W O 0.0000 -0.0701(19) 0.2500 0.247(9) Uani 1 2 d S . .


_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 N1 1.923(6) . ?
Cu1 O1 1.955(4) . ?
Cu1 O4 1.963(4) . ?
Cu1 N2 2.004(5) . ?
Cu1 Cu2 2.9980(10) . ?
Cu2 N3 1.919(5) . ?
Cu2 O1 1.954(4) . ?
Cu2 O4 1.968(4) . ?
Cu2 N4 2.021(5) . ?
Cu3 O8 1.944(4) 7_556 ?
Cu3 O7 1.948(4) 7_556 ?
Cu3 O5 1.984(4) . ?
Cu3 O6 1.989(4) . ?
Cu3 O4 2.153(4) . ?
Cu3 Cu3 2.5402(14) 7_556 ?
O1 C1 1.322(7) . ?
C1 C6 1.409(8) . ?
C1 C2 1.412(8) . ?
C2 C3 1.411(9) . ?
C2 C13 1.438(9) . ?
C3 C4 1.376(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.361(10) . ?
C4 C7 1.531(10) . ?
C5 C6 1.405(9) . ?
C5 H5 0.9300 . ?
C6 C8 1.442(9) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.265(8) . ?
C8 H8 0.9300 . ?
N1 C9A 1.495(13) . ?
N1 C9B 1.497(17) . ?
C9A C10A 1.567(19) . ?
C9A H9A1 0.9700 . ?
C9A H9A2 0.9700 . ?
C10A N2 1.502(15) . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
C9B C10B 1.42(2) . ?
C9B H9B1 0.9700 . ?
C9B H9B2 0.9700 . ?
C10B N2 1.470(17) . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
N2 C11 1.440(10) . ?
N2 H2A 0.9100 . ?
C11 C12 1.466(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2 1.387(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
O2 H2 0.8200 . ?
C13 N3 1.286(8) . ?
C13 H13 0.9300 . ?
N3 C14 1.464(8) . ?
C14 C15 1.505(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N4 1.476(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
N4 C16 1.479(9) . ?
N4 H4A 0.9100 . ?
C16 C17A 1.473(13) . ?
C16 C17B 1.489(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17A O3A 1.395(16) . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
O3A H3A 0.8200 . ?
C17B O3B 1.401(17) . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
O3B H3B 0.8200 . ?
O4 H4 0.9800 . ?
O6 C18 1.267(7) . ?
O8 C18 1.253(7) . ?
O8 Cu3 1.944(4) 7_556 ?
C18 C19 1.493(9) . ?
C19 C20 1.481(13) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O5 C21 1.267(8) . ?
O7 C21 1.247(8) . ?
O7 Cu3 1.948(4) 7_556 ?
C21 C22 1.503(9) . ?
C22 C23B 1.444(15) . ?
C22 C23A 1.453(13) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23A H23A 0.9600 . ?
C23A H23B 0.9600 . ?
C23A H23C 0.9600 . ?
C23B H23D 0.9600 . ?
C23B H23E 0.9600 . ?
C23B H23F 0.9600 . ?
Cl1 O10 1.399(6) . ?
Cl1 O11 1.417(5) . ?
Cl1 O9 1.443(6) . ?
Cl1 O12 1.494(6) . ?
Cl2 O15 1.396(7) . ?
Cl2 O14A 1.409(9) . ?
Cl2 O13A 1.413(8) . ?
Cl2 O16B 1.414(7) . ?
Cl2 O14B 1.416(8) . ?
Cl2 O16A 1.417(9) . ?
Cl2 O13B 1.427(8) . ?
O13A O16A 1.52(3) . ?

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 Cu1 O1 91.6(2) . . ?
N1 Cu1 O4 171.7(2) . . ?
O1 Cu1 O4 80.11(16) . . ?
N1 Cu1 N2 86.1(2) . . ?
O1 Cu1 N2 177.6(2) . . ?
O4 Cu1 N2 102.2(2) . . ?
N1 Cu1 Cu2 131.37(17) . . ?
O1 Cu1 Cu2 39.92(12) . . ?
O4 Cu1 Cu2 40.35(11) . . ?
N2 Cu1 Cu2 142.42(16) . . ?
N3 Cu2 O1 91.6(2) . . ?
N3 Cu2 O4 171.54(19) . . ?
O1 Cu2 O4 80.02(16) . . ?
N3 Cu2 N4 85.7(2) . . ?
O1 Cu2 N4 176.2(2) . . ?
O4 Cu2 N4 102.72(19) . . ?
N3 Cu2 Cu1 131.52(16) . . ?
O1 Cu2 Cu1 39.95(12) . . ?
O4 Cu2 Cu1 40.23(11) . . ?
N4 Cu2 Cu1 142.52(16) . . ?
O8 Cu3 O7 88.6(2) 7_556 7_556 ?
O8 Cu3 O5 91.41(19) 7_556 . ?
O7 Cu3 O5 170.69(18) 7_556 . ?
O8 Cu3 O6 170.96(18) 7_556 . ?
O7 Cu3 O6 90.86(19) 7_556 . ?
O5 Cu3 O6 87.63(19) . . ?
O8 Cu3 O4 101.88(17) 7_556 . ?
