# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_s2682b
_database_code_depnum_ccdc_archive 'CCDC 1046422'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu3(L)(CO3)(ClO4)3](ClO4)'
_chemical_formula_moiety         'C52 H69 Cl3 Cu3 N9 O18, Cl O4'
_chemical_formula_sum            'C52 H69 Cl4 Cu3 N9 O22'
_chemical_formula_weight         1504.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   18.6062(18)
_cell_length_b                   18.6062(18)
_cell_length_c                   30.69(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9201(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      25.29

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4650
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_T_max  0.7734
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21618
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.29
_reflns_number_total             3733
_reflns_number_gt                3366
_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)+(0.0738P)²+123.2831P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3733
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0770
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.75043(2) 0.49850(3) 0.076797(14) 0.01890(12) Uani 1 d . . .
Cl1 Cl 0.65035(6) 0.61966(7) 0.07212(4) 0.0373(3) Uani 1 d . . .
O1 O 0.64727(14) 0.39042(14) 0.07795(8) 0.0188(6) Uani 1 d . . .
N1 N 0.76381(18) 0.50142(18) 0.14196(11) 0.0228(8) Uani 1 d . . .
N3 N 0.73609(18) 0.51570(19) 0.01412(10) 0.0241(8) Uani 1 d . . .
N2 N 0.86711(18) 0.58905(19) 0.06378(11) 0.0235(8) Uani 1 d . . .
O2 O 0.62283(17) 0.66164(18) 0.10024(11) 0.0363(8) Uani 1 d . . .
O5 O 0.70172(18) 0.59589(18) 0.09600(10) 0.0380(8) Uani 1 d . . .
C5 C 0.8362(2) 0.5378(2) 0.16367(13) 0.0262(9) Uani 1 d . . .
C15 C 0.6667 0.3333 0.07829(19) 0.0159(13) Uani 1 d S . .
C10 C 0.7914(2) 0.5921(2) 0.00011(13) 0.0267(9) Uani 1 d . . .
C11 C 0.7840(2) 0.6212(3) -0.04089(14) 0.0337(10) Uani 1 d . . .
O3 O 0.7043(2) 0.6794(2) 0.03909(11) 0.045(3) Uani 1 d . . .
C9 C 0.8587(2) 0.6437(2) 0.03196(13) 0.0275(10) Uani 1 d . . .
H9A H 0.9118 0.6772 0.0163 0.033 Uiso 1 calc R . .
H9B H 0.8449 0.6821 0.0473 0.033 Uiso 1 calc R . .
C8 C 0.9115(2) 0.5508(3) 0.04239(14) 0.0309(10) Uani 1 d . . .
H8A H 0.9698 0.5932 0.0379 0.046 Uiso 1 calc R . .
H8B H 0.8856 0.5275 0.0142 0.046 Uiso 1 calc R . .
H8C H 0.9085 0.5066 0.0610 0.046 Uiso 1 calc R . .
C1 C 0.6917(3) 0.4608(2) 0.21046(14) 0.0305(11) Uani 1 d . . .
H1 H 0.6405 0.4343 0.2258 0.037 Uiso 1 calc R . .
C2 C 0.6930(2) 0.4647(2) 0.16560(13) 0.0245(9) Uani 1 d . . .
H2 H 0.6415 0.4405 0.1505 0.029 Uiso 1 calc R . .
C4 C 0.8382(3) 0.5350(2) 0.20900(13) 0.0301(10) Uani 1 d . . .
H4 H 0.8900 0.5604 0.2238 0.036 Uiso 1 calc R . .
O4 O 0.5869(2) 0.5540(2) 0.05026(14) 0.0553(11) Uani 1 d . . .
C3 C 0.7655(3) 0.4956(2) 0.23253(14) 0.0333(11) Uani 1 d . . .
H3 H 0.7666 0.4927 0.2634 0.040 Uiso 1 calc R . .
C14 C 0.6720(2) 0.4666(3) -0.01111(14) 0.0315(11) Uani 1 d . . .
H14 H 0.6323 0.4136 -0.0003 0.038 Uiso 1 calc R . .
C13 C 0.6603(3) 0.4888(3) -0.05215(14) 0.0404(12) Uani 1 d . . .
C7 C 0.9126(3) 0.6377(3) 0.10236(15) 0.0332(11) Uani 1 d . . .
H7A H 0.8854 0.6683 0.1134 0.040 Uiso 1 calc R . .
H7B H 0.9699 0.6791 0.0937 0.040 Uiso 1 calc R . .
C12 C 0.7188(2) 0.5670(3) -0.06662(13) 0.0385(11) Uani 1 d . . .
C6 C 0.9159(2) 0.5835(3) 0.13902(15) 0.0347(11) Uani 1 d . . .
H6A H 0.9296 0.5429 0.1264 0.042 Uiso 1 calc R . .
H6B H 0.9609 0.6190 0.1595 0.042 Uiso 1 calc R . .
O7 O 0.70743(19) 0.5919(2) -0.10673(10) 0.0513(9) Uani 1 d . . .
C18 C 0.8429(3) 0.7098(3) -0.05289(16) 0.0473(12) Uani 1 d . . .
H18A H 0.8304 0.7205 -0.0824 0.071 Uiso 1 calc R . .
