# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_(1)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Poly[μ₃-[1,3-bis(pyridazin-4-yl)adamantane-κ⁴N1:N2:N3)]-μ₄-
(1,3,5-benzenetricarboxylato)-μ₂-hydroxido-aquadicopper(II)]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 Cu2 N4 O8'
_chemical_formula_sum            'C27 H26 Cu2 N4 O8'
_chemical_formula_weight         661.60

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           monoclinic
_symmetry_space_group_name_H-M   C2/c
_space_group_name_Hall           '-C 2yc'
_symmetry_Int_Tables_number      15


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

_cell_length_a                   24.8536(18)
_cell_length_b                   10.8716(7)
_cell_length_c                   18.6837(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.581(8)
_cell_angle_gamma                90.00
_cell_volume                     4945.5(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      25.96

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2704
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6742
_exptl_absorpt_correction_T_max  0.7757
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      213(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  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       'φ oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16964
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.96
_reflns_number_total             4789
_reflns_number_gt                3592
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#


_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.

 The CH-hydrogen atoms were added geometrically, with Uiso = 1.2Ueq(C) 
 and OH-hydrogen atoms were located and included with fixed d(O-H) = 
 0.85 A and Uiso = 1.5Ueq(O). 

 Main feature of the crystal structure refinement was associated with 
 disorder within the binuclear cluster. It is equally disordered over two 
 positions (one Cu ion, hydroxido and aqua ligand; one of the pyridazine 
 cycles is also disordered by rotation along N1---C2 axis, adopting two 
 orientations). Attempted solution and refinements in space groups of 
 lower symmetry (either monoclinic C, monoclinic P or triclinic lattices 
 were considered) did not afford an ordered model. Both contributions of 
 the disorder (PART -1 and PART -2) were freely refined anisotropically, 
 without any restraints or constraints in the geometry and thermal motion, 
 and the hydrogen atoms of these fragments were added as stated above 
 with partial occupancy factors of 0.5. 
;

_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)+(0.0552P)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_number_reflns         4789
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0809
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_restrained_S_all      0.917
_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 0.409935(13) 0.15821(3) 0.52869(2) 0.03484(11) Uani 1 1 d . . .
Cu2A Cu 0.44234(3) 0.42890(5) 0.51526(3) 0.02307(14) Uani 0.50 1 d P . -1
O1A O 0.39257(14) 0.3205(3) 0.5491(2) 0.0281(8) Uani 0.50 1 d P . -1
H1OA H 0.3955 0.3293 0.5949 0.042 Uiso 0.50 1 d PR . -1
O2A O 0.49529(16) 0.5419(3) 0.48174(19) 0.0299(8) Uani 0.50 1 d P . -1
H1WA H 0.5174 0.5101 0.4577 0.045 Uiso 0.50 1 d PR . -1
H2WA H 0.5140 0.5771 0.5193 0.045 Uiso 0.50 1 d PR . -1
N2A N 0.50967(18) 0.3011(3) 0.5601(2) 0.0258(9) Uani 0.50 1 d P . -1
C1A C 0.5619(2) 0.3292(4) 0.5793(3) 0.0269(11) Uani 0.50 1 d P . -1
H1A H 0.5719 0.4122 0.5766 0.032 Uiso 0.50 1 calc PR . -1
C3A C 0.5884(2) 0.1231(4) 0.5940(3) 0.0277(11) Uani 0.50 1 d P . -1
H3A H 0.6148 0.0601 0.5999 0.033 Uiso 0.50 1 calc PR . -1
C4A C 0.5324(2) 0.0974(4) 0.5756(3) 0.0271(11) Uani 0.50 1 d P . -1
H4A H 0.5212 0.0148 0.5751 0.033 Uiso 0.50 1 calc PR . -1
Cu2B Cu 0.44074(2) 0.26516(5) 0.68701(3) 0.02225(14) Uani 0.50 1 d P . -2
O1B O 0.38975(14) 0.2719(3) 0.59688(19) 0.0249(7) Uani 0.50 1 d P . -2
H1OB H 0.3893 0.3442 0.5796 0.037 Uiso 0.50 1 d PR . -2
O2B O 0.49240(16) 0.2621(3) 0.78067(18) 0.0303(8) Uani 0.50 1 d P . -2
H1WB H 0.5137 0.2007 0.7816 0.045 Uiso 0.50 1 d PR . -2
H2WB H 0.5117 0.3250 0.7956 0.045 Uiso 0.50 1 d PR . -2
N2B N 0.50799(17) 0.2421(4) 0.6225(2) 0.0246(9) Uani 0.50 1 d P . -2
C1B C 0.5601(2) 0.2694(4) 0.6463(3) 0.0262(10) Uani 0.50 1 d P . -2
H1B H 0.5706 0.3060 0.6925 0.031 Uiso 0.50 1 calc PR . -2
C3B C 0.5850(2) 0.1819(4) 0.5436(3) 0.0250(10) Uani 0.50 1 d P . -2
H3B H 0.6103 0.1526 0.5164 0.030 Uiso 0.50 1 calc PR . -2
C4B C 0.5298(2) 0.1570(4) 0.5193(3) 0.0247(10) Uani 0.50 1 d P . -2
H4B H 0.5182 0.1184 0.4738 0.030 Uiso 0.50 1 calc PR . -2
O3 O 0.41797(8) 0.14349(19) 0.42239(10) 0.0387(5) Uani 1 1 d . . .
O4 O 0.42331(10) 0.3484(2) 0.41816(11) 0.0526(6) Uani 1 1 d . . .
O5 O 0.43172(11) 0.4574(2) 0.09162(12) 0.0598(7) Uani 1 1 d . . .
O6 O 0.43337(10) 0.55927(16) 0.19518(14) 0.0542(6) Uani 1 1 d . . .
O7 O 0.42682(7) 0.00679(15) 0.09348(10) 0.0330(4) Uani 1 1 d . . .
O8 O 0.42705(9) -0.09217(16) 0.19845(13) 0.0456(5) Uani 1 1 d . . .
N1 N 0.49311(8) 0.18616(17) 0.55835(11) 0.0235(4) Uani 1 1 d . . .
C2 C 0.60329(10) 0.2449(2) 0.60319(14) 0.0271(5) Uani 1 1 d . . .
N3 N 0.79633(10) 0.6565(2) 0.44248(14) 0.0409(6) Uani 1 1 d . . .
N4 N 0.82879(10) 0.6111(2) 0.50234(14) 0.0390(6) Uani 1 1 d . . .
C5 C 0.80850(12) 0.5396(3) 0.54756(17) 0.0407(7) Uani 1 1 d . . .
H5 H 0.8326 0.5129 0.5901 0.049 Uiso 1 1 calc R . .
C6 C 0.75392(11) 0.5007(2) 0.53690(15) 0.0320(6) Uani 1 1 d . . .
C7 C 0.72034(11) 0.5476(2) 0.47531(16) 0.0354(6) Uani 1 1 d . . .
H7 H 0.6828 0.5273 0.4634 0.042 Uiso 1 1 calc R . .
C8 C 0.74362(13) 0.6254(3) 0.43164(18) 0.0412(7) Uani 1 1 d . . .
H8 H 0.7201 0.6593 0.3906 0.049 Uiso 1 1 calc R . .
C9 C 0.73698(11) 0.4171(2) 0.59348(16) 0.0312(6) Uani 1 1 d . . .
C10 C 0.67764(10) 0.3720(2) 0.56990(15) 0.0305(6) Uani 1 1 d . . .
H10A H 0.6737 0.3267 0.5238 0.037 Uiso 1 1 calc R . .
H10B H 0.6528 0.4428 0.5618 0.037 Uiso 1 1 calc R . .
C11 C 0.66180(10) 0.2875(2) 0.62906(15) 0.0290(6) Uani 1 1 d . . .
C12 C 0.70136(12) 0.1773(2) 0.64138(17) 0.0368(6) Uani 1 1 d . . .
H12A H 0.6917 0.1228 0.6786 0.044 Uiso 1 1 calc R . .
H12B H 0.6982 0.1305 0.5959 0.044 Uiso 1 1 calc R . .
C13 C 0.76042(12) 0.2233(3) 0.66633(18) 0.0408(7) Uani 1 1 d . . .
H13 H 0.7856 0.1519 0.6745 0.049 Uiso 1 1 calc R . .
C14 C 0.77539(11) 0.3045(3) 0.60734(17) 0.0380(7) Uani 1 1 d . . .
H14A H 0.7724 0.2572 0.5621 0.046 Uiso 1 1 calc R . .
H14B H 0.8135 0.3322 0.6224 0.046 Uiso 1 1 calc R . .
C15 C 0.74122(12) 0.4887(3) 0.66522(16) 0.0366(6) Uani 1 1 d . . .
H15A H 0.7787 0.5201 0.6810 0.044 Uiso 1 1 calc R . .
H15B H 0.7161 0.5591 0.6573 0.044 Uiso 1 1 calc R . .
C16 C 0.72677(12) 0.4061(3) 0.72451(17) 0.0406(7) Uani 1 1 d . . .
H16 H 0.7299 0.4537 0.7703 0.049 Uiso 1 1 calc R . .
C17 C 0.66773(12) 0.3604(3) 0.70023(16) 0.0379(6) Uani 1 1 d . . .
H17A H 0.6580 0.3079 0.7384 0.046 Uiso 1 1 calc R . .
H17B H 0.6425 0.4307 0.6929 0.046 Uiso 1 1 calc R . .
C18 C 0.76580(13) 0.2961(3) 0.73776(18) 0.0463(7) Uani 1 1 d . . .
H18A H 0.7565 0.2434 0.7761 0.056 Uiso 1 1 calc R . .
H18B H 0.8037 0.3247 0.7539 0.056 Uiso 1 1 calc R . .
C19 C 0.42128(11) 0.2440(3) 0.38974(14) 0.0324(6) Uani 1 1 d . . .
C20 C 0.43134(11) 0.4637(2) 0.15831(16) 0.0306(6) Uani 1 1 d . . .
C21 C 0.42791(10) 0.0035(2) 0.16149(14) 0.0261(5) Uani 1 1 d . . .
C22 C 0.42341(10) 0.2377(2) 0.30982(13) 0.0245(5) Uani 1 1 d . . .
C23 C 0.42593(10) 0.3461(2) 0.27171(14) 0.0244(5) Uani 1 1 d . . .
H23 H 0.4259 0.4218 0.2960 0.029 Uiso 1 1 calc R . .
C24 C 0.42842(10) 0.3448(2) 0.19833(13) 0.0220(5) Uani 1 1 d . . .
C25 C 0.42903(10) 0.2335(2) 0.16259(13) 0.0213(5) Uani 1 1 d . . .
H25 H 0.4307 0.2320 0.1128 0.026 Uiso 1 1 calc R . .
C26 C 0.42723(9) 0.12400(19) 0.20030(13) 0.0205(5) Uani 1 1 d . . .
C27 C 0.42441(10) 0.1270(2) 0.27387(13) 0.0231(5) Uani 1 1 d . . .
H27 H 0.4232 0.0529 0.2994 0.028 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 O1A 1.873(3) . ?
Cu1 O1B 1.913(3) . ?
Cu1 O3 2.0418(18) . ?
Cu1 N4 2.043(2) 3_445 ?
Cu1 N1 2.053(2) . ?
Cu1 O7 2.1577(16) 6_556 ?
Cu2A O1A 1.906(3) . ?
Cu2A O5 1.946(2) 6_566 ?
Cu2A O4 1.984(2) . ?
Cu2A O2A 1.991(3) . ?
Cu2A N2A 2.207(4) . ?
O1A H1OA 0.8500 . ?
O2A H1WA 0.8500 . ?
O2A H2WA 0.8500 . ?
N2A C1A 1.312(6) . ?
N2A N1 1.314(4) . ?
C1A C2 1.383(6) . ?
C1A H1A 0.9400 . ?
C3A C2 1.377(5) . ?
C3A C4A 1.392(7) . ?
C3A H3A 0.9400 . ?
C4A N1 1.366(5) . ?
C4A H4A 0.9400 . ?
Cu2B O1B 1.895(4) . ?
Cu2B O6 1.9264(19) 6_566 ?
Cu2B O8 1.9307(18) 6_556 ?
Cu2B O2B 1.952(4) . ?
Cu2B N2B 2.262(4) . ?
O1B H1OB 0.8500 . ?
O2B H1WB 0.8500 . ?
O2B H2WB 0.8500 . ?
N2B C1B 1.317(6) . ?
N2B N1 1.329(4) . ?
C1B C2 1.488(5) . ?
C1B H1B 0.9400 . ?
C3B C2 1.308(6) . ?
C3B C4B 1.384(7) . ?
C3B H3B 0.9400 . ?
C4B N1 1.315(5) . ?
C4B H4B 0.9400 . ?
O3 C19 1.262(3) . ?
O4 C19 1.250(3) . ?
O5 C20 1.250(3) . ?
O5 Cu2A 1.946(2) 6_565 ?
O6 C20 1.242(3) . ?
O6 Cu2B 1.9264(19) 6_565 ?
O7 C21 1.266(3) . ?
O7 Cu1 2.1577(16) 6 ?
O8 C21 1.251(3) . ?
O8 Cu2B 1.9307(18) 6 ?
C2 C11 1.510(4) . ?
N3 C8 1.328(4) . ?
N3 N4 1.335(4) . ?
N4 C5 1.320(4) . ?
N4 Cu1 2.043(2) 3 ?
C5 C6 1.397(4) . ?
C5 H5 0.9400 . ?
C6 C7 1.376(4) . ?
C6 C9 1.517(4) . ?
C7 C8 1.380(4) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C10 1.532(4) . ?
C9 C15 1.535(4) . ?
C9 C14 1.541(4) . ?
C10 C11 1.548(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C17 1.529(4) . ?
C11 C12 1.537(3) . ?
C12 C13 1.532(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 C14 1.516(4) . ?
C13 C18 1.534(5) . ?
C13 H13 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.524(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 C18 1.528(4) . ?
C16 C17 1.529(4) . ?
C16 H16 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C22 1.506(3) . ?
C20 C24 1.503(3) . ?
C21 C26 1.499(3) . ?
C22 C27 1.381(3) . ?
C22 C23 1.385(3) . ?
C23 C24 1.385(3) . ?
C23 H23 0.9400 . ?
C24 C25 1.384(3) . ?
C25 C26 1.388(3) . ?
C25 H25 0.9400 . ?
C26 C27 1.391(3) . ?
C27 H27 0.9400 . ?