O7 Cu3 O4 102.36(17) 7_556 . ?
O5 Cu3 O4 86.73(16) . . ?
O6 Cu3 O4 87.05(16) . . ?
O8 Cu3 Cu3 86.91(13) 7_556 7_556 ?
O7 Cu3 Cu3 87.71(14) 7_556 7_556 ?
O5 Cu3 Cu3 83.01(13) . 7_556 ?
O6 Cu3 Cu3 84.05(13) . 7_556 ?
O4 Cu3 Cu3 166.66(11) . 7_556 ?
C1 O1 Cu2 129.9(4) . . ?
C1 O1 Cu1 129.7(4) . . ?
Cu2 O1 Cu1 100.13(18) . . ?
O1 C1 C6 121.0(6) . . ?
O1 C1 C2 120.4(5) . . ?
C6 C1 C2 118.7(6) . . ?
C3 C2 C1 118.6(6) . . ?
C3 C2 C13 116.1(6) . . ?
C1 C2 C13 125.3(6) . . ?
C4 C3 C2 122.9(6) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C5 C4 C3 117.4(6) . . ?
C5 C4 C7 121.9(7) . . ?
C3 C4 C7 120.7(7) . . ?
C4 C5 C6 123.3(6) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C1 119.1(6) . . ?
C5 C6 C8 117.2(6) . . ?
C1 C6 C8 123.7(6) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 127.2(6) . . ?
N1 C8 H8 116.4 . . ?
C6 C8 H8 116.4 . . ?
C8 N1 C9A 120.5(7) . . ?
C8 N1 C9B 120.5(8) . . ?
C9A N1 C9B 25.0(7) . . ?
C8 N1 Cu1 126.7(5) . . ?
C9A N1 Cu1 111.9(6) . . ?
C9B N1 Cu1 110.9(7) . . ?
N1 C9A C10A 101.2(9) . . ?
N1 C9A H9A1 111.5 . . ?
C10A C9A H9A1 111.5 . . ?
N1 C9A H9A2 111.5 . . ?
C10A C9A H9A2 111.5 . . ?
H9A1 C9A H9A2 109.4 . . ?
N2 C10A C9A 105.3(10) . . ?
N2 C10A H10A 110.7 . . ?
C9A C10A H10A 110.7 . . ?
N2 C10A H10B 110.7 . . ?
C9A C10A H10B 110.7 . . ?
H10A C10A H10B 108.8 . . ?
C10B C9B N1 108.5(13) . . ?
C10B C9B H9B1 110.0 . . ?
N1 C9B H9B1 110.0 . . ?
C10B C9B H9B2 110.0 . . ?
N1 C9B H9B2 110.0 . . ?
H9B1 C9B H9B2 108.4 . . ?
C9B C10B N2 115.3(13) . . ?
C9B C10B H10C 108.5 . . ?
N2 C10B H10C 108.5 . . ?
C9B C10B H10D 108.5 . . ?
N2 C10B H10D 108.5 . . ?
H10C C10B H10D 107.5 . . ?
C11 N2 C10B 123.8(9) . . ?
C11 N2 C10A 109.0(8) . . ?
C10B N2 C10A 26.3(7) . . ?
C11 N2 Cu1 120.1(5) . . ?
C10B N2 Cu1 107.3(7) . . ?
C10A N2 Cu1 103.3(6) . . ?
C11 N2 H2A 103.9 . . ?
C10B N2 H2A 91.1 . . ?
C10A N2 H2A 116.9 . . ?
Cu1 N2 H2A 104.2 . . ?
N2 C11 C12 118.0(8) . . ?
N2 C11 H11A 107.8 . . ?
C12 C11 H11A 107.8 . . ?
N2 C11 H11B 107.8 . . ?
C12 C11 H11B 107.8 . . ?
H11A C11 H11B 107.1 . . ?
O2 C12 C11 110.4(9) . . ?
O2 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
O2 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C12 O2 H2 107.9 . . ?
N3 C13 C2 125.2(6) . . ?
N3 C13 H13 117.4 . . ?
C2 C13 H13 117.4 . . ?
C13 N3 C14 119.8(6) . . ?
C13 N3 Cu2 127.5(4) . . ?
C14 N3 Cu2 112.7(4) . . ?
N3 C14 C15 107.4(6) . . ?
N3 C14 H14A 110.2 . . ?
C15 C14 H14A 110.2 . . ?
N3 C14 H14B 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
N4 C15 C14 109.0(6) . . ?
N4 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
N4 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C15 N4 C16 111.8(6) . . ?
C15 N4 Cu2 104.8(4) . . ?
C16 N4 Cu2 116.3(4) . . ?
C15 N4 H4A 108.1 . . ?
C16 N4 H4A 108.2 . . ?
Cu2 N4 H4A 107.3 . . ?
C17A C16 N4 119.8(9) . . ?
C17A C16 C17B 24.4(10) . . ?
N4 C16 C17B 115.0(13) . . ?
C17A C16 H16A 107.4 . . ?
N4 C16 H16A 107.4 . . ?
C17B C16 H16A 87.7 . . ?
C17A C16 H16B 107.4 . . ?
N4 C16 H16B 107.4 . . ?
C17B C16 H16B 128.3 . . ?
H16A C16 H16B 106.9 . . ?