H18B H 0.9000 0.7202 -0.0519 0.071 Uiso 1 calc R . .
H18C H 0.8369 0.7466 -0.0322 0.071 Uiso 1 calc R . .
C17 C 0.5859(3) 0.4299(5) -0.07928(17) 0.070(2) Uani 1 d . . .
H17A H 0.6049 0.4168 -0.1064 0.105 Uiso 1 calc R . .
H17B H 0.5527 0.4559 -0.0862 0.105 Uiso 1 calc R . .
H17C H 0.5519 0.3786 -0.0628 0.105 Uiso 1 calc R . .
C19 C 0.7585(4) 0.5865(5) -0.14081(18) 0.083(2) Uani 1 d . . .
H19A H 0.8169 0.6276 -0.1354 0.108 Uiso 1 calc R . .
H19B H 0.7416 0.5975 -0.1691 0.108 Uiso 1 calc R . .
H19C H 0.7517 0.5307 -0.1409 0.108 Uiso 1 calc R . .
Cl2 Cl 0.6667 0.3333 0.3333 0.0403(7) Uani 1 d S . .
O21 O 0.6667 0.3333 0.2895(3) 0.038(2) Uani 0.50 d SP . .
O22 O 0.7490(5) 0.3638(6) 0.3160(3) 0.069(3) Uani 0.50 d P . .
Cl3 Cl 0.6667 0.3333 0.86533(15) 0.0560(13) Uani 0.50 d SP A 1
O31 O 0.6667 0.3333 0.9117(4) 0.053(3) Uani 0.50 d SP A 1
O32 O 0.7066(6) 0.4165(6) 0.8498(3) 0.082(3) Uani 0.50 d P A 1


_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 1.967(2) . ?
Cu1 N3 1.990(4) . ?
Cu1 N1 2.013(4) . ?
Cu1 N2 2.013(3) . ?
Cl1 O4 1.376(3) . ?
Cl1 O2 1.420(4) . ?
Cl1 O5 1.438(4) . ?
Cl1 O3 1.468(3) . ?
O1 C15 1.281(3) . ?
N1 C5 1.344(5) . ?
N1 C2 1.353(5) . ?
N3 C14 1.329(5) . ?
N3 C10 1.342(5) . ?
N2 C7 1.474(5) . ?
N2 C9 1.474(5) . ?
N2 C8 1.486(6) . ?
C5 C4 1.393(6) . ?
C5 C6 1.495(6) . ?
C15 O1 1.281(3) 3_665 ?
C15 O1 1.281(3) 2_655 ?
C10 C11 1.403(6) . ?
C10 C9 1.497(5) . ?
C11 C12 1.375(6) . ?
C11 C18 1.499(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C1 C3 1.369(6) . ?
C1 C2 1.378(6) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C4 C3 1.377(6) . ?
C4 H4 0.9500 . ?
C3 H3 0.9500 . ?
C14 C13 1.377(6) . ?
C14 H14 0.9500 . ?
C13 C12 1.384(6) . ?
C13 C17 1.515(6) . ?
C7 C6 1.533(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C12 O7 1.369(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O7 C19 1.451(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N3 92.35(11) . . ?
O1 Cu1 N1 93.10(11) . . ?
N3 Cu1 N1 168.81(14) . . ?
O1 Cu1 N2 162.13(13) . . ?
N3 Cu1 N2 81.30(13) . . ?
N1 Cu1 N2 96.17(12) . . ?
O4 Cl1 O2 113.5(2) . . ?
O4 Cl1 O5 112.5(2) . . ?
O2 Cl1 O5 109.7(2) . . ?
O4 Cl1 O3 107.1(2) . . ?
O2 Cl1 O3 107.5(2) . . ?
O5 Cl1 O3 106.1(2) . . ?
C15 O1 Cu1 108.19(14) . . ?
C5 N1 C2 117.8(3) . . ?
C5 N1 Cu1 125.8(3) . . ?
C2 N1 Cu1 116.3(3) . . ?
C14 N3 C10 119.4(4) . . ?
C14 N3 Cu1 126.8(3) . . ?
C10 N3 Cu1 112.7(2) . . ?
C7 N2 C9 109.6(3) . . ?
C7 N2 C8 111.3(3) . . ?
C9 N2 C8 108.3(3) . . ?
C7 N2 Cu1 113.7(2) . . ?
C9 N2 Cu1 105.4(2) . . ?
C8 N2 Cu1 108.2(2) . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 119.7(4) . . ?
C4 C5 C6 119.3(3) . . ?
O1 C15 O1 119.993(10) 3_665 2_655 ?
O1 C15 O1 119.994(10) 3_665 . ?
O1 C15 O1 119.993(10) 2_655 . ?
N3 C10 C11 121.6(3) . . ?
N3 C10 C9 115.0(3) . . ?
C11 C10 C9 123.3(3) . . ?
C12 C11 C10 117.0(4) . . ?
C12 C11 C18 123.8(4) . . ?
C10 C11 C18 119.1(4) . . ?
N2 C9 C10 109.5(3) . . ?
N2 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
N2 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C1 C2 118.9(4) . . ?
C3 C1 H1 120.6 . . ?
C2 C1 H1 120.6 . . ?
N1 C2 C1 123.3(4) . . ?
N1 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C1 C3 C4 118.6(4) . . ?