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
O1A Cu1 O3 110.06(13) . . ?
O1B Cu1 O3 142.05(12) . . ?
O1A Cu1 N4 91.62(12) . 3_445 ?
O1B Cu1 N4 86.79(12) . 3_445 ?
O3 Cu1 N4 91.75(9) . 3_445 ?
O1A Cu1 N1 93.80(12) . . ?
O1B Cu1 N1 96.27(12) . . ?
O3 Cu1 N1 89.10(8) . . ?
N4 Cu1 N1 173.85(9) 3_445 . ?
O1A Cu1 O7 134.08(13) . 6_556 ?
O1B Cu1 O7 102.17(12) . 6_556 ?
O3 Cu1 O7 115.76(8) . 6_556 ?
N4 Cu1 O7 89.91(9) 3_445 6_556 ?
N1 Cu1 O7 84.24(7) . 6_556 ?
O1A Cu2A O5 87.56(13) . 6_566 ?
O1A Cu2A O4 88.78(14) . . ?
O5 Cu2A O4 155.29(11) 6_566 . ?
O1A Cu2A O2A 178.92(17) . . ?
O5 Cu2A O2A 91.94(13) 6_566 . ?
O4 Cu2A O2A 92.06(12) . . ?
O1A Cu2A N2A 88.73(14) . . ?
O5 Cu2A N2A 109.02(13) 6_566 . ?
O4 Cu2A N2A 95.32(13) . . ?
O2A Cu2A N2A 90.53(15) . . ?
Cu1 O1A Cu2A 108.89(16) . . ?
Cu1 O1A H1OA 109.5 . . ?
Cu2A O1A H1OA 109.5 . . ?
Cu2A O2A H1WA 116.9 . . ?
Cu2A O2A H2WA 107.7 . . ?
H1WA O2A H2WA 108.4 . . ?
C1A N2A N1 121.1(4) . . ?
C1A N2A Cu2A 126.2(3) . . ?
N1 N2A Cu2A 112.3(3) . . ?
N2A C1A C2 124.4(4) . . ?
N2A C1A H1A 117.8 . . ?
C2 C1A H1A 117.8 . . ?
C2 C3A C4A 117.0(4) . . ?
C2 C3A H3A 121.5 . . ?
C4A C3A H3A 121.5 . . ?
N1 C4A C3A 123.3(4) . . ?
N1 C4A H4A 118.4 . . ?
C3A C4A H4A 118.4 . . ?
O1B Cu2B O6 88.57(13) . 6_566 ?
O1B Cu2B O8 91.98(12) . 6_556 ?
O6 Cu2B O8 159.17(9) 6_566 6_556 ?
O1B Cu2B O2B 178.52(14) . . ?
O6 Cu2B O2B 90.11(12) 6_566 . ?
O8 Cu2B O2B 89.00(12) 6_556 . ?
O1B Cu2B N2B 87.98(15) . . ?
O6 Cu2B N2B 104.15(12) 6_566 . ?
O8 Cu2B N2B 96.68(12) 6_556 . ?
O2B Cu2B N2B 93.00(15) . . ?
Cu2B O1B Cu1 110.43(16) . . ?
Cu2B O1B H1OB 109.2 . . ?
Cu1 O1B H1OB 109.3 . . ?
Cu2B O2B H1WB 109.1 . . ?
Cu2B O2B H2WB 120.5 . . ?
H1WB O2B H2WB 108.4 . . ?
C1B N2B N1 119.0(3) . . ?
C1B N2B Cu2B 125.3(3) . . ?
N1 N2B Cu2B 115.5(2) . . ?
N2B C1B C2 123.0(4) . . ?
N2B C1B H1B 118.5 . . ?
C2 C1B H1B 118.5 . . ?
C2 C3B C4B 122.3(4) . . ?
C2 C3B H3B 118.8 . . ?
C4B C3B H3B 118.8 . . ?
N1 C4B C3B 121.5(4) . . ?
N1 C4B H4B 119.3 . . ?
C3B C4B H4B 119.3 . . ?
C19 O3 Cu1 115.53(17) . . ?
C19 O4 Cu2A 140.4(2) . . ?
C20 O5 Cu2A 136.48(19) . 6_565 ?
C20 O6 Cu2B 141.1(2) . 6_565 ?
C21 O7 Cu1 120.14(15) . 6 ?
C21 O8 Cu2B 136.52(19) . 6 ?
C4B N1 N2B 120.8(3) . . ?
N2A N1 C4A 117.4(3) . . ?
N2A N1 Cu1 116.2(2) . . ?
C4B N1 Cu1 125.9(3) . . ?
N2B N1 Cu1 113.2(2) . . ?
C4A N1 Cu1 126.4(2) . . ?
C3A C2 C1A 115.7(3) . . ?
C3B C2 C1B 112.9(3) . . ?
C3B C2 C11 125.5(3) . . ?
C3A C2 C11 123.5(3) . . ?
C1A C2 C11 120.4(3) . . ?
C1B C2 C11 121.6(3) . . ?
C8 N3 N4 116.5(2) . . ?
C5 N4 N3 120.6(2) . . ?
C5 N4 Cu1 118.6(2) . 3 ?
N3 N4 Cu1 120.73(18) . 3 ?
N4 C5 C6 124.9(3) . . ?
N4 C5 H5 117.6 . . ?
C6 C5 H5 117.6 . . ?
C7 C6 C5 114.6(3) . . ?
C7 C6 C9 126.7(2) . . ?
C5 C6 C9 118.7(3) . . ?
C6 C7 C8 117.7(3) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
N3 C8 C7 125.7(3) . . ?
N3 C8 H8 117.2 . . ?
C7 C8 H8 117.2 . . ?
C6 C9 C10 112.2(2) . . ?
C6 C9 C15 108.9(2) . . ?
C10 C9 C15 107.8(2) . . ?
C6 C9 C14 110.1(2) . . ?
C10 C9 C14 108.8(2) . . ?
C15 C9 C14 108.9(2) . . ?
C9 C10 C11 110.6(2) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C2 C11 C17 110.8(2) . . ?
C2 C11 C12 110.8(2) . . ?
C17 C11 C12 109.1(2) . . ?
C2 C11 C10 108.7(2) . . ?
C17 C11 C10 108.7(2) . . ?
C12 C11 C10 108.8(2) . . ?
C13 C12 C11 109.7(2) . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C12 109.2(2) . . ?
C14 C13 C18 109.9(2) . . ?
C12 C13 C18 110.1(2) . . ?
C14 C13 H13 109.2 . . ?
C12 C13 H13 109.2 . . ?
C18 C13 H13 109.2 . . ?
C13 C14 C9 110.5(2) . . ?
C13 C14 H14A 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C9 110.6(2) . . ?
C16 C15 H15A 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C9 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C15 C16 C18 110.1(2) . . ?
C15 C16 C17 109.1(3) . . ?
C18 C16 C17 109.5(2) . . ?
C15 C16 H16 109.4 . . ?
C18 C16 H16 109.4 . . ?
C17 C16 H16 109.4 . . ?
C11 C17 C16 110.2(2) . . ?
C11 C17 H17A 109.6 . . ?
C16 C17 H17A 109.6 . . ?
C11 C17 H17B 109.6 . . ?
C16 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C16 C18 C13 108.7(3) . . ?
C16 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 . . ?
C16 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O4 C19 O3 125.6(2) . . ?
O4 C19 C22 117.1(2) . . ?
O3 C19 C22 117.3(2) . . ?
O6 C20 O5 126.3(2) . . ?
O6 C20 C24 116.4(2) . . ?
O5 C20 C24 117.3(2) . . ?
O8 C21 O7 125.3(2) . . ?
O8 C21 C26 117.2(2) . . ?
O7 C21 C26 117.4(2) . . ?
C27 C22 C23 119.0(2) . . ?
C27 C22 C19 121.9(2) . . ?
C23 C22 C19 119.1(2) . . ?
C22 C23 C24 121.1(2) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 119.6(2) . . ?
C25 C24 C20 120.4(2) . . ?
C23 C24 C20 120.0(2) . . ?
C24 C25 C26 120.0(2) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C27 119.7(2) . . ?
C25 C26 C21 119.9(2) . . ?
C27 C26 C21 120.4(2) . . ?
C22 C27 C26 120.7(2) . . ?
C22 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Cu1 O1A Cu2A -49.1(2) . . . . ?
N4 Cu1 O1A Cu2A -141.57(18) 3_445 . . . ?
N1 Cu1 O1A Cu2A 41.32(18) . . . . ?
O7 Cu1 O1A Cu2A 126.98(15) 6_556 . . . ?
O5 Cu2A O1A Cu1 -151.67(19) 6_566 . . . ?
O4 Cu2A O1A Cu1 52.78(18) . . . . ?
N2A Cu2A O1A Cu1 -42.6(2) . . . . ?
O1A Cu2A N2A C1A -156.4(4) . . . . ?
O5 Cu2A N2A C1A -69.4(4) 6_566 . . . ?
O4 Cu2A N2A C1A 115.0(4) . . . . ?
O2A Cu2A N2A C1A 22.8(4) . . . . ?
O1A Cu2A N2A N1 31.1(3) . . . . ?
O5 Cu2A N2A N1 118.0(3) 6_566 . . . ?
O4 Cu2A N2A N1 -57.6(3) . . . . ?
O2A Cu2A N2A N1 -149.7(3) . . . . ?
N1 N2A C1A C2 -4.1(7) . . . . ?
Cu2A N2A C1A C2 -176.0(3) . . . . ?
C2 C3A C4A N1 7.8(7) . . . . ?
O6 Cu2B O1B Cu1 142.52(16) 6_566 . . . ?
O8 Cu2B O1B Cu1 -58.32(16) 6_556 . . . ?
N2B Cu2B O1B Cu1 38.30(17) . . . . ?
O1A Cu1 O1B Cu2B -125.6(3) . . . . ?
O3 Cu1 O1B Cu2B -135.00(15) . . . . ?
N4 Cu1 O1B Cu2B 136.26(17) 3_445 . . . ?
N1 Cu1 O1B Cu2B -38.39(16) . . . . ?
O7 Cu1 O1B Cu2B 47.05(17) 6_556 . . . ?
O1B Cu2B N2B C1B 156.6(4) . . . . ?
O6 Cu2B N2B C1B 68.6(4) 6_566 . . . ?
O8 Cu2B N2B C1B -111.6(4) 6_556 . . . ?
O2B Cu2B N2B C1B -22.3(4) . . . . ?
O1B Cu2B N2B N1 -29.6(3) . . . . ?
O6 Cu2B N2B N1 -117.6(3) 6_566 . . . ?
O8 Cu2B N2B N1 62.1(3) 6_556 . . . ?
O2B Cu2B N2B N1 151.5(3) . . . . ?
N1 N2B C1B C2 2.4(7) . . . . ?
Cu2B N2B C1B C2 176.0(3) . . . . ?
C2 C3B C4B N1 -6.1(7) . . . . ?
O1A Cu1 O3 C19 13.3(2) . . . . ?
O1B Cu1 O3 C19 18.7(3) . . . . ?
N4 Cu1 O3 C19 105.7(2) 3_445 . . . ?
N1 Cu1 O3 C19 -80.38(19) . . . . ?
O7 Cu1 O3 C19 -163.55(18) 6_556 . . . ?
O1A Cu2A O4 C19 -53.6(3) . . . . ?
O5 Cu2A O4 C19 -135.1(3) 6_566 . . . ?
O2A Cu2A O4 C19 125.8(3) . . . . ?
N2A Cu2A O4 C19 35.0(3) . . . . ?
C1A N2A N1 C4A -1.4(6) . . . . ?
Cu2A N2A N1 C4A 171.5(3) . . . . ?
C1A N2A N1 Cu1 179.1(3) . . . . ?
Cu2A N2A N1 Cu1 -7.9(3) . . . . ?
C3B C4B N1 N2B 0.8(6) . . . . ?
C3B C4B N1 Cu1 178.7(3) . . . . ?
C1B N2B N1 C4B 0.8(6) . . . . ?
Cu2B N2B N1 C4B -173.4(3) . . . . ?
C1B N2B N1 Cu1 -177.4(3) . . . . ?
Cu2B N2B N1 Cu1 8.4(3) . . . . ?
C3A C4A N1 N2A -0.6(6) . . . . ?
C3A C4A N1 Cu1 178.8(4) . . . . ?
O1A Cu1 N1 N2A -19.1(3) . . . . ?
O3 Cu1 N1 N2A 90.9(2) . . . . ?
O7 Cu1 N1 N2A -153.1(2) 6_556 . . . ?
O1B Cu1 N1 C4B -161.8(3) . . . . ?
O3 Cu1 N1 C4B -19.5(3) . . . . ?
O7 Cu1 N1 C4B 96.5(3) 6_556 . . . ?
O1B Cu1 N1 N2B 16.3(2) . . . . ?
O3 Cu1 N1 N2B 158.6(2) . . . . ?
O7 Cu1 N1 N2B -85.4(2) 6_556 . . . ?
O1A Cu1 N1 C4A 161.5(3) . . . . ?
O3 Cu1 N1 C4A -88.5(3) . . . . ?
O7 Cu1 N1 C4A 27.5(3) 6_556 . . . ?
C4B C3B C2 C1B 8.5(6) . . . . ?
C4B C3B C2 C11 -173.1(4) . . . . ?
C4A C3A C2 C1A -12.2(6) . . . . ?
C4A C3A C2 C11 174.9(4) . . . . ?
N2A C1A C2 C3A 11.1(6) . . . . ?
N2A C1A C2 C11 -175.7(4) . . . . ?
N2B C1B C2 C3B -7.0(6) . . . . ?
N2B C1B C2 C11 174.5(4) . . . . ?
C8 N3 N4 C5 -0.2(4) . . . . ?
C8 N3 N4 Cu1 -176.89(19) . . . 3 ?
N3 N4 C5 C6 2.8(4) . . . . ?
Cu1 N4 C5 C6 179.6(2) 3 . . . ?
N4 C5 C6 C7 -2.8(4) . . . . ?
N4 C5 C6 C9 179.2(3) . . . . ?
C5 C6 C7 C8 0.3(4) . . . . ?
C9 C6 C7 C8 178.2(3) . . . . ?
N4 N3 C8 C7 -2.4(4) . . . . ?
C6 C7 C8 N3 2.2(4) . . . . ?
C7 C6 C9 C10 8.3(4) . . . . ?
C5 C6 C9 C10 -174.0(2) . . . . ?
C7 C6 C9 C15 -111.0(3) . . . . ?
C5 C6 C9 C15 66.7(3) . . . . ?
C7 C6 C9 C14 129.6(3) . . . . ?
C5 C6 C9 C14 -52.7(3) . . . . ?
C6 C9 C10 C11 -179.7(2) . . . . ?
C15 C9 C10 C11 -59.8(3) . . . . ?
C14 C9 C10 C11 58.2(3) . . . . ?
C3B C2 C11 C17 179.1(3) . . . . ?
C3A C2 C11 C17 -119.7(4) . . . . ?
C1A C2 C11 C17 67.6(4) . . . . ?
C1B C2 C11 C17 -2.6(4) . . . . ?
C3B C2 C11 C12 -59.7(4) . . . . ?
C3A C2 C11 C12 1.4(4) . . . . ?
C1A C2 C11 C12 -171.2(3) . . . . ?
C1B C2 C11 C12 118.6(3) . . . . ?
C3B C2 C11 C10 59.8(4) . . . . ?
C3A C2 C11 C10 120.9(3) . . . . ?
C1A C2 C11 C10 -51.7(4) . . . . ?
C1B C2 C11 C10 -121.9(3) . . . . ?
C9 C10 C11 C2 -179.6(2) . . . . ?
C9 C10 C11 C17 59.7(3) . . . . ?
C9 C10 C11 C12 -58.9(3) . . . . ?
C2 C11 C12 C13 179.1(2) . . . . ?
C17 C11 C12 C13 -58.7(3) . . . . ?
C10 C11 C12 C13 59.7(3) . . . . ?
C11 C12 C13 C14 -61.1(3) . . . . ?
C11 C12 C13 C18 59.7(3) . . . . ?
C12 C13 C14 C9 60.9(3) . . . . ?
C18 C13 C14 C9 -60.0(3) . . . . ?
C6 C9 C14 C13 177.4(2) . . . . ?
C10 C9 C14 C13 -59.3(3) . . . . ?
C15 C9 C14 C13 58.0(3) . . . . ?
C6 C9 C15 C16 -177.7(2) . . . . ?
C10 C9 C15 C16 60.4(3) . . . . ?
C14 C9 C15 C16 -57.5(3) . . . . ?
C9 C15 C16 C18 59.5(3) . . . . ?
C9 C15 C16 C17 -60.7(3) . . . . ?
C2 C11 C17 C16 -178.3(2) . . . . ?
C12 C11 C17 C16 59.5(3) . . . . ?
C10 C11 C17 C16 -59.0(3) . . . . ?
C15 C16 C17 C11 59.9(3) . . . . ?
C18 C16 C17 C11 -60.7(3) . . . . ?
C15 C16 C18 C13 -59.8(3) . . . . ?
C17 C16 C18 C13 60.2(3) . . . . ?
C14 C13 C18 C16 60.2(3) . . . . ?
C12 C13 C18 C16 -60.1(3) . . . . ?
Cu2A O4 C19 O3 21.5(5) . . . . ?
Cu2A O4 C19 C22 -158.0(2) . . . . ?
Cu1 O3 C19 O4 4.5(4) . . . . ?
Cu1 O3 C19 C22 -175.97(17) . . . . ?
Cu2B O6 C20 O5 -3.5(6) 6_565 . . . ?
Cu2B O6 C20 C24 176.2(2) 6_565 . . . ?
Cu2A O5 C20 O6 7.5(5) 6_565 . . . ?
Cu2A O5 C20 C24 -172.2(2) 6_565 . . . ?
Cu2B O8 C21 O7 17.7(5) 6 . . . ?
Cu2B O8 C21 C26 -165.62(19) 6 . . . ?
Cu1 O7 C21 O8 10.0(4) 6 . . . ?
Cu1 O7 C21 C26 -166.64(15) 6 . . . ?
O4 C19 C22 C27 176.5(2) . . . . ?
O3 C19 C22 C27 -3.1(4) . . . . ?
O4 C19 C22 C23 -1.7(4) . . . . ?
O3 C19 C22 C23 178.7(2) . . . . ?
C27 C22 C23 C24 1.2(4) . . . . ?
C19 C22 C23 C24 179.4(2) . . . . ?
C22 C23 C24 C25 -0.7(4) . . . . ?
C22 C23 C24 C20 -179.8(2) . . . . ?
O6 C20 C24 C25 -176.5(3) . . . . ?
O5 C20 C24 C25 3.2(4) . . . . ?
O6 C20 C24 C23 2.5(4) . . . . ?
O5 C20 C24 C23 -177.7(3) . . . . ?
C23 C24 C25 C26 -0.1(4) . . . . ?
C20 C24 C25 C26 178.9(2) . . . . ?
C24 C25 C26 C27 0.5(4) . . . . ?
C24 C25 C26 C21 -180.0(2) . . . . ?
O8 C21 C26 C25 179.0(2) . . . . ?
O7 C21 C26 C25 -4.1(3) . . . . ?
O8 C21 C26 C27 -1.5(3) . . . . ?
O7 C21 C26 C27 175.4(2) . . . . ?
C23 C22 C27 C26 -0.8(4) . . . . ?
C19 C22 C27 C26 -179.0(2) . . . . ?
C25 C26 C27 C22 0.0(4) . . . . ?
C21 C26 C27 C22 -179.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.96
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.063