O3A C17A C16 105.9(12) . . ?
O3A C17A H17A 110.5 . . ?
C16 C17A H17A 110.5 . . ?
O3A C17A H17B 110.5 . . ?
C16 C17A H17B 110.5 . . ?
H17A C17A H17B 108.7 . . ?
C17A O3A H3A 109.5 . . ?
O3B C17B C16 104.4(17) . . ?
O3B C17B H17C 110.9 . . ?
C16 C17B H17C 110.9 . . ?
O3B C17B H17D 110.9 . . ?
C16 C17B H17D 110.9 . . ?
H17C C17B H17D 108.9 . . ?
C17B O3B H3B 109.5 . . ?
Cu1 O4 Cu2 99.42(17) . . ?
Cu1 O4 Cu3 103.74(17) . . ?
Cu2 O4 Cu3 102.05(16) . . ?
Cu1 O4 H4 116.4 . . ?
Cu2 O4 H4 116.3 . . ?
Cu3 O4 H4 116.4 . . ?
C18 O6 Cu3 122.5(4) . . ?
C18 O8 Cu3 121.8(4) . 7_556 ?
O8 C18 O6 124.4(6) . . ?
O8 C18 C19 117.7(6) . . ?
O6 C18 C19 117.8(6) . . ?
C20 C19 C18 111.3(7) . . ?
C20 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 O5 Cu3 124.0(4) . . ?
C21 O7 Cu3 121.0(4) . 7_556 ?
O7 C21 O5 124.1(6) . . ?
O7 C21 C22 118.0(6) . . ?
O5 C21 C22 117.9(6) . . ?
C23B C22 C23A 44.4(14) . . ?
C23B C22 C21 112.5(16) . . ?
C23A C22 C21 117.8(8) . . ?
C23B C22 H22A 68.2 . . ?
C23A C22 H22A 107.9 . . ?
C21 C22 H22A 107.9 . . ?
C23B C22 H22B 138.8 . . ?
C23A C22 H22B 107.9 . . ?
C21 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C22 C23A H23A 109.5 . . ?
C22 C23A H23B 109.5 . . ?
C22 C23A H23C 109.5 . . ?
C22 C23B H23D 109.5 . . ?
C22 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
O10 Cl1 O11 112.9(4) . . ?
O10 Cl1 O9 112.0(4) . . ?
O11 Cl1 O9 110.0(4) . . ?
O10 Cl1 O12 107.4(4) . . ?
O11 Cl1 O12 107.4(4) . . ?
O9 Cl1 O12 106.8(4) . . ?
O15 Cl2 O14A 93.5(18) . . ?
O15 Cl2 O13A 104.6(10) . . ?
O14A Cl2 O13A 99.7(19) . . ?
O15 Cl2 O16B 104.1(7) . . ?
O14A Cl2 O16B 144(2) . . ?
O13A Cl2 O16B 105.6(10) . . ?
O15 Cl2 O14B 117.0(8) . . ?
O14A Cl2 O14B 47.8(17) . . ?
O13A Cl2 O14B 126.1(11) . . ?
O16B Cl2 O14B 96.2(8) . . ?
O15 Cl2 O16A 123.3(10) . . ?
O14A Cl2 O16A 142(2) . . ?
O13A Cl2 O16A 64.9(12) . . ?
O16B Cl2 O16A 42.1(9) . . ?
O14B Cl2 O16A 111.6(11) . . ?
O15 Cl2 O13B 111.4(8) . . ?
O14A Cl2 O13B 64.3(17) . . ?
O13A Cl2 O13B 36.0(10) . . ?
O16B Cl2 O13B 132.6(9) . . ?
O14B Cl2 O13B 94.7(10) . . ?
O16A Cl2 O13B 91.3(12) . . ?
Cl2 O13A O16A 57.7(7) . . ?
Cl2 O16A O13A 57.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_complex_3
_database_code_depnum_ccdc_archive 'CCDC 1424794'
_audit_update_record             
;
2016-02-03 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H84 Cu6 N8 O16, 4(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C66 H88 Cl4 Cu6 N8 O34'
_chemical_formula_weight         2060.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   30.454(6)
_cell_length_b                   13.005(3)
_cell_length_c                   24.876(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.482(6)
_cell_angle_gamma                90.00
_cell_volume                     8966(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295
_cell_measurement_reflns_used    44447
_cell_measurement_theta_min      1.73
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4216
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44447
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         24.98
_reflns_number_total             7803
_reflns_number_gt                5314
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PLATON (Spek, 2009)'

_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)+(0.1154P)²+84.2126P] 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         7803
_refine_ls_number_parameters     525
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0800
_refine_ls_wR_factor_ref         0.2579
_refine_ls_wR_factor_gt          0.2120
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.09466(3) 0.27971(8) -0.06028(4) 0.0556(3) Uani 1 1 d . B .
Cu2 Cu 0.13584(4) 0.19752(9) 0.06220(4) 0.0603(3) Uani 1 1 d . B .
Cu3 Cu 0.20808(3) 0.21731(7) -0.00674(4) 0.0475(3) Uani 1 1 d . . .
O1 O 0.0995(2) 0.3162(5) 0.0172(2) 0.0604(14) Uani 1 1 d . . .