C1 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
N3 C14 C13 123.3(4) . . ?
N3 C14 H14 118.3 . . ?
C13 C14 H14 118.3 . . ?
C14 C13 C12 116.7(4) . . ?
C14 C13 C17 120.7(4) . . ?
C12 C13 C17 122.6(4) . . ?
N2 C7 C6 112.6(3) . . ?
N2 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
O7 C12 C11 119.9(4) . . ?
O7 C12 C13 118.1(4) . . ?
C11 C12 C13 121.9(4) . . ?
C5 C6 C7 113.0(4) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C12 O7 C19 114.1(4) . . ?
C11 C18 H18A 109.5 . . ?
C11 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C11 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O7 C19 H19A 109.5 . . ?
O7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
C2 N1 C5 C4 2.4(6) . . . . ?
C2 N1 C5 C6 -176.3(4) . . . . ?
C14 N3 C10 C11 -1.0(6) . . . . ?
C14 N3 C10 C9 177.0(4) . . . . ?
N3 C10 C11 C12 -1.7(7) . . . . ?
C9 C10 C11 C12 -179.5(4) . . . . ?
N3 C10 C11 C18 174.1(4) . . . . ?
C9 C10 C11 C18 -3.8(7) . . . . ?
C7 N2 C9 C10 -162.2(3) . . . . ?
C8 N2 C9 C10 76.2(4) . . . . ?
N3 C10 C9 N2 21.7(5) . . . . ?
C11 C10 C9 N2 -160.3(4) . . . . ?
C5 N1 C2 C1 -2.0(6) . . . . ?
C3 C1 C2 N1 0.1(7) . . . . ?
N1 C5 C4 C3 -0.8(7) . . . . ?
C6 C5 C4 C3 177.8(4) . . . . ?
C2 C1 C3 C4 1.5(7) . . . . ?
C5 C4 C3 C1 -1.1(7) . . . . ?
C10 N3 C14 C13 2.3(7) . . . . ?
N3 C14 C13 C12 -0.8(8) . . . . ?
N3 C14 C13 C17 179.9(5) . . . . ?
C9 N2 C7 C6 173.9(3) . . . . ?
C8 N2 C7 C6 -66.3(4) . . . . ?
C10 C11 C12 O7 179.1(4) . . . . ?
C18 C11 C12 O7 3.5(7) . . . . ?
C10 C11 C12 C13 3.3(7) . . . . ?
C18 C11 C12 C13 -172.3(5) . . . . ?
C14 C13 C12 O7 -178.0(4) . . . . ?
C17 C13 C12 O7 1.3(8) . . . . ?
C14 C13 C12 C11 -2.1(8) . . . . ?
C17 C13 C12 C11 177.2(5) . . . . ?
N1 C5 C6 C7 42.8(6) . . . . ?
C4 C5 C6 C7 -135.9(4) . . . . ?
N2 C7 C6 C5 -76.7(5) . . . . ?
C11 C12 O7 C19 82.2(6) . . . . ?
C13 C12 O7 C19 -101.8(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.29
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.128
####################################################################### 
# 
# 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_s2649a
_database_code_depnum_ccdc_archive 'CCDC 1046423'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu2(L2)2(CO3)](ClO4)2.H2O'
_chemical_formula_moiety         'C31 H72 Cu2 N8 O3, 2(Cl O4), H2 O'
_chemical_formula_sum            'C31 H74 Cl2 Cu2 N8 O12'
_chemical_formula_weight         948.98

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.5041(11)
_cell_length_b                   23.516(3)
_cell_length_c                   18.0212(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.48(2)
_cell_angle_gamma                90.00
_cell_volume                     4362.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1000
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      26.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2016
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_T_max  0.8095
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30734
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8520
_reflns_number_gt                6848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0754P)²+9.5040P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8520
_refine_ls_number_parameters     538
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1542
_refine_ls_wR_factor_gt          0.1441
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.047
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.43351(5) 0.25555(2) 0.94730(3) 0.02724(15) Uani 1 d . . .
Cu2 Cu 0.26414(5) 0.44516(2) 0.75386(3) 0.02863(15) Uani 1 d . . .
N6 N 0.2410(3) 0.49386(15) 0.65771(19) 0.0305(8) Uani 1 d . . .
N2 N 0.5089(3) 0.17825(15) 0.9850(2) 0.0299(8) Uani 1 d . . .
N3 N 0.3197(3) 0.20936(14) 0.8606(2) 0.0329(8) Uani 1 d . . .
H3 H 0.3405 0.2245 0.8168 0.039 Uiso 1 calc R . .
N7 N 0.1482(3) 0.51865(14) 0.79370(19) 0.0281(7) Uani 1 d . . .
H7 H 0.2094 0.5445 0.8181 0.034 Uiso 1 calc R . .
N1 N 0.6309(3) 0.27215(14) 0.93202(19) 0.0284(7) Uani 1 d . . .
H1 H 0.6309 0.2617 0.8822 0.034 Uiso 1 calc R . .
N4 N 0.4163(4) 0.26833(19) 1.0624(2) 0.0428(10) Uani 1 d . . .
H4 H 0.4989 0.2800 1.0863 0.051 Uiso 1 calc R A 1
N5 N 0.4605(4) 0.46617(19) 0.7659(2) 0.0451(10) Uani 1 d . . .