_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL ip1350 in C2/c
CELL  0.71073  24.8536  10.8716  18.6837   90.000  101.581   90.000
ZERR     8.00   0.0018   0.0007   0.0014    0.000    0.008    0.000
LATT   7
SYMM  - X,   Y, 1/2 - Z
SFAC  C    H    N    O    CU
UNIT  216   208   32   64   16
 
MERG   2
OMIT     4   4   4
OMIT     5   3   3
FMAP   2
PLAN   10
SIZE     0.15   0.21   0.24
RTAB O..O Cu1 Cu2A
RTAB O..O Cu1 Cu2B
 
EQIV $1 1-X, Y, 0.5-Z
EQIV $2 1-X, 1-Y, 1-Z
EQIV $3 1-X, -Y, 1-Z
EQIV $4 X, 1-Y, 0.5+Z
 
RTAB H..O H1WA O5_$1
RTAB H..O H2WA O4_$2
RTAB H..O H1WB O8_$3
RTAB H..O H2WB O6_$2
RTAB H..O H1OA O6_$4
RTAB H..O H1OB O5_$4
 
RTAB O..O O2A O5_$1
RTAB O..O O2A O4_$2
RTAB O..O O2B O8_$3
RTAB O..O O2B O6_$2
RTAB O..O O1A O6_$4
RTAB O..O O1B O5_$4
 
RTAB XHY O2A H1WA O5_$1
RTAB XHY O2A H2WA O4_$2
RTAB XHY O2B H1WB O8_$3
RTAB XHY O2B H2WB O6_$2
RTAB XHY O1A H1OA O6_$4
RTAB XHY O1B H1OB O5_$4
 
ACTA
BOND   $H
CONF
LIST   4
L.S.   4
TEMP   -60.00
WGHT    0.055200
FVAR       1.00555
CU1   5    0.409935    0.158208    0.528689    11.00000    0.02323    0.03347 =
         0.05020   -0.01578    0.01308   -0.00964
PART   -1
CU2A  5    0.442336    0.428900    0.515255    10.50000    0.02866    0.01752 =
         0.02360   -0.00083    0.00665   -0.00025
O1A   4    0.392570    0.320470    0.549065    10.50000    0.02412    0.02385 =
         0.03729   -0.00159    0.00871    0.00321
AFIX   3
H1OA  2    0.395540    0.329280    0.594895    10.50000   -1.50000
AFIX   0
O2A   4    0.495291    0.541920    0.481745    10.50000    0.04094    0.02161 =
         0.02847   -0.00335    0.01028   -0.00665
AFIX   3
H1WA  2    0.517401    0.510080    0.457705    10.50000   -1.50000
H2WA  2    0.513971    0.577100    0.519275    10.50000   -1.50000
AFIX   0
N2A   3    0.509667    0.301097    0.560107    10.50000    0.02714    0.02241 =
         0.02886    0.00424    0.00825   -0.00089
C1A   1    0.561922    0.329178    0.579298    10.50000    0.02060    0.02606 =
         0.03414    0.00182    0.00582   -0.00671
AFIX  43
H1A   2    0.571907    0.412195    0.576624    10.50000   -1.20000
AFIX   0
C3A   1    0.588401    0.123081    0.594024    10.50000    0.02514    0.02449 =
         0.03513    0.00160    0.00989    0.00419
AFIX  43
H3A   2    0.614828    0.060080    0.599919    10.50000   -1.20000
AFIX   0
C4A   1    0.532446    0.097355    0.575633    10.50000    0.02394    0.02129 =
         0.03789    0.00071    0.01019   -0.00046
AFIX  43
H4A   2    0.521181    0.014762    0.575083    10.50000   -1.20000
AFIX   0
PART   -2
CU2B  5    0.440741    0.265164    0.687006    10.50000    0.03014    0.01456 =
         0.02293   -0.00050    0.00747   -0.00072
O1B   4    0.389747    0.271857    0.596879    10.50000    0.02374    0.02006 =
         0.02955    0.00135    0.00234    0.00174
AFIX   3
H1OB  2    0.389287    0.344247    0.579569    10.50000   -1.50000
AFIX   0
O2B   4    0.492397    0.262054    0.780673    10.50000    0.04407    0.01860 =
         0.02637   -0.00180    0.00273    0.00173
AFIX   3
H1WB  2    0.513737    0.200733    0.781583    10.50000   -1.50000
H2WB  2    0.511727    0.324954    0.795593    10.50000   -1.50000
AFIX   0
N2B   3    0.507992    0.242064    0.622504    10.50000    0.02460    0.02868 =
         0.02165   -0.00029    0.00735   -0.00254
C1B   1    0.560141    0.269390    0.646255    10.50000    0.02478    0.03270 =
         0.02264   -0.00614    0.00839   -0.00411
AFIX  43
H1B   2    0.570590    0.306041    0.692531    10.50000   -1.20000
AFIX   0
C3B   1    0.584997    0.181947    0.543612    10.50000    0.02178    0.02574 =
         0.02914   -0.00513    0.00903   -0.00173
AFIX  43
H3B   2    0.610272    0.152599    0.516380    10.50000   -1.20000
AFIX   0
C4B   1    0.529763    0.157026    0.519264    10.50000    0.03021    0.02198 =
         0.02286   -0.00296    0.00784   -0.00474
AFIX  43
H4B   2    0.518165    0.118406    0.473766    10.50000   -1.20000
AFIX   0
PART    0
O3    4    0.417973    0.143487    0.422395    11.00000    0.03498    0.05963 =
         0.02207    0.00691    0.00674    0.00034
O4    4    0.423312    0.348377    0.418161    11.00000    0.06138    0.06349 =
         0.02991   -0.02143    0.00224    0.01035
O5    4    0.431716    0.457360    0.091617    11.00000    0.08550    0.05485 =
         0.03328    0.01901   -0.00159   -0.03278
O6    4    0.433370    0.559273    0.195182    11.00000    0.06244    0.01707 =
         0.08931   -0.00336    0.03028   -0.00555
O7    4    0.426823    0.006791    0.093484    11.00000    0.03117    0.02530 =
         0.04377   -0.01547    0.01043   -0.00086
O8    4    0.427050   -0.092173    0.198453    11.00000    0.05271    0.01649 =
         0.06765    0.00313    0.01184    0.00479
N1    3    0.493111    0.186160    0.558349    11.00000    0.02452    0.02238 =
         0.02444    0.00181    0.00677   -0.00498
C2    1    0.603291    0.244906    0.603190    11.00000    0.02205    0.02497 =
         0.03336    0.00176    0.00313   -0.00022
N3    3    0.796327    0.656454    0.442482    11.00000    0.03643    0.04011 =
         0.04744   -0.00327    0.01155   -0.00699
N4    3    0.828795    0.611138    0.502338    11.00000    0.03020    0.03945 =
         0.04813   -0.00924    0.00948   -0.00848
C5    1    0.808505    0.539639    0.547561    11.00000    0.02716    0.04890 =
         0.04411   -0.00112    0.00260   -0.00797
AFIX  43
H5    2    0.832598    0.512929    0.590104    11.00000   -1.20000
AFIX   0
C6    1    0.753920    0.500738    0.536904    11.00000    0.02242    0.03329 =
         0.03972   -0.00602    0.00458   -0.00353
C7    1    0.720344    0.547588    0.475315    11.00000    0.02308    0.03796 =
         0.04429   -0.00335    0.00486   -0.00081
AFIX  43
H7    2    0.682841    0.527314    0.463406    11.00000   -1.20000
AFIX   0
C8    1    0.743620    0.625355    0.431637    11.00000    0.03429    0.04297 =
         0.04543    0.00158    0.00600   -0.00166
AFIX  43
H8    2    0.720134    0.659265    0.390650    11.00000   -1.20000
AFIX   0
C9    1    0.736984    0.417078    0.593479    11.00000    0.02138    0.03279 =
         0.03778   -0.00205    0.00209   -0.00053
C10   1    0.677640    0.372020    0.569905    11.00000    0.02230    0.02929 =
         0.03796    0.00005    0.00105    0.00050
AFIX  23
H10A  2    0.673695    0.326668    0.523814    11.00000   -1.20000
H10B  2    0.652769    0.442849    0.561774    11.00000   -1.20000
AFIX   0
C11   1    0.661804    0.287539    0.629065    11.00000    0.02037    0.02601 =
         0.03850   -0.00117    0.00118   -0.00012
C12   1    0.701357    0.177338    0.641379    11.00000    0.03077    0.02937 =
         0.04648    0.00099   -0.00097    0.00302
AFIX  23
H12A  2    0.691699    0.122750    0.678598    11.00000   -1.20000
H12B  2    0.698220    0.130524    0.595904    11.00000   -1.20000
AFIX   0
C13   1    0.760422    0.223284    0.666331    11.00000    0.02789    0.03812 =
         0.05229    0.00175   -0.00193    0.00777
AFIX  13
H13   2    0.785618    0.151853    0.674484    11.00000   -1.20000
AFIX   0
C14   1    0.775392    0.304533    0.607335    11.00000    0.02160    0.04701 =
         0.04332   -0.00509    0.00167    0.00290
AFIX  23
H14A  2    0.772400    0.257216    0.562062    11.00000   -1.20000
H14B  2    0.813510    0.332244    0.622395    11.00000   -1.20000
AFIX   0
C15   1    0.741215    0.488662    0.665218    11.00000    0.02837    0.03616 =
         0.04427   -0.00617    0.00482   -0.00521
AFIX  23
H15A  2    0.778677    0.520083    0.681033    11.00000   -1.20000
H15B  2    0.716117    0.559104    0.657298    11.00000   -1.20000
AFIX   0
C16   1    0.726771    0.406105    0.724510    11.00000    0.03373    0.05144 =
         0.03478   -0.00989    0.00227   -0.00534
AFIX  13
H16   2    0.729936    0.453721    0.770333    11.00000   -1.20000
AFIX   0
C17   1    0.667726    0.360383    0.700234    11.00000    0.03119    0.04242 =
         0.04035   -0.00615    0.00764   -0.00418
AFIX  23
H17A  2    0.657998    0.307902    0.738354    11.00000   -1.20000
H17B  2    0.642543    0.430696    0.692939    11.00000   -1.20000
AFIX   0
C18   1    0.765801    0.296105    0.737764    11.00000    0.03408    0.05823 =
         0.04054    0.00818   -0.00680   -0.00665
AFIX  23
H18A  2    0.756507    0.243369    0.776060    11.00000   -1.20000
H18B  2    0.803696    0.324705    0.753853    11.00000   -1.20000
AFIX   0
C19   1    0.421282    0.243977    0.389742    11.00000    0.02617    0.04982 =
         0.02036    0.00000    0.00227    0.00221
C20   1    0.431342    0.463729    0.158312    11.00000    0.02898    0.02023 =
         0.04089    0.00688    0.00320   -0.00378
C21   1    0.427915    0.003483    0.161487    11.00000    0.02102    0.02059 =
         0.03652   -0.00608    0.00555    0.00250
C22   1    0.423406    0.237743    0.309821    11.00000    0.01890    0.03206 =
         0.02127    0.00027    0.00084   -0.00182
C23   1    0.425928    0.346134    0.271709    11.00000    0.02458    0.01924 =
         0.02842   -0.00651    0.00331    0.00009
AFIX  43
H23   2    0.425949    0.421824    0.296035    11.00000   -1.20000
AFIX   0
C24   1    0.428418    0.344808    0.198328    11.00000    0.02147    0.01715 =
         0.02706    0.00044    0.00400   -0.00092
C25   1    0.429025    0.233480    0.162586    11.00000    0.02222    0.02103 =
         0.02114   -0.00092    0.00554   -0.00173
AFIX  43
H25   2    0.430651    0.231979    0.112761    11.00000   -1.20000
AFIX   0
C26   1    0.427233    0.124004    0.200300    11.00000    0.01564    0.01711 =
         0.02764    0.00029    0.00175    0.00119
C27   1    0.424407    0.126995    0.273870    11.00000    0.02052    0.02095 =
         0.02647    0.00550    0.00175   -0.00133
AFIX  43
H27   2    0.423165    0.052879    0.299398    11.00000   -1.20000
HKLF    4
 