C1 C 0.0868(3) 0.4024(7) 0.0351(4) 0.060(2) Uani 1 1 d . . .
C2 C 0.0964(3) 0.4163(8) 0.0953(4) 0.070(2) Uani 1 1 d . . .
C3 C 0.0840(4) 0.5102(10) 0.1141(5) 0.088(3) Uani 1 1 d . . .
H3 H 0.0907 0.5188 0.1539 0.106 Uiso 1 1 calc R . .
C4 C 0.0621(4) 0.5896(11) 0.0751(7) 0.098(4) Uani 1 1 d . . .
C5 C 0.0529(4) 0.5751(9) 0.0173(5) 0.086(3) Uani 1 1 d . . .
H5 H 0.0383 0.6283 -0.0090 0.103 Uiso 1 1 calc R . .
C6 C 0.0641(3) 0.4858(8) -0.0049(4) 0.067(2) Uani 1 1 d . . .
C7 C 0.0506(6) 0.6903(12) 0.0980(8) 0.142(6) Uani 1 1 d . . .
H7A H 0.0327 0.7343 0.0652 0.213 Uiso 1 1 calc R . .
H7B H 0.0802 0.7237 0.1231 0.213 Uiso 1 1 calc R . .
H7C H 0.0318 0.6763 0.1200 0.213 Uiso 1 1 calc R . .
C8 C 0.0550(3) 0.4812(8) -0.0652(5) 0.079(3) Uani 1 1 d . . .
H8 H 0.0407 0.5392 -0.0873 0.094 Uiso 1 1 calc R . .
N1 N 0.0638(3) 0.4084(7) -0.0935(3) 0.074(2) Uani 1 1 d . . .
C9 C 0.0534(5) 0.4164(10) -0.1571(5) 0.102(4) Uani 1 1 d . . .
H9A H 0.0212 0.3907 -0.1810 0.122 Uiso 1 1 calc R . .
H9B H 0.0551 0.4876 -0.1677 0.122 Uiso 1 1 calc R . .
C10 C 0.0897(4) 0.3545(11) -0.1677(4) 0.100(4) Uani 1 1 d . . .
H10A H 0.1208 0.3884 -0.1504 0.120 Uiso 1 1 calc R . .
H10B H 0.0804 0.3475 -0.2098 0.120 Uiso 1 1 calc R . .
N2 N 0.0929(3) 0.2513(7) -0.1405(3) 0.071(2) Uani 1 1 d . . .
H2 H 0.1213 0.2215 -0.1356 0.085 Uiso 1 1 d R . .
C11 C 0.0536(4) 0.1818(10) -0.1765(4) 0.084(3) Uani 1 1 d . . .
H11A H 0.0613 0.1516 -0.2072 0.101 Uiso 1 1 calc R . .
H11B H 0.0241 0.2212 -0.1955 0.101 Uiso 1 1 calc R . .
C12 C 0.0455(4) 0.0990(10) -0.1411(5) 0.097(4) Uani 1 1 d . . .
H12A H 0.0197 0.0541 -0.1662 0.116 Uiso 1 1 calc R . .
H12B H 0.0746 0.0583 -0.1221 0.116 Uiso 1 1 calc R . .
O2 O 0.0329(2) 0.1470(6) -0.0980(3) 0.0819(19) Uani 1 1 d . . .
H2A H 0.0282 0.1027 -0.0775 0.123 Uiso 1 1 d R . .
C13 C 0.1199(4) 0.3425(10) 0.1404(5) 0.085(3) Uani 1 1 d . . .
H13 H 0.1220 0.3579 0.1779 0.102 Uiso 1 1 calc R . .
N3 N 0.1389(3) 0.2554(8) 0.1346(3) 0.078(2) Uani 1 1 d . B .
C14 C 0.1649(6) 0.1845(11) 0.1848(5) 0.128(6) Uani 1 1 d D . .
H14A H 0.1989 0.2024 0.2029 0.154 Uiso 1 1 calc R A 1
H14B H 0.1521 0.1917 0.2144 0.154 Uiso 1 1 calc R A 1
C15A C 0.1598(7) 0.0833(12) 0.1653(7) 0.090(5) Uiso 0.70 1 d PD B 1
H15A H 0.1272 0.0599 0.1560 0.108 Uiso 0.70 1 calc PR B 1
H15B H 0.1819 0.0397 0.1963 0.108 Uiso 0.70 1 calc PR B 1
C15B C 0.1899(14) 0.102(3) 0.1760(8) 0.115(15) Uiso 0.30 1 d PD B 2
H15C H 0.1868 0.0432 0.1981 0.138 Uiso 0.30 1 calc PR B 2
H15D H 0.2239 0.1194 0.1905 0.138 Uiso 0.30 1 calc PR B 2
N4 N 0.1702(4) 0.0749(7) 0.1104(4) 0.087(3) Uani 1 1 d D . .
H40 H 0.2021 0.0794 0.1179 0.104 Uiso 1 1 d R B .
C16 C 0.1523(6) -0.0368(13) 0.0893(9) 0.152(7) Uani 1 1 d D B .