H5 H 0.4973 0.4348 0.7470 0.054 Uiso 1 calc R . .
N8 N 0.1475(6) 0.3880(2) 0.6891(3) 0.0796(17) Uani 1 d . . .
H8A H 0.1939 0.3545 0.7010 0.103 Uiso 1 calc R . .
O9 O 0.2970(3) 0.39955(12) 0.84284(17) 0.0376(7) Uani 1 d . . .
O10 O 0.3592(3) 0.32770(11) 0.91674(16) 0.0310(6) Uani 1 d . . .
O11 O 0.3562(3) 0.31906(12) 0.79255(17) 0.0333(7) Uani 1 d . . .
C9 C 0.3383(3) 0.34765(16) 0.8485(2) 0.0254(8) Uani 1 d . . .
C1 C 0.3724(4) 0.15048(17) 0.8636(3) 0.0354(10) Uani 1 d . . .
H1A H 0.4445 0.1486 0.8357 0.042 Uiso 1 calc R . .
H1B H 0.3035 0.1238 0.8395 0.042 Uiso 1 calc R . .
C6 C 0.6845(4) 0.33101(18) 0.9392(2) 0.0313(9) Uani 1 d . . .
H6 H 0.6330 0.3536 0.8965 0.047 Uiso 1 calc R . .
C15 C 0.0873(4) 0.5452(2) 0.7213(3) 0.0372(10) Uani 1 d . . .
H15A H 0.0548 0.5835 0.7307 0.045 Uiso 1 calc R . .
H15B H 0.0125 0.5219 0.6961 0.045 Uiso 1 calc R . .
C10 C 0.1856(5) 0.54988(19) 0.6705(3) 0.0396(11) Uani 1 d . . .
H10A H 0.1431 0.5664 0.6212 0.048 Uiso 1 calc R . .
H10B H 0.2564 0.5758 0.6940 0.048 Uiso 1 calc R . .
C2 C 0.4212(4) 0.13373(18) 0.9458(3) 0.0350(10) Uani 1 d . . .
H2A H 0.3466 0.1288 0.9712 0.042 Uiso 1 calc R . .
H2B H 0.4683 0.0971 0.9482 0.042 Uiso 1 calc R . .
C3 C 0.7121(4) 0.22879(19) 0.9788(2) 0.0320(9) Uani 1 d . . .
H3A H 0.7277 0.2399 1.0328 0.038 Uiso 1 calc R . .
H3B H 0.7971 0.2255 0.9633 0.038 Uiso 1 calc R . .
C14 C 0.1242(5) 0.48303(19) 0.9191(2) 0.0354(10) Uani 1 d . . .
H14A H 0.1723 0.4493 0.9084 0.053 Uiso 1 calc R . .
H14B H 0.0601 0.4720 0.9492 0.053 Uiso 1 calc R . .
H14C H 0.1847 0.5107 0.9474 0.053 Uiso 1 calc R . .
C13 C 0.0549(4) 0.50952(18) 0.8449(2) 0.0308(9) Uani 1 d . . .
H13 H -0.0122 0.4818 0.8196 0.037 Uiso 1 calc R . .
C4 C 0.6414(4) 0.17288(18) 0.9677(3) 0.0327(10) Uani 1 d . . .
H4A H 0.6343 0.1601 0.9146 0.039 Uiso 1 calc R . .
H4B H 0.6914 0.1439 1.0012 0.039 Uiso 1 calc R . .
C8 C 0.1749(4) 0.21398(19) 0.8474(3) 0.0406(11) Uani 1 d . . .
H8 H 0.1539 0.2546 0.8562 0.049 Uiso 1 calc R . .
C7 C 0.6650(5) 0.3587(2) 1.0119(3) 0.0406(11) Uani 1 d . . .
H7A H 0.5722 0.3590 1.0134 0.061 Uiso 1 calc R . .
H7B H 0.6975 0.3978 1.0141 0.061 Uiso 1 calc R . .
H7C H 0.7125 0.3372 1.0552 0.061 Uiso 1 calc R . .
C5 C 0.5157(4) 0.1752(2) 1.0686(3) 0.0393(11) Uani 1 d . . .
H5A H 0.6005 0.1900 1.0956 0.047 Uiso 1 calc R . .
H5B H 0.5082 0.1351 1.0839 0.047 Uiso 1 calc R . .
C11 C 0.3721(4) 0.5008(2) 0.6399(3) 0.0398(11) Uani 1 d . . .
H11A H 0.3712 0.5328 0.6041 0.048 Uiso 1 calc R . .
H11B H 0.3963 0.4658 0.6155 0.048 Uiso 1 calc R . .
C12 C -0.0154(5) 0.5640(2) 0.8597(3) 0.0462(12) Uani 1 d . . .
H12A H 0.0486 0.5940 0.8767 0.069 Uiso 1 calc R . .
H12B H -0.0659 0.5568 0.8990 0.069 Uiso 1 calc R . .
H12C H -0.0738 0.5760 0.8130 0.069 Uiso 1 calc R . .
C24 C 0.1535(5) 0.4629(2) 0.5962(3) 0.0453(12) Uani 1 d . . .
H24A H 0.1756 0.4720 0.5466 0.054 Uiso 1 calc R . .
