# Electronic Supplementary Material (ESI) for Metallomics.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pgaprime

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H18 Cl Cu N3 O, C H4 O'
_chemical_formula_sum            'C17 H22 Cl Cu N3 O2'
_chemical_formula_weight         399.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cu Cu 0.1330 1.4803
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_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                   7.9513(4)
_cell_length_b                   10.1551(5)
_cell_length_c                   11.4377(5)
_cell_angle_alpha                103.3680(10)
_cell_angle_beta                 96.2100(10)
_cell_angle_gamma                100.2460(10)
_cell_volume                     873.38(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6302
_cell_measurement_theta_min      3.24
_cell_measurement_theta_max      33.60

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             414
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI US'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            8951
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         31.10
_reflns_number_total             4258
_reflns_number_gt                3941
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_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. All non-hydrogens were 
 refined anistropically. Hydrogens were found in difference Fourier maps,
 placed geometrically on their carrier atom and refined with a riding
 model, except that on the lattice methanol oxygen O2 that was refined 
 freely with its thermal parameter 1.2 times that of O2 and a distance
 restraint.
;

_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)+(0.1111P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4258
_refine_ls_number_parameters     221
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1622
_refine_ls_wR_factor_gt          0.1601
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.116
_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 0.27458(3) 0.42721(3) 0.59412(2) 0.01196(14) Uani 1 1 d . . .
Cl1 Cl 0.29679(8) 0.29406(6) 0.72536(5) 0.01695(17) Uani 1 1 d . . .
O1 O 0.4368(2) 0.57453(18) 0.70093(16) 0.0163(4) Uani 1 1 d . . .
N1 N 0.2617(3) 0.5316(2) 0.47134(18) 0.0136(4) Uani 1 1 d . . .
N2 N 0.1389(3) 0.4668(2) 0.37220(19) 0.0164(4) Uani 1 1 d . . .
H2A H 0.1238 0.5023 0.3095 0.020 Uiso 1 1 calc R . .
N3 N 0.0802(3) 0.2992(2) 0.47573(19) 0.0136(4) Uani 1 1 d . . .
C1 C 0.5155(3) 0.6937(2) 0.6859(2) 0.0144(5) Uani 1 1 d . . .
C2 C 0.6304(3) 0.7896(2) 0.7861(2) 0.0147(5) Uani 1 1 d . . .
C3 C 0.7157(3) 0.9135(2) 0.7675(2) 0.0177(5) Uani 1 1 d . . .
H3A H 0.7960 0.9764 0.8326 0.021 Uiso 1 1 calc R . .
C4 C 0.6880(3) 0.9496(3) 0.6563(2) 0.0188(5) Uani 1 1 d . . .
H4A H 0.7474 1.0358 0.6477 0.023 Uiso 1 1 calc R . .
C5 C 0.5754(3) 0.8598(3) 0.5612(2) 0.0168(5) Uani 1 1 d . . .
H5A H 0.5558 0.8839 0.4862 0.020 Uiso 1 1 calc R . .
C6 C 0.4874(3) 0.7307(2) 0.5735(2) 0.0131(4) Uani 1 1 d . . .
C7 C 0.6521(3) 0.7596(2) 0.9123(2) 0.0158(5) Uani 1 1 d . . .
C8 C 0.7841(4) 0.8749(3) 1.0050(2) 0.0229(5) Uani 1 1 d . . .
H8A H 0.8966 0.8840 0.9768 0.034 Uiso 1 1 calc R . .
H8B H 0.7949 0.8520 1.0838 0.034 Uiso 1 1 calc R . .
H8C H 0.7451 0.9625 1.0138 0.034 Uiso 1 1 calc R . .
C9 C 0.7158(4) 0.6239(3) 0.9075(2) 0.0196(5) Uani 1 1 d . . .
H9A H 0.6347 0.5472 0.8487 0.029 Uiso 1 1 calc R . .
H9B H 0.7227 0.6057 0.9882 0.029 Uiso 1 1 calc R . .
H9C H 0.8306 0.6326 0.8827 0.029 Uiso 1 1 calc R . .
C10 C 0.4771(4) 0.7482(3) 0.9597(2) 0.0232(6) Uani 1 1 d . . .
H10A H 0.3904 0.6747 0.9018 0.035 Uiso 1 1 calc R . .
H10B H 0.4397 0.8364 0.9686 0.035 Uiso 1 1 calc R . .
H10C H 0.4899 0.7262 1.0388 0.035 Uiso 1 1 calc R . .
C11 C 0.3606(3) 0.6489(2) 0.4726(2) 0.0145(5) Uani 1 1 d . . .
H11A H 0.3478 0.6823 0.4019 0.017 Uiso 1 1 calc R . .
C12 C 0.0404(3) 0.3431(2) 0.3760(2) 0.0148(5) Uani 1 1 d . . .
C13 C -0.0944(3) 0.2689(3) 0.2811(2) 0.0166(5) Uani 1 1 d . . .
H13A H -0.1205 0.3030 0.2121 0.020 Uiso 1 1 calc R . .
C14 C -0.1876(3) 0.1450(3) 0.2913(2) 0.0183(5) Uani 1 1 d . . .
H14A H -0.2797 0.0922 0.2290 0.022 Uiso 1 1 calc R . .
C15 C -0.1457(3) 0.0976(3) 0.3939(2) 0.0189(5) Uani 1 1 d . . .
H15A H -0.2082 0.0120 0.4016 0.023 Uiso 1 1 calc R . .
C16 C -0.0137(3) 0.1761(2) 0.4832(2) 0.0160(5) Uani 1 1 d . . .
H16A H 0.0136 0.1436 0.5529 0.019 Uiso 1 1 calc R . .
O1S O 0.0419(4) 0.6116(3) 0.2089(2) 0.0435(7) Uani 1 1 d D . .
H1S H -0.049(4) 0.646(4) 0.224(4) 0.052 Uiso 1 1 d D . .
C1S C 0.1344(4) 0.6778(3) 0.1328(3) 0.0251(6) Uani 1 1 d . . .
H1S1 H 0.1062 0.7689 0.1381 0.038 Uiso 1 1 calc R . .
H1S2 H 0.1026 0.6214 0.0486 0.038 Uiso 1 1 calc R . .
H1S3 H 0.2589 0.6892 0.1587 0.038 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.8768(18) . ?
Cu1 N1 1.950(2) . ?
Cu1 N3 1.983(2) . ?
Cu1 Cl1 2.2537(6) . ?
O1 C1 1.317(3) . ?
N1 C11 1.301(3) . ?
N1 N2 1.364(3) . ?
N2 C12 1.369(3) . ?
N2 H2A 0.8800 . ?
N3 C12 1.344(3) . ?
N3 C16 1.363(3) . ?
C1 C6 1.427(3) . ?
C1 C2 1.428(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.540(3) . ?
C3 C4 1.408(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.362(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.417(3) . ?
C5 H5A 0.9500 . ?
C6 C11 1.430(3) . ?
C7 C8 1.532(4) . ?
C7 C9 1.542(3) . ?
C7 C10 1.542(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9500 . ?
C12 C13 1.406(4) . ?
C13 C14 1.378(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.397(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.369(4) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
O1S C1S 1.409(3) . ?
O1S H1S 0.876(19) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 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 N1 91.27(8) . . ?
O1 Cu1 N3 169.17(8) . . ?
N1 Cu1 N3 80.94(9) . . ?
O1 Cu1 Cl1 90.92(6) . . ?
N1 Cu1 Cl1 175.51(6) . . ?
N3 Cu1 Cl1 97.38(6) . . ?
C1 O1 Cu1 131.01(16) . . ?
C11 N1 N2 118.9(2) . . ?
C11 N1 Cu1 127.29(18) . . ?
N2 N1 Cu1 113.71(15) . . ?
N1 N2 C12 116.0(2) . . ?
N1 N2 H2A 122.0 . . ?
C12 N2 H2A 122.0 . . ?
C12 N3 C16 117.9(2) . . ?
C12 N3 Cu1 113.49(16) . . ?
C16 N3 Cu1 128.61(17) . . ?
O1 C1 C6 122.1(2) . . ?
O1 C1 C2 118.8(2) . . ?
C6 C1 C2 119.1(2) . . ?
C3 C2 C1 117.9(2) . . ?
C3 C2 C7 121.2(2) . . ?
C1 C2 C7 120.8(2) . . ?
C2 C3 C4 122.8(2) . . ?
C2 C3 H3A 118.6 . . ?
C4 C3 H3A 118.6 . . ?
C5 C4 C3 119.5(2) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C4 C5 C6 120.4(2) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C11 116.4(2) . . ?
C1 C6 C11 123.2(2) . . ?
C8 C7 C2 111.8(2) . . ?
C8 C7 C9 106.9(2) . . ?
C2 C7 C9 111.67(19) . . ?
C8 C7 C10 108.0(2) . . ?
C2 C7 C10 109.4(2) . . ?
C9 C7 C10 108.9(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C6 124.3(2) . . ?
N1 C11 H11A 117.8 . . ?
C6 C11 H11A 117.8 . . ?
N3 C12 N2 115.8(2) . . ?
N3 C12 C13 122.9(2) . . ?
N2 C12 C13 121.3(2) . . ?
C14 C13 C12 117.9(2) . . ?
C14 C13 H13A 121.0 . . ?
C12 C13 H13A 121.0 . . ?
C13 C14 C15 119.6(2) . . ?
C13 C14 H14A 120.2 . . ?
C15 C14 H14A 120.2 . . ?
C16 C15 C14 119.2(2) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
N3 C16 C15 122.5(2) . . ?
N3 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C1S O1S H1S 111(3) . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        31.10
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.141
_database_code_depnum_ccdc_archive 'CCDC 964834'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pgbprime

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H76 Cl6 Cu3 N12 O4, 6(C H4 O)'
_chemical_formula_sum            'C86 H100 Cl6 Cu3 N12 O10'
_chemical_formula_weight         1865.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cu Cu 0.1330 1.4803
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_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                   10.9272(10)
_cell_length_b                   11.8160(11)
_cell_length_c                   18.887(2)
_cell_angle_alpha                73.7590(10)
_cell_angle_beta                 81.8970(10)
_cell_angle_gamma                72.6210(10)
_cell_volume                     2230.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6454
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.11

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             969
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI US'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            16072
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.13
_reflns_number_total             7548
_reflns_number_gt                6349
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_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. All non-hydrogens were
 refined anisotropically. One of the terbutyl groups (C37 > C40) is
 heavily disordered and was refined with strong displacement parameters
 restraints. Two of the lattice methanol molecules (O1S and O3S) were
 also refined with displacement parameters restraints due to large 
 thermal disorder. Hydrogens were placed geometrically on their carrier
 atom and refined with a riding model. The crystals were rather small
 and showed very poor diffraction at resolutions better than 0.8 angstrom.
 The present data were cut at 0.85 angstrom for this reason.
;

_vrf_PLAT027_pgbprime            
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      27.10 Deg.
RESPONSE: Significant diffraction was only detected up to a resolution
of ca. 0.80 angstrom, even with longer acquisition time. The present data
were thus cut at 0.85 angstrom, resulting relatively low thetamax and 
thetafull values.
;

_vrf_PLAT220_pgbprime            
;
PROBLEM: Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        4.9 Ratio
RESPONSE: One of the terbutyl groups (C37 > C40) was highly disordered and 
was refined with displacement parameters restraints. Even like this, the
Ueq of the corresponding carbon atoms remain much higher than those of the
rest of the main residue, thus resulting in a large Ueq(max)/Ueq(min)
ratio. The same occurs for the hydrogens carried by these atoms, resulting 
in a large Uiso(max)/Uiso(min).
;

_vrf_PLAT222_pgbprime            
;
PROBLEM: Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        5.7 Ratio
RESPONSE: One of the terbutyl groups (C37 > C40) was highly disordered and 
was refined with displacement parameters restraints. Even like this, the
Ueq of the corresponding carbon atoms remain much higher than those of the
rest of the main residue, thus resulting in a large Ueq(max)/Ueq(min)
ratio. The same occurs for the hydrogens carried by these atoms, resulting 
in a large Uiso(max)/Uiso(min).
;

_vrf_PLAT417_pgbprime            
;
PROBLEM: Short Inter D-H..H-D       H1S    ..  H3S     ..       1.99 Ang.
RESPONSE: Hydrogens were placed at calculated positions. Since two of the
methanol lattice molecules (O1S-C1S and O3S-C3S) showed some disorder and
were refined with displacement parameters restraints, the positions of the 
corresponding hydrogens may be ill-defined, resulting short H H contacts.
;

_vrf_PLAT413_pgbprime            
;
PROBLEM: Short Inter XH3 .. XHn     H2S3   ..  H39B    ..       2.10 Ang.
RESPONSE: Hydrogens were placed at calculated positions. Since two of the
methanol lattice molecules (O1S-C1S and O3S-C3S) showed some disorder and
were refined with displacement parameters restraints, the positions of the 
corresponding hydrogens may be ill-defined, resulting short H H contacts.
;

_vrf_THETM01_pgbprime            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: Significant diffraction was only detected up to a resolution
of ca. 0.80 angstrom, even with longer acquisition time. The present data
were thus cut at 0.85 angstrom, resulting relatively low thetamax and 
thetafull values.
;