REM  ip1350 in C2/c
REM R1 =  0.0335 for   3592 Fo > 4sig(Fo)  and  0.0465 for all   4789 data
REM    433 parameters refined using      0 restraints
 
END
 
WGHT      0.0552      0.0000
REM Highest difference peak  0.443,  deepest hole -0.784,  1-sigma level  0.063
Q1    1   0.3911  0.2077  0.5112  11.00000  0.05    0.44
Q2    1   0.4186 -0.0413  0.0766  11.00000  0.05    0.32
Q3    1   0.4262  0.2958  0.4269  11.00000  0.05    0.30
Q4    1   0.4394  0.5808  0.2122  11.00000  0.05    0.30
Q5    1   0.4366  0.3940  0.1859  11.00000  0.05    0.29
Q6    1   0.8099  0.6484  0.3771  11.00000  0.05    0.28
Q7    1   0.4211 -0.0827  0.1632  11.00000  0.05    0.27
Q8    1   0.7532  0.6477  0.3356  11.00000  0.05    0.27
Q9    1   0.6804  0.2418  0.6346  11.00000  0.05    0.26
Q10   1   0.7131  0.6413  0.3640  11.00000  0.05    0.26
;
_database_code_depnum_ccdc_archive 'CCDC 967343'
#######################################################################
#
#                 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_(2)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Poly[bis-[μ₃-[1,3-bis(pyridazin-4-yl)adamantane-κ⁴N1:N2:N3)]]-
bis[μ₃-(1,3,5-adamantanetricarboxylato)]-di(μ₃-hydroxido)-
diaquatetracopper(II)] monohydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H76 Cu4 N8 O18, H2 O'
_chemical_formula_sum            'C62 H78 Cu4 N8 O19'
_chemical_formula_weight         1493.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_space_group_name_Hall           '-P 1'
_symmetry_Int_Tables_number      2


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

_cell_length_a                   11.1208(9)
_cell_length_b                   11.5078(10)
_cell_length_c                   13.8841(13)
_cell_angle_alpha                83.981(6)
_cell_angle_beta                 67.507(6)
_cell_angle_gamma                62.065(5)
_cell_volume                     1444.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    15505
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      26.94

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             774
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7379
_exptl_absorpt_correction_T_max  0.9409
_exptl_absorpt_process_details   'face indexed (SADABS; Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(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 APEX2 area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15505
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.1269
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         26.94
_reflns_number_total             6248
_reflns_number_gt                3870
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 The CH-hydrogen atoms were added geometrically, with Uiso = 1.2Ueq(C) 
 and OH-hydrogen atoms were located and included with fixed d(O-H) = 0.85 A 
 and Uiso = 1.5Ueq(O). 

 The refinement was essentially standard. The solvate water molecule (O3W) 
 is equally disordered over two closely separated positions related by 
 inversion [i.e. O3W...O3W (1-x, 1-y, 1-z) = 1.36 A]. The O3W atom was 
 refined with 0.5 occupancy factor and it was left isotropic due to the 
 relatively high value of Uiso = 0.244(9) A². The hydrogen atoms were 
 not added to this disordered water molecule. 
;

_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)+(0.0278P)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_number_reflns         6248
_refine_ls_number_parameters     419
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_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 0.31127(5) 0.93994(5) 0.32959(4) 0.01933(14) Uani 1 1 d . . .
Cu2 Cu 0.07996(5) 0.84025(5) 0.48897(4) 0.01976(14) Uani 1 1 d . . .
O1 O 0.1110(3) 0.9677(2) 0.3899(2) 0.0172(6) Uani 1 1 d . . .
H1O H 0.1000 0.9400 0.3416 0.026 Uiso 1 1 d R . .
O2 O 0.5233(3) 0.8747(3) 0.2809(2) 0.0239(7) Uani 1 1 d . . .
O3 O 0.5766(4) 0.7028(3) 0.1868(3) 0.0554(12) Uani 1 1 d . . .
O4 O 0.7588(4) 0.4593(3) 0.5238(3) 0.0558(11) Uani 1 1 d . . .
O5 O 0.9411(3) 0.2879(3) 0.4107(2) 0.0276(7) Uani 1 1 d . . .
O6 O 0.9582(3) 0.8049(3) 0.4384(2) 0.0231(7) Uani 1 1 d . . .
O7 O 1.0086(3) 0.8714(3) 0.2782(2) 0.0338(8) Uani 1 1 d . . .
N1 N 0.3172(3) 0.8923(3) 0.4761(3) 0.0145(7) Uani 1 1 d . . .
N2 N 0.2207(3) 0.8536(3) 0.5398(3) 0.0159(7) Uani 1 1 d . . .
N3 N 0.2998(4) 1.1092(3) 1.1584(3) 0.0232(8) Uani 1 1 d . . .
N4 N 0.3052(3) 0.9921(3) 1.1869(3) 0.0194(8) Uani 1 1 d . . .
C1 C 0.4087(4) 0.9015(4) 0.5090(3) 0.0235(10) Uani 1 1 d . . .
H1 H 0.4740 0.9303 0.4637 0.028 Uiso 1 1 calc R . .
C2 C 0.4141(5) 0.8711(4) 0.6063(3) 0.0227(9) Uani 1 1 d . . .
H2 H 0.4819 0.8784 0.6255 0.027 Uiso 1 1 calc R . .
C3 C 0.3172(4) 0.8298(4) 0.6746(3) 0.0173(9) Uani 1 1 d . . .
C4 C 0.2206(4) 0.8249(3) 0.6347(3) 0.0205(9) Uani 1 1 d . . .
H4 H 0.1513 0.7994 0.6785 0.025 Uiso 1 1 calc R . .
C5 C 0.3008(5) 1.1398(4) 1.0646(3) 0.0291(11) Uani 1 1 d . . .
H5 H 0.2953 1.2215 1.0455 0.035 Uiso 1 1 calc R . .
C6 C 0.3096(5) 1.0590(4) 0.9908(4) 0.0278(10) Uani 1 1 d . . .
H6 H 0.3123 1.0851 0.9246 0.033 Uiso 1 1 calc R . .
C7 C 0.3140(4) 0.9397(4) 1.0199(3) 0.0161(9) Uani 1 1 d . . .
C8 C 0.3108(4) 0.9130(4) 1.1211(3) 0.0240(10) Uani 1 1 d . . .
H8 H 0.3126 0.8334 1.1439 0.029 Uiso 1 1 calc R . .
C9 C 0.3171(4) 0.7863(4) 0.7811(3) 0.0176(9) Uani 1 1 d . . .
C10 C 0.3128(4) 0.8889(4) 0.8455(3) 0.0175(9) Uani 1 1 d . . .
H10A H 0.2231 0.9709 0.8565 0.021 Uiso 1 1 calc R . .
H10B H 0.3954 0.9060 0.8070 0.021 Uiso 1 1 calc R . .
C11 C 0.3190(4) 0.8420(3) 0.9516(3) 0.0157(9) Uani 1 1 d . . .
C12 C 0.4632(4) 0.7097(4) 0.9311(4) 0.0261(10) Uani 1 1 d . . .
H12A H 0.5475 0.7240 0.8916 0.031 Uiso 1 1 calc R . .
H12B H 0.4702 0.6780 0.9972 0.031 Uiso 1 1 calc R . .
C13 C 0.4641(5) 0.6063(4) 0.8697(4) 0.0306(11) Uani 1 1 d . . .
H13 H 0.5544 0.5231 0.8587 0.037 Uiso 1 1 calc R . .
C14 C 0.4609(4) 0.6546(4) 0.7636(3) 0.0273(10) Uani 1 1 d . . .
H14A H 0.4646 0.5887 0.7228 0.033 Uiso 1 1 calc R . .
H14B H 0.5459 0.6686 0.7253 0.033 Uiso 1 1 calc R . .
C15 C 0.1851(4) 0.7604(4) 0.8429(3) 0.0233(10) Uani 1 1 d . . .
H15A H 0.0941 0.8412 0.8542 0.028 Uiso 1 1 calc R . .
H15B H 0.1869 0.6948 0.8031 0.028 Uiso 1 1 calc R . .
C16 C 0.1917(5) 0.7115(4) 0.9478(4) 0.0279(11) Uani 1 1 d . . .
H16 H 0.1066 0.6964 0.9867 0.033 Uiso 1 1 calc R . .
C17 C 0.1865(4) 0.8171(4) 1.0107(3) 0.0237(10) Uani 1 1 d . . .
H17A H 0.0961 0.8985 1.0219 0.028 Uiso 1 1 calc R . .
H17B H 0.1876 0.7877 1.0786 0.028 Uiso 1 1 calc R . .
C18 C 0.3313(5) 0.5837(4) 0.9321(4) 0.0336(12) Uani 1 1 d . . .
H18A H 0.3332 0.5160 0.8946 0.040 Uiso 1 1 calc R . .
H18B H 0.3346 0.5541 0.9995 0.040 Uiso 1 1 calc R . .
C19 C 0.6115(5) 0.7561(4) 0.2355(4) 0.0242(10) Uani 1 1 d . . .
C20 C 0.8576(5) 0.4123(4) 0.4370(4) 0.0272(11) Uani 1 1 d . . .
C21 C 0.9717(4) 0.7993(4) 0.3432(3) 0.0185(9) Uani 1 1 d . . .
C22 C 0.7576(4) 0.6832(3) 0.2493(3) 0.0172(9) Uani 1 1 d . . .
C23 C 0.7396(4) 0.5861(3) 0.3338(3) 0.0202(9) Uani 1 1 d . . .
H23A H 0.6605 0.6357 0.3986 0.024 Uiso 1 1 calc R . .
H23B H 0.7137 0.5273 0.3109 0.024 Uiso 1 1 calc R . .
C24 C 0.8840(4) 0.5037(3) 0.3533(3) 0.0176(9) Uani 1 1 d . . .
C25 C 0.9187(4) 0.6009(4) 0.3923(3) 0.0223(10) Uani 1 1 d . . .
H25A H 0.8393 0.6495 0.4573 0.027 Uiso 1 1 calc R . .
H25B H 1.0082 0.5519 0.4059 0.027 Uiso 1 1 calc R . .
C26 C 0.9378(4) 0.6985(4) 0.3104(3) 0.0191(9) Uani 1 1 d . . .
C27 C 0.7954(4) 0.7760(3) 0.2901(3) 0.0187(9) Uani 1 1 d . . .
H27A H 0.8063 0.8384 0.2392 0.022 Uiso 1 1 calc R . .
H27B H 0.7153 0.8257 0.3546 0.022 Uiso 1 1 calc R . .
C28 C 0.8829(4) 0.6037(4) 0.1480(3) 0.0249(10) Uani 1 1 d . . .
H28A H 0.8601 0.5432 0.1237 0.030 Uiso 1 1 calc R . .
H28B H 0.8952 0.6627 0.0942 0.030 Uiso 1 1 calc R . .
C29 C 1.0243(4) 0.5264(4) 0.1687(3) 0.0207(9) Uani 1 1 d . . .
H29 H 1.1050 0.4772 0.1031 0.025 Uiso 1 1 calc R . .
C30 C 1.0093(4) 0.4288(4) 0.2495(4) 0.0267(11) Uani 1 1 d . . .
H30A H 1.1008 0.3787 0.2604 0.032 Uiso 1 1 calc R . .
H30B H 0.9886 0.3673 0.2243 0.032 Uiso 1 1 calc R . .
C31 C 1.0628(4) 0.6185(4) 0.2090(3) 0.0220(10) Uani 1 1 d . . .
H31A H 1.1528 0.5667 0.2216 0.026 Uiso 1 1 calc R . .
H31B H 1.0790 0.6780 0.1566 0.026 Uiso 1 1 calc R . .
O1W O 0.2768(3) 1.1495(3) 0.3718(2) 0.0302(8) Uani 1 1 d . . .
H1W H 0.2709 1.1873 0.3166 0.045 Uiso 1 1 d R . .
H2W H 0.2027 1.1994 0.4241 0.045 Uiso 1 1 d R . .
O2W O 0.3185(4) 0.6818(3) 0.3117(3) 0.0615(12) Uani 1 1 d . . .
H3W H 0.4029 0.6776 0.2928 0.092 Uiso 1 1 d R . .
H4W H 0.3243 0.6081 0.3333 0.092 Uiso 1 1 d R . .
O3W O 0.464(2) 0.5628(16) 0.5225(17) 0.244(9) Uiso 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.931(2) . ?
Cu1 O2 1.952(3) . ?
Cu1 N4 2.026(3) 1_554 ?
Cu1 N1 2.068(3) . ?
Cu1 O1W 2.359(3) . ?
Cu2 O6 1.948(3) 1_455 ?
Cu2 O5 1.953(3) 2_666 ?
Cu2 O1 1.962(2) . ?
Cu2 N2 2.016(3) . ?
Cu2 O1 2.423(2) 2_576 ?
O1 Cu2 2.423(2) 2_576 ?
O1 H1O 0.8419 . ?
O2 C19 1.294(5) . ?
O3 C19 1.222(5) . ?
O4 C20 1.232(5) . ?
O5 C20 1.284(5) . ?
O5 Cu2 1.953(3) 2_666 ?
O6 C21 1.277(5) . ?
O6 Cu2 1.948(3) 1_655 ?
O7 C21 1.246(4) . ?
N1 C1 1.312(5) . ?
N1 N2 1.330(4) . ?
N2 C4 1.325(5) . ?
N3 C5 1.310(5) . ?
N3 N4 1.344(4) . ?
N4 C8 1.322(5) . ?
C1 C2 1.377(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.407(5) . ?
C3 C9 1.510(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.401(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.373(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.396(5) . ?
C7 C11 1.513(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.527(5) . ?
C9 C15 1.541(5) . ?
C9 C14 1.556(5) . ?
C10 C11 1.531(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C17 1.533(5) . ?
C11 C12 1.558(5) . ?
C12 C13 1.528(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.527(6) . ?
C13 C18 1.527(6) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.521(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C18 1.513(6) . ?
C16 C17 1.537(5) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C22 1.519(5) . ?
C20 C24 1.521(5) . ?
C21 C26 1.531(5) . ?
C22 C28 1.528(6) . ?
C22 C27 1.539(5) . ?
C22 C23 1.556(5) . ?
C23 C24 1.550(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C30 1.537(5) . ?
C24 C25 1.544(5) . ?
C25 C26 1.540(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C31 1.529(5) . ?
C26 C27 1.533(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.526(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.522(5) . ?
C29 C31 1.534(5) . ?
C29 H29 0.9800 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
O1W H1W 0.8500 . ?
O1W H2W 0.8500 . ?
O2W H3W 0.8499 . ?
O2W H4W 0.8500 . ?