H24B H 0.0620 0.4739 0.5946 0.054 Uiso 1 calc R . .
C17 C 0.5391(5) 0.4737(3) 0.8439(3) 0.0517(14) Uani 1 d . . .
H17 H 0.5363 0.4366 0.8707 0.062 Uiso 1 calc R . .
C22 C -0.0004(5) 0.3567(2) 0.7718(3) 0.0415(11) Uani 1 d . . .
H22A H 0.0194 0.3166 0.7830 0.062 Uiso 1 calc R . .
H22B H -0.0924 0.3639 0.7719 0.062 Uiso 1 calc R . .
H22C H 0.0536 0.3804 0.8105 0.062 Uiso 1 calc R . .
C26 C 0.1124(5) 0.1999(2) 0.7658(3) 0.0522(14) Uani 1 d . . .
H26A H 0.1442 0.2264 0.7316 0.078 Uiso 1 calc R . .
H26B H 0.0178 0.2034 0.7590 0.078 Uiso 1 calc R . .
H26C H 0.1349 0.1609 0.7542 0.078 Uiso 1 calc R . .
C18 C 0.4798(5) 0.5177(3) 0.8882(3) 0.0555(15) Uani 1 d . . .
H18A H 0.4672 0.5534 0.8595 0.083 Uiso 1 calc R . .
H18B H 0.5381 0.5243 0.9371 0.083 Uiso 1 calc R . .
H18C H 0.3958 0.5039 0.8966 0.083 Uiso 1 calc R . .
C16 C 0.8257(5) 0.3338(2) 0.9309(3) 0.0481(12) Uani 1 d . . .
H16A H 0.8806 0.3147 0.9740 0.072 Uiso 1 calc R . .
H16B H 0.8523 0.3736 0.9293 0.072 Uiso 1 calc R . .
H16C H 0.8351 0.3148 0.8838 0.072 Uiso 1 calc R . .
C27 C 0.1160(5) 0.1782(2) 0.9020(3) 0.0462(12) Uani 1 d . . .
H27A H 0.1290 0.1378 0.8924 0.069 Uiso 1 calc R . .
H27B H 0.0228 0.1862 0.8948 0.069 Uiso 1 calc R . .
H27C H 0.1582 0.1875 0.9541 0.069 Uiso 1 calc R . .
C20 C 0.4711(5) 0.5124(3) 0.7117(3) 0.0504(14) Uani 1 d . . .
H20A H 0.5597 0.5132 0.7006 0.061 Uiso 1 calc R . .
H20B H 0.4537 0.5496 0.7333 0.061 Uiso 1 calc R . .
C23 C -0.0460(5) 0.3266(3) 0.6362(3) 0.0518(13) Uani 1 d . . .
H23A H -0.0429 0.3377 0.5842 0.078 Uiso 1 calc R . .
H23B H -0.1367 0.3247 0.6420 0.078 Uiso 1 calc R . .
H23C H -0.0051 0.2893 0.6472 0.078 Uiso 1 calc R . .
C31 C 0.4066(5) 0.2100(3) 1.0900(3) 0.0490(13) Uani 1 d . . .
H31A H 0.3215 0.1933 1.0667 0.059 Uiso 1 calc R . .
H31B H 0.4145 0.2100 1.1456 0.059 Uiso 1 calc R . .
C19 C 0.6824(5) 0.4853(3) 0.8424(3) 0.0640(17) Uani 1 d . . .
H19A H 0.7142 0.4563 0.8115 0.096 Uiso 1 calc R . .
H19B H 0.7338 0.4840 0.8941 0.096 Uiso 1 calc R . .
H19C H 0.6907 0.5230 0.8206 0.096 Uiso 1 calc R . .
C21 C 0.0205(6) 0.3706(4) 0.6928(3) 0.0739(18) Uani 1 d . . .
H21 H -0.0311 0.4047 0.6793 0.089 Uiso 1 calc R . .
C25 C 0.1716(8) 0.4003(3) 0.6125(3) 0.079(2) Uani 1 d . . .
H25A H 0.1105 0.3782 0.5744 0.094 Uiso 1 calc R . .
H25B H 0.2612 0.3889 0.6096 0.094 Uiso 1 calc R . .