_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)+(0.0506P)²+5.2591P] 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         7548
_refine_ls_number_parameters     535
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1233
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.091
_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 0.5000 0.5000 0.5000 0.01843(16) Uani 1 2 d S . .
Cu2 Cu 0.76753(4) 0.45237(4) 0.57856(2) 0.01820(13) Uani 1 1 d . . .
Cl1 Cl 0.41736(8) 0.65153(8) 0.39843(5) 0.0216(2) Uani 1 1 d . . .
Cl2 Cl 0.75445(8) 0.49884(8) 0.45341(5) 0.0217(2) Uani 1 1 d . . .
Cl3 Cl 0.93245(9) 0.28237(9) 0.57998(5) 0.0288(2) Uani 1 1 d . . .
O1 O 0.6078(2) 0.7535(3) 0.74021(14) 0.0277(6) Uani 1 1 d . . .
H1 H 0.5535 0.7402 0.7185 0.042 Uiso 1 1 calc R . .
O2 O 0.8192(3) 0.1509(3) 0.89134(17) 0.0432(8) Uani 1 1 d . . .
H2 H 0.8494 0.1864 0.8507 0.065 Uiso 1 1 calc R . .
N1 N 0.5112(3) 0.6251(3) 0.54892(17) 0.0199(7) Uani 1 1 d . . .
N2 N 0.6261(3) 0.6114(3) 0.57680(16) 0.0191(6) Uani 1 1 d . . .
N3 N 0.5022(3) 0.7930(3) 0.58080(16) 0.0191(7) Uani 1 1 d . . .
N4 N 0.7900(3) 0.4386(3) 0.68445(17) 0.0214(7) Uani 1 1 d . . .
N5 N 0.6948(3) 0.4143(3) 0.73711(17) 0.0239(7) Uani 1 1 d . . .
N6 N 0.8639(3) 0.4035(3) 0.79283(17) 0.0223(7) Uani 1 1 d . . .
C1 C 0.6213(3) 0.7108(3) 0.59598(19) 0.0185(8) Uani 1 1 d . . .
C2 C 0.4475(4) 0.9146(3) 0.5880(2) 0.0208(8) Uani 1 1 d . . .
C3 C 0.5171(4) 0.9823(4) 0.6063(2) 0.0244(8) Uani 1 1 d . . .
H3A H 0.6059 0.9479 0.6145 0.029 Uiso 1 1 calc R . .
C4 C 0.4562(4) 1.0997(4) 0.6125(2) 0.0295(9) Uani 1 1 d . . .
H4A H 0.5036 1.1460 0.6251 0.035 Uiso 1 1 calc R . .
C5 C 0.3262(4) 1.1514(4) 0.6004(2) 0.0310(9) Uani 1 1 d . . .
H5A H 0.2849 1.2319 0.6057 0.037 Uiso 1 1 calc R . .
C6 C 0.2579(4) 1.0852(4) 0.5808(2) 0.0291(9) Uani 1 1 d . . .
H6A H 0.1693 1.1209 0.5725 0.035 Uiso 1 1 calc R . .
C7 C 0.3163(4) 0.9665(3) 0.5730(2) 0.0218(8) Uani 1 1 d . . .
C8 C 0.2476(4) 0.9002(4) 0.5471(2) 0.0255(8) Uani 1 1 d . . .
H8A H 0.1593 0.9365 0.5381 0.031 Uiso 1 1 calc R . .
C9 C 0.3046(4) 0.7890(4) 0.5356(2) 0.0233(8) Uani 1 1 d . . .
H9A H 0.2593 0.7480 0.5163 0.028 Uiso 1 1 calc R . .
C10 C 0.4359(3) 0.7340(3) 0.5531(2) 0.0192(8) Uani 1 1 d . . .
C11 C 0.7293(3) 0.7278(3) 0.6266(2) 0.0191(8) Uani 1 1 d . . .
C12 C 0.8456(3) 0.7189(3) 0.5834(2) 0.0202(8) Uani 1 1 d . . .
H12A H 0.8539 0.6992 0.5372 0.024 Uiso 1 1 calc R . .
C13 C 0.9474(4) 0.7389(4) 0.6086(2) 0.0251(8) Uani 1 1 d . . .
H13A H 1.0269 0.7325 0.5801 0.030 Uiso 1 1 calc R . .
C14 C 0.9329(4) 0.7687(4) 0.6761(2) 0.0272(9) Uani 1 1 d . . .
H14A H 1.0030 0.7856 0.6918 0.033 Uiso 1 1 calc R . .
C15 C 0.8211(4) 0.7748(4) 0.7218(2) 0.0245(8) Uani 1 1 d . . .
C16 C 0.7179(3) 0.7504(4) 0.6965(2) 0.0224(8) Uani 1 1 d . . .
C17 C 0.8056(4) 0.8141(4) 0.7943(2) 0.0308(9) Uani 1 1 d . . .
C18 C 0.9311(4) 0.8331(5) 0.8109(3) 0.0409(11) Uani 1 1 d . . .
H18A H 0.9989 0.7556 0.8170 0.061 Uiso 1 1 calc R . .
H18B H 0.9174 0.8606 0.8565 0.061 Uiso 1 1 calc R . .
H18C H 0.9568 0.8950 0.7698 0.061 Uiso 1 1 calc R . .
C19 C 0.7691(5) 0.7184(4) 0.8606(2) 0.0377(11) Uani 1 1 d . . .
H19A H 0.8355 0.6402 0.8651 0.057 Uiso 1 1 calc R . .
H19B H 0.6866 0.7077 0.8534 0.057 Uiso 1 1 calc R . .
H19C H 0.7618 0.7460 0.9057 0.057 Uiso 1 1 calc R . .
C20 C 0.7021(4) 0.9384(4) 0.7857(3) 0.0380(11) Uani 1 1 d . . .
H20A H 0.7273 0.9988 0.7434 0.057 Uiso 1 1 calc R . .
H20B H 0.6937 0.9668 0.8307 0.057 Uiso 1 1 calc R . .
H20C H 0.6196 0.9286 0.7777 0.057 Uiso 1 1 calc R . .
C21 C 0.7399(4) 0.3909(4) 0.8021(2) 0.0245(8) Uani 1 1 d . . .
C22 C 0.9529(4) 0.3951(4) 0.8434(2) 0.0248(8) Uani 1 1 d . . .
C23 C 0.9233(4) 0.3742(4) 0.9195(2) 0.0321(10) Uani 1 1 d . . .
H23A H 0.8420 0.3626 0.9399 0.038 Uiso 1 1 calc R . .
C24 C 1.0145(4) 0.3707(4) 0.9649(2) 0.0362(10) Uani 1 1 d . . .
H24A H 0.9955 0.3564 1.0168 0.043 Uiso 1 1 calc R . .
C25 C 1.1332(4) 0.3879(5) 0.9352(2) 0.0385(11) Uani 1 1 d . . .
H25A H 1.1944 0.3858 0.9669 0.046 Uiso 1 1 calc R . .
C26 C 1.1632(4) 0.4080(4) 0.8605(2) 0.0355(10) Uani 1 1 d . . .
H26A H 1.2450 0.4191 0.8410 0.043 Uiso 1 1 calc R . .
C27 C 1.0729(4) 0.4120(4) 0.8123(2) 0.0272(9) Uani 1 1 d . . .
C28 C 1.1019(4) 0.4346(4) 0.7337(2) 0.0287(9) Uani 1 1 d . . .
H28A H 1.1846 0.4429 0.7142 0.034 Uiso 1 1 calc R . .
C29 C 1.0140(4) 0.4444(4) 0.6871(2) 0.0243(8) Uani 1 1 d . . .
H29A H 1.0338 0.4596 0.6353 0.029 Uiso 1 1 calc R . .
C30 C 0.8916(3) 0.4313(3) 0.7179(2) 0.0212(8) Uani 1 1 d . . .
C31 C 0.6695(4) 0.3496(4) 0.8723(2) 0.0277(9) Uani 1 1 d . . .
C32 C 0.5577(4) 0.4296(4) 0.8947(2) 0.0347(10) Uani 1 1 d . . .
H32A H 0.5272 0.5108 0.8654 0.042 Uiso 1 1 calc R . .
C33 C 0.4924(4) 0.3882(5) 0.9606(3) 0.0407(12) Uani 1 1 d . . .
H33A H 0.4140 0.4398 0.9756 0.049 Uiso 1 1 calc R . .
C34 C 0.5410(4) 0.2723(5) 1.0045(3) 0.0403(12) Uani 1 1 d . . .
H34A H 0.4967 0.2474 1.0506 0.048 Uiso 1 1 calc R . .
C35 C 0.6522(4) 0.1900(5) 0.9842(2) 0.0378(11) Uani 1 1 d . . .
C36 C 0.7128(4) 0.2304(4) 0.9143(2) 0.0312(9) Uani 1 1 d . . .
C37 C 0.7093(6) 0.0640(6) 1.0353(3) 0.0641(13) Uani 1 1 d U . .
C38 C 0.7120(9) -0.0385(6) 0.9995(4) 0.0904(19) Uani 1 1 d U . .
H38A H 0.7635 -0.0291 0.9524 0.136 Uiso 1 1 calc R . .
H38B H 0.6241 -0.0337 0.9906 0.136 Uiso 1 1 calc R . .
H38C H 0.7499 -0.1183 1.0325 0.136 Uiso 1 1 calc R . .
C39 C 0.8437(7) 0.0587(7) 1.0536(3) 0.0867(18) Uani 1 1 d U . .
H39A H 0.8982 0.0712 1.0079 0.130 Uiso 1 1 calc R . .
H39B H 0.8815 -0.0216 1.0862 0.130 Uiso 1 1 calc R . .
H39C H 0.8370 0.1230 1.0785 0.130 Uiso 1 1 calc R . .
C40 C 0.6287(7) 0.0419(7) 1.1094(3) 0.0767(18) Uani 1 1 d U . .
H40A H 0.6256 0.1045 1.1349 0.115 Uiso 1 1 calc R . .
H40B H 0.6680 -0.0394 1.1404 0.115 Uiso 1 1 calc R . .
H40C H 0.5412 0.0465 1.0998 0.115 Uiso 1 1 calc R . .
O1S O 0.4304(4) 0.6470(5) 0.7293(2) 0.0765(13) Uani 1 1 d U . .
H1S H 0.4358 0.5781 0.7228 0.115 Uiso 1 1 calc R . .
C1S C 0.3060(7) 0.6993(9) 0.7518(5) 0.105(2) Uani 1 1 d U . .
H1S1 H 0.2879 0.6571 0.8031 0.157 Uiso 1 1 calc R . .
H1S2 H 0.2467 0.6921 0.7200 0.157 Uiso 1 1 calc R . .
H1S3 H 0.2949 0.7861 0.7485 0.157 Uiso 1 1 calc R . .
O2S O 0.9169(3) 0.1541(3) 0.75214(16) 0.0349(7) Uani 1 1 d . . .
H2S H 0.8964 0.1964 0.7096 0.052 Uiso 1 1 calc R . .
C2S C 1.0534(5) 0.1130(5) 0.7534(3) 0.0506(13) Uani 1 1 d . . .
H2S1 H 1.0885 0.1839 0.7409 0.076 Uiso 1 1 calc R . .
H2S2 H 1.0882 0.0640 0.7173 0.076 Uiso 1 1 calc R . .
H2S3 H 1.0773 0.0627 0.8029 0.076 Uiso 1 1 calc R . .
O3S O 0.4142(4) 0.4155(5) 0.7374(2) 0.0836(13) Uani 1 1 d U . .
H3S H 0.4499 0.4244 0.6946 0.125 Uiso 1 1 calc R . .
C3S C 0.4640(9) 0.2668(9) 0.7850(5) 0.109(2) Uani 1 1 d U . .
H3S1 H 0.5561 0.2345 0.7735 0.163 Uiso 1 1 calc R . .
H3S2 H 0.4164 0.2190 0.7708 0.163 Uiso 1 1 calc R . .
H3S3 H 0.4483 0.2609 0.8381 0.163 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.989(3) 2_666 ?
Cu1 N1 1.989(3) . ?
Cu1 Cl1 2.3027(9) . ?
Cu1 Cl1 2.3027(9) 2_666 ?
Cu2 N4 2.005(3) . ?
Cu2 N2 2.041(3) . ?
Cu2 Cl3 2.2593(10) . ?
Cu2 Cl2 2.2872(10) . ?
Cu2 Cl1 2.5911(10) 2_666 ?
Cl1 Cu2 2.5911(10) 2_666 ?
O1 C16 1.357(4) . ?
O1 H1 0.8400 . ?
O2 C36 1.362(5) . ?
O2 H2 0.8400 . ?
N1 C10 1.321(5) . ?
N1 N2 1.378(4) . ?
N2 C1 1.307(5) . ?
N3 C10 1.377(5) . ?
N3 C1 1.384(5) . ?
N3 C2 1.419(5) . ?
N4 C30 1.323(5) . ?
N4 N5 1.371(4) . ?
N5 C21 1.313(5) . ?
N6 C30 1.371(5) . ?
N6 C21 1.388(5) . ?
N6 C22 1.421(5) . ?
C1 C11 1.472(5) . ?
C2 C3 1.389(5) . ?
C2 C7 1.415(5) . ?
C3 C4 1.377(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.376(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.397(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.444(5) . ?
C8 C9 1.340(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.431(5) . ?
C9 H9A 0.9500 . ?
C11 C16 1.399(5) . ?
C11 C12 1.402(5) . ?
C12 C13 1.374(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.392(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.388(6) . ?
C14 H14A 0.9500 . ?
C15 C16 1.416(5) . ?
C15 C17 1.538(5) . ?
C17 C19 1.530(6) . ?
C17 C18 1.540(6) . ?
C17 C20 1.546(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C31 1.470(6) . ?
C22 C23 1.396(6) . ?
C22 C27 1.407(6) . ?
C23 C24 1.388(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.389(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.372(6) . ?
C25 H25A 0.9500 . ?
C26 C27 1.416(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.438(6) . ?
C28 C29 1.350(5) . ?
C28 H28A 0.9500 . ?
C29 C30 1.417(5) . ?
C29 H29A 0.9500 . ?
C31 C36 1.386(6) . ?
C31 C32 1.398(6) . ?
C32 C33 1.383(7) . ?
C32 H32A 0.9500 . ?
C33 C34 1.378(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.392(7) . ?
C34 H34A 0.9500 . ?
C35 C36 1.413(6) . ?
C35 C37 1.533(8) . ?
C37 C39 1.534(10) . ?
C37 C38 1.537(9) . ?
C37 C40 1.544(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O1S C1S 1.376(9) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.425(6) . ?
O2S H2S 0.8400 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
O3S C3S 1.696(11) . ?
O3S H3S 0.8400 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 180.00(13) 2_666 . ?
N1 Cu1 Cl1 89.37(9) 2_666 . ?
N1 Cu1 Cl1 90.63(9) . . ?
N1 Cu1 Cl1 90.63(9) 2_666 2_666 ?
N1 Cu1 Cl1 89.37(9) . 2_666 ?
Cl1 Cu1 Cl1 180.00(3) . 2_666 ?
N4 Cu2 N2 88.91(12) . . ?
N4 Cu2 Cl3 90.36(9) . . ?
N2 Cu2 Cl3 176.70(9) . . ?
N4 Cu2 Cl2 169.73(10) . . ?
N2 Cu2 Cl2 86.74(9) . . ?
Cl3 Cu2 Cl2 93.46(4) . . ?
N4 Cu2 Cl1 97.52(9) . 2_666 ?
N2 Cu2 Cl1 85.80(9) . 2_666 ?
Cl3 Cu2 Cl1 97.48(4) . 2_666 ?
Cl2 Cu2 Cl1 91.44(3) . 2_666 ?
Cu1 Cl1 Cu2 84.33(3) . 2_666 ?
C16 O1 H1 109.5 . . ?
C36 O2 H2 109.5 . . ?
C10 N1 N2 107.2(3) . . ?
C10 N1 Cu1 133.8(2) . . ?
N2 N1 Cu1 118.3(2) . . ?
C1 N2 N1 109.3(3) . . ?
C1 N2 Cu2 132.6(2) . . ?
N1 N2 Cu2 118.1(2) . . ?
C10 N3 C1 105.7(3) . . ?
C10 N3 C2 121.9(3) . . ?
C1 N3 C2 132.4(3) . . ?
C30 N4 N5 108.7(3) . . ?
C30 N4 Cu2 131.3(3) . . ?
N5 N4 Cu2 119.3(2) . . ?
C21 N5 N4 107.6(3) . . ?
C30 N6 C21 105.2(3) . . ?
C30 N6 C22 121.9(3) . . ?
C21 N6 C22 132.9(3) . . ?
N2 C1 N3 108.5(3) . . ?
N2 C1 C11 123.4(3) . . ?
N3 C1 C11 128.0(3) . . ?
C3 C2 C7 120.8(3) . . ?
C3 C2 N3 123.2(3) . . ?
C7 C2 N3 116.0(3) . . ?
C4 C3 C2 119.4(4) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 120.9(4) . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 H4A 119.5 . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 H6A 119.4 . . ?
C7 C6 H6A 119.4 . . ?
C6 C7 C2 117.9(4) . . ?
C6 C7 C8 121.5(3) . . ?
C2 C7 C8 120.6(3) . . ?
C9 C8 C7 122.0(3) . . ?
C9 C8 H8A 119.0 . . ?
C7 C8 H8A 119.0 . . ?
C8 C9 C10 117.8(4) . . ?
C8 C9 H9A 121.1 . . ?
C10 C9 H9A 121.1 . . ?
N1 C10 N3 109.3(3) . . ?
N1 C10 C9 129.3(3) . . ?
N3 C10 C9 121.4(3) . . ?
C16 C11 C12 120.9(3) . . ?
C16 C11 C1 121.7(3) . . ?
C12 C11 C1 117.4(3) . . ?
C13 C12 C11 119.4(3) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C12 C13 C14 119.4(4) . . ?
C12 C13 H13A 120.3 . . ?
C14 C13 H13A 120.3 . . ?
C15 C14 C13 123.2(3) . . ?
C15 C14 H14A 118.4 . . ?
C13 C14 H14A 118.4 . . ?
C14 C15 C16 117.0(3) . . ?
C14 C15 C17 122.0(3) . . ?
C16 C15 C17 120.9(3) . . ?
O1 C16 C11 121.4(3) . . ?
O1 C16 C15 118.6(3) . . ?
C11 C16 C15 119.9(3) . . ?
C19 C17 C15 112.0(3) . . ?
C19 C17 C18 107.1(4) . . ?
C15 C17 C18 111.4(3) . . ?
C19 C17 C20 110.6(4) . . ?
C15 C17 C20 108.3(3) . . ?
C18 C17 C20 107.3(4) . . ?
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 . . ?
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 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 N6 109.5(3) . . ?
N5 C21 C31 123.4(3) . . ?
N6 C21 C31 126.9(3) . . ?
C23 C22 C27 121.3(4) . . ?
C23 C22 N6 122.6(4) . . ?
C27 C22 N6 116.1(3) . . ?
C24 C23 C22 118.9(4) . . ?
C24 C23 H23A 120.5 . . ?
C22 C23 H23A 120.5 . . ?
C23 C24 C25 120.6(4) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C26 C25 C24 120.8(4) . . ?
C26 C25 H25A 119.6 . . ?
C24 C25 H25A 119.6 . . ?
C25 C26 C27 120.4(4) . . ?
C25 C26 H26A 119.8 . . ?
C27 C26 H26A 119.8 . . ?
C22 C27 C26 118.0(4) . . ?
C22 C27 C28 120.8(3) . . ?
C26 C27 C28 121.2(4) . . ?
C29 C28 C27 121.5(4) . . ?
C29 C28 H28A 119.2 . . ?
C27 C28 H28A 119.2 . . ?
C28 C29 C30 117.9(4) . . ?
C28 C29 H29A 121.0 . . ?
C30 C29 H29A 121.0 . . ?
N4 C30 N6 108.9(3) . . ?
N4 C30 C29 129.4(3) . . ?
N6 C30 C29 121.6(3) . . ?
C36 C31 C32 120.8(4) . . ?
C36 C31 C21 119.5(4) . . ?
C32 C31 C21 119.7(4) . . ?
C33 C32 C31 118.6(5) . . ?
C33 C32 H32A 120.7 . . ?
C31 C32 H32A 120.7 . . ?
C34 C33 C32 120.1(4) . . ?
C34 C33 H33A 119.9 . . ?
C32 C33 H33A 119.9 . . ?
C33 C34 C35 122.9(4) . . ?
C33 C34 H34A 118.5 . . ?
C35 C34 H34A 118.5 . . ?
C34 C35 C36 116.3(4) . . ?
C34 C35 C37 122.4(4) . . ?
C36 C35 C37 121.3(4) . . ?
O2 C36 C31 120.9(4) . . ?
O2 C36 C35 118.1(4) . . ?
C31 C36 C35 120.9(4) . . ?
C35 C37 C39 108.6(5) . . ?
C35 C37 C38 110.6(5) . . ?
C39 C37 C38 112.2(6) . . ?
C35 C37 C40 111.9(5) . . ?
C39 C37 C40 107.1(5) . . ?
C38 C37 C40 106.5(6) . . ?
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 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C3S O3S H3S 109.5 . . ?
O3S C3S H3S1 109.5 . . ?
O3S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
O3S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.080


_database_code_depnum_ccdc_archive 'CCDC 964839'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pgd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H20 Cu N4 O4'
_chemical_formula_sum            'C20 H20 Cu N4 O4'
_chemical_formula_weight         443.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cu Cu 0.1330 1.4803
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   17.2957(12)
_cell_length_b                   6.6675(5)
_cell_length_c                   18.3318(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.727(5)
_cell_angle_gamma                90.00
_cell_volume                     1835.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2788
_cell_measurement_theta_min      3.64
_cell_measurement_theta_max      32.42

_exptl_crystal_description       lath
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             916
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI US'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            15267
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         32.55
_reflns_number_total             5093
_reflns_number_gt                3448
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_structure_solution    'SIR92 (Altomare 1993)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_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. All non-hydrogens were
 refined anisotropically. Hydrogens were found in a difference Fourier map,
 placed geometrically on their carrier atom and refined with a riding 
 model.
;

_vrf_PLAT112_pgd                 
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem...          Z
RESPONSE: PLATON/ADDSYM was used to pass from the original P21/n space 
group in which the structure was solved into P21/c. Indeed ADDSYM also
indicated a possible pseudo translational symmetry, but since ADDSYM_shelx
did not produce additional symmetry element, nor were we able to find a
better model, the structural model was left as is.
;