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 O2 167.55(11) . . ?
O1 Cu1 N4 94.38(12) . 1_554 ?
O2 Cu1 N4 93.50(12) . 1_554 ?
O1 Cu1 N1 86.13(12) . . ?
O2 Cu1 N1 86.29(12) . . ?
N4 Cu1 N1 178.20(13) 1_554 . ?
O1 Cu1 O1W 100.77(10) . . ?
O2 Cu1 O1W 88.75(10) . . ?
N4 Cu1 O1W 90.72(12) 1_554 . ?
N1 Cu1 O1W 87.49(11) . . ?
O6 Cu2 O5 85.36(12) 1_455 2_666 ?
O6 Cu2 O1 97.84(11) 1_455 . ?
O5 Cu2 O1 176.64(12) 2_666 . ?
O6 Cu2 N2 173.27(12) 1_455 . ?
O5 Cu2 N2 90.36(12) 2_666 . ?
O1 Cu2 N2 86.36(12) . . ?
O6 Cu2 O1 99.00(10) 1_455 2_576 ?
O5 Cu2 O1 95.01(11) 2_666 2_576 ?
O1 Cu2 O1 85.52(10) . 2_576 ?
N2 Cu2 O1 86.53(11) . 2_576 ?
Cu1 O1 Cu2 114.38(12) . . ?
Cu1 O1 Cu2 120.24(12) . 2_576 ?
Cu2 O1 Cu2 94.48(10) . 2_576 ?
Cu1 O1 H1O 104.5 . . ?
Cu2 O1 H1O 96.8 . . ?
Cu2 O1 H1O 123.5 2_576 . ?
C19 O2 Cu1 119.2(3) . . ?
C20 O5 Cu2 120.6(3) . 2_666 ?
C21 O6 Cu2 126.3(2) . 1_655 ?
C1 N1 N2 119.3(3) . . ?
C1 N1 Cu1 123.1(3) . . ?
N2 N1 Cu1 117.6(2) . . ?
C4 N2 N1 118.7(3) . . ?
C4 N2 Cu2 122.1(3) . . ?
N1 N2 Cu2 119.2(3) . . ?
C5 N3 N4 117.5(4) . . ?
C8 N4 N3 119.9(4) . . ?
C8 N4 Cu1 121.9(3) . 1_556 ?
N3 N4 Cu1 118.2(3) . 1_556 ?
N1 C1 C2 124.1(4) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 114.1(4) . . ?
C2 C3 C9 123.9(4) . . ?
C4 C3 C9 122.0(4) . . ?
N2 C4 C3 125.1(4) . . ?
N2 C4 H4 117.4 . . ?
C3 C4 H4 117.4 . . ?
N3 C5 C6 125.1(4) . . ?
N3 C5 H5 117.4 . . ?
C6 C5 H5 117.4 . . ?
C7 C6 C5 117.5(4) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
C6 C7 C8 115.0(4) . . ?
C6 C7 C11 124.6(4) . . ?
C8 C7 C11 120.4(3) . . ?
N4 C8 C7 125.0(4) . . ?
N4 C8 H8 117.5 . . ?
C7 C8 H8 117.5 . . ?
C3 C9 C10 111.7(3) . . ?
C3 C9 C15 111.2(3) . . ?
C10 C9 C15 108.8(3) . . ?
C3 C9 C14 107.5(3) . . ?
C10 C9 C14 109.3(3) . . ?
C15 C9 C14 108.3(3) . . ?
C9 C10 C11 111.5(3) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C7 C11 C10 114.3(3) . . ?
C7 C11 C17 108.0(3) . . ?
C10 C11 C17 108.0(3) . . ?
C7 C11 C12 109.5(3) . . ?
C10 C11 C12 107.9(3) . . ?
C17 C11 C12 109.1(3) . . ?
C13 C12 C11 110.1(3) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C14 C13 C18 111.1(4) . . ?
C14 C13 C12 108.9(4) . . ?
C18 C13 C12 109.5(4) . . ?
C14 C13 H13 109.1 . . ?
C18 C13 H13 109.1 . . ?
C12 C13 H13 109.1 . . ?
C13 C14 C9 109.1(3) . . ?
C13 C14 H14A 109.9 . . ?
C9 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
C9 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
C16 C15 C9 109.9(3) . . ?
C16 C15 H15A 109.7 . . ?
C9 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
C9 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C18 C16 C15 110.6(4) . . ?
C18 C16 C17 109.6(4) . . ?
C15 C16 C17 109.2(3) . . ?
C18 C16 H16 109.1 . . ?
C15 C16 H16 109.1 . . ?
C17 C16 H16 109.1 . . ?
C11 C17 C16 110.1(3) . . ?
C11 C17 H17A 109.6 . . ?
C16 C17 H17A 109.6 . . ?
C11 C17 H17B 109.6 . . ?
C16 C17 H17B 109.6 . . ?
H17A C17 H17B 108.2 . . ?
C16 C18 C13 109.3(3) . . ?
C16 C18 H18A 109.8 . . ?
C13 C18 H18A 109.8 . . ?
C16 C18 H18B 109.8 . . ?
C13 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?
O3 C19 O2 121.5(4) . . ?
O3 C19 C22 121.2(4) . . ?
O2 C19 C22 117.2(4) . . ?
O4 C20 O5 123.9(4) . . ?
O4 C20 C24 119.7(4) . . ?
O5 C20 C24 116.4(4) . . ?
O7 C21 O6 123.5(4) . . ?
O7 C21 C26 119.8(4) . . ?
O6 C21 C26 116.7(3) . . ?
C19 C22 C28 111.5(4) . . ?
C19 C22 C27 112.6(3) . . ?
C28 C22 C27 110.1(3) . . ?
C19 C22 C23 106.1(3) . . ?
C28 C22 C23 108.8(3) . . ?
C27 C22 C23 107.5(3) . . ?
C24 C23 C22 110.8(3) . . ?
C24 C23 H23A 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C20 C24 C30 112.9(3) . . ?
C20 C24 C25 110.4(4) . . ?
C30 C24 C25 109.0(3) . . ?
C20 C24 C23 107.8(3) . . ?
C30 C24 C23 109.0(3) . . ?
C25 C24 C23 107.6(3) . . ?
C26 C25 C24 110.8(3) . . ?
C26 C25 H25A 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C31 C26 C21 109.2(3) . . ?
C31 C26 C27 109.0(4) . . ?
C21 C26 C27 107.4(3) . . ?
C31 C26 C25 108.0(3) . . ?
C21 C26 C25 114.2(4) . . ?
C27 C26 C25 109.0(3) . . ?
C26 C27 C22 111.3(3) . . ?
C26 C27 H27A 109.4 . . ?
C22 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C22 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C29 C28 C22 109.0(3) . . ?
C29 C28 H28A 109.9 . . ?
C22 C28 H28A 109.9 . . ?
C29 C28 H28B 109.9 . . ?
C22 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
C30 C29 C28 110.7(3) . . ?
C30 C29 C31 108.3(3) . . ?
C28 C29 C31 111.5(3) . . ?
C30 C29 H29 108.8 . . ?
C28 C29 H29 108.8 . . ?
C31 C29 H29 108.8 . . ?
C29 C30 C24 109.7(3) . . ?
C29 C30 H30A 109.7 . . ?
C24 C30 H30A 109.7 . . ?
C29 C30 H30B 109.7 . . ?
C24 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
C26 C31 C29 110.1(3) . . ?
C26 C31 H31A 109.6 . . ?
C29 C31 H31A 109.6 . . ?
C26 C31 H31B 109.6 . . ?
C29 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
Cu1 O1W H1W 101.5 . . ?
Cu1 O1W H2W 120.5 . . ?
H1W O1W H2W 108.4 . . ?
H3W O2W H4W 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu1 O1 Cu2 14.1(6) . . . . ?
N4 Cu1 O1 Cu2 143.20(15) 1_554 . . . ?
N1 Cu1 O1 Cu2 -38.53(14) . . . . ?
O1W Cu1 O1 Cu2 -125.23(14) . . . . ?
O2 Cu1 O1 Cu2 125.4(5) . . . 2_576 ?
N4 Cu1 O1 Cu2 -105.47(15) 1_554 . . 2_576 ?
N1 Cu1 O1 Cu2 72.80(14) . . . 2_576 ?
O1W Cu1 O1 Cu2 -13.90(16) . . . 2_576 ?
O6 Cu2 O1 Cu1 -135.34(14) 1_455 . . . ?
N2 Cu2 O1 Cu1 39.37(14) . . . . ?
O1 Cu2 O1 Cu1 126.17(17) 2_576 . . . ?
O6 Cu2 O1 Cu2 98.48(11) 1_455 . . 2_576 ?
N2 Cu2 O1 Cu2 -86.80(11) . . . 2_576 ?
O1 Cu2 O1 Cu2 0.0 2_576 . . 2_576 ?
O1 Cu1 O2 C19 46.2(7) . . . . ?
N4 Cu1 O2 C19 -83.0(3) 1_554 . . . ?
N1 Cu1 O2 C19 98.8(3) . . . . ?
O1W Cu1 O2 C19 -173.6(3) . . . . ?
O1 Cu1 N1 C1 -156.4(3) . . . . ?
O2 Cu1 N1 C1 33.5(3) . . . . ?
O1W Cu1 N1 C1 -55.4(3) . . . . ?
O1 Cu1 N1 N2 22.0(2) . . . . ?
O2 Cu1 N1 N2 -148.1(2) . . . . ?
O1W Cu1 N1 N2 123.0(2) . . . . ?
C1 N1 N2 C4 -0.3(5) . . . . ?
Cu1 N1 N2 C4 -178.8(2) . . . . ?
C1 N1 N2 Cu2 179.8(3) . . . . ?
Cu1 N1 N2 Cu2 1.3(3) . . . . ?
O5 Cu2 N2 C4 -24.1(3) 2_666 . . . ?
O1 Cu2 N2 C4 156.6(3) . . . . ?
O1 Cu2 N2 C4 70.9(3) 2_576 . . . ?
O5 Cu2 N2 N1 155.7(3) 2_666 . . . ?
O1 Cu2 N2 N1 -23.5(2) . . . . ?
O1 Cu2 N2 N1 -109.3(2) 2_576 . . . ?
C5 N3 N4 C8 -0.2(5) . . . . ?
C5 N3 N4 Cu1 177.8(3) . . . 1_556 ?
N2 N1 C1 C2 1.2(6) . . . . ?
Cu1 N1 C1 C2 179.6(3) . . . . ?
N1 C1 C2 C3 -0.7(6) . . . . ?
C1 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C9 176.4(4) . . . . ?
N1 N2 C4 C3 -1.0(5) . . . . ?
Cu2 N2 C4 C3 178.8(3) . . . . ?
C2 C3 C4 N2 1.4(6) . . . . ?
C9 C3 C4 N2 -175.6(3) . . . . ?
N4 N3 C5 C6 -1.1(6) . . . . ?
N3 C5 C6 C7 1.6(7) . . . . ?
C5 C6 C7 C8 -0.7(6) . . . . ?
C5 C6 C7 C11 178.1(4) . . . . ?
N3 N4 C8 C7 1.1(6) . . . . ?
Cu1 N4 C8 C7 -176.8(3) 1_556 . . . ?
C6 C7 C8 N4 -0.6(6) . . . . ?
C11 C7 C8 N4 -179.4(4) . . . . ?
C2 C3 C9 C10 52.2(5) . . . . ?
C4 C3 C9 C10 -131.1(4) . . . . ?
C2 C3 C9 C15 173.9(4) . . . . ?
C4 C3 C9 C15 -9.4(5) . . . . ?
C2 C3 C9 C14 -67.7(5) . . . . ?
C4 C3 C9 C14 109.0(4) . . . . ?
C3 C9 C10 C11 -177.7(3) . . . . ?
C15 C9 C10 C11 59.2(4) . . . . ?
C14 C9 C10 C11 -58.9(4) . . . . ?
C6 C7 C11 C10 -2.2(5) . . . . ?
C8 C7 C11 C10 176.5(3) . . . . ?
C6 C7 C11 C17 -122.4(4) . . . . ?
C8 C7 C11 C17 56.3(5) . . . . ?
C6 C7 C11 C12 118.9(4) . . . . ?
C8 C7 C11 C12 -62.3(5) . . . . ?
C9 C10 C11 C7 -179.6(3) . . . . ?
C9 C10 C11 C17 -59.4(4) . . . . ?
C9 C10 C11 C12 58.4(4) . . . . ?
C7 C11 C12 C13 175.4(3) . . . . ?
C10 C11 C12 C13 -59.7(4) . . . . ?
C17 C11 C12 C13 57.4(5) . . . . ?
C11 C12 C13 C14 62.2(4) . . . . ?
C11 C12 C13 C18 -59.4(5) . . . . ?
C18 C13 C14 C9 59.3(4) . . . . ?
C12 C13 C14 C9 -61.3(4) . . . . ?
C3 C9 C14 C13 -179.2(3) . . . . ?
C10 C9 C14 C13 59.4(4) . . . . ?
C15 C9 C14 C13 -59.0(5) . . . . ?
C3 C9 C15 C16 177.7(3) . . . . ?
C10 C9 C15 C16 -58.9(4) . . . . ?
C14 C9 C15 C16 59.8(4) . . . . ?
C9 C15 C16 C18 -60.6(4) . . . . ?
C9 C15 C16 C17 60.2(4) . . . . ?
C7 C11 C17 C16 -176.3(3) . . . . ?
C10 C11 C17 C16 59.6(4) . . . . ?
C12 C11 C17 C16 -57.5(4) . . . . ?
C18 C16 C17 C11 60.3(4) . . . . ?
C15 C16 C17 C11 -61.0(4) . . . . ?
C15 C16 C18 C13 58.9(5) . . . . ?
C17 C16 C18 C13 -61.6(5) . . . . ?
C14 C13 C18 C16 -58.8(5) . . . . ?
C12 C13 C18 C16 61.4(5) . . . . ?
Cu1 O2 C19 O3 28.4(6) . . . . ?
Cu1 O2 C19 C22 -148.8(3) . . . . ?
Cu2 O5 C20 O4 -1.7(6) 2_666 . . . ?
Cu2 O5 C20 C24 179.5(3) 2_666 . . . ?
Cu2 O6 C21 O7 -36.0(5) 1_655 . . . ?
Cu2 O6 C21 C26 144.8(3) 1_655 . . . ?
O3 C19 C22 C28 42.5(5) . . . . ?
O2 C19 C22 C28 -140.3(4) . . . . ?
O3 C19 C22 C27 166.9(4) . . . . ?
O2 C19 C22 C27 -15.9(5) . . . . ?
O3 C19 C22 C23 -75.8(5) . . . . ?
O2 C19 C22 C23 101.5(4) . . . . ?
C19 C22 C23 C24 179.0(3) . . . . ?
C28 C22 C23 C24 58.9(4) . . . . ?
C27 C22 C23 C24 -60.3(4) . . . . ?
O4 C20 C24 C30 -179.0(4) . . . . ?
O5 C20 C24 C30 -0.1(5) . . . . ?
O4 C20 C24 C25 58.7(5) . . . . ?
O5 C20 C24 C25 -122.4(4) . . . . ?
O4 C20 C24 C23 -58.6(5) . . . . ?
O5 C20 C24 C23 120.3(4) . . . . ?
C22 C23 C24 C20 179.6(3) . . . . ?
C22 C23 C24 C30 -57.6(4) . . . . ?
C22 C23 C24 C25 60.6(4) . . . . ?
C20 C24 C25 C26 -177.1(3) . . . . ?
C30 C24 C25 C26 58.3(4) . . . . ?
C23 C24 C25 C26 -59.8(4) . . . . ?
O7 C21 C26 C31 49.4(5) . . . . ?
O6 C21 C26 C31 -131.3(4) . . . . ?
O7 C21 C26 C27 -68.6(5) . . . . ?
O6 C21 C26 C27 110.6(4) . . . . ?
O7 C21 C26 C25 170.4(3) . . . . ?
O6 C21 C26 C25 -10.3(5) . . . . ?
C24 C25 C26 C31 -58.7(4) . . . . ?
C24 C25 C26 C21 179.6(3) . . . . ?
C24 C25 C26 C27 59.6(4) . . . . ?
C31 C26 C27 C22 58.0(4) . . . . ?
C21 C26 C27 C22 176.1(3) . . . . ?
C25 C26 C27 C22 -59.7(4) . . . . ?
C19 C22 C27 C26 176.1(3) . . . . ?
C28 C22 C27 C26 -58.8(4) . . . . ?
C23 C22 C27 C26 59.6(4) . . . . ?
C19 C22 C28 C29 -176.6(3) . . . . ?
C27 C22 C28 C29 57.7(4) . . . . ?
C23 C22 C28 C29 -59.9(4) . . . . ?
C22 C28 C29 C30 62.0(4) . . . . ?
C22 C28 C29 C31 -58.6(4) . . . . ?
C28 C29 C30 C24 -60.9(4) . . . . ?
C31 C29 C30 C24 61.5(4) . . . . ?
C20 C24 C30 C29 177.5(3) . . . . ?
C25 C24 C30 C29 -59.4(4) . . . . ?
C23 C24 C30 C29 57.8(4) . . . . ?
C21 C26 C31 C29 -174.4(3) . . . . ?
C27 C26 C31 C29 -57.4(4) . . . . ?
C25 C26 C31 C29 60.9(4) . . . . ?
C30 C29 C31 C26 -62.9(4) . . . . ?
C28 C29 C31 C26 59.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.94
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.116