C28 C 0.187(4) 0.3033(13) 1.037(2) 0.042(4) Uani 0.482(12) d P B 1
H28A H 0.1612 0.2698 1.0622 0.063 Uiso 0.482(12) calc PR B 1
H28B H 0.1822 0.2947 0.9829 0.063 Uiso 0.482(12) calc PR B 1
H28C H 0.1288 0.3350 1.0414 0.063 Uiso 0.482(12) calc PR B 1
C29 C 0.3273(10) 0.3198(6) 1.0733(7) 0.029(3) Uani 0.482(12) d PU B 1
H29 H 0.3538 0.3538 1.0467 0.035 Uiso 0.482(12) calc PR B 1
C30 C 0.3406(10) 0.3332(5) 1.1567(6) 0.043(3) Uani 0.482(12) d PU B 1
H30A H 0.3160 0.2997 1.1831 0.065 Uiso 0.482(12) calc PR B 1
H30B H 0.2836 0.3651 1.1628 0.065 Uiso 0.482(12) calc PR B 1
H30C H 0.4309 0.3434 1.1782 0.065 Uiso 0.482(12) calc PR B 1
C48 C 0.177(4) 0.2880(11) 1.046(2) 0.042(4) Uani 0.518(12) d P B 2
H48A H 0.1137 0.3115 1.0662 0.063 Uiso 0.518(12) calc PR B 2
H48B H 0.1528 0.2479 1.0485 0.063 Uiso 0.518(12) calc PR B 2
H48C H 0.1761 0.2988 0.9938 0.063 Uiso 0.518(12) calc PR B 2
C49 C 0.3103(11) 0.2973(6) 1.0936(7) 0.039(3) Uani 0.518(12) d PU B 2
H49 H 0.3127 0.2844 1.1467 0.047 Uiso 0.518(12) calc PR B 2
C50 C 0.3478(8) 0.3587(5) 1.0934(6) 0.042(3) Uani 0.518(12) d PU B 2
H50A H 0.4358 0.3636 1.1234 0.063 Uiso 0.518(12) calc PR B 2
H50B H 0.2867 0.3815 1.1155 0.063 Uiso 0.518(12) calc PR B 2
H50C H 0.3455 0.3711 1.0413 0.063 Uiso 0.518(12) calc PR B 2
Cl1 Cl 0.30651(12) 0.70115(5) 0.75722(6) 0.0423(3) Uani 1 d . . .
O3 O 0.2102(4) 0.6981(2) 0.6921(2) 0.0692(12) Uani 1 d . . .
O2 O 0.4282(4) 0.7151(2) 0.7338(3) 0.0820(14) Uani 1 d . . .
O4 O 0.3185(5) 0.6490(2) 0.7974(3) 0.0904(16) Uani 1 d . . .
O1 O 0.2885(6) 0.7432(2) 0.8082(3) 0.108(2) Uani 1 d . . .
Cl2 Cl 0.25322(10) 0.52252(4) 0.40617(6) 0.0321(2) Uani 1 d . . .
O5 O 0.1811(3) 0.55490(14) 0.45144(18) 0.0406(8) Uani 1 d . . .
O6 O 0.2127(4) 0.46508(16) 0.4079(3) 0.0780(14) Uani 1 d . . .
O8 O 0.3871(4) 0.5249(2) 0.4389(3) 0.0800(15) Uani 1 d . . .
O7 O 0.2239(6) 0.5426(3) 0.3317(3) 0.109(2) Uani 1 d . . .
O12 O 0.5750(5) 0.35382(18) 0.7480(2) 0.0664(12) Uani 1 d D . .
H90 H 0.624(5) 0.333(2) 0.730(4) 0.100 Uiso 1 d D . .
H91 H 0.510(4) 0.337(2) 0.754(4) 0.100 Uiso 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O10 1.903(3) . ?
Cu1 N2 2.044(3) . ?
Cu1 N3 2.075(3) . ?
Cu1 N4 2.139(4) . ?
Cu1 N1 2.181(4) . ?
Cu2 O9 1.903(3) . ?
Cu2 N8 2.025(5) . ?
Cu2 N6 2.051(3) . ?
Cu2 N5 2.090(4) . ?
Cu2 N7 2.309(3) . ?
N6 C10 1.477(6) . ?
N6 C11 1.484(5) . ?
N6 C24 1.483(6) . ?
N2 C2 1.478(6) . ?
N2 C4 1.492(5) . ?
N2 C5 1.495(6) . ?
N3 C1 1.488(5) . ?
N3 C8 1.496(6) . ?
N3 H3 0.9300 . ?
N7 C15 1.473(5) . ?
N7 C13 1.489(5) . ?
N7 H7 0.9300 . ?
N1 C3 1.480(5) . ?
N1 C6 1.490(5) . ?
N1 H1 0.9300 . ?
N4 C31 1.471(7) . ?
N4 C49 1.507(12) . ?
N4 C29 1.565(12) . ?
N4 H4 0.9300 . ?
N5 C20 1.481(6) . ?
N5 C17 1.492(7) . ?
N5 H5 0.9300 . ?
N8 C25 1.479(7) . ?
O9 C9 1.293(5) . ?
O10 C9 1.294(5) . ?
O11 C9 1.257(5) . ?
C1 C2 1.519(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C6 C7 1.513(6) . ?
C6 C16 1.521(6) . ?
C6 H6 1.0000 . ?
C15 C10 1.514(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.503(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C14 C13 1.523(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 C12 1.528(6) . ?
C13 H13 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C8 C27 1.516(7) . ?
C8 C26 1.523(7) . ?
C8 H8 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C5 C31 1.518(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C11 C20 1.514(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C24 C25 1.505(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C17 C18 1.513(8) . ?
C17 C19 1.536(7) . ?
C17 H17 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C28 C29 1.54(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.515(16) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C48 C49 1.51(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.496(16) . ?
C49 H49 1.0000 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
Cl1 O1 1.388(4) . ?
Cl1 O3 1.391(4) . ?
Cl1 O4 1.418(5) . ?
Cl1 O2 1.462(4) . ?
Cl2 O7 1.397(4) . ?
Cl2 O8 1.414(4) . ?
Cl2 O6 1.418(4) . ?
Cl2 O5 1.437(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
O10 Cu1 N2 176.97(13) . . ?