_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)+(0.0573P)²+0.2509P] 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         5093
_refine_ls_number_parameters     265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1199
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.593573(18) 0.24009(4) 0.357932(18) 0.01688(10) Uani 1 1 d . . .
O1 O 0.71482(11) 0.2455(2) 0.44064(11) 0.0196(3) Uani 1 1 d . . .
O2 O 0.56928(11) 0.1156(3) 0.44162(11) 0.0207(4) Uani 1 1 d . . .
O3 O 0.58898(12) 0.4067(3) 0.50056(13) 0.0303(4) Uani 1 1 d . . .
O4 O 0.59608(13) 0.1359(3) 0.56945(12) 0.0349(5) Uani 1 1 d . . .
N1 N 0.46885(13) 0.2646(3) 0.26114(13) 0.0175(4) Uani 1 1 d . . .
N2 N 0.54859(14) 0.2582(3) 0.19108(13) 0.0208(4) Uani 1 1 d . . .
H2B H 0.5527 0.2590 0.1451 0.025 Uiso 1 1 calc R . .
N3 N 0.62258(13) 0.2601(3) 0.26954(13) 0.0181(4) Uani 1 1 d . . .
N4 N 0.58569(13) 0.2232(3) 0.50580(13) 0.0213(4) Uani 1 1 d . . .
C1 C 0.38663(15) 0.2701(3) 0.25835(15) 0.0185(4) Uani 1 1 d . . .
C2 C 0.38317(17) 0.2982(4) 0.33233(16) 0.0225(5) Uani 1 1 d . . .
H2A H 0.4367 0.3154 0.3843 0.027 Uiso 1 1 calc R . .
C3 C 0.30227(17) 0.3011(4) 0.33005(18) 0.0260(6) Uani 1 1 d . . .
H3A H 0.3007 0.3188 0.3807 0.031 Uiso 1 1 calc R . .
C4 C 0.22230(17) 0.2782(4) 0.25403(19) 0.0276(6) Uani 1 1 d . . .
H4A H 0.1671 0.2780 0.2534 0.033 Uiso 1 1 calc R . .
C5 C 0.22422(16) 0.2561(4) 0.18090(18) 0.0251(5) Uani 1 1 d . . .
H5A H 0.1700 0.2431 0.1293 0.030 Uiso 1 1 calc R . .
C6 C 0.30599(16) 0.2525(3) 0.18109(16) 0.0220(5) Uani 1 1 d . . .
C7 C 0.31097(17) 0.2345(3) 0.10633(16) 0.0236(5) Uani 1 1 d . . .
H7A H 0.2577 0.2194 0.0540 0.028 Uiso 1 1 calc R . .
C8 C 0.38980(17) 0.2385(3) 0.10843(16) 0.0235(5) Uani 1 1 d . . .
H8A H 0.3928 0.2306 0.0582 0.028 Uiso 1 1 calc R . .
C9 C 0.46877(15) 0.2550(3) 0.18822(15) 0.0186(4) Uani 1 1 d . . .
C10 C 0.70070(16) 0.2661(3) 0.27572(16) 0.0198(5) Uani 1 1 d . . .
H10A H 0.7036 0.2734 0.2254 0.024 Uiso 1 1 calc R . .
C11 C 0.78259(16) 0.2623(3) 0.35376(15) 0.0192(4) Uani 1 1 d . . .
C12 C 0.86186(17) 0.2686(4) 0.34925(17) 0.0240(5) Uani 1 1 d . . .
H12A H 0.8585 0.2783 0.2961 0.029 Uiso 1 1 calc R . .
C13 C 0.94283(17) 0.2610(4) 0.42028(19) 0.0277(6) Uani 1 1 d . . .
H13A H 0.9959 0.2640 0.4169 0.033 Uiso 1 1 calc R . .
C14 C 0.94691(17) 0.2486(4) 0.49879(18) 0.0254(5) Uani 1 1 d . . .
H14A H 1.0037 0.2447 0.5481 0.030 Uiso 1 1 calc R . .
C15 C 0.87203(16) 0.2420(3) 0.50738(16) 0.0213(5) Uani 1 1 d . . .
C16 C 0.78613(15) 0.2502(3) 0.43285(16) 0.0184(4) Uani 1 1 d . . .
C17 C 0.87926(16) 0.2294(3) 0.59452(16) 0.0212(5) Uani 1 1 d . . .
C18 C 0.97638(17) 0.2241(4) 0.66588(18) 0.0297(6) Uani 1 1 d . . .
H18A H 1.0064 0.1070 0.6589 0.045 Uiso 1 1 calc R . .
H18B H 0.9780 0.2154 0.7200 0.045 Uiso 1 1 calc R . .
H18C H 1.0069 0.3466 0.6643 0.045 Uiso 1 1 calc R . .
C19 C 0.83523(17) 0.4139(4) 0.60901(17) 0.0251(5) Uani 1 1 d . . .
H19A H 0.8656 0.5357 0.6066 0.038 Uiso 1 1 calc R . .
H19B H 0.8397 0.4040 0.6643 0.038 Uiso 1 1 calc R . .
H19C H 0.7724 0.4195 0.5654 0.038 Uiso 1 1 calc R . .
C20 C 0.83366(17) 0.0381(4) 0.60109(17) 0.0265(6) Uani 1 1 d . . .
H20A H 0.8631 -0.0796 0.5939 0.040 Uiso 1 1 calc R . .
H20B H 0.7709 0.0391 0.5572 0.040 Uiso 1 1 calc R . .
H20C H 0.8379 0.0329 0.6564 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.8827(17) . ?
Cu1 N3 1.924(2) . ?
Cu1 O2 1.9644(17) . ?
Cu1 N1 2.008(2) . ?
O1 C16 1.310(3) . ?
O2 N4 1.284(3) . ?
O3 N4 1.231(3) . ?
O4 N4 1.235(3) . ?
N1 C9 1.338(3) . ?
N1 C1 1.398(3) . ?
N2 C9 1.355(3) . ?
N2 N3 1.372(3) . ?
N2 H2B 0.8800 . ?
N3 C10 1.299(3) . ?
C1 C2 1.399(3) . ?
C1 C6 1.416(3) . ?
C2 C3 1.379(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.403(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.365(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.413(3) . ?
C5 H5A 0.9500 . ?
C6 C7 1.420(4) . ?
C7 C8 1.345(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.427(3) . ?
C8 H8A 0.9500 . ?
C10 C11 1.430(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.415(3) . ?
C11 C16 1.423(3) . ?
C12 C13 1.360(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.408(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.381(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.437(3) . ?
C15 C17 1.542(4) . ?
C17 C18 1.535(3) . ?
C17 C20 1.535(3) . ?
C17 C19 1.538(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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 91.45(8) . . ?
O1 Cu1 O2 87.90(7) . . ?
N3 Cu1 O2 158.93(8) . . ?
O1 Cu1 N1 171.72(7) . . ?
N3 Cu1 N1 82.22(8) . . ?
O2 Cu1 N1 99.92(7) . . ?
C16 O1 Cu1 130.20(16) . . ?
N4 O2 Cu1 116.34(14) . . ?
C9 N1 C1 117.9(2) . . ?
C9 N1 Cu1 110.33(15) . . ?
C1 N1 Cu1 131.45(17) . . ?
C9 N2 N3 116.3(2) . . ?
C9 N2 H2B 121.8 . . ?
N3 N2 H2B 121.8 . . ?
C10 N3 N2 118.7(2) . . ?
C10 N3 Cu1 128.53(18) . . ?
N2 N3 Cu1 112.65(15) . . ?
O3 N4 O4 123.5(2) . . ?
O3 N4 O2 118.8(2) . . ?
O4 N4 O2 117.7(2) . . ?
N1 C1 C2 120.0(2) . . ?
N1 C1 C6 120.9(2) . . ?
C2 C1 C6 119.1(2) . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C5 C6 C1 119.3(2) . . ?
C5 C6 C7 122.6(2) . . ?
C1 C6 C7 118.1(2) . . ?
C8 C7 C6 121.1(2) . . ?
C8 C7 H7A 119.5 . . ?
C6 C7 H7A 119.5 . . ?
C7 C8 C9 118.2(2) . . ?
C7 C8 H8A 120.9 . . ?
C9 C8 H8A 120.9 . . ?
N1 C9 N2 117.7(2) . . ?
N1 C9 C8 123.7(2) . . ?
N2 C9 C8 118.7(2) . . ?
N3 C10 C11 123.9(2) . . ?
N3 C10 H10A 118.0 . . ?
C11 C10 H10A 118.0 . . ?
C12 C11 C16 120.5(2) . . ?
C12 C11 C10 116.7(2) . . ?
C16 C11 C10 122.8(2) . . ?
C13 C12 C11 120.7(2) . . ?
C13 C12 H12A 119.6 . . ?
C11 C12 H12A 119.6 . . ?
C12 C13 C14 119.1(2) . . ?
C12 C13 H13A 120.4 . . ?
C14 C13 H13A 120.4 . . ?
C15 C14 C13 123.0(2) . . ?
C15 C14 H14A 118.5 . . ?
C13 C14 H14A 118.5 . . ?
C14 C15 C16 118.5(2) . . ?
C14 C15 C17 121.4(2) . . ?
C16 C15 C17 120.1(2) . . ?
O1 C16 C11 123.0(2) . . ?
O1 C16 C15 118.7(2) . . ?
C11 C16 C15 118.2(2) . . ?
C18 C17 C20 107.6(2) . . ?
C18 C17 C19 107.3(2) . . ?
C20 C17 C19 109.5(2) . . ?
C18 C17 C15 112.1(2) . . ?
C20 C17 C15 110.2(2) . . ?
C19 C17 C15 110.0(2) . . ?
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 . . ?
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 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        32.55
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 964835'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_l3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C24 H30 Cl2 Cu2 N6 O11), (C H4 O)'
_chemical_formula_sum            'C25 H34 Cl2 Cu2 N6 O12'
_chemical_formula_weight         808.56

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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   11.893(9)
_cell_length_b                   21.582(9)
_cell_length_c                   12.732(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.466(9)
_cell_angle_gamma                90.00
_cell_volume                     3265(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    570
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      26.35

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5767
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Bruker Apex-II SADABS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD area-detector'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            19288
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         26.35
_reflns_number_total             6441
_reflns_number_gt                2833
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (2008)'
_computing_cell_refinement       'APEX-II (2008)'
_computing_data_reduction        'SAINT (2008)'
_computing_structure_solution    'SIR97 (Giacovazzo and co., 1999)'
_computing_structure_refinement  
'SHELXL97, G. M. Sheldrick, Acta Cryst. A, 2008,A64,112-122.'
_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.
;

_vrf_PLAT201_l3                  
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s)
RESPONSE: The tert-butyl moiety of the ligand is disordered over two 
positions with occupancy factors 0.6 and 0.4. The atoms with occupancy
factors 0.4 are the ones with isotropic thermal parameters.
;

_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)+(0.0508P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6441
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1700
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1479
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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 0.29306(6) 0.14067(4) 1.04783(6) 0.0597(3) Uani 1 1 d . . .
Cu2 Cu 0.05293(6) 0.16414(3) 0.99769(6) 0.0507(2) Uani 1 1 d . . .
O1 O 0.1838(3) 0.13065(18) 0.9318(3) 0.0509(11) Uani 1 1 d . . .
N1 N 0.4065(4) 0.0984(3) 0.9706(5) 0.0610(15) Uani 1 1 d . . .
N2 N 0.5032(5) 0.0897(3) 1.0292(5) 0.0796(18) Uani 1 1 d . . .
H2N H 0.5579 0.0680 1.0066 0.096 Uiso 1 1 calc R . .
N3 N 0.4165(4) 0.1473(2) 1.1531(5) 0.0634(15) Uani 1 1 d . . .
N4 N -0.0310(4) 0.1611(2) 0.8644(4) 0.0484(12) Uani 1 1 d . . .
N5 N -0.1370(4) 0.1850(2) 0.8709(4) 0.0569(14) Uani 1 1 d . . .
H5N H -0.1833 0.1858 0.8171 0.068 Uiso 1 1 calc R . .
N6 N -0.0841(4) 0.2065(2) 1.0422(4) 0.0512(13) Uani 1 1 d . . .
C1 C 0.1970(5) 0.1095(3) 0.8359(5) 0.0508(16) Uani 1 1 d . . .
C2 C 0.3007(6) 0.0836(3) 0.8062(5) 0.0557(17) Uani 1 1 d . . .
C3 C 0.3086(6) 0.0630(3) 0.7021(6) 0.067(2) Uani 1 1 d . . .
H3 H 0.3769 0.0462 0.6835 0.081 Uiso 1 1 calc R . .
C4 C 0.2248(6) 0.0656(3) 0.6261(5) 0.0607(18) Uani 1 1 d . A .
C5 C 0.1240(5) 0.0910(3) 0.6557(5) 0.0563(17) Uani 1 1 d . . .
H5 H 0.0646 0.0939 0.6060 0.068 Uiso 1 1 calc R . .
C6 C 0.1083(5) 0.1128(3) 0.7586(5) 0.0489(15) Uani 1 1 d . . .
C7 C 0.2425(6) 0.0422(3) 0.5130(5) 0.072(2) Uani 1 1 d . . .
C8 C 0.3352(10) 0.0817(6) 0.4668(9) 0.089(4) Uiso 0.60 1 d P A 1
H8A H 0.3118 0.1243 0.4642 0.134 Uiso 0.60 1 calc PR A 1
H8B H 0.3490 0.0676 0.3970 0.134 Uiso 0.60 1 calc PR A 1
H8C H 0.4030 0.0781 0.5101 0.134 Uiso 0.60 1 calc PR A 1
C9 C 0.2774(14) -0.0235(7) 0.5156(11) 0.109(5) Uiso 0.60 1 d P A 1
H9A H 0.2876 -0.0378 0.4452 0.163 Uiso 0.60 1 calc PR A 1
H9B H 0.2204 -0.0479 0.5470 0.163 Uiso 0.60 1 calc PR A 1