_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk25 in P-1
CELL  0.71073  11.1208  11.5078  13.8841   83.981   67.507   62.065
ZERR     1.00   0.0009   0.0010   0.0013    0.006    0.006    0.005
LATT   1
SFAC  C    H    N    O    CU
UNIT  62   78   8    19   4
MERG   2
OMIT     0.00 180.00
SHEL 0.784 8
FMAP   2
PLAN   10
SIZE     0.04   0.08   0.21
ACTA
BOND
 
EQIV $1 X, Y, -1+Z
EQIV $2 1-X, 2-Y, 1-Z
EQIV $3 1-X, 1-Y, 1-Z
EQIV $4 -1+X, Y, Z
 
RTAB H..O H1O O7_$4
RTAB H..O H1W N3_$1
RTAB H..O H2W O6_$2
RTAB H..O H3W O3
RTAB H..O H4W O4_$3
 
RTAB O..O O1 O7_$4
RTAB O..O O1W N3_$1
RTAB O..O O1W O6_$2
RTAB O..O O2W O3
RTAB O..O O2W O4_$3
RTAB O..O O3W O4
RTAB O..O O3W O4_$3
 
RTAB XHY O1 H1O O7_$4
RTAB XHY O1W H1W N3_$1
RTAB XHY O1W H2W O6_$2
RTAB XHY O2W H3W O3
RTAB XHY O2W H4W O4_$3
 
BOND   $H
CONF
LIST   4
L.S.   6
TEMP    -100
WGHT    0.027800
FVAR       0.60669
CU1   5    0.311268    0.939939    0.329590    11.00000    0.01662    0.02930 =
         0.01343    0.00159   -0.00723   -0.01048
CU2   5    0.079957    0.840255    0.488973    11.00000    0.02934    0.02103 =
         0.02404    0.01190   -0.01935   -0.01810
O1    4    0.110968    0.967707    0.389857    11.00000    0.02044    0.02029 =
         0.01388   -0.00051   -0.00790   -0.01030
AFIX   3
H1O   2    0.099973    0.939981    0.341648    11.00000   -1.50000
AFIX   0
O2    4    0.523338    0.874709    0.280933    11.00000    0.01957    0.02873 =
         0.02179   -0.00336   -0.01106   -0.00639
O3    4    0.576611    0.702810    0.186836    11.00000    0.04713    0.02703 =
         0.10923   -0.00731   -0.05642   -0.00702
O4    4    0.758777    0.459278    0.523782    11.00000    0.05236    0.05310 =
         0.03998    0.01528    0.00304   -0.02595
O5    4    0.941080    0.287900    0.410676    11.00000    0.04957    0.02146 =
         0.03064    0.01542   -0.02794   -0.02368
O6    4    0.958239    0.804947    0.438372    11.00000    0.03265    0.03392 =
         0.01536    0.00099   -0.01254   -0.02239
O7    4    1.008618    0.871447    0.278184    11.00000    0.05811    0.04052 =
         0.02700    0.01242   -0.02396   -0.03730
N1    3    0.317210    0.892274    0.476078    11.00000    0.01869    0.01387 =
         0.01547    0.00287   -0.00797   -0.01033
N2    3    0.220728    0.853633    0.539762    11.00000    0.01997    0.01831 =
         0.01101    0.00198   -0.00925   -0.00773
N3    3    0.299784    1.109245    1.158411    11.00000    0.03804    0.02360 =
         0.01218    0.00140   -0.01024   -0.01695
N4    3    0.305193    0.992114    1.186866    11.00000    0.02198    0.02555 =
         0.01533   -0.00181   -0.00803   -0.01318
C1    1    0.408704    0.901456    0.508999    11.00000    0.02813    0.03661 =
         0.01971    0.00343   -0.01193   -0.02364
AFIX  43
H1    2    0.474005    0.930269    0.463743    11.00000   -1.20000
AFIX   0
C2    1    0.414065    0.871108    0.606330    11.00000    0.03560    0.03609 =
         0.01062    0.00030   -0.01163   -0.02492
AFIX  43
H2    2    0.481888    0.878407    0.625530    11.00000   -1.20000
AFIX   0
C3    1    0.317156    0.829797    0.674573    11.00000    0.02036    0.02054 =
         0.01388    0.00257   -0.01214   -0.00755
C4    1    0.220592    0.824876    0.634709    11.00000    0.01803    0.01486 =
         0.02538    0.00163   -0.00641   -0.00649
AFIX  43
H4    2    0.151260    0.799443    0.678456    11.00000   -1.20000
AFIX   0
C5    1    0.300803    1.139773    1.064626    11.00000    0.05211    0.01915 =
         0.02359    0.01028   -0.02417   -0.01641
AFIX  43
H5    2    0.295271    1.221516    1.045532    11.00000   -1.20000
AFIX   0
C6    1    0.309570    1.058979    0.990816    11.00000    0.04373    0.03291 =
         0.02014    0.01068   -0.02247   -0.02161
AFIX  43
H6    2    0.312277    1.085142    0.924646    11.00000   -1.20000
AFIX   0
C7    1    0.314016    0.939676    1.019898    11.00000    0.02409    0.02093 =
         0.01465    0.00635   -0.01238   -0.01612
C8    1    0.310757    0.912965    1.121065    11.00000    0.03045    0.02671 =
         0.01743    0.00587   -0.01177   -0.01402
AFIX  43
H8    2    0.312646    0.833423    1.143878    11.00000   -1.20000
AFIX   0
C9    1    0.317140    0.786295    0.781056    11.00000    0.02216    0.01722 =
         0.01934    0.00243   -0.01175   -0.01083
C10   1    0.312771    0.888891    0.845483    11.00000    0.02152    0.01910 =
         0.02190    0.00438   -0.01463   -0.01261
AFIX  23
H10A  2    0.223092    0.970940    0.856480    11.00000   -1.20000
H10B  2    0.395448    0.905966    0.806981    11.00000   -1.20000
AFIX   0
C11   1    0.318968    0.842049    0.951619    11.00000    0.02428    0.01625 =
         0.01333    0.00562   -0.00958   -0.01361
C12   1    0.463159    0.709657    0.931052    11.00000    0.02564    0.02824 =
         0.02461    0.00212   -0.01377   -0.00934
AFIX  23
H12A  2    0.547533    0.724041    0.891644    11.00000   -1.20000
H12B  2    0.470204    0.678035    0.997224    11.00000   -1.20000
AFIX   0
C13   1    0.464079    0.606262    0.869721    11.00000    0.03896    0.01328 =
         0.03176   -0.00468   -0.01906   -0.00052
AFIX  13
H13   2    0.554372    0.523108    0.858743    11.00000   -1.20000
AFIX   0
C14   1    0.460933    0.654619    0.763620    11.00000    0.02925    0.02220 =
         0.02462   -0.00036   -0.01297   -0.00491
AFIX  23
H14A  2    0.464552    0.588749    0.722832    11.00000   -1.20000
H14B  2    0.545853    0.668609    0.725298    11.00000   -1.20000
AFIX   0
C15   1    0.185113    0.760415    0.842909    11.00000    0.03428    0.03625 =
         0.01996    0.01085   -0.01794   -0.02791
AFIX  23
H15A  2    0.094118    0.841228    0.854204    11.00000   -1.20000
H15B  2    0.186924    0.694817    0.803077    11.00000   -1.20000
AFIX   0
C16   1    0.191674    0.711513    0.947773    11.00000    0.04557    0.03694 =
         0.02663    0.01369   -0.02083   -0.03537
AFIX  13
H16   2    0.106587    0.696428    0.986671    11.00000   -1.20000
AFIX   0
C17   1    0.186469    0.817061    1.010745    11.00000    0.03355    0.02805 =
         0.01258    0.00435   -0.00959   -0.01660
AFIX  23
H17A  2    0.096122    0.898499    1.021902    11.00000   -1.20000
H17B  2    0.187572    0.787673    1.078626    11.00000   -1.20000
AFIX   0
C18   1    0.331298    0.583729    0.932073    11.00000    0.06703    0.03108 =
         0.02348    0.01134   -0.02662   -0.03328
AFIX  23
H18A  2    0.333151    0.515975    0.894598    11.00000   -1.20000
H18B  2    0.334642    0.554088    0.999460    11.00000   -1.20000
AFIX   0
C19   1    0.611478    0.756115    0.235490    11.00000    0.03128    0.02863 =
         0.03183    0.00756   -0.02025   -0.02319
C20   1    0.857628    0.412283    0.437014    11.00000    0.03076    0.03584 =
         0.03766    0.01822   -0.02498   -0.02649
C21   1    0.971684    0.799264    0.343202    11.00000    0.01491    0.02452 =
         0.02090    0.00234   -0.00654   -0.01313
C22   1    0.757552    0.683220    0.249312    11.00000    0.02134    0.01388 =
         0.02898    0.00738   -0.01872   -0.01189
C23   1    0.739602    0.586127    0.333819    11.00000    0.02431    0.01419 =
         0.02336    0.00288   -0.00959   -0.00979
AFIX  23
H23A  2    0.660492    0.635655    0.398649    11.00000   -1.20000
H23B  2    0.713651    0.527334    0.310883    11.00000   -1.20000
AFIX   0
C24   1    0.883975    0.503676    0.353334    11.00000    0.02365    0.01366 =
         0.01716    0.00544   -0.00550   -0.01252
C25   1    0.918703    0.600889    0.392288    11.00000    0.02178    0.02214 =
         0.02371    0.00551   -0.01003   -0.01041
AFIX  23
H25A  2    0.839292    0.649477    0.457320    11.00000   -1.20000
H25B  2    1.008207    0.551850    0.405949    11.00000   -1.20000
AFIX   0
C26   1    0.937842    0.698498    0.310416    11.00000    0.01824    0.01775 =
         0.02713   -0.00184   -0.01112   -0.01002
C27   1    0.795367    0.776014    0.290148    11.00000    0.01954    0.01658 =
         0.03037   -0.00093   -0.01428   -0.01213
AFIX  23
H27A  2    0.806333    0.838406    0.239161    11.00000   -1.20000
H27B  2    0.715288    0.825676    0.354589    11.00000   -1.20000
AFIX   0
C28   1    0.882892    0.603664    0.148010    11.00000    0.04002    0.03111 =
         0.02209    0.01093   -0.02029   -0.02574
AFIX  23
H28A  2    0.860123    0.543246    0.123706    11.00000   -1.20000
H28B  2    0.895244    0.662704    0.094212    11.00000   -1.20000
AFIX   0
C29   1    1.024306    0.526365    0.168652    11.00000    0.01914    0.01796 =
         0.01609   -0.00415   -0.00127   -0.00494
AFIX  13
H29   2    1.104962    0.477243    0.103114    11.00000   -1.20000
AFIX   0
C30   1    1.009296    0.428783    0.249495    11.00000    0.02553    0.01944 =
         0.04079    0.00588   -0.01819   -0.01107
AFIX  23
H30A  2    1.100834    0.378702    0.260371    11.00000   -1.20000
H30B  2    0.988618    0.367323    0.224328    11.00000   -1.20000
AFIX   0
C31   1    1.062798    0.618507    0.208975    11.00000    0.02302    0.02365 =
         0.02415    0.00764   -0.00830   -0.01618
AFIX  23
H31A  2    1.152810    0.566738    0.221574    11.00000   -1.20000
H31B  2    1.078953    0.677968    0.156555    11.00000   -1.20000
AFIX   0
O1W   4    0.276838    1.149534    0.371785    11.00000    0.03292    0.02646 =
         0.02980   -0.00786   -0.01077   -0.01158
AFIX   3
H1W   2    0.270856    1.187255    0.316581    11.00000   -1.50000
H2W   2    0.202739    1.199400    0.424115    11.00000   -1.50000
AFIX   0
O2W   4    0.318535    0.681778    0.311685    11.00000    0.05911    0.02204 =
         0.08121    0.00276   -0.01868   -0.00769
AFIX   3
H3W   2    0.402859    0.677554    0.292789    11.00000   -1.50000
H4W   2    0.324307    0.608146    0.333282    11.00000   -1.50000
AFIX   0
O3W   4    0.463776    0.562835    0.522533    10.50000    0.24429
HKLF    4
 