O10 Cu1 N3 96.14(13) . . ?
N2 Cu1 N3 84.95(14) . . ?
O10 Cu1 N4 92.65(14) . . ?
N2 Cu1 N4 84.51(15) . . ?
N3 Cu1 N4 131.03(16) . . ?
O10 Cu1 N1 98.61(13) . . ?
N2 Cu1 N1 83.46(13) . . ?
N3 Cu1 N1 114.72(14) . . ?
N4 Cu1 N1 111.32(14) . . ?
O9 Cu2 N8 95.71(18) . . ?
O9 Cu2 N6 176.36(14) . . ?
N8 Cu2 N6 85.80(18) . . ?
O9 Cu2 N5 92.05(15) . . ?
N8 Cu2 N5 133.5(2) . . ?
N6 Cu2 N5 84.53(14) . . ?
O9 Cu2 N7 100.28(12) . . ?
N8 Cu2 N7 112.3(2) . . ?
N6 Cu2 N7 82.16(13) . . ?
N5 Cu2 N7 111.18(15) . . ?
C10 N6 C11 110.3(4) . . ?
C10 N6 C24 110.5(4) . . ?
C11 N6 C24 110.9(4) . . ?
C10 N6 Cu2 110.5(3) . . ?
C11 N6 Cu2 106.6(3) . . ?
C24 N6 Cu2 108.0(3) . . ?
C2 N2 C4 111.0(3) . . ?
C2 N2 C5 110.4(3) . . ?
C4 N2 C5 110.4(3) . . ?
C2 N2 Cu1 107.9(2) . . ?
C4 N2 Cu1 108.8(2) . . ?
C5 N2 Cu1 108.4(3) . . ?
C1 N3 C8 115.6(3) . . ?
C1 N3 Cu1 107.8(2) . . ?
C8 N3 Cu1 119.8(3) . . ?
C1 N3 H3 103.9 . . ?
C8 N3 H3 103.9 . . ?
Cu1 N3 H3 103.9 . . ?
C15 N7 C13 112.7(3) . . ?
C15 N7 Cu2 101.8(2) . . ?
C13 N7 Cu2 122.5(2) . . ?
C15 N7 H7 106.2 . . ?
C13 N7 H7 106.2 . . ?
Cu2 N7 H7 106.2 . . ?
C3 N1 C6 115.2(3) . . ?
C3 N1 Cu1 105.0(2) . . ?
C6 N1 Cu1 120.5(3) . . ?
C3 N1 H1 104.9 . . ?
C6 N1 H1 104.9 . . ?
Cu1 N1 H1 104.9 . . ?
C31 N4 C49 101.0(6) . . ?
C31 N4 C29 126.6(6) . . ?
C31 N4 Cu1 102.8(3) . . ?
C49 N4 Cu1 129.6(5) . . ?
C29 N4 Cu1 113.5(5) . . ?
C31 N4 H4 103.8 . . ?
C49 N4 H4 112.6 . . ?
C29 N4 H4 103.8 . . ?
Cu1 N4 H4 103.8 . . ?
C20 N5 C17 115.7(4) . . ?
C20 N5 Cu2 107.9(3) . . ?
C17 N5 Cu2 118.4(3) . . ?
C20 N5 H5 104.4 . . ?
C17 N5 H5 104.4 . . ?
Cu2 N5 H5 104.4 . . ?
C25 N8 Cu2 102.2(4) . . ?
C9 O9 Cu2 126.9(3) . . ?
C9 O10 Cu1 125.5(3) . . ?
O11 C9 O10 123.0(3) . . ?
O11 C9 O9 122.9(4) . . ?
O10 C9 O9 114.1(4) . . ?
N3 C1 C2 109.2(4) . . ?
N3 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N3 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
N1 C6 C7 111.1(3) . . ?
N1 C6 C16 113.0(4) . . ?
C7 C6 C16 111.7(4) . . ?
N1 C6 H6 106.9 . . ?
C7 C6 H6 106.9 . . ?
C16 C6 H6 106.9 . . ?
N7 C15 C10 109.8(3) . . ?
N7 C15 H15A 109.7 . . ?
C10 C15 H15A 109.7 . . ?
N7 C15 H15B 109.7 . . ?
C10 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
N6 C10 C15 111.5(4) . . ?
N6 C10 H10A 109.3 . . ?
C15 C10 H10A 109.3 . . ?
N6 C10 H10B 109.3 . . ?
C15 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
N2 C2 C1 109.9(3) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C4 108.3(3) . . ?
N1 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
N1 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
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 . . ?
N7 C13 C14 110.1(3) . . ?
N7 C13 C12 112.8(4) . . ?
C14 C13 C12 110.6(4) . . ?
N7 C13 H13 107.7 . . ?
C14 C13 H13 107.7 . . ?
C12 C13 H13 107.7 . . ?
N2 C4 C3 110.8(3) . . ?
N2 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N3 C8 C27 113.0(4) . . ?
N3 C8 C26 111.5(4) . . ?
C27 C8 C26 110.7(4) . . ?
N3 C8 H8 107.1 . . ?
C27 C8 H8 107.1 . . ?
C26 C8 H8 107.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C5 C31 110.1(3) . . ?
N2 C5 H5A 109.6 . . ?
C31 C5 H5A 109.6 . . ?