H9C H 0.3469 -0.0276 0.5562 0.163 Uiso 0.60 1 calc PR A 1
C10 C 0.1377(12) 0.0497(7) 0.4403(11) 0.104(5) Uiso 0.60 1 d P A 1
H10A H 0.1149 0.0923 0.4391 0.157 Uiso 0.60 1 calc PR A 1
H10B H 0.0780 0.0246 0.4656 0.157 Uiso 0.60 1 calc PR A 1
H10C H 0.1545 0.0368 0.3705 0.157 Uiso 0.60 1 calc PR A 1
C8' C 0.1831(19) -0.0202(10) 0.4971(16) 0.099(7) Uiso 0.40 1 d P A 2
H8'1 H 0.2126 -0.0493 0.5482 0.148 Uiso 0.40 1 calc PR A 2
H8'2 H 0.1957 -0.0354 0.4277 0.148 Uiso 0.40 1 calc PR A 2
H8'3 H 0.1038 -0.0150 0.5054 0.148 Uiso 0.40 1 calc PR A 2
C9' C 0.199(2) 0.0878(13) 0.4304(18) 0.128(9) Uiso 0.40 1 d P A 2
H9'1 H 0.2355 0.1271 0.4418 0.192 Uiso 0.40 1 calc PR A 2
H9'2 H 0.1194 0.0926 0.4353 0.192 Uiso 0.40 1 calc PR A 2
H9'3 H 0.2155 0.0726 0.3619 0.192 Uiso 0.40 1 calc PR A 2
C10' C 0.360(2) 0.0183(13) 0.4968(18) 0.128(8) Uiso 0.40 1 d P A 2
H10D H 0.3818 -0.0093 0.5531 0.192 Uiso 0.40 1 calc PR A 2
H10E H 0.4114 0.0525 0.4958 0.192 Uiso 0.40 1 calc PR A 2
H10F H 0.3609 -0.0035 0.4311 0.192 Uiso 0.40 1 calc PR A 2
C11 C 0.3970(6) 0.0782(3) 0.8753(6) 0.0658(19) Uani 1 1 d . . .
H11 H 0.4593 0.0582 0.8494 0.079 Uiso 1 1 calc R . .
C12 C 0.5093(6) 0.1173(3) 1.1268(6) 0.0622(18) Uani 1 1 d . . .
C13 C 0.6078(6) 0.1147(4) 1.1879(7) 0.084(2) Uani 1 1 d . . .
H13 H 0.6700 0.0931 1.1655 0.101 Uiso 1 1 calc R . .
C14 C 0.6111(7) 0.1445(4) 1.2810(7) 0.087(2) Uani 1 1 d . . .
H14 H 0.6764 0.1439 1.3238 0.104 Uiso 1 1 calc R . .
C15 C 0.5189(7) 0.1754(4) 1.3123(6) 0.085(2) Uani 1 1 d . . .
H15 H 0.5201 0.1958 1.3767 0.102 Uiso 1 1 calc R . .
C16 C 0.4226(6) 0.1760(3) 1.2463(6) 0.074(2) Uani 1 1 d . . .
H16 H 0.3596 0.1972 1.2680 0.089 Uiso 1 1 calc R . .
C17 C -0.0013(5) 0.1392(3) 0.7752(5) 0.0531(16) Uani 1 1 d . . .
H17 H -0.0533 0.1405 0.7186 0.064 Uiso 1 1 calc R . .
C18 C -0.1663(6) 0.2074(3) 0.9659(5) 0.0538(17) Uani 1 1 d . . .
C19 C -0.2724(5) 0.2313(3) 0.9827(5) 0.0644(19) Uani 1 1 d . . .
H19 H -0.3279 0.2317 0.9290 0.077 Uiso 1 1 calc R . .
C20 C -0.2932(6) 0.2543(3) 1.0792(6) 0.070(2) Uani 1 1 d . . .
H20 H -0.3641 0.2698 1.0925 0.085 Uiso 1 1 calc R . .
C21 C -0.2090(6) 0.2546(3) 1.1580(6) 0.074(2) Uani 1 1 d . . .
H21 H -0.2219 0.2715 1.2236 0.088 Uiso 1 1 calc R . .
C22 C -0.1083(6) 0.2301(3) 1.1375(5) 0.0623(18) Uani 1 1 d . . .
H22 H -0.0526 0.2292 1.1911 0.075 Uiso 1 1 calc R . .
Cl1 Cl 0.38718(18) 0.28599(10) 0.95371(16) 0.0767(6) Uani 1 1 d . . .
O2 O 0.2800(6) 0.2645(4) 0.9573(5) 0.175(3) Uani 1 1 d . . .
O3 O 0.3876(6) 0.3357(3) 0.8869(6) 0.142(2) Uani 1 1 d . . .
O4 O 0.4525(7) 0.2404(4) 0.9061(6) 0.182(3) Uani 1 1 d . . .
O5 O 0.4319(6) 0.2989(4) 1.0542(5) 0.167(3) Uani 1 1 d . . .
Cl2 Cl 0.27135(15) -0.02249(8) 1.14996(15) 0.0667(5) Uani 1 1 d . . .
O6 O 0.2984(4) -0.0692(3) 1.0799(5) 0.138(3) Uani 1 1 d . . .
O7 O 0.2290(5) 0.0289(3) 1.0967(6) 0.160(3) Uani 1 1 d . . .
O8 O 0.3710(4) -0.0046(3) 1.2088(4) 0.1082(18) Uani 1 1 d . . .
O9 O 0.1897(4) -0.0459(3) 1.2160(4) 0.1089(19) Uani 1 1 d . . .
C1S C 0.1240(8) 0.3413(4) 1.1592(8) 0.134(4) Uani 1 1 d . . .
H1S1 H 0.0771 0.3546 1.2144 0.201 Uiso 1 1 calc R . .
H1S2 H 0.0790 0.3201 1.1061 0.201 Uiso 1 1 calc R . .
H1S3 H 0.1590 0.3767 1.1288 0.201 Uiso 1 1 calc R . .
O1S O 0.2040(5) 0.3026(3) 1.1989(4) 0.112(2) Uani 1 1 d . . .
H1S H 0.2136 0.2744 1.1572 0.168 Uiso 1 1 calc R . .
C2S C -0.0745(8) 0.0505(4) 1.1377(7) 0.123(3) Uani 1 1 d . . .
H2S1 H -0.0834 0.0862 1.1815 0.185 Uiso 1 1 calc R . .
H2S2 H -0.0393 0.0178 1.1784 0.185 Uiso 1 1 calc R . .
H2S3 H -0.1470 0.0369 1.1107 0.185 Uiso 1 1 calc R . .
O2S O -0.0074(4) 0.0657(2) 1.0543(4) 0.0901(16) Uani 1 1 d . . .
H2S H 0.0566 0.0526 1.0663 0.135 Uiso 1 1 calc R . .
C3S C 0.1418(9) 0.1558(5) 1.2122(10) 0.167(5) Uani 1 1 d . . .
H3S1 H 0.1296 0.1916 1.2551 0.250 Uiso 1 1 calc R . .
H3S2 H 0.2057 0.1332 1.2404 0.250 Uiso 1 1 calc R . .
H3S3 H 0.0763 0.1298 1.2116 0.250 Uiso 1 1 calc R . .
O3S O 0.1617(3) 0.17445(19) 1.1108(3) 0.0544(12) Uani 1 1 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 O3S 1.930(4) . ?
Cu1 N1 1.932(5) . ?
Cu1 O1 1.937(4) . ?
Cu1 N3 1.949(5) . ?
Cu1 Cu2 2.943(2) . ?
Cu2 O3S 1.907(4) . ?
Cu2 N4 1.933(5) . ?
Cu2 O1 1.939(4) . ?
Cu2 N6 1.973(5) . ?
O1 C1 1.319(6) . ?
N1 C11 1.289(7) . ?
N1 N2 1.357(7) . ?
N2 C12 1.378(8) . ?
N2 H2N 0.8600 . ?
N3 C12 1.335(8) . ?
N3 C16 1.338(8) . ?
N4 C17 1.293(7) . ?
N4 N5 1.366(6) . ?
N5 C18 1.362(7) . ?
N5 H5N 0.8600 . ?
N6 C18 1.348(7) . ?
N6 C22 1.358(7) . ?
C1 C6 1.413(8) . ?
C1 C2 1.420(8) . ?
C2 C3 1.405(8) . ?
C2 C11 1.419(9) . ?
C3 C4 1.359(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(8) . ?
C4 C7 1.549(9) . ?
C5 C6 1.412(7) . ?
C5 H5 0.9300 . ?
C6 C17 1.447(8) . ?
C7 C9 1.478(15) . ?
C7 C9' 1.51(2) . ?
C7 C10' 1.51(2) . ?
C7 C8' 1.53(2) . ?
C7 C8 1.531(13) . ?
C7 C10 1.529(15) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C8' H8'1 0.9600 . ?
C8' H8'2 0.9600 . ?
C8' H8'3 0.9600 . ?
C9' H9'1 0.9600 . ?
C9' H9'2 0.9600 . ?
C9' H9'3 0.9600 . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?
C11 H11 0.9300 . ?
C12 C13 1.379(9) . ?
C13 C14 1.348(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.357(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.391(9) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.389(8) . ?
C19 C20 1.357(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.386(9) . ?
C20 H20 0.9300 . ?
C21 C22 1.346(8) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
Cl1 O2 1.358(6) . ?
Cl1 O3 1.368(6) . ?
Cl1 O5 1.393(6) . ?
Cl1 O4 1.407(7) . ?
Cl2 O7 1.384(6) . ?
Cl2 O6 1.392(5) . ?
Cl2 O9 1.406(5) . ?
Cl2 O8 1.428(5) . ?
C1S O1S 1.346(9) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
O1S H1S 0.8200 . ?
C2S O2S 1.395(8) . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?
O2S H2S 0.8200 . ?
C3S O3S 1.382(12) . ?
C3S H3S1 0.9600 . ?
C3S H3S2 0.9600 . ?
C3S H3S3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3S Cu1 N1 170.2(2) . . ?
O3S Cu1 O1 80.24(17) . . ?
N1 Cu1 O1 91.1(2) . . ?
O3S Cu1 N3 106.6(2) . . ?
N1 Cu1 N3 82.1(3) . . ?
O1 Cu1 N3 173.1(2) . . ?
O3S Cu1 Cu2 39.62(13) . . ?
N1 Cu1 Cu2 131.52(19) . . ?
O1 Cu1 Cu2 40.63(11) . . ?
N3 Cu1 Cu2 146.22(17) . . ?
O3S Cu2 N4 167.19(18) . . ?
O3S Cu2 O1 80.75(17) . . ?
N4 Cu2 O1 90.10(19) . . ?
O3S Cu2 N6 105.7(2) . . ?
N4 Cu2 N6 82.3(2) . . ?
O1 Cu2 N6 170.11(19) . . ?
O3S Cu2 Cu1 40.18(12) . . ?
N4 Cu2 Cu1 130.14(15) . . ?
O1 Cu2 Cu1 40.57(11) . . ?
N6 Cu2 Cu1 145.41(16) . . ?
C1 O1 Cu1 130.0(4) . . ?
C1 O1 Cu2 131.2(4) . . ?
Cu1 O1 Cu2 98.80(17) . . ?
C11 N1 N2 120.5(6) . . ?
C11 N1 Cu1 127.1(5) . . ?
N2 N1 Cu1 112.3(4) . . ?
N1 N2 C12 116.5(6) . . ?
N1 N2 H2N 121.8 . . ?
C12 N2 H2N 121.8 . . ?
C12 N3 C16 115.6(6) . . ?
C12 N3 Cu1 113.5(5) . . ?
C16 N3 Cu1 130.9(5) . . ?
C17 N4 N5 118.6(5) . . ?
C17 N4 Cu2 129.2(4) . . ?
N5 N4 Cu2 112.2(4) . . ?
C18 N5 N4 117.3(5) . . ?
C18 N5 H5N 121.3 . . ?
N4 N5 H5N 121.3 . . ?
C18 N6 C22 117.6(5) . . ?
C18 N6 Cu2 112.4(4) . . ?
C22 N6 Cu2 129.7(5) . . ?
O1 C1 C6 120.8(5) . . ?
O1 C1 C2 121.4(6) . . ?
C6 C1 C2 117.7(6) . . ?
C3 C2 C1 118.0(6) . . ?
C3 C2 C11 118.3(6) . . ?
C1 C2 C11 123.7(6) . . ?
C4 C3 C2 125.6(6) . . ?
C4 C3 H3 117.2 . . ?
C2 C3 H3 117.2 . . ?
C3 C4 C5 116.0(6) . . ?
C3 C4 C7 121.6(6) . . ?
C5 C4 C7 122.4(7) . . ?
C4 C5 C6 122.3(6) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 120.3(6) . . ?
C5 C6 C17 115.0(6) . . ?
C1 C6 C17 124.6(5) . . ?
C9 C7 C9' 136.5(12) . . ?
C9 C7 C10' 54.2(10) . . ?
C9' C7 C10' 114.5(13) . . ?
C9 C7 C8' 44.4(8) . . ?
C9' C7 C8' 109.8(14) . . ?
C10' C7 C8' 96.0(13) . . ?
C9 C7 C8 109.7(9) . . ?
C9' C7 C8 66.4(11) . . ?
C10' C7 C8 56.9(10) . . ?
C8' C7 C8 140.8(10) . . ?
C9 C7 C10 109.6(9) . . ?
C9' C7 C10 42.9(10) . . ?
C10' C7 C10 133.4(11) . . ?
C8' C7 C10 69.7(10) . . ?
C8 C7 C10 106.9(9) . . ?
C9 C7 C4 109.9(8) . . ?
C9' C7 C4 112.2(11) . . ?
C10' C7 C4 113.7(10) . . ?
C8' C7 C4 109.2(9) . . ?
C8 C7 C4 107.8(7) . . ?
C10 C7 C4 112.9(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8' H8'1 109.5 . . ?
C7 C8' H8'2 109.5 . . ?
H8'1 C8' H8'2 109.5 . . ?
C7 C8' H8'3 109.5 . . ?
H8'1 C8' H8'3 109.5 . . ?
H8'2 C8' H8'3 109.5 . . ?
C7 C9' H9'1 109.5 . . ?
C7 C9' H9'2 109.5 . . ?
H9'1 C9' H9'2 109.5 . . ?
C7 C9' H9'3 109.5 . . ?
H9'1 C9' H9'3 109.5 . . ?
H9'2 C9' H9'3 109.5 . . ?
C7 C10' H10D 109.5 . . ?
C7 C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
C7 C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
N1 C11 C2 126.3(6) . . ?
N1 C11 H11 116.9 . . ?
C2 C11 H11 116.9 . . ?
N3 C12 C13 124.8(7) . . ?
N3 C12 N2 115.1(6) . . ?
C13 C12 N2 120.1(7) . . ?
C14 C13 C12 117.9(8) . . ?
C14 C13 H13 121.0 . . ?
C12 C13 H13 121.0 . . ?
C13 C14 C15 119.9(7) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 118.8(7) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
N3 C16 C15 122.9(7) . . ?
N3 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
N4 C17 C6 123.7(6) . . ?
N4 C17 H17 118.1 . . ?
C6 C17 H17 118.1 . . ?
N6 C18 N5 115.5(6) . . ?
N6 C18 C19 122.0(6) . . ?
N5 C18 C19 122.5(7) . . ?
C20 C19 C18 118.5(7) . . ?
C20 C19 H19 120.8 . . ?
C18 C19 H19 120.8 . . ?
C19 C20 C21 120.2(7) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C22 C21 C20 118.6(7) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C21 C22 N6 123.0(6) . . ?
C21 C22 H22 118.5 . . ?
N6 C22 H22 118.5 . . ?
O2 Cl1 O3 108.4(5) . . ?
O2 Cl1 O5 111.1(4) . . ?
O3 Cl1 O5 113.7(5) . . ?
O2 Cl1 O4 108.2(5) . . ?
O3 Cl1 O4 105.3(5) . . ?
O5 Cl1 O4 109.9(4) . . ?
O7 Cl2 O6 110.8(5) . . ?
O7 Cl2 O9 109.6(4) . . ?
O6 Cl2 O9 107.8(4) . . ?
O7 Cl2 O8 108.4(4) . . ?
O6 Cl2 O8 108.8(3) . . ?
O9 Cl2 O8 111.3(4) . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S O1S H1S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O3S C3S H3S1 109.5 . . ?
O3S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
O3S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
C3S O3S Cu2 122.3(5) . . ?
C3S O3S Cu1 116.9(5) . . ?
Cu2 O3S Cu1 100.20(19) . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.082
_database_code_depnum_ccdc_archive 'CCDC 964836'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pgc