H16A H 0.1708 -0.0817 0.1221 0.183 Uiso 1 1 calc R C 1
H16B H 0.1192 -0.0399 0.0852 0.183 Uiso 1 1 calc R C 1
C17A C 0.1523(8) -0.0832(18) 0.0391(7) 0.100 Uiso 0.50 1 d PD B 1
H17A H 0.1426 -0.1545 0.0376 0.120 Uiso 0.50 1 calc PR B 1
H17B H 0.1847 -0.0816 0.0406 0.120 Uiso 0.50 1 calc PR B 1
C17B C 0.1617(7) -0.057(2) 0.0399(7) 0.100 Uiso 0.50 1 d PD B 2
H17C H 0.1695 -0.1288 0.0390 0.120 Uiso 0.50 1 calc PR B 2
H17D H 0.1891 -0.0161 0.0419 0.120 Uiso 0.50 1 calc PR B 2
O3 O 0.1200(4) -0.0307(7) -0.0124(5) 0.140(4) Uani 1 1 d D . .
H3O H 0.1041 -0.0202 -0.0564 0.150 Uiso 1 1 d . . .
O4 O 0.13872(17) 0.1718(4) -0.0126(2) 0.0497(12) Uani 1 1 d . . .
H4 H 0.1292 0.1020 -0.0279 0.060 Uiso 1 1 calc R B .
O5 O 0.1873(2) 0.3614(4) -0.0247(2) 0.0614(14) Uani 1 1 d . . .
O7 O 0.2606(2) 0.4162(4) -0.0106(3) 0.0630(15) Uani 1 1 d . . .
C18 C 0.2177(3) 0.4311(6) -0.0203(3) 0.058(2) Uani 1 1 d . B .
C19 C 0.2001(4) 0.5422(7) -0.0258(4) 0.073(3) Uani 1 1 d . . .
H19A H 0.2138 0.5815 -0.0484 0.088 Uiso 1 1 calc R B .
H19B H 0.1653 0.5438 -0.0470 0.088 Uiso 1 1 calc R . .
C20 C 0.2145(3) 0.5909(6) 0.0342(4) 0.068(2) Uani 1 1 d . B .
C21 C 0.1924(5) 0.5602(13) 0.0702(6) 0.126(5) Uani 1 1 d . . .
H21 H 0.1692 0.5086 0.0574 0.151 Uiso 1 1 calc R B .
C22 C 0.2043(6) 0.605(2) 0.1248(8) 0.183(10) Uani 1 1 d . B .
H22 H 0.1902 0.5818 0.1494 0.220 Uiso 1 1 calc R . .
C23 C 0.2367(7) 0.6821(15) 0.1421(7) 0.133(6) Uani 1 1 d . . .
H23 H 0.2419 0.7190 0.1762 0.160 Uiso 1 1 calc R B .
C24 C 0.2623(8) 0.7067(11) 0.1090(8) 0.145(7) Uani 1 1 d . B .
H24 H 0.2871 0.7549 0.1228 0.174 Uiso 1 1 calc R . .
C25 C 0.2506(5) 0.6591(9) 0.0555(6) 0.102(4) Uani 1 1 d . . .
H25 H 0.2681 0.6745 0.0336 0.123 Uiso 1 1 calc R B .
O6 O 0.30315(19) 0.3012(4) 0.0906(2) 0.0555(13) Uani 1 1 d . . .
O8 O 0.22931(19) 0.2518(4) 0.0781(2) 0.0558(13) Uani 1 1 d . . .
C26 C 0.2699(3) 0.2880(6) 0.1086(3) 0.0502(18) Uani 1 1 d . B .
C27 C 0.2813(3) 0.3163(7) 0.1719(4) 0.063(2) Uani 1 1 d . . .
H27A H 0.2841 0.2533 0.1940 0.076 Uiso 1 1 calc R B .
H27B H 0.2542 0.3545 0.1725 0.076 Uiso 1 1 calc R . .
C28 C 0.3265(3) 0.3790(7) 0.2035(3) 0.055(2) Uani 1 1 d . B .
C29 C 0.3618(3) 0.3457(7) 0.2560(4) 0.063(2) Uani 1 1 d . . .
H29 H 0.3579 0.2829 0.2714 0.076 Uiso 1 1 calc R B .
C30 C 0.4026(3) 0.4026(9) 0.2865(4) 0.074(3) Uani 1 1 d . B .
H30 H 0.4260 0.3779 0.3218 0.089 Uiso 1 1 calc R . .
C31 C 0.4089(3) 0.4960(8) 0.2646(4) 0.071(3) Uani 1 1 d . . .
H31 H 0.4361 0.5356 0.2855 0.086 Uiso 1 1 calc R B .
C32 C 0.3749(4) 0.5296(7) 0.2124(5) 0.077(3) Uani 1 1 d . B .
H32 H 0.3795 0.5915 0.1967 0.093 Uiso 1 1 calc R . .
C33 C 0.3330(3) 0.4721(7) 0.1817(4) 0.067(2) Uani 1 1 d . . .
H33 H 0.3095 0.4970 0.1465 0.081 Uiso 1 1 calc R B .
Cl1 Cl 0.01495(15) 0.1270(4) 0.0540(2) 0.1562(19) Uani 1 1 d D . .
O9 O 0.0182(7) 0.0446(13) 0.0934(6) 0.251(9) Uani 1 1 d D D .