N2 C5 H5B 109.6 . . ?
C31 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
N6 C11 C20 110.2(4) . . ?
N6 C11 H11A 109.6 . . ?
C20 C11 H11A 109.6 . . ?
N6 C11 H11B 109.6 . . ?
C20 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N6 C24 C25 107.4(4) . . ?
N6 C24 H24A 110.2 . . ?
C25 C24 H24A 110.2 . . ?
N6 C24 H24B 110.2 . . ?
C25 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
N5 C17 C18 111.7(4) . . ?
N5 C17 C19 111.4(4) . . ?
C18 C17 C19 113.3(5) . . ?
N5 C17 H17 106.7 . . ?
C18 C17 H17 106.7 . . ?
C19 C17 H17 106.7 . . ?
C8 C26 H26A 109.5 . . ?
C8 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C8 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C6 C16 H16A 109.5 . . ?
C6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C27 H27A 109.5 . . ?
C8 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C8 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N5 C20 C11 107.6(4) . . ?
N5 C20 H20A 110.2 . . ?
C11 C20 H20A 110.2 . . ?
N5 C20 H20B 110.2 . . ?
C11 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C31 C5 108.1(4) . . ?
N4 C31 H31A 110.1 . . ?
C5 C31 H31A 110.1 . . ?
N4 C31 H31B 110.1 . . ?
C5 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N8 C25 C24 109.5(5) . . ?
N8 C25 H25A 109.8 . . ?
C24 C25 H25A 109.8 . . ?
N8 C25 H25B 109.8 . . ?
C24 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
C30 C29 C28 111.6(17) . . ?
C30 C29 N4 110.2(8) . . ?
C28 C29 N4 107.2(16) . . ?
C30 C29 H29 109.2 . . ?
C28 C29 H29 109.2 . . ?
N4 C29 H29 109.2 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 C48 110.8(12) . . ?
C50 C49 N4 102.8(9) . . ?
C48 C49 N4 113.5(17) . . ?
C50 C49 H49 109.8 . . ?
C48 C49 H49 109.8 . . ?
N4 C49 H49 109.8 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O1 Cl1 O3 115.1(4) . . ?
O1 Cl1 O4 106.7(4) . . ?
O3 Cl1 O4 111.3(3) . . ?
O1 Cl1 O2 105.9(3) . . ?
O3 Cl1 O2 107.4(3) . . ?
O4 Cl1 O2 110.4(3) . . ?
O7 Cl2 O8 113.4(4) . . ?
O7 Cl2 O6 109.5(4) . . ?
O8 Cl2 O6 107.8(3) . . ?
O7 Cl2 O5 109.0(2) . . ?
O8 Cl2 O5 109.6(2) . . ?
O6 Cl2 O5 107.3(3) . . ?

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
C8 N3 C1 C2 -101.3(4) . . . . ?
C3 N1 C6 C7 -77.1(5) . . . . ?
C3 N1 C6 C16 49.3(5) . . . . ?
C13 N7 C15 C10 -176.6(4) . . . . ?
C11 N6 C10 C15 -154.1(4) . . . . ?
C24 N6 C10 C15 82.9(4) . . . . ?
N7 C15 C10 N6 56.8(5) . . . . ?
C4 N2 C2 C1 -79.8(4) . . . . ?
C5 N2 C2 C1 157.6(4) . . . . ?
N3 C1 C2 N2 -50.8(5) . . . . ?
C6 N1 C3 C4 177.4(3) . . . . ?
C15 N7 C13 C14 -179.0(4) . . . . ?
C15 N7 C13 C12 -54.9(5) . . . . ?
C2 N2 C4 C3 156.4(3) . . . . ?
C5 N2 C4 C3 -80.9(4) . . . . ?
N1 C3 C4 N2 -55.3(4) . . . . ?
C1 N3 C8 C27 52.0(5) . . . . ?
C1 N3 C8 C26 -73.4(5) . . . . ?
C2 N2 C5 C31 -87.0(5) . . . . ?
C4 N2 C5 C31 150.0(4) . . . . ?
C10 N6 C11 C20 77.7(5) . . . . ?
C24 N6 C11 C20 -159.6(4) . . . . ?
C10 N6 C24 C25 -150.2(4) . . . . ?
C11 N6 C24 C25 87.2(5) . . . . ?
C20 N5 C17 C18 74.7(5) . . . . ?
C20 N5 C17 C19 -53.1(6) . . . . ?
C17 N5 C20 C11 -172.7(4) . . . . ?
N6 C11 C20 N5 54.2(5) . . . . ?
C49 N4 C31 C5 -175.5(6) . . . . ?
C29 N4 C31 C5 -178.1(6) . . . . ?
N2 C5 C31 N4 -56.0(5) . . . . ?
N6 C24 C25 N8 55.8(7) . . . . ?
C31 N4 C29 C30 62.4(11) . . . . ?
C49 N4 C29 C30 56.6(15) . . . . ?
C31 N4 C29 C28 -59.3(16) . . . . ?
C49 N4 C29 C28 -65(2) . . . . ?
C31 N4 C49 C50 159.2(7) . . . . ?
C29 N4 C49 C50 -25.5(13) . . . . ?
C31 N4 C49 C48 -81.1(12) . . . . ?
C29 N4 C49 C48 94(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.096