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H32 Cl Cu2 N6 O7, Cl O4'
_chemical_formula_sum            'C31 H32 Cl2 Cu2 N6 O11'
_chemical_formula_weight         862.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cu Cu 0.1330 1.4803
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_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                   7.629(3)
_cell_length_b                   13.448(4)
_cell_length_c                   17.723(5)
_cell_angle_alpha                110.693(4)
_cell_angle_beta                 97.801(4)
_cell_angle_gamma                94.246(4)
_cell_volume                     1670.6(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4857
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      28.95

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI US'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            13570
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         28.96
_reflns_number_total             6721
_reflns_number_gt                5309
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_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. All non-hydrogens were 
 refined anistropically. Hydrogens were found in difference Fourier maps,
 placed geometrically on their carrier atom and refined with a riding
 model, except those on the coordinated hydroxo and methoxo oxygens O2
 and O3, that were refined freely with their thermal parameter 1.2 times
 that of their carrier oxygen.
;

_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)+(0.1113P)²+6.3655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6721
_refine_ls_number_parameters     475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.2123
_refine_ls_wR_factor_gt          0.2024
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_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 0.73103(10) 0.39484(5) 0.88426(4) 0.0218(2) Uani 1 1 d . . .
Cu2 Cu 0.66288(10) 0.31541(5) 0.70183(4) 0.0218(2) Uani 1 1 d . . .
O1 O 0.6131(6) 0.4373(3) 0.7969(2) 0.0235(8) Uani 1 1 d . . .
O2 O 0.7915(6) 0.2872(3) 0.7913(2) 0.0232(8) Uani 1 1 d . . .
H2 H 0.899(10) 0.280(6) 0.804(4) 0.028 Uiso 1 1 d . . .
O3 O 0.9289(6) 0.4005(4) 0.6797(3) 0.0292(9) Uani 1 1 d . . .
H3 H 0.919(10) 0.456(6) 0.668(5) 0.035 Uiso 1 1 d . . .
N1 N 0.6847(7) 0.5284(4) 0.9644(3) 0.0232(10) Uani 1 1 d . . .
N2 N 0.7519(7) 0.5379(4) 1.0435(3) 0.0246(10) Uani 1 1 d . . .
H2A H 0.7424 0.5948 1.0860 0.029 Uiso 1 1 calc R . .
N3 N 0.8370(7) 0.3708(4) 0.9851(3) 0.0234(10) Uani 1 1 d . . .
N4 N 0.5304(7) 0.3734(4) 0.6283(3) 0.0233(10) Uani 1 1 d . . .
N5 N 0.5227(7) 0.3072(4) 0.5484(3) 0.0253(11) Uani 1 1 d . . .
H5B H 0.4728 0.3246 0.5078 0.030 Uiso 1 1 calc R . .
N6 N 0.6600(7) 0.1906(4) 0.5981(3) 0.0228(10) Uani 1 1 d . . .
C1 C 0.5469(8) 0.5262(4) 0.7988(3) 0.0210(11) Uani 1 1 d . . .
C2 C 0.5454(8) 0.6112(4) 0.8748(3) 0.0230(12) Uani 1 1 d . . .
C3 C 0.4836(8) 0.7080(5) 0.8755(4) 0.0251(12) Uani 1 1 d . . .
H3A H 0.4823 0.7629 0.9268 0.030 Uiso 1 1 calc R . .
C4 C 0.4253(8) 0.7263(5) 0.8054(4) 0.0259(12) Uani 1 1 d . . .
C5 C 0.4199(8) 0.6408(5) 0.7310(4) 0.0267(12) Uani 1 1 d . . .
H5A H 0.3751 0.6500 0.6816 0.032 Uiso 1 1 calc R . .
C6 C 0.4776(8) 0.5423(4) 0.7261(4) 0.0230(12) Uani 1 1 d . . .
C7 C 0.3820(8) 0.8361(5) 0.8052(4) 0.0263(13) Uani 1 1 d . . .
C8 C 0.3669(10) 0.9131(5) 0.8912(4) 0.0323(14) Uani 1 1 d . . .
H8A H 0.4776 0.9204 0.9291 0.048 Uiso 1 1 calc R . .
H8B H 0.2666 0.8845 0.9100 0.048 Uiso 1 1 calc R . .
H8C H 0.3470 0.9834 0.8894 0.048 Uiso 1 1 calc R . .
C9 C 0.5367(9) 0.8848(5) 0.7762(4) 0.0321(14) Uani 1 1 d . . .
H9A H 0.6489 0.8908 0.8127 0.048 Uiso 1 1 calc R . .
H9B H 0.5150 0.9561 0.7771 0.048 Uiso 1 1 calc R . .
H9C H 0.5447 0.8383 0.7203 0.048 Uiso 1 1 calc R . .
C10 C 0.2082(9) 0.8255(5) 0.7477(4) 0.0317(14) Uani 1 1 d . . .
H10A H 0.1097 0.7943 0.7659 0.048 Uiso 1 1 calc R . .
H10B H 0.2176 0.7790 0.6920 0.048 Uiso 1 1 calc R . .
H10C H 0.1856 0.8966 0.7482 0.048 Uiso 1 1 calc R . .
C11 C 0.6146(8) 0.6079(5) 0.9534(3) 0.0240(12) Uani 1 1 d . . .
H11A H 0.6084 0.6685 1.0007 0.029 Uiso 1 1 calc R . .
C12 C 0.8333(8) 0.4550(4) 1.0523(3) 0.0218(11) Uani 1 1 d . . .
C13 C 0.9082(8) 0.4647(5) 1.1335(3) 0.0265(13) Uani 1 1 d . . .
H13A H 0.9009 0.5266 1.1796 0.032 Uiso 1 1 calc R . .
C14 C 0.9900(8) 0.3822(5) 1.1421(4) 0.0263(12) Uani 1 1 d . . .
H14A H 1.0419 0.3863 1.1951 0.032 Uiso 1 1 calc R . .
C15 C 0.9989(8) 0.2901(5) 1.0730(4) 0.0243(12) Uani 1 1 d . . .
C16 C 1.0879(8) 0.2045(5) 1.0791(4) 0.0273(13) Uani 1 1 d . . .
H16A H 1.1413 0.2070 1.1315 0.033 Uiso 1 1 calc R . .
C17 C 1.0991(9) 0.1180(5) 1.0111(4) 0.0293(13) Uani 1 1 d . . .
H17A H 1.1643 0.0624 1.0159 0.035 Uiso 1 1 calc R . .
C18 C 1.0117(9) 0.1118(5) 0.9326(4) 0.0288(13) Uani 1 1 d . . .
H18A H 1.0155 0.0504 0.8855 0.035 Uiso 1 1 calc R . .
C19 C 0.9221(9) 0.1935(5) 0.9245(4) 0.0262(12) Uani 1 1 d . . .
H19A H 0.8622 0.1879 0.8722 0.031 Uiso 1 1 calc R . .
C20 C 0.9199(8) 0.2856(4) 0.9942(4) 0.0231(12) Uani 1 1 d . . .
C21 C 0.4714(8) 0.4645(5) 0.6440(4) 0.0255(12) Uani 1 1 d . . .
H21A H 0.4206 0.4820 0.5991 0.031 Uiso 1 1 calc R . .
C22 C 0.5945(8) 0.2139(4) 0.5335(3) 0.0206(11) Uani 1 1 d . . .
C23 C 0.5939(9) 0.1474(5) 0.4512(4) 0.0269(13) Uani 1 1 d . . .
H23A H 0.5458 0.1675 0.4072 0.032 Uiso 1 1 calc R . .
C24 C 0.6645(9) 0.0537(5) 0.4370(4) 0.0279(13) Uani 1 1 d . . .
H24A H 0.6688 0.0084 0.3825 0.033 Uiso 1 1 calc R . .
C25 C 0.7316(8) 0.0233(5) 0.5032(4) 0.0254(12) Uani 1 1 d . . .
C26 C 0.8002(8) -0.0752(5) 0.4910(4) 0.0288(13) Uani 1 1 d . . .
H26A H 0.8030 -0.1231 0.4371 0.035 Uiso 1 1 calc R . .
C27 C 0.8626(9) -0.1017(5) 0.5569(4) 0.0310(13) Uani 1 1 d . . .
H27A H 0.9103 -0.1674 0.5483 0.037 Uiso 1 1 calc R . .
C28 C 0.8562(9) -0.0327(5) 0.6367(4) 0.0308(14) Uani 1 1 d . . .
H28A H 0.8971 -0.0526 0.6817 0.037 Uiso 1 1 calc R . .
C29 C 0.7908(9) 0.0645(5) 0.6505(4) 0.0286(13) Uani 1 1 d . . .
H29A H 0.7887 0.1114 0.7048 0.034 Uiso 1 1 calc R . .
C30 C 0.7276(8) 0.0936(4) 0.5840(4) 0.0236(12) Uani 1 1 d . . .
C31 C 1.0390(10) 0.3406(6) 0.6260(5) 0.0436(17) Uani 1 1 d . . .
H31A H 1.1394 0.3891 0.6242 0.065 Uiso 1 1 calc R . .
H31B H 0.9688 0.3049 0.5709 0.065 Uiso 1 1 calc R . .
H31C H 1.0846 0.2867 0.6461 0.065 Uiso 1 1 calc R . .
Cl1 Cl 0.31940(19) 0.21267(11) 0.79354(8) 0.0244(3) Uani 1 1 d . . .
O4 O 0.3847(6) 0.2076(4) 0.7201(3) 0.0314(10) Uani 1 1 d . . .
O5 O 0.4619(6) 0.2611(4) 0.8642(3) 0.0312(10) Uani 1 1 d . . .
O6 O 0.1781(6) 0.2820(4) 0.8056(3) 0.0339(10) Uani 1 1 d . . .
O7 O 0.2523(7) 0.1085(4) 0.7881(3) 0.0377(11) Uani 1 1 d . . .
Cl2 Cl 0.1966(2) 0.39606(12) 0.41292(9) 0.0318(4) Uani 1 1 d . . .
O8 O 0.2618(7) 0.5026(4) 0.4725(3) 0.0410(12) Uani 1 1 d . . .
O9 O 0.0551(7) 0.3475(4) 0.4382(3) 0.0452(12) Uani 1 1 d . . .
O10 O 0.1339(7) 0.4043(4) 0.3344(3) 0.0381(11) Uani 1 1 d . . .
O11 O 0.3424(7) 0.3323(4) 0.4040(3) 0.0424(12) Uani 1 1 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 O2 1.908(4) . ?
Cu1 N1 1.948(5) . ?
Cu1 O1 1.963(4) . ?
Cu1 N3 2.002(5) . ?
Cu1 Cu2 2.9809(12) . ?
Cu2 O2 1.919(4) . ?
Cu2 N4 1.950(5) . ?
Cu2 O1 1.996(4) . ?
Cu2 N6 2.000(5) . ?
Cu2 O3 2.402(5) . ?
O1 C1 1.323(7) . ?
O2 H2 0.84(7) . ?
O3 C31 1.426(8) . ?
O3 H3 0.85(8) . ?
N1 C11 1.293(7) . ?
N1 N2 1.383(7) . ?
N2 C12 1.361(7) . ?
N2 H2A 0.8800 . ?
N3 C12 1.327(7) . ?
N3 C20 1.395(7) . ?
N4 C21 1.288(7) . ?
N4 N5 1.371(7) . ?
N5 C22 1.361(7) . ?
N5 H5B 0.8800 . ?
N6 C22 1.333(7) . ?
N6 C30 1.391(7) . ?
C1 C6 1.420(8) . ?
C1 C2 1.428(8) . ?
C2 C3 1.413(8) . ?
C2 C11 1.439(8) . ?
C3 C4 1.373(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.403(8) . ?
C4 C7 1.538(8) . ?
C5 C6 1.404(8) . ?
C5 H5A 0.9500 . ?
C6 C21 1.453(8) . ?
C7 C10 1.523(8) . ?
C7 C8 1.536(8) . ?
C7 C9 1.541(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9500 . ?
C12 C13 1.431(8) . ?
C13 C14 1.357(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.414(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.407(8) . ?
C15 C20 1.424(8) . ?
C16 C17 1.366(9) . ?
C16 H16A 0.9500 . ?
C17 C18 1.429(9) . ?
C17 H17A 0.9500 . ?
C18 C19 1.376(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.410(8) . ?
C19 H19A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 C23 1.416(8) . ?
C23 C24 1.361(8) . ?
C23 H23A 0.9500 . ?
C24 C25 1.417(9) . ?
C24 H24A 0.9500 . ?
C25 C30 1.416(8) . ?
C25 C26 1.416(8) . ?
C26 C27 1.373(9) . ?
C26 H26A 0.9500 . ?
C27 C28 1.400(9) . ?
C27 H27A 0.9500 . ?
C28 C29 1.386(8) . ?
C28 H28A 0.9500 . ?
C29 C30 1.406(8) . ?
C29 H29A 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Cl1 O7 1.421(5) . ?
Cl1 O4 1.437(4) . ?
Cl1 O5 1.457(5) . ?
Cl1 O6 1.465(5) . ?
Cl2 O9 1.423(6) . ?
Cl2 O11 1.446(5) . ?
Cl2 O8 1.448(5) . ?
Cl2 O10 1.454(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N1 165.43(19) . . ?
O2 Cu1 O1 80.37(17) . . ?
N1 Cu1 O1 88.88(18) . . ?
O2 Cu1 N3 108.45(19) . . ?
N1 Cu1 N3 82.4(2) . . ?
O1 Cu1 N3 171.19(18) . . ?
O2 Cu1 Cu2 38.98(12) . . ?
N1 Cu1 Cu2 130.26(14) . . ?
O1 Cu1 Cu2 41.58(11) . . ?
N3 Cu1 Cu2 147.20(14) . . ?
O2 Cu2 N4 167.99(19) . . ?
O2 Cu2 O1 79.28(17) . . ?
N4 Cu2 O1 89.05(18) . . ?
O2 Cu2 N6 108.78(18) . . ?
N4 Cu2 N6 83.2(2) . . ?
O1 Cu2 N6 168.39(19) . . ?
O2 Cu2 O3 92.12(17) . . ?
N4 Cu2 O3 86.81(19) . . ?
O1 Cu2 O3 98.50(16) . . ?
N6 Cu2 O3 89.69(18) . . ?
O2 Cu2 Cu1 38.71(12) . . ?
N4 Cu2 Cu1 129.78(14) . . ?
O1 Cu2 Cu1 40.75(11) . . ?
N6 Cu2 Cu1 145.80(14) . . ?
O3 Cu2 Cu1 99.79(11) . . ?
C1 O1 Cu1 131.8(3) . . ?
C1 O1 Cu2 129.7(3) . . ?
Cu1 O1 Cu2 97.66(17) . . ?
Cu1 O2 Cu2 102.31(19) . . ?
Cu1 O2 H2 107(5) . . ?
Cu2 O2 H2 134(5) . . ?
C31 O3 Cu2 121.4(4) . . ?
C31 O3 H3 105(5) . . ?
Cu2 O3 H3 117(5) . . ?
C11 N1 N2 118.4(5) . . ?
C11 N1 Cu1 129.8(4) . . ?
N2 N1 Cu1 111.6(3) . . ?
C12 N2 N1 116.7(5) . . ?
C12 N2 H2A 121.6 . . ?
N1 N2 H2A 121.6 . . ?
C12 N3 C20 117.8(5) . . ?
C12 N3 Cu1 111.3(4) . . ?
C20 N3 Cu1 130.7(4) . . ?
C21 N4 N5 119.4(5) . . ?
C21 N4 Cu2 129.9(4) . . ?
N5 N4 Cu2 110.2(3) . . ?
C22 N5 N4 118.2(5) . . ?
C22 N5 H5B 120.9 . . ?
N4 N5 H5B 120.9 . . ?
C22 N6 C30 118.2(5) . . ?
C22 N6 Cu2 110.3(4) . . ?
C30 N6 Cu2 131.2(4) . . ?
O1 C1 C6 121.9(5) . . ?
O1 C1 C2 120.9(5) . . ?
C6 C1 C2 117.1(5) . . ?
C3 C2 C1 120.1(5) . . ?
C3 C2 C11 116.1(5) . . ?
C1 C2 C11 123.7(5) . . ?
C4 C3 C2 123.0(5) . . ?
C4 C3 H3A 118.5 . . ?
C2 C3 H3A 118.5 . . ?
C3 C4 C5 116.5(5) . . ?
C3 C4 C7 123.4(5) . . ?
C5 C4 C7 120.0(5) . . ?
C4 C5 C6 123.3(5) . . ?
C4 C5 H5A 118.4 . . ?
C6 C5 H5A 118.4 . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 C21 116.0(5) . . ?
C1 C6 C21 124.0(5) . . ?
C10 C7 C8 108.5(5) . . ?
C10 C7 C4 111.5(5) . . ?
C8 C7 C4 111.7(5) . . ?
C10 C7 C9 109.3(5) . . ?
C8 C7 C9 108.3(5) . . ?
C4 C7 C9 107.5(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C2 124.7(5) . . ?
N1 C11 H11A 117.7 . . ?
C2 C11 H11A 117.7 . . ?
N3 C12 N2 117.8(5) . . ?
N3 C12 C13 124.6(5) . . ?
N2 C12 C13 117.6(5) . . ?
C14 C13 C12 117.5(5) . . ?
C14 C13 H13A 121.3 . . ?
C12 C13 H13A 121.3 . . ?
C13 C14 C15 120.8(5) . . ?
C13 C14 H14A 119.6 . . ?
C15 C14 H14A 119.6 . . ?
C16 C15 C14 122.5(5) . . ?
C16 C15 C20 118.9(5) . . ?
C14 C15 C20 118.6(5) . . ?
C17 C16 C15 121.3(6) . . ?
C17 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 . . ?
C16 C17 C18 119.4(5) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C19 C18 C17 120.9(6) . . ?
C19 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C18 C19 C20 119.6(5) . . ?
C18 C19 H19A 120.2 . . ?
C20 C19 H19A 120.2 . . ?
N3 C20 C19 119.5(5) . . ?
N3 C20 C15 120.7(5) . . ?
C19 C20 C15 119.8(5) . . ?
N4 C21 C6 124.2(5) . . ?
N4 C21 H21A 117.9 . . ?
C6 C21 H21A 117.9 . . ?
N6 C22 N5 117.4(5) . . ?
N6 C22 C23 124.1(5) . . ?
N5 C22 C23 118.4(5) . . ?
C24 C23 C22 117.9(5) . . ?
C24 C23 H23A 121.0 . . ?
C22 C23 H23A 121.0 . . ?
C23 C24 C25 120.5(5) . . ?
C23 C24 H24A 119.8 . . ?
C25 C24 H24A 119.8 . . ?
C30 C25 C26 119.1(6) . . ?
C30 C25 C24 118.6(5) . . ?
C26 C25 C24 122.3(6) . . ?
C27 C26 C25 120.4(6) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C28 120.4(6) . . ?
C26 C27 H27A 119.8 . . ?
C28 C27 H27A 119.8 . . ?
C29 C28 C27 120.6(6) . . ?
C29 C28 H28A 119.7 . . ?
C27 C28 H28A 119.7 . . ?
C28 C29 C30 119.9(6) . . ?
C28 C29 H29A 120.0 . . ?
C30 C29 H29A 120.0 . . ?
N6 C30 C29 119.7(5) . . ?
N6 C30 C25 120.6(5) . . ?
C29 C30 C25 119.7(5) . . ?
O3 C31 H31A 109.5 . . ?
O3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O7 Cl1 O4 110.5(3) . . ?
O7 Cl1 O5 110.0(3) . . ?
O4 Cl1 O5 109.9(3) . . ?
O7 Cl1 O6 110.0(3) . . ?
O4 Cl1 O6 109.1(3) . . ?
O5 Cl1 O6 107.2(3) . . ?
O9 Cl2 O11 110.4(3) . . ?
O9 Cl2 O8 110.4(3) . . ?
O11 Cl2 O8 108.9(3) . . ?
O9 Cl2 O10 110.0(3) . . ?
O11 Cl2 O10 108.4(3) . . ?
O8 Cl2 O10 108.7(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O6 0.84(7) 2.12(7) 2.933(6) 160(7) 1_655
O3 H3 O10 0.85(8) 1.96(8) 2.792(6) 165(7) 2_666
N2 H2A O6 0.88 2.02 2.855(7) 157.4 2_667
N5 H5B O11 0.88 2.01 2.878(7) 168.4 .

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        28.95
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.152
_database_code_depnum_ccdc_archive 'CCDC 964837'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ll3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C88 H84 Cu8 N28 O21), 3(NO3), (C H3 O), 0.5(O2), 7(O)'
_chemical_formula_sum            'C93 H125 Cu8 N31 O43'
_chemical_formula_weight         2873.56

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'

_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                   15.8661(5)
_cell_length_b                   15.9224(5)
_cell_length_c                   26.4434(9)
_cell_angle_alpha                76.0760(10)
_cell_angle_beta                 87.3960(10)
_cell_angle_gamma                68.3660(10)
_cell_volume                     6020.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    2912
_cell_measurement_theta_min      0.79
_cell_measurement_theta_max      31.88


_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2952
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_process_details   'Bruker Apex-II SADABS'


_exptl_special_details           
; 
The calculated molar mass, density and absorption coefficient include 
eight disordered methanol molecules per cell which do not appear in 
the final files because of the  refinements
carried out with data subjected to SQUEEZE.
;

_diffrn_ambient_temperature      190(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 APEX-II CCD area-detector'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            100899
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         31.88
_reflns_number_total             38648
_reflns_number_gt                27862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (2008)'
_computing_cell_refinement       'APEX-II (2008)'
_computing_data_reduction        'SAINT (2008)'
_computing_structure_solution    'SIR97 (Giacovazzo and co., 1999)'
_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. 

In view of the presence of disordered methanol molecules which could not be 
properly
modelled, the structure was subjected to SQUEEZE (P. v.d. Sluis and
A. L. Spek, 
Acta Crystallogr., Sect A 1990, 46, 194-201). The program calculated a void
volume of 525.3   A³ and 150 electrons per unit cell, which correspond 
to eight methanol molecules per unit cell.
;

_vrf_PLAT601_ll3                 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 429 A^3^
RESPONSE: The structure contains disordered methanol molecules 
that could not be properly modeled, and that occupy the voids in the
lattice. The structure was therefore subjected to SQUEEZE. 
;

_vrf_CHEMW03_ll3                 
;
PROBLEM: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.95 <> 1.05
RESPONSE: The calculated molar mass includes 
eight disordered methanol molecules per cell which do not appear in 
the final files because of the  refinements
carried out with data subjected to SQUEEZE.
;