O10 O 0.0509(4) 0.1144(9) 0.0312(6) 0.155(4) Uani 1 1 d D D .
O11 O 0.0196(7) 0.2276(11) 0.0812(11) 0.298(12) Uani 1 1 d D D .
O12A O -0.0352(5) 0.146(3) 0.0162(13) 0.185(11) Uiso 0.50 1 d PD D 1
O12B O -0.0220(11) 0.105(3) -0.0043(8) 0.224(15) Uiso 0.50 1 d PD D 2
Cl2 Cl 0.30626(14) 0.0022(3) 0.20889(14) 0.1093(11) Uani 1 1 d D . .
O13 O 0.2922(6) -0.0827(10) 0.2291(7) 0.217(7) Uani 1 1 d D E .
O14 O 0.2848(5) 0.0289(13) 0.1510(4) 0.204(7) Uani 1 1 d D E .
O15A O 0.3364(8) 0.0720(16) 0.2475(9) 0.151(8) Uiso 0.50 1 d PD E 1
O16A O 0.3393(9) -0.062(2) 0.2028(14) 0.195(11) Uiso 0.50 1 d PD E 1
O15B O 0.2889(11) 0.0757(19) 0.2345(13) 0.201(12) Uiso 0.50 1 d PD E 2
O16B O 0.3544(4) 0.025(2) 0.2348(11) 0.156(8) Uiso 0.50 1 d PD E 2
O1W O 0.4228(15) -0.260(3) 0.1242(17) 0.241(15) Uiso 0.50 1 d P . .
O2W O 0.0863(13) 0.685(3) -0.2146(15) 0.219(13) Uiso 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.929(8) . ?
Cu1 O1 1.930(5) . ?
Cu1 O4 1.964(5) . ?
Cu1 N2 2.008(7) . ?
Cu1 O2 2.436(7) . ?
Cu1 Cu2 2.9719(15) . ?
Cu2 N3 1.917(8) . ?
Cu2 O4 1.929(5) . ?
Cu2 O1 1.958(6) . ?
Cu2 N4 2.009(9) . ?
Cu3 O7 1.941(6) 7 ?
Cu3 O5 1.970(6) . ?
Cu3 O6 1.983(5) 7 ?
Cu3 O8 1.986(5) . ?
Cu3 O4 2.139(5) . ?
Cu3 Cu3 2.5781(18) 7 ?
O1 C1 1.321(10) . ?
C1 C2 1.414(12) . ?
C1 C6 1.440(13) . ?
C2 C3 1.414(14) . ?
C2 C13 1.424(15) . ?
C3 C4 1.384(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.360(16) . ?
C4 C7 1.525(17) . ?
C5 C6 1.387(14) . ?
C5 H5 0.9300 . ?
C6 C8 1.411(14) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.272(12) . ?
C8 H8 0.9300 . ?
N1 C9 1.483(12) . ?
C9 C10 1.476(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.488(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C11 1.470(13) . ?
N2 H2 0.9101 . ?
C11 C12 1.474(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2 1.427(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
O2 H2A 0.8201 . ?
C13 N3 1.307(15) . ?
C13 H13 0.9300 . ?
N3 C14 1.490(15) . ?
C14 C15B 1.38(2) . ?
C14 C15A 1.388(18) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15A N4 1.529(15) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C15B N4 1.530(17) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
N4 C16 1.56(2) . ?
N4 H40 0.9099 . ?
C16 C17A 1.39(2) . ?
C16 C17B 1.40(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17A O3 1.425(16) . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
C17B O3 1.431(16) . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
O3 H3O 1.006(10) . ?
O4 H4 0.9800 . ?
O5 C18 1.266(10) . ?
O7 C18 1.244(10) . ?
O7 Cu3 1.941(6) 7 ?
C18 C19 1.527(12) . ?
C19 C20 1.510(13) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C25 1.339(14) . ?
C20 C21 1.383(16) . ?
C21 C22 1.381(19) . ?
C21 H21 0.9300 . ?
C22 C23 1.35(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.39(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.37(2) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
O6 C26 1.279(9) . ?
O6 Cu3 1.983(5) 7 ?
O8 C26 1.243(9) . ?
C26 C27 1.509(11) . ?
C27 C28 1.511(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C33 1.373(12) . ?
C28 C29 1.374(11) . ?
C29 C30 1.374(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.376(14) . ?
C30 H30 0.9300 . ?
C31 C32 1.354(14) . ?
C31 H31 0.9300 . ?
C32 C33 1.401(13) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
Cl1 O9 1.429(9) . ?
Cl1 O10 1.435(8) . ?
Cl1 O12A 1.446(10) . ?
Cl1 O12B 1.447(10) . ?
Cl1 O11 1.453(9) . ?
Cl2 O13 1.355(8) . ?
Cl2 O14 1.357(7) . ?
Cl2 O15A 1.363(10) . ?
Cl2 O16A 1.365(10) . ?
Cl2 O16B 1.365(10) . ?
Cl2 O15B 1.370(10) . ?

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 Cu1 O1 92.1(3) . . ?
N1 Cu1 O4 165.5(3) . . ?
O1 Cu1 O4 79.8(2) . . ?
N1 Cu1 N2 85.7(3) . . ?
O1 Cu1 N2 175.5(3) . . ?