REM  dk25 in P-1
REM R1 =  0.0554 for   3870 Fo > 4sig(Fo)  and  0.1149 for all   6248 data
REM    419 parameters refined using      0 restraints
 
END
 
WGHT      0.0275      0.0000
REM Highest difference peak  0.580,  deepest hole -0.593,  1-sigma level  0.116
Q1    1   0.6359  0.7386  0.1283  11.00000  0.05    0.48
Q2    1   0.1817  0.5652  0.9875  11.00000  0.05    0.47
Q3    1   0.3167  0.6786  0.5366  11.00000  0.05    0.47
Q4    1   0.7387  0.4585  0.4416  11.00000  0.05    0.46
Q5    1   0.2552  1.2181  1.2065  11.00000  0.05    0.44
Q6    1   0.0000  1.0000  0.5000  10.50000  0.05    0.44
Q7    1   0.3617  1.2787  0.9774  11.00000  0.05    0.44
Q8    1   0.8620  0.4587  0.3876  11.00000  0.05    0.44
Q9    1   0.5223  0.7020  1.0887  11.00000  0.05    0.43
Q10   1   0.0077  0.8034  0.8372  11.00000  0.05    0.43
;
_database_code_depnum_ccdc_archive 'CCDC 967344'
#######################################################################
#
#                 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_(3)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Poly[bis-[μ₃-[1,3-bis(pyridazin-4-yl)adamantane-κ⁴N1:N2:N3)]]-
tris[μ₂-(2,5-thiophenedicarboxylato)]-di(μ₃-hydroxido)-
diaquatetracopper(II)] heptahydrate
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H52 Cu4 N8 O16 S3, 7(H2 O)'
_chemical_formula_sum            'C54 H66 Cu4 N8 O23 S3'
_chemical_formula_weight         1545.49

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_space_group_name_Hall           '-P 2yn'
_symmetry_Int_Tables_number      14


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                   13.3933(4)
_cell_length_b                   9.9035(3)
_cell_length_c                   23.7661(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.036(2)
_cell_angle_gamma                90.00
_cell_volume                     3121.39(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    29009
_cell_measurement_theta_min      4.12
_cell_measurement_theta_max      27.10

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1588
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7009
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_process_details   'face indexed (SADABS; Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(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 APEX2 area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29009
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         4.12
_diffrn_reflns_theta_max         27.10
_reflns_number_total             6862
_reflns_number_gt                4502
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 One of the present thiophenedicarboxylate ligands is equally disordered 
 over center of inversion, giving two overlapping orientations. The 
 disorder was resolved without any restraints in geometry and all atoms 
 were refined anisotropically, with similarity restraints (SIMU) for the 
 thermal motion of carbon atoms and rigid bond restrains for the thermal 
 motion of carboxylic groups (DELU). The H-atoms were added to the 
 disordered fragment with partial occupancy factors of 0.5. Further, 
 the disorder of bulky organic ligand effects partial disordering in the 
 region of neighboring solvate water molecules. Two water molecules 
 (O3W and O4W) are situated closely to this thiophenedicarboxylate 
 (TDC²⁻) fragment and have corresponding partial occupancies of 0.5, 
 depending on orientation of the disordered TDC²⁻. These oxygen atoms 
 were refined anisotropically, but H-atoms were not added. Another 
 water molecule is similarly disordered nearly TDC²⁻, but its 
 0.5 partially occupied position is also splitted between two closely 
 separated positions (O51W to O52W 1.40 A). In this case the refined 
 partial contributions were 0.30 and 0.20, these atoms O51W and O52W 
 were refined isotropically and H-atoms were not added. 

 Two other solvate water molecules (O1W and O2W) are ordered, their 
 refinement was standard, in the anisotropic approximation, OH-hydrogen 
 atoms were located and included with fixed d(O-H) = 0.85 A and 
 Uiso = 1.5Ueq(O). 
;