_vrf_PLAT306_ll3                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: All the isolated oxygen atoms are water molecules for which 
the hydrogen atoms could not be found in the difference Fourier map
;
_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)+(0.0829P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         38648
_refine_ls_number_parameters     1537
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1400
_refine_ls_wR_factor_gt          0.1316
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_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
Cu1A Cu 1.135344(19) -0.086484(19) 0.726350(10) 0.02507(6) Uani 1 1 d . . .
Cu2A Cu 1.14389(2) -0.003891(19) 0.810244(10) 0.02661(7) Uani 1 1 d . . .
Cu1B Cu 0.97695(2) -0.089522(19) 0.828197(11) 0.02704(7) Uani 1 1 d . . .
Cu2B Cu 0.920528(18) 0.093133(18) 0.754256(10) 0.02199(6) Uani 1 1 d . . .
Cu1C Cu 0.41723(2) 0.234062(19) 0.812824(10) 0.02517(6) Uani 1 1 d . . .
Cu2C Cu 0.408157(19) 0.392545(18) 0.729554(10) 0.02432(6) Uani 1 1 d . . .
Cu1D Cu 0.584740(19) 0.305774(18) 0.827657(10) 0.02345(6) Uani 1 1 d . . .
Cu2D Cu 0.626624(18) 0.185134(17) 0.754117(10) 0.02067(6) Uani 1 1 d . . .
O1A O 1.10545(11) 0.03926(11) 0.73559(6) 0.0254(3) Uani 1 1 d . . .
O2A O 1.13224(11) -0.11665(11) 0.80147(6) 0.0258(3) Uani 1 1 d . . .
N1A N 1.11542(13) -0.03675(14) 0.65119(7) 0.0274(4) Uani 1 1 d . . .
N2A N 1.11779(15) -0.10305(15) 0.62542(8) 0.0348(5) Uani 1 1 d . . .
N3A N 1.14232(13) -0.20073(14) 0.70813(8) 0.0290(4) Uani 1 1 d . . .
N4A N 1.14075(14) 0.11904(14) 0.81033(7) 0.0274(4) Uani 1 1 d . . .
N5A N 1.15073(17) 0.12841(16) 0.85958(8) 0.0387(5) Uani 1 1 d . . .
N6A N 1.17743(13) -0.02930(15) 0.88439(8) 0.0302(4) Uani 1 1 d . . .
N7A N 1.33675(14) -0.09875(14) 0.75473(9) 0.0321(4) Uani 1 1 d . . .
O3A O 1.30019(12) -0.05207(14) 0.78722(8) 0.0396(4) Uani 1 1 d . . .
O4A O 1.28960(12) -0.10984(14) 0.72183(8) 0.0398(4) Uani 1 1 d . . .
O5A O 1.42010(13) -0.13271(16) 0.75464(10) 0.0543(6) Uani 1 1 d . . .
O1B O 0.93732(11) -0.03430(11) 0.75480(6) 0.0264(3) Uani 1 1 d . . .
O2B O 0.97468(10) 0.03457(11) 0.82433(6) 0.0251(3) Uani 1 1 d . . .
N1B N 0.97458(14) -0.20703(14) 0.82138(8) 0.0306(4) Uani 1 1 d . . .
N2B N 1.00097(19) -0.27425(16) 0.86711(9) 0.0463(6) Uani 1 1 d . . .
N3B N 1.00183(14) -0.15455(15) 0.90181(8) 0.0310(4) Uani 1 1 d . . .
N4B N 0.88659(12) 0.13117(12) 0.68023(7) 0.0230(4) Uani 1 1 d . . .
N5B N 0.87048(13) 0.22384(13) 0.65953(8) 0.0277(4) Uani 1 1 d . . .
N6B N 0.90852(12) 0.22385(13) 0.74290(8) 0.0249(4) Uani 1 1 d . . .
N7B N 0.76156(15) -0.04294(16) 0.89504(9) 0.0365(5) Uani 1 1 d . . .
O3B O 0.79848(13) -0.04314(14) 0.85191(7) 0.0442(5) Uani 1 1 d . . .
O4B O 0.69097(15) 0.02450(15) 0.89889(8) 0.0523(5) Uani 1 1 d . . .
O5B O 0.79393(16) -0.10794(16) 0.93308(9) 0.0618(7) Uani 1 1 d . . .
O1E O 0.77606(11) 0.12326(12) 0.78647(6) 0.0294(3) Uani 1 1 d . . .
O1C O 0.43720(11) 0.26014(10) 0.73750(6) 0.0245(3) Uani 1 1 d . . .
O2C O 0.42506(10) 0.35509(11) 0.80445(6) 0.0247(3) Uani 1 1 d . . .
N1C N 0.41243(13) 0.41115(13) 0.65415(7) 0.0269(4) Uani 1 1 d . . .
N2C N 0.40418(15) 0.50058(14) 0.62941(8) 0.0333(4) Uani 1 1 d . . .
N3C N 0.39767(13) 0.52236(13) 0.71309(8) 0.0274(4) Uani 1 1 d . . .
N4C N 0.41571(14) 0.11398(13) 0.81019(7) 0.0263(4) Uani 1 1 d . . .
N5C N 0.41360(17) 0.05979(15) 0.85922(8) 0.0376(5) Uani 1 1 d . . .
N6C N 0.39564(14) 0.19209(14) 0.88701(7) 0.0290(4) Uani 1 1 d . . .
N7C N 0.20936(14) 0.38427(16) 0.75708(10) 0.0379(5) Uani 1 1 d . . .
O3C O 0.25093(13) 0.42027(14) 0.72284(8) 0.0446(5) Uani 1 1 d . . .
O4C O 0.25051(14) 0.31493(16) 0.79299(9) 0.0519(5) Uani 1 1 d . . .
O5C O 0.12500(14) 0.41639(16) 0.75537(11) 0.0636(7) Uani 1 1 d . . .
O1D O 0.61067(11) 0.31238(10) 0.75396(6) 0.0241(3) Uani 1 1 d . . .
O2D O 0.58437(10) 0.18527(10) 0.82445(6) 0.0225(3) Uani 1 1 d . . .
N1D N 0.58787(14) 0.42887(13) 0.81951(7) 0.0260(4) Uani 1 1 d . . .
N2D N 0.57188(17) 0.45727(15) 0.86511(8) 0.0384(5) Uani 1 1 d . . .
N3D N 0.57437(13) 0.30943(14) 0.90139(7) 0.0269(4) Uani 1 1 d . . .
N4D N 0.64647(12) 0.21019(12) 0.68003(7) 0.0223(4) Uani 1 1 d . . .
N5D N 0.65791(13) 0.13502(13) 0.65964(7) 0.0256(4) Uani 1 1 d . . .
N6D N 0.63577(12) 0.06412(12) 0.74335(7) 0.0239(4) Uani 1 1 d . . .
N7D N 0.81174(16) 0.21593(16) 0.88675(8) 0.0352(5) Uani 1 1 d . . .
O3D O 0.76243(13) 0.24324(16) 0.84553(8) 0.0465(5) Uani 1 1 d . . .
O4D O 0.79836(17) 0.26869(16) 0.91578(8) 0.0564(6) Uani 1 1 d . . .
O5D O 0.87266(17) 0.13814(16) 0.89693(8) 0.0608(7) Uani 1 1 d . . .
C1A C 1.11041(14) 0.11313(15) 0.70104(8) 0.0240(4) Uani 1 1 d . . .
C2A C 1.10200(15) 0.12163(16) 0.64666(9) 0.0261(4) Uani 1 1 d . . .
C3A C 1.09686(16) 0.20487(16) 0.61106(9) 0.0293(5) Uani 1 1 d . . .
H3A H 1.0877 0.2104 0.5750 0.035 Uiso 1 1 calc R . .
C4A C 1.10456(15) 0.27905(16) 0.62636(9) 0.0284(5) Uani 1 1 d . . .
C5A C 1.11650(16) 0.26875(16) 0.67967(9) 0.0289(5) Uani 1 1 d . . .
H5A H 1.1227 0.3183 0.6913 0.035 Uiso 1 1 calc R . .
C6A C 1.11979(15) 0.18774(16) 0.71698(9) 0.0251(4) Uani 1 1 d . . .
C7A C 1.10304(17) 0.36896(17) 0.58764(10) 0.0320(5) Uani 1 1 d . . .
C8A C 1.1957(2) 0.3782(2) 0.59172(14) 0.0579(9) Uani 1 1 d . . .
H8A1 H 1.2436 0.3245 0.5831 0.087 Uiso 1 1 calc R . .
H8A2 H 1.2072 0.3806 0.6274 0.087 Uiso 1 1 calc R . .
H8A3 H 1.1951 0.4355 0.5673 0.087 Uiso 1 1 calc R . .
C9A C 1.0316(3) 0.4538(2) 0.60059(14) 0.0612(10) Uani 1 1 d . . .
H9A1 H 1.0317 0.5099 0.5753 0.092 Uiso 1 1 calc R . .
H9A2 H 1.0450 0.4571 0.6357 0.092 Uiso 1 1 calc R . .
H9A3 H 0.9718 0.4494 0.5992 0.092 Uiso 1 1 calc R . .
C10A C 1.0853(3) 0.3685(2) 0.53185(12) 0.0565(9) Uani 1 1 d . . .
H10A H 1.1329 0.3153 0.5226 0.085 Uiso 1 1 calc R . .
H10B H 1.0854 0.4264 0.5084 0.085 Uiso 1 1 calc R . .
H10C H 1.0261 0.3636 0.5286 0.085 Uiso 1 1 calc R . .
C11A C 1.10028(16) 0.04709(17) 0.62446(9) 0.0294(5) Uani 1 1 d . . .
H11A H 1.0872 0.0610 0.5880 0.035 Uiso 1 1 calc R . .
C12A C 1.13422(16) -0.19080(17) 0.65662(10) 0.0302(5) Uani 1 1 d . . .
C13A C 1.14257(18) -0.26465(19) 0.63475(11) 0.0379(6) Uani 1 1 d . . .
H13A H 1.1393 -0.2564 0.5980 0.045 Uiso 1 1 calc R . .
C14A C 1.15578(19) -0.34991(19) 0.66806(12) 0.0432(7) Uani 1 1 d . . .
H14A H 1.1609 -0.4015 0.6545 0.052 Uiso 1 1 calc R . .
C15A C 1.1617(2) -0.36030(19) 0.72184(13) 0.0447(7) Uani 1 1 d . . .
H15A H 1.1693 -0.4184 0.7453 0.054 Uiso 1 1 calc R . .
C16A C 1.15617(18) -0.28529(17) 0.74000(11) 0.0355(5) Uani 1 1 d . . .
H16A H 1.1624 -0.2928 0.7766 0.043 Uiso 1 1 calc R . .
C17A C 1.13152(16) 0.18895(17) 0.77108(9) 0.0291(5) Uani 1 1 d . . .
H17A H 1.1324 0.2445 0.7780 0.035 Uiso 1 1 calc R . .
C18A C 1.17002(17) 0.04868(19) 0.89871(9) 0.0326(5) Uani 1 1 d . . .
C19A C 1.1820(2) 0.0485(2) 0.95127(10) 0.0430(7) Uani 1 1 d . . .
H19A H 1.1753 0.1042 0.9610 0.052 Uiso 1 1 calc R . .
C20A C 1.2036(2) -0.0340(2) 0.98771(11) 0.0479(7) Uani 1 1 d . . .
H20A H 1.2117 -0.0361 1.0234 0.057 Uiso 1 1 calc R . .
C21A C 1.2138(2) -0.1144(2) 0.97297(10) 0.0441(7) Uani 1 1 d . . .
H21A H 1.2298 -0.1721 0.9982 0.053 Uiso 1 1 calc R . .
C22A C 1.20035(17) -0.10988(19) 0.92121(10) 0.0355(5) Uani 1 1 d . . .
H22A H 1.2075 -0.1654 0.9111 0.043 Uiso 1 1 calc R . .
C1B C 0.91808(15) -0.07083(15) 0.71812(8) 0.0238(4) Uani 1 1 d . . .
C2B C 0.92556(15) -0.16432(16) 0.72964(9) 0.0262(4) Uani 1 1 d . . .
C3B C 0.90953(16) -0.20189(16) 0.68975(9) 0.0287(5) Uani 1 1 d . . .
H3B H 0.9150 -0.2652 0.6981 0.034 Uiso 1 1 calc R . .
C4B C 0.88601(15) -0.15024(16) 0.63860(9) 0.0267(4) Uani 1 1 d . . .
C5B C 0.87646(15) -0.05766(16) 0.62836(9) 0.0267(4) Uani 1 1 d . . .
H5B H 0.8592 -0.0204 0.5938 0.032 Uiso 1 1 calc R . .
C6B C 0.89118(14) -0.01605(15) 0.66688(8) 0.0223(4) Uani 1 1 d . . .
C7B C 0.86984(18) -0.19226(18) 0.59514(10) 0.0341(5) Uani 1 1 d . . .
C8B C 0.9256(2) -0.1701(3) 0.54768(12) 0.0556(9) Uani 1 1 d . . .
H8B1 H 0.9199 -0.2021 0.5214 0.083 Uiso 1 1 calc R . .
H8B2 H 0.9896 -0.1914 0.5590 0.083 Uiso 1 1 calc R . .
H8B3 H 0.9027 -0.1028 0.5326 0.083 Uiso 1 1 calc R . .
C9B C 0.9008(3) -0.2985(2) 0.61243(13) 0.0547(8) Uani 1 1 d . . .
H9B1 H 0.8646 -0.3156 0.6413 0.082 Uiso 1 1 calc R . .
H9B2 H 0.9651 -0.3250 0.6240 0.082 Uiso 1 1 calc R . .
H9B3 H 0.8925 -0.3228 0.5831 0.082 Uiso 1 1 calc R . .
C10B C 0.7690(2) -0.1512(2) 0.57905(13) 0.0532(8) Uani 1 1 d . . .
H10D H 0.7338 -0.1613 0.6098 0.080 Uiso 1 1 calc R . .
H10E H 0.7576 -0.1815 0.5534 0.080 Uiso 1 1 calc R . .
H10F H 0.7507 -0.0842 0.5636 0.080 Uiso 1 1 calc R . .
C11B C 0.95253(17) -0.22853(17) 0.78065(10) 0.0326(5) Uani 1 1 d . . .
H11B H 0.9542 -0.2900 0.7845 0.039 Uiso 1 1 calc R . .
C12B C 1.0129(2) -0.2435(2) 0.90985(10) 0.0413(6) Uani 1 1 d . . .
C13B C 1.0356(3) -0.3051(3) 0.95940(13) 0.0649(10) Uani 1 1 d . . .
H13B H 1.0452 -0.3691 0.9643 0.078 Uiso 1 1 calc R . .
C14B C 1.0434(3) -0.2693(3) 1.00054(13) 0.0702(11) Uani 1 1 d . . .
H14B H 1.0596 -0.3093 1.0345 0.084 Uiso 1 1 calc R . .
C15B C 1.0282(2) -0.1767(3) 0.99311(11) 0.0525(8) Uani 1 1 d . . .
H15B H 1.0321 -0.1516 1.0217 0.063 Uiso 1 1 calc R . .
C16B C 1.00715(18) -0.1210(2) 0.94344(10) 0.0385(6) Uani 1 1 d . . .
H16B H 0.9959 -0.0565 0.9381 0.046 Uiso 1 1 calc R . .
C17B C 0.87745(15) 0.08153(15) 0.64973(9) 0.0246(4) Uani 1 1 d . . .
H17B H 0.8607 0.1114 0.6140 0.030 Uiso 1 1 calc R . .
C18B C 0.88203(15) 0.27201(15) 0.69341(9) 0.0262(4) Uani 1 1 d . . .
C19B C 0.86614(17) 0.36674(17) 0.67699(11) 0.0346(5) Uani 1 1 d . . .
H19B H 0.8475 0.3995 0.6418 0.042 Uiso 1 1 calc R . .
C20B C 0.8780(2) 0.41152(19) 0.71270(12) 0.0424(6) Uani 1 1 d . . .
H20B H 0.8675 0.4761 0.7025 0.051 Uiso 1 1 calc R . .
C21B C 0.9057(2) 0.3616(2) 0.76449(12) 0.0419(6) Uani 1 1 d . . .
H21B H 0.9143 0.3919 0.7896 0.050 Uiso 1 1 calc R . .
C22B C 0.91989(17) 0.26974(18) 0.77794(10) 0.0316(5) Uani 1 1 d . . .
H22B H 0.9384 0.2360 0.8130 0.038 Uiso 1 1 calc R . .
C17C C 0.41773(17) 0.07962(17) 0.77077(9) 0.0289(5) Uani 1 1 d . . .
H17C H 0.4178 0.0183 0.7771 0.035 Uiso 1 1 calc R . .
C1C C 0.42629(14) 0.21709(15) 0.70169(8) 0.0221(4) Uani 1 1 d . . .
C2C C 0.42543(15) 0.25739(16) 0.64781(8) 0.0250(4) Uani 1 1 d . . .
C3C C 0.42397(15) 0.20608(16) 0.61151(9) 0.0281(5) Uani 1 1 d . . .
H3C H 0.4260 0.2329 0.5755 0.034 Uiso 1 1 calc R . .
C4C C 0.41966(16) 0.11809(17) 0.62609(9) 0.0282(5) Uani 1 1 d . . .
C5C C 0.41743(16) 0.08113(16) 0.67909(9) 0.0279(5) Uani 1 1 d . . .
H5C H 0.4140 0.0211 0.6901 0.033 Uiso 1 1 calc R . .
C6C C 0.41994(15) 0.12854(15) 0.71719(8) 0.0235(4) Uani 1 1 d . . .
C7C C 0.41379(18) 0.06342(18) 0.58638(10) 0.0354(6) Uani 1 1 d . . .
C8C C 0.3194(3) 0.0521(3) 0.59004(18) 0.0816(13) Uani 1 1 d . . .
H8C1 H 0.3140 0.0193 0.5641 0.122 Uiso 1 1 calc R . .
H8C2 H 0.2706 0.1137 0.5833 0.122 Uiso 1 1 calc R . .
H8C3 H 0.3145 0.0162 0.6250 0.122 Uiso 1 1 calc R . .
C9C C 0.4224(4) 0.1109(3) 0.53085(14) 0.0901(16) Uani 1 1 d . . .
H9C1 H 0.4820 0.1164 0.5272 0.135 Uiso 1 1 calc R . .
H9C2 H 0.3747 0.1731 0.5218 0.135 Uiso 1 1 calc R . .
H9C3 H 0.4160 0.0741 0.5074 0.135 Uiso 1 1 calc R . .
C10C C 0.4812(3) -0.0355(3) 0.60059(16) 0.0824(14) Uani 1 1 d . . .
H10G H 0.4673 -0.0717 0.5793 0.124 Uiso 1 1 calc R . .
H10H H 0.4774 -0.0631 0.6376 0.124 Uiso 1 1 calc R . .
H10I H 0.5426 -0.0359 0.5941 0.124 Uiso 1 1 calc R . .
C11C C 0.42137(16) 0.35179(16) 0.62646(9) 0.0282(5) Uani 1 1 d . . .
H11C H 0.4255 0.3712 0.5899 0.034 Uiso 1 1 calc R . .
C12C C 0.39440(16) 0.55910(16) 0.66162(10) 0.0292(5) Uani 1 1 d . . .
C13C C 0.38303(18) 0.65291(17) 0.64094(11) 0.0369(6) Uani 1 1 d . . .