O4 Cu1 N2 101.5(3) . . ?
N1 Cu1 O2 106.8(3) . . ?
O1 Cu1 O2 106.6(2) . . ?
O4 Cu1 O2 87.2(2) . . ?
N2 Cu1 O2 77.8(3) . . ?
N1 Cu1 Cu2 132.5(2) . . ?
O1 Cu1 Cu2 40.51(18) . . ?
O4 Cu1 Cu2 39.81(15) . . ?
N2 Cu1 Cu2 141.2(2) . . ?
O2 Cu1 Cu2 94.02(17) . . ?
N3 Cu2 O4 166.0(3) . . ?
N3 Cu2 O1 91.4(3) . . ?
O4 Cu2 O1 80.0(2) . . ?
N3 Cu2 N4 86.6(4) . . ?
O4 Cu2 N4 102.5(3) . . ?
O1 Cu2 N4 176.6(3) . . ?
N3 Cu2 Cu1 131.1(3) . . ?
O4 Cu2 Cu1 40.68(15) . . ?
O1 Cu2 Cu1 39.80(16) . . ?
N4 Cu2 Cu1 142.3(3) . . ?
O7 Cu3 O5 169.6(2) 7 . ?
O7 Cu3 O6 88.9(2) 7 7 ?
O5 Cu3 O6 88.7(2) . 7 ?
O7 Cu3 O8 93.0(2) 7 . ?
O5 Cu3 O8 87.6(2) . . ?
O6 Cu3 O8 169.6(2) 7 . ?
O7 Cu3 O4 98.5(2) 7 . ?
O5 Cu3 O4 91.9(2) . . ?
O6 Cu3 O4 99.2(2) 7 . ?
O8 Cu3 O4 90.7(2) . . ?
O7 Cu3 Cu3 84.11(18) 7 7 ?
O5 Cu3 Cu3 85.58(18) . 7 ?
O6 Cu3 Cu3 84.64(15) 7 7 ?
O8 Cu3 Cu3 85.34(16) . 7 ?
O4 Cu3 Cu3 175.41(15) . 7 ?
C1 O1 Cu1 129.3(6) . . ?
C1 O1 Cu2 130.6(5) . . ?
Cu1 O1 Cu2 99.7(3) . . ?
O1 C1 C2 120.4(9) . . ?
O1 C1 C6 122.0(8) . . ?
C2 C1 C6 117.6(8) . . ?
C1 C2 C3 119.7(11) . . ?
C1 C2 C13 124.3(9) . . ?
C3 C2 C13 115.9(10) . . ?
C4 C3 C2 121.9(11) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C5 C4 C3 117.8(11) . . ?
C5 C4 C7 122.3(15) . . ?
C3 C4 C7 119.8(13) . . ?
C4 C5 C6 124.0(12) . . ?
C4 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C8 119.1(10) . . ?
C5 C6 C1 118.9(9) . . ?
C8 C6 C1 121.9(9) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 128.9(10) . . ?
N1 C8 H8 115.6 . . ?
C6 C8 H8 115.6 . . ?
C8 N1 C9 122.5(9) . . ?
C8 N1 Cu1 125.8(7) . . ?
C9 N1 Cu1 111.7(7) . . ?
C10 C9 N1 107.9(9) . . ?
C10 C9 H9A 110.1 . . ?
N1 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
N1 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C9 C10 N2 108.9(9) . . ?
C9 C10 H10A 109.9 . . ?
N2 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
N2 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C11 N2 C10 113.2(8) . . ?
C11 N2 Cu1 113.5(6) . . ?
C10 N2 Cu1 104.8(6) . . ?
C11 N2 H2 108.0 . . ?
C10 N2 H2 108.9 . . ?
Cu1 N2 H2 108.2 . . ?
N2 C11 C12 112.4(8) . . ?
N2 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N2 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
O2 C12 C11 107.0(9) . . ?
O2 C12 H12A 110.3 . . ?
C11 C12 H12A 110.3 . . ?
O2 C12 H12B 110.3 . . ?
C11 C12 H12B 110.3 . . ?
H12A C12 H12B 108.6 . . ?
C12 O2 Cu1 101.2(6) . . ?
C12 O2 H2A 109.4 . . ?
Cu1 O2 H2A 124.4 . . ?
N3 C13 C2 126.8(9) . . ?
N3 C13 H13 116.6 . . ?
C2 C13 H13 116.6 . . ?
C13 N3 C14 123.4(10) . . ?
C13 N3 Cu2 126.3(7) . . ?
C14 N3 Cu2 110.3(8) . . ?
C15B C14 C15A 37(2) . . ?
C15B C14 N3 118.9(16) . . ?
C15A C14 N3 110.5(11) . . ?
C15B C14 H14A 73.1 . . ?
C15A C14 H14A 109.5 . . ?
N3 C14 H14A 109.5 . . ?
C15B C14 H14B 128.0 . . ?
C15A C14 H14B 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15A N4 110.1(12) . . ?
C14 C15A H15A 109.6 . . ?
N4 C15A H15A 109.6 . . ?
C14 C15A H15B 109.6 . . ?
N4 C15A H15B 109.6 . . ?
H15A C15A H15B 108.1 . . ?
C14 C15B N4 110.5(14) . . ?