H13C H 0.3793 0.6784 0.6044 0.044 Uiso 1 1 calc R . .
C14C C 0.37759(19) 0.70638(17) 0.67586(12) 0.0399(6) Uani 1 1 d . . .
H14C H 0.3701 0.7700 0.6633 0.048 Uiso 1 1 calc R . .
C15C C 0.38296(19) 0.66829(18) 0.72918(11) 0.0387(6) Uani 1 1 d . . .
H15C H 0.3801 0.7048 0.7533 0.046 Uiso 1 1 calc R . .
C16C C 0.39244(17) 0.57735(17) 0.74622(10) 0.0333(5) Uani 1 1 d . . .
H16C H 0.3955 0.5513 0.7827 0.040 Uiso 1 1 calc R . .
C18C C 0.40117(17) 0.10374(18) 0.89957(9) 0.0309(5) Uani 1 1 d . . .
C19C C 0.39533(19) 0.0558(2) 0.95051(10) 0.0385(6) Uani 1 1 d . . .
H19C H 0.4016 -0.0077 0.9583 0.046 Uiso 1 1 calc R . .
C20C C 0.3802(2) 0.1039(2) 0.98907(10) 0.0436(7) Uani 1 1 d . . .
H20C H 0.3753 0.0739 1.0242 0.052 Uiso 1 1 calc R . .
C21C C 0.3720(2) 0.1959(2) 0.97646(11) 0.0466(7) Uani 1 1 d . . .
H21C H 0.3608 0.2297 1.0027 0.056 Uiso 1 1 calc R . .
C22C C 0.38031(19) 0.2384(2) 0.92564(10) 0.0372(6) Uani 1 1 d . . .
H22C H 0.3752 0.3016 0.9173 0.045 Uiso 1 1 calc R . .
C1D C 0.62277(14) 0.38011(14) 0.71685(8) 0.0210(4) Uani 1 1 d . . .
C2D C 0.61745(15) 0.46393(15) 0.72748(8) 0.0232(4) Uani 1 1 d . . .
C3D C 0.62540(15) 0.53608(15) 0.68692(9) 0.0261(4) Uani 1 1 d . . .
H3D H 0.6220 0.5923 0.6949 0.031 Uiso 1 1 calc R . .
C4D C 0.63806(15) 0.52804(15) 0.63569(9) 0.0252(4) Uani 1 1 d . . .
C5D C 0.64605(15) 0.44404(16) 0.62598(9) 0.0255(4) Uani 1 1 d . . .
H5D H 0.6563 0.4364 0.5914 0.031 Uiso 1 1 calc R . .
C6D C 0.63964(14) 0.36904(14) 0.66514(8) 0.0217(4) Uani 1 1 d . . .
C7D C 0.64469(18) 0.60741(16) 0.59125(9) 0.0320(5) Uani 1 1 d . . .
C8D C 0.5805(2) 0.6239(2) 0.54524(12) 0.0528(8) Uani 1 1 d . . .
H8D1 H 0.5191 0.6340 0.5574 0.079 Uiso 1 1 calc R . .
H8D2 H 0.6015 0.5694 0.5303 0.079 Uiso 1 1 calc R . .
H8D3 H 0.5799 0.6789 0.5186 0.079 Uiso 1 1 calc R . .
C9D C 0.6192(2) 0.69835(19) 0.60912(12) 0.0489(7) Uani 1 1 d . . .
H9D1 H 0.6668 0.6925 0.6336 0.073 Uiso 1 1 calc R . .
H9D2 H 0.5614 0.7105 0.6264 0.073 Uiso 1 1 calc R . .
H9D3 H 0.6132 0.7500 0.5788 0.073 Uiso 1 1 calc R . .
C10D C 0.7429(2) 0.5801(2) 0.57353(13) 0.0558(9) Uani 1 1 d . . .
H10J H 0.7468 0.6285 0.5436 0.084 Uiso 1 1 calc R . .
H10K H 0.7611 0.5207 0.5635 0.084 Uiso 1 1 calc R . .
H10L H 0.7835 0.5738 0.6022 0.084 Uiso 1 1 calc R . .
C11D C 0.60197(16) 0.48417(16) 0.77853(9) 0.0270(4) Uani 1 1 d . . .
H11D H 0.6022 0.5421 0.7820 0.032 Uiso 1 1 calc R . .
C12D C 0.56776(17) 0.39180(17) 0.90874(9) 0.0306(5) Uani 1 1 d . . .
C13D C 0.5581(2) 0.4117(2) 0.95793(10) 0.0432(7) Uani 1 1 d . . .
H13D H 0.5526 0.4711 0.9620 0.052 Uiso 1 1 calc R . .
C14D C 0.5570(2) 0.3421(2) 1.00001(11) 0.0462(7) Uani 1 1 d . . .
H14D H 0.5495 0.3535 1.0339 0.055 Uiso 1 1 calc R . .
C15D C 0.5667(2) 0.2552(2) 0.99339(10) 0.0421(6) Uani 1 1 d . . .
H15D H 0.5676 0.2064 1.0226 0.051 Uiso 1 1 calc R . .
C16D C 0.57493(18) 0.24101(18) 0.94376(9) 0.0334(5) Uani 1 1 d . . .
H16D H 0.5812 0.1818 0.9390 0.040 Uiso 1 1 calc R . .
C17D C 0.64989(15) 0.28507(15) 0.64922(8) 0.0241(4) Uani 1 1 d . . .
H17D H 0.6598 0.2851 0.6135 0.029 Uiso 1 1 calc R . .
C18D C 0.65194(14) 0.05840(15) 0.69416(9) 0.0239(4) Uani 1 1 d . . .
C19D C 0.66285(17) -0.02165(17) 0.67744(10) 0.0332(5) Uani 1 1 d . . .
H19D H 0.6751 -0.0242 0.6422 0.040 Uiso 1 1 calc R . .
C20D C 0.6554(2) -0.09659(18) 0.71333(12) 0.0427(6) Uani 1 1 d . . .
H20D H 0.6617 -0.1517 0.7031 0.051 Uiso 1 1 calc R . .
C21D C 0.6385(2) -0.09130(18) 0.76519(11) 0.0415(6) Uani 1 1 d . . .
H21D H 0.6333 -0.1426 0.7905 0.050 Uiso 1 1 calc R . .
C22D C 0.62957(17) -0.01126(16) 0.77869(10) 0.0305(5) Uani 1 1 d . . .
H22D H 0.6187 -0.0078 0.8139 0.037 Uiso 1 1 calc R . .
N1 N 1.3222(2) -0.31854(17) 0.86535(10) 0.0473(6) Uani 1 1 d . . .
O1 O 1.3548(2) -0.25680(17) 0.85356(12) 0.0732(8) Uani 1 1 d . . .
O2 O 1.23986(16) -0.29951(16) 0.86077(10) 0.0594(6) Uani 1 1 d . . .
O3 O 1.37590(16) -0.40147(15) 0.88264(11) 0.0650(7) Uani 1 1 d . . .
N2 N 0.8517(2) 0.2828(2) 0.52465(10) 0.0552(7) Uani 1 1 d . . .
O4 O 0.8298(2) 0.3219(2) 0.47805(10) 0.0993(12) Uani 1 1 d . . .
O5 O 0.90940(17) 0.20080(18) 0.53813(10) 0.0654(7) Uani 1 1 d . . .
O6 O 0.8132(2) 0.3217(2) 0.55797(9) 0.0859(10) Uani 1 1 d . . .
N3 N 0.6572(2) 0.1966(2) 0.52368(10) 0.0537(7) Uani 1 1 d . . .
O7 O 0.60151(17) 0.26487(17) 0.53669(9) 0.0618(6) Uani 1 1 d . . .
O8 O 0.6986(2) 0.12520(18) 0.55743(9) 0.0794(9) Uani 1 1 d . . .
O9 O 0.6745(2) 0.1999(2) 0.47745(9) 0.1003(12) Uani 1 1 d . . .
C1S C 0.2206(3) 0.4933(3) 0.86521(16) 0.0717(11) Uani 1 1 d . . .
H1S1 H 0.2015 0.4996 0.9003 0.107 Uiso 1 1 calc R . .
H1S2 H 0.2048 0.4441 0.8567 0.107 Uiso 1 1 calc R . .
H1S3 H 0.1896 0.5524 0.8399 0.107 Uiso 1 1 calc R . .
O1S O 0.31289(18) 0.47069(16) 0.86340(10) 0.0632(7) Uani 1 1 d . . .
O1W O 0.63460(18) 0.42971(17) 0.47668(9) 0.0652(7) Uani 1 1 d . . .
O2W O 0.8668(2) 0.08223(19) 0.48087(9) 0.0738(8) Uani 1 1 d . . .
O3W O 0.54536(18) 0.64663(17) 0.84759(13) 0.0773(8) Uani 1 1 d . . .
O4W O 0.6673(3) 0.5596(3) 0.95368(16) 0.0642(11) Uani 0.60 1 d P . .
O4W' O 0.7046(5) 0.5228(5) 1.0021(3) 0.088(2) Uani 0.40 1 d P . .
O5W O 0.6169(3) 0.7381(3) 0.90349(17) 0.0810(12) Uani 0.70 1 d P . .
O5W' O 0.6672 0.7539(10) 0.8948(6) 0.113(5) Uiso 0.30 1 d P . .
O7W O 0.7673(3) 0.4597(3) 0.88640(17) 0.1245(14) Uani 1 1 d . . .
O6W O 0.4439(2) -0.12468(17) 0.87928(9) 0.0801(9) Uani 1 1 d . . .
O8W O 0.1412(7) 0.2916(7) 0.8751(3) 0.087(3) Uani 0.50 1 d P . .
O8W' O 0.0911(9) 0.3098(9) 0.8748(6) 0.146(5) Uani 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
Cu1A O2A 1.9309(16) . ?
Cu1A N1A 1.9475(19) . ?
Cu1A O1A 1.9540(15) . ?
Cu1A N3A 1.955(2) . ?
Cu1A O4A 2.3380(19) . ?
Cu1A Cu2A 2.8692(4) . ?
Cu2A O2A 1.9392(16) . ?
Cu2A N4A 1.940(2) . ?
Cu2A N6A 1.9610(19) . ?
Cu2A O1A 1.9719(15) . ?
Cu2A O3A 2.4071(18) . ?
Cu1B N1B 1.936(2) . ?
Cu1B O2B 1.9408(16) . ?
Cu1B N3B 1.953(2) . ?
Cu1B O1B 1.9538(15) . ?
Cu1B Cu2B 2.9301(4) . ?
Cu2B O2B 1.9401(15) . ?
Cu2B N4B 1.9425(18) . ?
Cu2B O1B 1.9431(15) . ?
Cu2B N6B 1.9673(19) . ?
Cu2B O1E 2.3277(16) . ?
Cu1C O2C 1.9356(15) . ?
Cu1C N4C 1.9389(19) . ?
Cu1C O1C 1.9702(15) . ?
Cu1C N6C 1.9722(19) . ?
Cu1C Cu2C 2.8851(4) . ?
Cu2C O2C 1.9266(15) . ?
Cu2C O1C 1.9443(15) . ?
Cu2C N1C 1.9458(19) . ?
Cu2C N3C 1.9518(19) . ?
Cu2C O3C 2.3748(19) . ?
Cu1D N1D 1.9386(19) . ?
Cu1D O2D 1.9431(15) . ?
Cu1D O1D 1.9591(15) . ?
Cu1D N3D 1.9623(19) . ?
Cu1D O2C 2.4195(16) . ?
Cu1D Cu2D 2.9415(4) . ?
Cu2D N4D 1.9382(18) . ?
Cu2D O1D 1.9461(15) . ?
Cu2D O2D 1.9483(15) . ?
Cu2D N6D 1.9670(18) . ?
Cu2D O1E 2.3196(16) . ?
O1A C1A 1.330(3) . ?
N1A C11A 1.290(3) . ?
N1A N2A 1.377(3) . ?
N2A C12A 1.377(3) . ?
N3A C12A 1.339(3) . ?
N3A C16A 1.350(3) . ?
N4A C17A 1.294(3) . ?
N4A N5A 1.369(3) . ?
N5A C18A 1.373(3) . ?
N6A C18A 1.347(3) . ?
N6A C22A 1.347(3) . ?
N7A O5A 1.231(3) . ?
N7A O3A 1.253(3) . ?
N7A O4A 1.256(3) . ?
O1B C1B 1.342(3) . ?
N1B C11B 1.304(3) . ?
N1B N2B 1.370(3) . ?
N2B C12B 1.381(4) . ?
N3B C12B 1.326(4) . ?
N3B C16B 1.353(3) . ?
N4B C17B 1.303(3) . ?
N4B N5B 1.374(2) . ?
N5B C18B 1.369(3) . ?
N6B C18B 1.344(3) . ?
N6B C22B 1.365(3) . ?
N7B O5B 1.225(3) . ?
N7B O4B 1.254(3) . ?
N7B O3B 1.259(3) . ?
O1C C1C 1.346(3) . ?
N1C C11C 1.294(3) . ?
N1C N2C 1.377(3) . ?
N2C C12C 1.371(3) . ?
N3C C12C 1.341(3) . ?
N3C C16C 1.360(3) . ?
N4C C17C 1.283(3) . ?
N4C N5C 1.380(3) . ?
N5C C18C 1.380(3) . ?
N6C C18C 1.336(3) . ?
N6C C22C 1.361(3) . ?
N7C O5C 1.243(3) . ?
N7C O3C 1.248(3) . ?
N7C O4C 1.252(3) . ?
O1D C1D 1.338(2) . ?
N1D C11D 1.290(3) . ?
N1D N2D 1.369(3) . ?
N2D C12D 1.374(3) . ?
N3D C12D 1.337(3) . ?
N3D C16D 1.360(3) . ?
N4D C17D 1.290(3) . ?
N4D N5D 1.378(2) . ?
N5D C18D 1.368(3) . ?
N6D C18D 1.332(3) . ?
N6D C22D 1.365(3) . ?
N7D O4D 1.226(3) . ?
N7D O5D 1.233(3) . ?
N7D O3D 1.260(3) . ?
C1A C6A 1.410(3) . ?
C1A C2A 1.419(3) . ?
C2A C3A 1.406(3) . ?
C2A C11A 1.454(3) . ?
C3A C4A 1.384(3) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.393(3) . ?
C4A C7A 1.539(3) . ?
C5A C6A 1.408(3) . ?
C5A H5A 0.9500 . ?
C6A C17A 1.457(3) . ?
C7A C9A 1.512(4) . ?
C7A C10A 1.517(4) . ?
C7A C8A 1.541(4) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C11A H11A 0.9500 . ?
C12A C13A 1.393(3) . ?
C13A C14A 1.376(4) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.395(4) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.364(4) . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
C17A H17A 0.9500 . ?
C18A C19A 1.410(3) . ?
C19A C20A 1.364(4) . ?
C19A H19A 0.9500 . ?
C20A C21A 1.378(4) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.375(4) . ?
C21A H21A 0.9500 . ?
C22A H22A 0.9500 . ?
C1B C2B 1.406(3) . ?
C1B C6B 1.410(3) . ?
C2B C3B 1.405(3) . ?
C2B C11B 1.454(3) . ?
C3B C4B 1.389(3) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.384(3) . ?
C4B C7B 1.536(3) . ?
C5B C6B 1.411(3) . ?
C5B H5B 0.9500 . ?
C6B C17B 1.445(3) . ?
C7B C10B 1.525(4) . ?
C7B C9B 1.532(4) . ?
C7B C8B 1.549(4) . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11B H11B 0.9500 . ?
C12B C13B 1.404(4) . ?
C13B C14B 1.373(5) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.369(5) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.373(4) . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
C17B H17B 0.9500 . ?
C18B C19B 1.393(3) . ?
C19B C20B 1.369(4) . ?
C19B H19B 0.9500 . ?
C20B C21B 1.405(4) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.354(4) . ?
C21B H21B 0.9500 . ?
C22B H22B 0.9500 . ?
C17C C6C 1.449(3) . ?
C17C H17C 0.9500 . ?
C1C C6C 1.410(3) . ?
C1C C2C 1.413(3) . ?
C2C C3C 1.408(3) . ?
C2C C11C 1.451(3) . ?
C3C C4C 1.387(3) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.388(3) . ?
C4C C7C 1.542(3) . ?
C5C C6C 1.406(3) . ?
C5C H5C 0.9500 . ?
C7C C9C 1.507(4) . ?
C7C C10C 1.508(4) . ?
C7C C8C 1.570(5) . ?
C8C H8C1 0.9800 . ?
C8C H8C2 0.9800 . ?
C8C H8C3 0.9800 . ?
C9C H9C1 0.9800 . ?
C9C H9C2 0.9800 . ?
C9C H9C3 0.9800 . ?
C10C H10G 0.9800 . ?
C10C H10H 0.9800 . ?
C10C H10I 0.9800 . ?
C11C H11C 0.9500 . ?
C12C C13C 1.407(3) . ?
C13C C14C 1.379(4) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.387(4) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.362(4) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C18C C19C 1.397(3) . ?
C19C C20C 1.380(4) . ?
C19C H19C 0.9500 . ?
C20C C21C 1.379(4) . ?
C20C H20C 0.9500 . ?
C21C C22C 1.376(4) . ?
C21C H21C 0.9500 . ?
C22C H22C 0.9500 . ?
C1D C2D 1.401(3) . ?
C1D C6D 1.421(3) . ?
C2D C3D 1.410(3) . ?
C2D C11D 1.452(3) . ?
C3D C4D 1.390(3) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.381(3) . ?
C4D C7D 1.537(3) . ?
C5D C6D 1.412(3) . ?
C5D H5D 0.9500 . ?
C6D C17D 1.448(3) . ?
C7D C8D 1.532(4) . ?
C7D C9D 1.537(4) . ?
C7D C10D 1.540(4) . ?
C8D H8D1 0.9800 . ?
C8D H8D2 0.9800 . ?
C8D H8D3 0.9800 . ?
C9D H9D1 0.9800 . ?
C9D H9D2 0.9800 . ?
C9D H9D3 0.9800 . ?
C10D H10J 0.9800 . ?
C10D H10K 0.9800 . ?
C10D H10L 0.9800 . ?
C11D H11D 0.9500 . ?
C12D C13D 1.400(3) . ?
C13D C14D 1.373(4) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.388(4) . ?
C14D H14D 0.9500 . ?
C15D C16D 1.377(4) . ?
C15D H15D 0.9500 . ?
C16D H16D 0.9500 . ?
C17D H17D 0.9500 . ?
C18D C19D 1.397(3) . ?
C19D C20D 1.374(4) . ?
C19D H19D 0.9500 . ?
C20D C21D 1.402(4) . ?
C20D H20D 0.9500 . ?
C21D C22D 1.361(4) . ?
C21D H21D 0.9500 . ?
C22D H22D 0.9500 . ?
N1 O2 1.232(3) . ?
N1 O1 1.242(3) . ?
N1 O3 1.262(3) . ?
N2 O6 1.212(3) . ?
N2 O4 1.240(3) . ?
N2 O5 1.262(4) . ?
N3 O9 1.233(3) . ?
N3 O7 1.235(3) . ?
N3 O8 1.239(3) . ?
C1S O1S 1.375(5) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O4W O4W' 1.336(7) . ?
O5W O5W' 0.927(9) . ?
O8W O8W' 0.739(17) . ?