C14 C15B H15C 109.6 . . ?
N4 C15B H15C 109.6 . . ?
C14 C15B H15D 109.6 . . ?
N4 C15B H15D 109.6 . . ?
H15C C15B H15D 108.1 . . ?
C15A N4 C15B 33.3(18) . . ?
C15A N4 C16 101.1(10) . . ?
C15B N4 C16 120(2) . . ?
C15A N4 Cu2 103.1(8) . . ?
C15B N4 Cu2 109.3(12) . . ?
C16 N4 Cu2 120.9(8) . . ?
C15A N4 H40 114.1 . . ?
C15B N4 H40 81.5 . . ?
C16 N4 H40 108.9 . . ?
Cu2 N4 H40 108.6 . . ?
C17A C16 C17B 18.3(19) . . ?
C17A C16 N4 125.0(16) . . ?
C17B C16 N4 107.1(15) . . ?
C17A C16 H16A 106.1 . . ?
C17B C16 H16A 111.5 . . ?
N4 C16 H16A 106.1 . . ?
C17A C16 H16B 106.1 . . ?
C17B C16 H16B 118.9 . . ?
N4 C16 H16B 106.1 . . ?
H16A C16 H16B 106.3 . . ?
C16 C17A O3 110.0(14) . . ?
C16 C17A H17A 109.7 . . ?
O3 C17A H17A 109.7 . . ?
C16 C17A H17B 109.7 . . ?
O3 C17A H17B 109.7 . . ?
H17A C17A H17B 108.2 . . ?
C16 C17B O3 109.0(14) . . ?
C16 C17B H17C 109.9 . . ?
O3 C17B H17C 109.9 . . ?
C16 C17B H17D 109.9 . . ?
O3 C17B H17D 109.9 . . ?
H17C C17B H17D 108.3 . . ?
C17A O3 C17B 17.9(18) . . ?
C17A O3 H3O 152.2(13) . . ?
C17B O3 H3O 150.0(14) . . ?
Cu2 O4 Cu1 99.5(2) . . ?
Cu2 O4 Cu3 108.9(2) . . ?
Cu1 O4 Cu3 104.6(2) . . ?
Cu2 O4 H4 114.2 . . ?
Cu1 O4 H4 114.2 . . ?
Cu3 O4 H4 114.2 . . ?
C18 O5 Cu3 120.5(5) . . ?
C18 O7 Cu3 124.2(6) . 7 ?
O7 C18 O5 125.2(8) . . ?
O7 C18 C19 117.8(8) . . ?
O5 C18 C19 117.0(8) . . ?
C20 C19 C18 111.1(7) . . ?
C20 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C25 C20 C21 118.4(11) . . ?
C25 C20 C19 121.6(11) . . ?
C21 C20 C19 119.9(9) . . ?
C22 C21 C20 121.1(14) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C23 C22 C21 119.1(17) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 120.0(15) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.1(15) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C20 C25 C24 121.6(14) . . ?
C20 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C26 O6 Cu3 122.4(5) . 7 ?
C26 O8 Cu3 122.5(5) . . ?
O8 C26 O6 124.7(7) . . ?
O8 C26 C27 118.0(7) . . ?
O6 C26 C27 117.4(7) . . ?
C26 C27 C28 116.2(7) . . ?
C26 C27 H27A 108.2 . . ?
C28 C27 H27A 108.2 . . ?
C26 C27 H27B 108.2 . . ?
C28 C27 H27B 108.2 . . ?
H27A C27 H27B 107.4 . . ?
C33 C28 C29 118.0(8) . . ?
C33 C28 C27 121.3(8) . . ?
C29 C28 C27 120.6(8) . . ?
C28 C29 C30 121.8(9) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
C29 C30 C31 120.0(9) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 119.2(9) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 120.7(9) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C28 C33 C32 120.2(9) . . ?
C28 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
O9 Cl1 O10 109.8(11) . . ?
O9 Cl1 O12A 109.2(15) . . ?
O10 Cl1 O12A 122.5(15) . . ?
O9 Cl1 O12B 110.2(18) . . ?
O10 Cl1 O12B 89.3(18) . . ?
O12A Cl1 O12B 37.7(17) . . ?
O9 Cl1 O11 112.9(13) . . ?
O10 Cl1 O11 110.1(9) . . ?
O12A Cl1 O11 91.2(17) . . ?
O12B Cl1 O11 122(2) . . ?
O13 Cl2 O14 121.1(10) . . ?
O13 Cl2 O15A 120.4(13) . . ?
O14 Cl2 O15A 117.7(13) . . ?
O13 Cl2 O16A 84.4(15) . . ?
O14 Cl2 O16A 95.3(15) . . ?
O15A Cl2 O16A 100.0(14) . . ?
O13 Cl2 O16B 116.1(13) . . ?
O14 Cl2 O16B 113.3(13) . . ?
O15A Cl2 O16B 41.2(13) . . ?
O16A Cl2 O16B 59.1(10) . . ?
O13 Cl2 O15B 98.9(16) . . ?
O14 Cl2 O15B 101.9(15) . . ?
O15A Cl2 O15B 59.0(10) . . ?
O16A Cl2 O15B 157.4(19) . . ?
O16B Cl2 O15B 100.2(14) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.598
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.143