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
O2A Cu1A N1A 168.69(7) . . ?
O2A Cu1A O1A 82.69(6) . . ?
N1A Cu1A O1A 89.91(7) . . ?
O2A Cu1A N3A 103.45(8) . . ?
N1A Cu1A N3A 82.43(8) . . ?
O1A Cu1A N3A 168.26(7) . . ?
O2A Cu1A O4A 96.98(7) . . ?
N1A Cu1A O4A 91.72(8) . . ?
O1A Cu1A O4A 91.42(7) . . ?
N3A Cu1A O4A 97.67(7) . . ?
O2A Cu1A Cu2A 42.26(5) . . ?
N1A Cu1A Cu2A 132.50(6) . . ?
O1A Cu1A Cu2A 43.29(4) . . ?
N3A Cu1A Cu2A 145.07(6) . . ?
O4A Cu1A Cu2A 83.54(5) . . ?
O2A Cu2A N4A 170.98(7) . . ?
O2A Cu2A N6A 105.22(8) . . ?
N4A Cu2A N6A 82.50(8) . . ?
O2A Cu2A O1A 82.01(6) . . ?
N4A Cu2A O1A 90.11(7) . . ?
N6A Cu2A O1A 172.40(8) . . ?
O2A Cu2A O3A 93.00(6) . . ?
N4A Cu2A O3A 91.33(7) . . ?
N6A Cu2A O3A 92.19(7) . . ?
O1A Cu2A O3A 89.74(7) . . ?
O2A Cu2A Cu1A 42.04(5) . . ?
N4A Cu2A Cu1A 131.48(6) . . ?
N6A Cu2A Cu1A 144.80(6) . . ?
O1A Cu2A Cu1A 42.80(4) . . ?
O3A Cu2A Cu1A 79.87(4) . . ?
N1B Cu1B O2B 171.74(7) . . ?
N1B Cu1B N3B 82.77(9) . . ?
O2B Cu1B N3B 105.48(8) . . ?
N1B Cu1B O1B 90.09(7) . . ?
O2B Cu1B O1B 81.66(6) . . ?
N3B Cu1B O1B 170.46(8) . . ?
N1B Cu1B Cu2B 130.88(6) . . ?
O2B Cu1B Cu2B 40.97(4) . . ?
N3B Cu1B Cu2B 144.69(7) . . ?
O1B Cu1B Cu2B 41.11(4) . . ?
O2B Cu2B N4B 168.30(7) . . ?
O2B Cu2B O1B 81.95(6) . . ?
N4B Cu2B O1B 90.06(7) . . ?
O2B Cu2B N6B 104.70(7) . . ?
N4B Cu2B N6B 82.55(8) . . ?
O1B Cu2B N6B 171.53(7) . . ?
O2B Cu2B O1E 90.45(6) . . ?
N4B Cu2B O1E 98.50(7) . . ?
O1B Cu2B O1E 92.73(7) . . ?
N6B Cu2B O1E 92.47(7) . . ?
O2B Cu2B Cu1B 40.98(5) . . ?
N4B Cu2B Cu1B 131.43(5) . . ?
O1B Cu2B Cu1B 41.38(4) . . ?
N6B Cu2B Cu1B 145.65(6) . . ?
O1E Cu2B Cu1B 87.52(4) . . ?
O2C Cu1C N4C 171.06(7) . . ?
O2C Cu1C O1C 81.49(6) . . ?
N4C Cu1C O1C 89.69(7) . . ?
O2C Cu1C N6C 106.42(7) . . ?
N4C Cu1C N6C 82.42(8) . . ?
O1C Cu1C N6C 172.08(7) . . ?
O2C Cu1C Cu2C 41.55(5) . . ?
N4C Cu1C Cu2C 130.26(5) . . ?
O1C Cu1C Cu2C 42.18(4) . . ?
N6C Cu1C Cu2C 145.22(6) . . ?
O2C Cu2C O1C 82.39(6) . . ?
O2C Cu2C N1C 169.32(7) . . ?
O1C Cu2C N1C 90.44(7) . . ?
O2C Cu2C N3C 103.39(8) . . ?
O1C Cu2C N3C 169.44(7) . . ?
N1C Cu2C N3C 82.54(8) . . ?
O2C Cu2C O3C 98.58(7) . . ?
O1C Cu2C O3C 90.23(7) . . ?
N1C Cu2C O3C 89.31(8) . . ?
N3C Cu2C O3C 97.53(7) . . ?
O2C Cu2C Cu1C 41.79(5) . . ?
O1C Cu2C Cu1C 42.87(4) . . ?
N1C Cu2C Cu1C 132.80(6) . . ?
N3C Cu2C Cu1C 144.66(6) . . ?
O3C Cu2C Cu1C 85.22(5) . . ?
N1D Cu1D O2D 171.24(7) . . ?
N1D Cu1D O1D 89.81(7) . . ?
O2D Cu1D O1D 81.45(6) . . ?
N1D Cu1D N3D 82.59(8) . . ?
O2D Cu1D N3D 106.16(7) . . ?
O1D Cu1D N3D 169.97(7) . . ?
N1D Cu1D O2C 97.07(7) . . ?
O2D Cu1D O2C 82.33(6) . . ?
O1D Cu1D O2C 88.96(6) . . ?
N3D Cu1D O2C 98.43(7) . . ?
N1D Cu1D Cu2D 130.41(6) . . ?
O2D Cu1D Cu2D 40.96(4) . . ?
O1D Cu1D Cu2D 40.96(4) . . ?
N3D Cu1D Cu2D 145.16(6) . . ?
O2C Cu1D Cu2D 89.12(4) . . ?
N4D Cu2D O1D 89.98(7) . . ?
N4D Cu2D O2D 167.61(7) . . ?
O1D Cu2D O2D 81.64(6) . . ?
N4D Cu2D N6D 82.52(8) . . ?
O1D Cu2D N6D 171.42(7) . . ?
O2D Cu2D N6D 105.07(7) . . ?
N4D Cu2D O1E 99.48(7) . . ?
O1D Cu2D O1E 94.17(6) . . ?
O2D Cu2D O1E 90.27(6) . . ?
N6D Cu2D O1E 91.16(7) . . ?
N4D Cu2D Cu1D 131.25(5) . . ?
O1D Cu2D Cu1D 41.30(4) . . ?
O2D Cu2D Cu1D 40.83(4) . . ?
N6D Cu2D Cu1D 145.86(6) . . ?
O1E Cu2D Cu1D 88.03(4) . . ?
C1A O1A Cu1A 127.89(14) . . ?
C1A O1A Cu2A 128.36(14) . . ?
Cu1A O1A Cu2A 93.91(7) . . ?
Cu1A O2A Cu2A 95.70(7) . . ?
C11A N1A N2A 118.9(2) . . ?
C11A N1A Cu1A 128.69(16) . . ?
N2A N1A Cu1A 112.41(15) . . ?
N1A N2A C12A 115.4(2) . . ?
C12A N3A C16A 118.3(2) . . ?
C12A N3A Cu1A 112.94(17) . . ?
C16A N3A Cu1A 128.74(18) . . ?
C17A N4A N5A 118.9(2) . . ?
C17A N4A Cu2A 128.75(16) . . ?
N5A N4A Cu2A 112.34(15) . . ?
N4A N5A C18A 115.7(2) . . ?
C18A N6A C22A 118.7(2) . . ?
C18A N6A Cu2A 111.93(16) . . ?
C22A N6A Cu2A 129.27(18) . . ?
O5A N7A O3A 119.3(2) . . ?
O5A N7A O4A 119.8(2) . . ?
O3A N7A O4A 121.0(2) . . ?
N7A O3A Cu2A 127.64(15) . . ?
N7A O4A Cu1A 126.02(15) . . ?
C1B O1B Cu2B 131.13(14) . . ?
C1B O1B Cu1B 130.99(14) . . ?
Cu2B O1B Cu1B 97.51(7) . . ?
Cu2B O2B Cu1B 98.05(7) . . ?
C11B N1B N2B 118.8(2) . . ?
C11B N1B Cu1B 129.28(16) . . ?
N2B N1B Cu1B 111.95(16) . . ?
N1B N2B C12B 115.3(2) . . ?
C12B N3B C16B 118.5(2) . . ?
C12B N3B Cu1B 112.23(17) . . ?
C16B N3B Cu1B 129.24(19) . . ?
C17B N4B N5B 118.76(19) . . ?
C17B N4B Cu2B 128.92(16) . . ?
N5B N4B Cu2B 112.32(14) . . ?
C18B N5B N4B 115.99(19) . . ?
C18B N6B C22B 118.6(2) . . ?
C18B N6B Cu2B 112.19(15) . . ?
C22B N6B Cu2B 129.17(17) . . ?
O5B N7B O4B 120.0(2) . . ?
O5B N7B O3B 120.5(2) . . ?
O4B N7B O3B 119.5(2) . . ?
Cu2D O1E Cu2B 138.23(8) . . ?
C1C O1C Cu2C 127.94(13) . . ?
C1C O1C Cu1C 129.21(14) . . ?
Cu2C O1C Cu1C 94.95(7) . . ?
Cu2C O2C Cu1C 96.66(7) . . ?
Cu2C O2C Cu1D 108.79(7) . . ?
Cu1C O2C Cu1D 99.02(6) . . ?
C11C N1C N2C 119.1(2) . . ?
C11C N1C Cu2C 128.51(16) . . ?
N2C N1C Cu2C 112.36(15) . . ?
C12C N2C N1C 115.3(2) . . ?
C12C N3C C16C 118.5(2) . . ?
C12C N3C Cu2C 112.64(16) . . ?
C16C N3C Cu2C 128.83(17) . . ?
C17C N4C N5C 118.1(2) . . ?
C17C N4C Cu1C 129.73(16) . . ?
N5C N4C Cu1C 112.14(15) . . ?
C18C N5C N4C 115.6(2) . . ?
C18C N6C C22C 118.1(2) . . ?
C18C N6C Cu1C 112.37(15) . . ?
C22C N6C Cu1C 129.49(18) . . ?
O5C N7C O3C 119.8(3) . . ?
O5C N7C O4C 118.6(3) . . ?
O3C N7C O4C 121.6(2) . . ?
N7C O3C Cu2C 124.40(16) . . ?
C1D O1D Cu2D 131.20(13) . . ?
C1D O1D Cu1D 130.74(13) . . ?
Cu2D O1D Cu1D 97.74(6) . . ?
Cu1D O2D Cu2D 98.21(6) . . ?
C11D N1D N2D 118.72(19) . . ?
C11D N1D Cu1D 129.39(16) . . ?
N2D N1D Cu1D 111.90(15) . . ?
N1D N2D C12D 116.2(2) . . ?
C12D N3D C16D 118.5(2) . . ?
C12D N3D Cu1D 112.36(15) . . ?
C16D N3D Cu1D 129.10(17) . . ?
C17D N4D N5D 118.57(18) . . ?
C17D N4D Cu2D 129.15(15) . . ?
N5D N4D Cu2D 112.28(13) . . ?
C18D N5D N4D 115.66(18) . . ?
C18D N6D C22D 118.6(2) . . ?
C18D N6D Cu2D 112.27(15) . . ?
C22D N6D Cu2D 129.13(16) . . ?
O4D N7D O5D 121.3(2) . . ?
O4D N7D O3D 118.5(2) . . ?
O5D N7D O3D 120.1(2) . . ?
O1A C1A C6A 121.4(2) . . ?
O1A C1A C2A 121.0(2) . . ?
C6A C1A C2A 117.6(2) . . ?
C3A C2A C1A 120.0(2) . . ?
C3A C2A C11A 116.5(2) . . ?
C1A C2A C11A 123.6(2) . . ?
C4A C3A C2A 122.8(2) . . ?
C4A C3A H3A 118.6 . . ?
C2A C3A H3A 118.6 . . ?
C3A C4A C5A 116.9(2) . . ?
C3A C4A C7A 123.3(2) . . ?
C5A C4A C7A 119.8(2) . . ?
C4A C5A C6A 122.5(2) . . ?
C4A C5A H5A 118.7 . . ?
C6A C5A H5A 118.7 . . ?
C5A C6A C1A 120.2(2) . . ?
C5A C6A C17A 115.4(2) . . ?
C1A C6A C17A 124.4(2) . . ?
C9A C7A C10A 108.9(2) . . ?
C9A C7A C4A 111.1(2) . . ?
C10A C7A C4A 111.8(2) . . ?
C9A C7A C8A 107.4(3) . . ?
C10A C7A C8A 108.6(3) . . ?
C4A C7A C8A 109.0(2) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7A C9A H9A1 109.5 . . ?
C7A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C7A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C7A C10A H10A 109.5 . . ?
C7A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C7A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
N1A C11A C2A 124.1(2) . . ?
N1A C11A H11A 118.0 . . ?
C2A C11A H11A 118.0 . . ?
N3A C12A N2A 116.7(2) . . ?
N3A C12A C13A 122.7(2) . . ?
N2A C12A C13A 120.6(2) . . ?
C14A C13A C12A 117.9(3) . . ?
C14A C13A H13A 121.1 . . ?
C12A C13A H13A 121.1 . . ?
C13A C14A C15A 119.8(3) . . ?
C13A C14A H14A 120.1 . . ?
C15A C14A H14A 120.1 . . ?
C16A C15A C14A 118.6(3) . . ?
C16A C15A H15A 120.7 . . ?
C14A C15A H15A 120.7 . . ?
N3A C16A C15A 122.7(3) . . ?
N3A C16A H16A 118.7 . . ?
C15A C16A H16A 118.7 . . ?
N4A C17A C6A 124.0(2) . . ?
N4A C17A H17A 118.0 . . ?
C6A C17A H17A 118.0 . . ?
N6A C18A N5A 116.7(2) . . ?
N6A C18A C19A 121.7(3) . . ?
N5A C18A C19A 121.6(3) . . ?
C20A C19A C18A 118.1(3) . . ?
C20A C19A H19A 120.9 . . ?
C18A C19A H19A 120.9 . . ?
C19A C20A C21A 120.3(3) . . ?
C19A C20A H20A 119.9 . . ?
C21A C20A H20A 119.9 . . ?
C22A C21A C20A 119.1(3) . . ?
C22A C21A H21A 120.5 . . ?
C20A C21A H21A 120.5 . . ?
N6A C22A C21A 122.1(3) . . ?
N6A C22A H22A 118.9 . . ?
C21A C22A H22A 118.9 . . ?
O1B C1B C2B 121.0(2) . . ?
O1B C1B C6B 120.28(19) . . ?
C2B C1B C6B 118.7(2) . . ?
C3B C2B C1B 119.6(2) . . ?
C3B C2B C11B 115.8(2) . . ?
C1B C2B C11B 124.5(2) . . ?
C4B C3B C2B 122.7(2) . . ?
C4B C3B H3B 118.7 . . ?
C2B C3B H3B 118.7 . . ?
C5B C4B C3B 116.8(2) . . ?
C5B C4B C7B 120.9(2) . . ?
C3B C4B C7B 122.3(2) . . ?
C4B C5B C6B 123.0(2) . . ?
C4B C5B H5B 118.5 . . ?
C6B C5B H5B 118.5 . . ?
C1B C6B C5B 119.1(2) . . ?
C1B C6B C17B 125.00(19) . . ?
C5B C6B C17B 115.9(2) . . ?
C10B C7B C9B 109.2(2) . . ?
C10B C7B C4B 109.2(2) . . ?
C9B C7B C4B 112.0(2) . . ?
C10B C7B C8B 110.0(3) . . ?
C9B C7B C8B 106.7(2) . . ?
C4B C7B C8B 109.7(2) . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7B C9B H9B1 109.5 . . ?
C7B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C7B C10B H10D 109.5 . . ?
C7B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C7B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
N1B C11B C2B 124.1(2) . . ?
N1B C11B H11B 117.9 . . ?
C2B C11B H11B 117.9 . . ?
N3B C12B N2B 117.2(2) . . ?
N3B C12B C13B 122.3(3) . . ?
N2B C12B C13B 120.5(3) . . ?
C14B C13B C12B 117.5(3) . . ?
C14B C13B H13B 121.2 . . ?
C12B C13B H13B 121.2 . . ?
C15B C14B C13B 120.7(3) . . ?
C15B C14B H14B 119.7 . . ?
C13B C14B H14B 119.7 . . ?
C14B C15B C16B 118.5(3) . . ?
C14B C15B H15B 120.8 . . ?
C16B C15B H15B 120.8 . . ?
N3B C16B C15B 122.3(3) . . ?
N3B C16B H16B 118.8 . . ?
C15B C16B H16B 118.8 . . ?
N4B C17B C6B 124.1(2) . . ?
N4B C17B H17B 118.0 . . ?
C6B C17B H17B 118.0 . . ?
N6B C18B N5B 116.9(2) . . ?
N6B C18B C19B 122.1(2) . . ?
N5B C18B C19B 121.0(2) . . ?
C20B C19B C18B 118.5(3) . . ?
C20B C19B H19B 120.8 . . ?
C18B C19B H19B 120.8 . . ?
C19B C20B C21B 119.8(2) . . ?
C19B C20B H20B 120.1 . . ?
C21B C20B H20B 120.1 . . ?
C22B C21B C20B 118.8(3) . . ?
C22B C21B H21B 120.6 . . ?
C20B C21B H21B 120.6 . . ?
C21B C22B N6B 122.3(3) . . ?
C21B C22B H22B 118.9 . . ?
N6B C22B H22B 118.9 . . ?
N4C C17C C6C 124.1(2) . . ?
N4C C17C H17C 118.0 . . ?
C6C C17C H17C 118.0 . . ?
O1C C1C C6C 120.60(19) . . ?
O1C C1C C2C 120.8(2) . . ?
C6C C1C C2C 118.5(2) . . ?
C3C C2C C1C 119.4(2) . . ?
C3C C2C C11C 116.5(2) . . ?
C1C C2C C11C 124.1(2) . . ?
C4C C3C C2C 122.8(2) . . ?
C4C C3C H3C 118.6 . . ?
C2C C3C H3C 118.6 . . ?
C5C C4C C3C 116.8(2) . . ?
C5C C4C C7C 120.1(2) . . ?
C3C C4C C7C 123.0(2) . . ?
C4C C5C C6C 122.9(2) . . ?
C4C C5C H5C 118.5 . . ?
C6C C5C H5C 118.5 . . ?
C5C C6C C1C 119.5(2) . . ?
C5C C6C C17C 115.8(2) . . ?
C1C C6C C17C 124.8(2) . . ?
C9C C7C C10C 111.2(3) . . ?
C9C C7C C4C 113.3(2) . . ?
C10C C7C C4C 111.5(2) . . ?
C9C C7C C8C 107.9(3) . . ?
C10C C7C C8C 103.6(3) . . ?
C4C C7C C8C 108.8(2) . . ?
C7C C8C H8C1 109.5 . . ?
C7C C8C H8C2 109.5 . . ?
H8C1 C8C H8C2 109.5 . . ?
C7C C8C H8C3 109.5 . . ?
H8C1 C8C H8C3 109.5 . . ?
H8C2 C8C H8C3 109.5 . . ?
C7C C9C H9C1 109.5 . . ?
C7C C9C H9C2 109.5 . . ?
H9C1 C9C H9C2 109.5 . . ?
C7C C9C H9C3 109.5 . . ?
H9C1 C9C H9C3 109.5 . . ?
H9C2 C9C H9C3 109.5 . . ?
C7C C10C H10G 109.5 . . ?
C7C C10C H10H 109.5 . . ?
H10G C10C H10H 109.5 . . ?
C7C C10C H10I 109.5 . . ?
H10G C10C H10I 109.5 . . ?
H10H C10C H10I 109.5 . . ?
N1C C11C C2C 124.1(2) . . ?
N1C C11C H11C 117.9 . . ?
C2C C11C H11C 117.9 . . ?
N3C C12C N2C 117.0(2) . . ?
N3C C12C C13C 122.2(2) . . ?
N2C C12C C13C 120.8(2) . . ?
C14C C13C C12C 117.4(2) . . ?
C14C C13C H13C 121.3 . . ?
C12C C13C H13C 121.3 . . ?
C13C C14C C15C 120.7(2) . . ?
C13C C14C H14C 119.7 . . ?
C15C C14C H14C 119.7 . . ?
C16C C15C C14C 118.5(3) . . ?
C16C C15C H15C 120.7 . . ?
C14C C15C H15C 120.7 . . ?
N3C C16C C15C 122.6(3) . . ?
N3C C16C H16C 118.7 . . ?
C15C C16C H16C 118.7 . . ?
N6C C18C N5C 116.6(2) . . ?
N6C C18C C19C 123.3(2) . . ?
N5C C18C C19C 120.1(2) . . ?
C20C C19C C18C 117.6(3) . . ?
C20C C19C H19C 121.2 . . ?
C18C C19C H19C 121.2 . . ?
C21C C20C C19C 119.7(2) . . ?
C21C C20C H20C 120.1 . . ?
C19C C20C H20C 120.1 . . ?
C22C C21C C20C 119.7(3) . . ?
C22C C21C H21C 120.2 . . ?
C20C C21C H21C 120.2 . . ?
N6C C22C C21C 121.6(3) . . ?
N6C C22C H22C 119.2 . . ?
C21C C22C H22C 119.2 . . ?
O1D C1D C2D 121.24(19) . . ?
O1D C1D C6D 120.34(19) . . ?
C2D C1D C6D 118.41(19) . . ?
C1D C2D C3D 120.0(2) . . ?
C1D C2D C11D 124.31(19) . . ?
C3D C2D C11D 115.71(19) . . ?
C4D C3D C2D 122.4(2) . . ?
C4D C3D H3D 118.8 . . ?
C2D C3D H3D 118.8 . . ?
C5D C4D C3D 117.1(2) . . ?
C5D C4D C7D 120.5(2) . . ?
C3D C4D C7D 122.5(2) . . ?
C4D C5D C6D 122.9(2) . . ?
C4D C5D H5D 118.5 . . ?
C6D C5D H5D 118.5 . . ?
C5D C6D C1D 119.10(19) . . ?
C5D C6D C17D 116.76(19) . . ?
C1D C6D C17D 124.13(19) . . ?
C8D C7D C9D 108.8(2) . . ?
C8D C7D C4D 109.7(2) . . ?
C9D C7D C4D 111.3(2) . . ?
C8D C7D C10D 109.4(3) . . ?
C9D C7D C10D 108.6(2) . . ?
C4D C7D C10D 109.0(2) . . ?
C7D C8D H8D1 109.5 . . ?
C7D C8D H8D2 109.5 . . ?
H8D1 C8D H8D2 109.5 . . ?
C7D C8D H8D3 109.5 . . ?
H8D1 C8D H8D3 109.5 . . ?
H8D2 C8D H8D3 109.5 . . ?
C7D C9D H9D1 109.5 . . ?
C7D C9D H9D2 109.5 . . ?
H9D1 C9D H9D2 109.5 . . ?
C7D C9D H9D3 109.5 . . ?
H9D1 C9D H9D3 109.5 . . ?
H9D2 C9D H9D3 109.5 . . ?
C7D C10D H10J 109.5 . . ?
C7D C10D H10K 109.5 . . ?
H10J C10D H10K 109.5 . . ?
C7D C10D H10L 109.5 . . ?
H10J C10D H10L 109.5 . . ?
H10K C10D H10L 109.5 . . ?
N1D C11D C2D 124.5(2) . . ?
N1D C11D H11D 117.8 . . ?
C2D C11D H11D 117.8 . . ?
N3D C12D N2D 116.5(2) . . ?
N3D C12D C13D 122.9(2) . . ?
N2D C12D C13D 120.7(2) . . ?
C14D C13D C12D 117.5(3) . . ?
C14D C13D H13D 121.2 . . ?
C12D C13D H13D 121.2 . . ?
C13D C14D C15D 120.5(2) . . ?
C13D C14D H14D 119.8 . . ?
C15D C14D H14D 119.8 . . ?
C16D C15D C14D 118.7(3) . . ?
C16D C15D H15D 120.6 . . ?
C14D C15D H15D 120.6 . . ?
N3D C16D C15D 121.8(2) . . ?
N3D C16D H16D 119.1 . . ?
C15D C16D H16D 119.1 . . ?
N4D C17D C6D 124.7(2) . . ?
N4D C17D H17D 117.6 . . ?
C6D C17D H17D 117.6 . . ?
N6D C18D N5D 117.25(19) . . ?
N6D C18D C19D 122.6(2) . . ?
N5D C18D C19D 120.2(2) . . ?
C20D C19D C18D 118.2(2) . . ?
C20D C19D H19D 120.9 . . ?
C18D C19D H19D 120.9 . . ?
C19D C20D C21D 119.7(2) . . ?
C19D C20D H20D 120.2 . . ?
C21D C20D H20D 120.2 . . ?
C22D C21D C20D 118.8(2) . . ?
C22D C21D H21D 120.6 . . ?
C20D C21D H21D 120.6 . . ?
C21D C22D N6D 122.2(2) . . ?
C21D C22D H22D 118.9 . . ?
N6D C22D H22D 118.9 . . ?
O2 N1 O1 121.1(3) . . ?
O2 N1 O3 120.9(3) . . ?
O1 N1 O3 118.0(3) . . ?
O6 N2 O4 119.4(3) . . ?
O6 N2 O5 119.3(3) . . ?
O4 N2 O5 121.2(3) . . ?
O9 N3 O7 120.5(3) . . ?
O9 N3 O8 119.5(3) . . ?
O7 N3 O8 119.9(3) . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.933
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.091
_database_code_depnum_ccdc_archive 'CCDC 964838'