_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)+(0.0454P)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_number_reflns         6862
_refine_ls_number_parameters     477
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.991
_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 0.39009(3) 1.03859(5) 0.010910(17) 0.01965(12) Uani 1 1 d . . .
Cu2 Cu 0.57011(3) 1.11753(4) 0.117346(17) 0.01986(12) Uani 1 1 d . . .
S1 S 0.02963(14) 0.9703(2) 0.00252(8) 0.0264(5) Uani 0.50 1 d P A -1
O2 O 0.2467(7) 1.0111(9) -0.0014(6) 0.0293(19) Uani 0.50 1 d PU A -1
O3 O 0.2445(4) 1.2314(6) 0.0135(3) 0.0473(17) Uani 0.50 1 d PU A -1
O4 O -0.1827(7) 0.8500(10) -0.0107(5) 0.042(3) Uani 0.50 1 d PU A -1
O5 O -0.2559(7) 1.0485(7) 0.0034(6) 0.0229(17) Uani 0.50 1 d PU . -1
C19 C 0.2040(11) 1.1248(17) 0.0019(7) 0.028(2) Uani 0.50 1 d PU A -1
C20 C -0.1821(6) 0.9714(10) -0.0052(3) 0.0256(14) Uani 0.50 1 d PU A -1
C21 C 0.0915(5) 1.1176(9) -0.0086(3) 0.0278(14) Uani 0.50 1 d PU A -1
C22 C 0.0249(5) 1.2222(9) -0.0215(3) 0.0316(15) Uani 0.50 1 d PU . -1
H22 H 0.0459 1.3122 -0.0293 0.038 Uiso 0.50 1 d PR . -1
C23 C -0.0771(5) 1.1828(9) -0.0218(3) 0.0307(15) Uani 0.50 1 d PU A -1
H23 H -0.1335 1.2427 -0.0307 0.037 Uiso 0.50 1 d PR A -1
C24 C -0.0864(6) 1.0519(9) -0.0085(3) 0.0274(14) Uani 0.50 1 d PU A -1
S2 S 0.73916(7) 1.28657(10) 0.33632(4) 0.0256(2) Uani 1 1 d . A .
O1 O 0.51950(16) 1.1159(2) 0.03771(9) 0.0184(5) Uani 1 1 d . . .
H1H H 0.5262 1.1951 0.0250 0.028 Uiso 1 1 d R . .
O6 O 0.63034(17) 1.0971(2) 0.19732(10) 0.0225(6) Uani 1 1 d . A .
O7 O 0.5860(2) 1.2925(3) 0.23498(11) 0.0409(8) Uani 1 1 d . A .
O8 O 0.86687(17) 1.3683(2) 0.43784(10) 0.0249(6) Uani 1 1 d . . .
O9 O 0.94988(18) 1.1745(3) 0.45794(11) 0.0301(6) Uani 1 1 d . . .
O10 O 0.45700(18) 1.2694(3) 0.13792(11) 0.0335(7) Uani 1 1 d . A .
H1W H 0.4860 1.3029 0.1689 0.050 Uiso 1 1 d R . .
H2W H 0.4492 1.3315 0.1130 0.050 Uiso 1 1 d R . .
N1 N 0.4032(2) 0.9277(3) 0.08451(12) 0.0237(7) Uani 1 1 d . A .
N2 N 0.47106(19) 0.9640(3) 0.12819(12) 0.0182(6) Uani 1 1 d . A .
N3 N 0.8119(2) 0.8089(4) 0.43514(15) 0.0434(10) Uani 1 1 d . . .
N4 N 0.8022(2) 0.7100(3) 0.39646(12) 0.0234(7) Uani 1 1 d . . .
C1 C 0.3444(3) 0.8234(5) 0.09110(17) 0.0464(13) Uani 1 1 d . . .
H1 H 0.2974 0.7959 0.0595 0.056 Uiso 1 1 calc R A .
C2 C 0.3470(3) 0.7522(5) 0.14086(17) 0.0422(12) Uani 1 1 d . A .
H2 H 0.3021 0.6788 0.1432 0.051 Uiso 1 1 calc R . .
C3 C 0.4148(2) 0.7876(4) 0.18708(15) 0.0230(8) Uani 1 1 d . . .
C4 C 0.4763(3) 0.8968(4) 0.17651(15) 0.0248(8) Uani 1 1 d . A .
H4 H 0.5259 0.9248 0.2067 0.030 Uiso 1 1 calc R . .
C5 C 0.7284(3) 0.8704(6) 0.4437(2) 0.0734(19) Uani 1 1 d . . .
H5 H 0.7339 0.9417 0.4707 0.088 Uiso 1 1 calc R . .
C6 C 0.6333(3) 0.8393(5) 0.4164(2) 0.0625(16) Uani 1 1 d . . .
H6 H 0.5763 0.8883 0.4248 0.075 Uiso 1 1 calc R . .
C7 C 0.6217(3) 0.7380(4) 0.37738(16) 0.0276(9) Uani 1 1 d . . .
C8 C 0.7124(3) 0.6760(4) 0.36922(15) 0.0247(9) Uani 1 1 d . . .
H8 H 0.7095 0.6047 0.3423 0.030 Uiso 1 1 calc R . .
C9 C 0.4200(2) 0.7234(4) 0.24462(15) 0.0218(8) Uani 1 1 d . A .
C10 C 0.5187(2) 0.7603(4) 0.28267(14) 0.0210(8) Uani 1 1 d . . .
H10A H 0.5239 0.8597 0.2864 0.025 Uiso 1 1 calc R A .
H10B H 0.5768 0.7280 0.2648 0.025 Uiso 1 1 calc R . .
C11 C 0.5228(3) 0.6964(4) 0.34227(16) 0.0261(9) Uani 1 1 d . A .
C12 C 0.5146(3) 0.5423(4) 0.33593(17) 0.0341(10) Uani 1 1 d . . .
H12A H 0.5170 0.5002 0.3739 0.041 Uiso 1 1 calc R A .
H12B H 0.5723 0.5076 0.3183 0.041 Uiso 1 1 calc R . .
C13 C 0.4149(3) 0.5045(4) 0.29860(17) 0.0345(10) Uani 1 1 d . A .
H13 H 0.4106 0.4041 0.2947 0.041 Uiso 1 1 calc R . .
C14 C 0.4134(3) 0.5677(4) 0.23961(17) 0.0298(9) Uani 1 1 d . . .
H14A H 0.3504 0.5420 0.2150 0.036 Uiso 1 1 calc R A .
H14B H 0.4710 0.5332 0.2219 0.036 Uiso 1 1 calc R . .
C15 C 0.3300(2) 0.7726(4) 0.27298(15) 0.0272(9) Uani 1 1 d . . .
H15A H 0.3325 0.8722 0.2767 0.033 Uiso 1 1 calc R A .
H15B H 0.2662 0.7482 0.2489 0.033 Uiso 1 1 calc R . .
C16 C 0.3327(3) 0.7086(4) 0.33175(17) 0.0338(10) Uani 1 1 d . A .
H16 H 0.2744 0.7424 0.3499 0.041 Uiso 1 1 calc R . .
C17 C 0.4314(3) 0.7482(4) 0.36829(15) 0.0307(10) Uani 1 1 d . . .
H17A H 0.4328 0.7101 0.4069 0.037 Uiso 1 1 calc R A .
H17B H 0.4351 0.8478 0.3717 0.037 Uiso 1 1 calc R . .
C18 C 0.3259(3) 0.5549(5) 0.32569(18) 0.0421(11) Uani 1 1 d . . .
H18A H 0.3265 0.5129 0.3635 0.050 Uiso 1 1 calc R A .
H18B H 0.2621 0.5297 0.3017 0.050 Uiso 1 1 calc R . .
C25 C 0.6376(3) 1.1887(4) 0.23549(15) 0.0243(9) Uani 1 1 d . . .
C26 C 0.8882(2) 1.2475(4) 0.42733(15) 0.0220(8) Uani 1 1 d . A .
C27 C 0.7166(3) 1.1643(4) 0.28492(15) 0.0211(8) Uani 1 1 d . A .
C28 C 0.7798(3) 1.0569(4) 0.29628(16) 0.0291(9) Uani 1 1 d . . .
H28 H 0.7789 0.9796 0.2726 0.035 Uiso 1 1 calc R A .
C29 C 0.8466(3) 1.0735(4) 0.34706(16) 0.0292(9) Uani 1 1 d . A .
H29 H 0.8954 1.0080 0.3614 0.035 Uiso 1 1 calc R . .
C30 C 0.8341(2) 1.1917(4) 0.37328(15) 0.0208(8) Uani 1 1 d . . .
O1W O 1.0829(2) 0.9702(3) 0.44384(11) 0.0395(7) Uani 1 1 d . . .
H3W H 1.0435 1.0372 0.4448 0.059 Uiso 1 1 d R . .
H4W H 1.0779 0.9201 0.4724 0.059 Uiso 1 1 d R . .
O2W O 1.2836(3) 0.9730(6) 0.43004(18) 0.132(2) Uani 1 1 d . . .
H5W H 1.3037 0.9045 0.4500 0.198 Uiso 1 1 d R . .
H6W H 1.2209 0.9831 0.4310 0.198 Uiso 1 1 d R . .
O3W O 0.4267(6) 1.1138(9) 0.2859(6) 0.135(5) Uani 0.50 1 d P . .
O4W O 1.3951(7) 1.1291(9) 0.3919(6) 0.145(5) Uani 0.50 1 d P . .
O51W O -0.0714(9) 0.6215(13) 0.0132(6) 0.076(4) Uiso 0.30 1 d P . .
O52W O -0.0850(14) 0.6654(19) 0.0675(8) 0.076(6) Uiso 0.20 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.920(2) . ?
Cu1 O2 1.921(10) . ?
Cu1 O8 1.952(2) 4_585 ?
Cu1 O5 1.979(10) 3_575 ?
Cu1 N1 2.052(3) . ?
Cu1 O1 2.352(2) 3_675 ?
Cu2 O1 1.919(2) . ?
Cu2 O6 1.969(2) . ?
Cu2 N4 2.006(3) 2_655 ?
Cu2 N2 2.058(3) . ?
Cu2 O10 2.236(2) . ?
S1 C21 1.716(8) . ?
S1 C24 1.739(9) . ?
O2 C19 1.270(17) . ?
O3 C19 1.201(18) . ?
O4 C20 1.210(13) . ?
O5 C20 1.288(11) . ?
O5 Cu1 1.979(10) 3_575 ?
C19 C21 1.495(15) . ?
C20 C24 1.520(11) . ?
C21 C22 1.373(11) . ?
C22 C23 1.420(9) . ?
C22 H22 0.9600 . ?
C23 C24 1.345(11) . ?
C23 H23 0.9600 . ?
S2 C27 1.716(4) . ?
S2 C30 1.720(3) . ?
O1 Cu1 2.352(2) 3_675 ?
O1 H1H 0.8500 . ?
O6 C25 1.277(4) . ?
O7 C25 1.238(4) . ?
O8 C26 1.264(4) . ?
O8 Cu1 1.952(2) 4_686 ?
O9 C26 1.252(4) . ?
O10 H1W 0.8500 . ?
O10 H2W 0.8500 . ?
N1 C1 1.321(5) . ?
N1 N2 1.330(4) . ?
N2 C4 1.321(4) . ?
N3 C5 1.314(5) . ?
N3 N4 1.337(4) . ?
N4 C8 1.328(4) . ?
N4 Cu2 2.006(3) 2_645 ?
C1 C2 1.373(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.370(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.402(5) . ?
C3 C9 1.501(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.360(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(5) . ?
C7 C11 1.521(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.537(4) . ?
C9 C15 1.541(5) . ?
C9 C14 1.549(5) . ?
C10 C11 1.545(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C17 1.535(5) . ?
C11 C12 1.536(5) . ?
C12 C13 1.542(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.517(6) . ?
C13 C14 1.533(5) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.530(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.528(5) . ?
C16 C18 1.530(6) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C25 C27 1.486(5) . ?
C26 C30 1.490(5) . ?
C27 C28 1.363(5) . ?
C28 C29 1.408(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.348(5) . ?
C29 H29 0.9500 . ?
O1W H3W 0.8500 . ?
O1W H4W 0.8499 . ?
O2W H5W 0.8499 . ?
O2W H6W 0.8500 . ?

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 O2 160.7(3) . . ?
O1 Cu1 O8 97.53(10) . 4_585 ?
O2 Cu1 O8 84.3(4) . 4_585 ?
O1 Cu1 O5 170.5(4) . 3_575 ?
O2 Cu1 O5 17.8(3) . 3_575 ?
O8 Cu1 O5 91.5(4) 4_585 3_575 ?
O1 Cu1 N1 88.00(10) . . ?
O2 Cu1 N1 91.0(4) . . ?
O8 Cu1 N1 174.25(11) 4_585 . ?
O5 Cu1 N1 83.1(4) 3_575 . ?
O1 Cu1 O1 85.38(9) . 3_675 ?
O2 Cu1 O1 113.9(3) . 3_675 ?
O8 Cu1 O1 84.21(9) 4_585 3_675 ?
O5 Cu1 O1 98.6(3) 3_575 3_675 ?
N1 Cu1 O1 94.72(10) . 3_675 ?
O1 Cu2 O6 172.67(10) . . ?
O1 Cu2 N4 91.96(10) . 2_655 ?
O6 Cu2 N4 87.77(11) . 2_655 ?
O1 Cu2 N2 88.41(10) . . ?
O6 Cu2 N2 89.29(10) . . ?
N4 Cu2 N2 159.51(12) 2_655 . ?
O1 Cu2 O10 93.71(9) . . ?
O6 Cu2 O10 93.24(10) . . ?
N4 Cu2 O10 110.34(11) 2_655 . ?
N2 Cu2 O10 90.07(10) . . ?
C21 S1 C24 91.3(4) . . ?
C19 O2 Cu1 108.3(10) . . ?
C20 O5 Cu1 114.4(6) . 3_575 ?
O3 C19 O2 126.9(14) . . ?
O3 C19 C21 119.5(12) . . ?
O2 C19 C21 113.5(13) . . ?
O4 C20 O5 127.8(9) . . ?
O4 C20 C24 120.6(8) . . ?
O5 C20 C24 111.6(8) . . ?
C22 C21 C19 127.5(10) . . ?
C22 C21 S1 111.3(5) . . ?
C19 C21 S1 120.8(9) . . ?
C21 C22 C23 112.8(8) . . ?
C21 C22 H22 123.0 . . ?
C23 C22 H22 124.1 . . ?
C24 C23 C22 112.6(8) . . ?
C24 C23 H23 123.5 . . ?
C22 C23 H23 123.9 . . ?
C23 C24 C20 128.6(8) . . ?
C23 C24 S1 111.9(6) . . ?
C20 C24 S1 119.4(7) . . ?
C27 S2 C30 91.29(17) . . ?
Cu2 O1 Cu1 120.57(12) . . ?
Cu2 O1 Cu1 110.79(10) . 3_675 ?
Cu1 O1 Cu1 94.62(9) . 3_675 ?
Cu2 O1 H1H 107.7 . . ?
Cu1 O1 H1H 112.6 . . ?
Cu1 O1 H1H 109.8 3_675 . ?
C25 O6 Cu2 126.4(2) . . ?
C26 O8 Cu1 127.7(2) . 4_686 ?
Cu2 O10 H1W 102.2 . . ?
Cu2 O10 H2W 110.8 . . ?
H1W O10 H2W 108.5 . . ?
C1 N1 N2 118.2(3) . . ?
C1 N1 Cu1 122.6(2) . . ?
N2 N1 Cu1 119.2(2) . . ?
C4 N2 N1 119.3(3) . . ?
C4 N2 Cu2 121.7(2) . . ?
N1 N2 Cu2 119.0(2) . . ?
C5 N3 N4 116.3(3) . . ?
C8 N4 N3 121.0(3) . . ?
C8 N4 Cu2 122.7(3) . 2_645 ?
N3 N4 Cu2 116.3(2) . 2_645 ?
N1 C1 C2 124.0(4) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 113.2(3) . . ?
C2 C3 C9 124.3(3) . . ?
C4 C3 C9 122.4(3) . . ?
N2 C4 C3 125.7(3) . . ?
N2 C4 H4 117.2 . . ?
C3 C4 H4 117.2 . . ?
N3 C5 C6 124.9(4) . . ?
N3 C5 H5 117.6 . . ?
C6 C5 H5 117.6 . . ?
C7 C6 C5 119.7(4) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C8 113.6(4) . . ?
C6 C7 C11 125.5(3) . . ?
C8 C7 C11 120.8(3) . . ?
N4 C8 C7 124.5(4) . . ?
N4 C8 H8 117.7 . . ?
C7 C8 H8 117.7 . . ?
C3 C9 C10 111.2(3) . . ?
C3 C9 C15 109.0(3) . . ?
C10 C9 C15 109.2(3) . . ?
C3 C9 C14 110.9(3) . . ?
C10 C9 C14 108.5(3) . . ?
C15 C9 C14 108.0(3) . . ?
C9 C10 C11 111.1(3) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C7 C11 C17 111.8(3) . . ?
C7 C11 C12 111.6(3) . . ?
C17 C11 C12 108.7(3) . . ?
C7 C11 C10 108.0(3) . . ?
C17 C11 C10 107.7(3) . . ?
C12 C11 C10 108.9(3) . . ?
C11 C12 C13 110.0(3) . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C18 C13 C14 110.1(3) . . ?
C18 C13 C12 110.2(4) . . ?
C14 C13 C12 109.1(3) . . ?
C18 C13 H13 109.2 . . ?
C14 C13 H13 109.2 . . ?
C12 C13 H13 109.2 . . ?
C13 C14 C9 110.1(3) . . ?
C13 C14 H14A 109.7 . . ?
C9 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C9 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C16 C15 C9 110.4(3) . . ?
C16 C15 H15A 109.6 . . ?
C9 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C9 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C15 108.7(3) . . ?
C17 C16 C18 110.1(3) . . ?
C15 C16 C18 109.4(3) . . ?
C17 C16 H16 109.5 . . ?
C15 C16 H16 109.5 . . ?
C18 C16 H16 109.5 . . ?
C16 C17 C11 111.1(3) . . ?
C16 C17 H17A 109.4 . . ?
C11 C17 H17A 109.4 . . ?
C16 C17 H17B 109.4 . . ?
C11 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C13 C18 C16 109.1(3) . . ?
C13 C18 H18A 109.9 . . ?
C16 C18 H18A 109.9 . . ?
C13 C18 H18B 109.9 . . ?
C16 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O7 C25 O6 126.6(3) . . ?
O7 C25 C27 118.5(3) . . ?
O6 C25 C27 114.9(3) . . ?
O9 C26 O8 125.5(3) . . ?
O9 C26 C30 119.3(3) . . ?
O8 C26 C30 115.2(3) . . ?
C28 C27 C25 129.6(3) . . ?
C28 C27 S2 111.5(3) . . ?
C25 C27 S2 118.9(3) . . ?
C27 C28 C29 112.4(3) . . ?
C27 C28 H28 123.8 . . ?
C29 C28 H28 123.8 . . ?
C30 C29 C28 113.1(3) . . ?
C30 C29 H29 123.4 . . ?
C28 C29 H29 123.4 . . ?
C29 C30 C26 130.1(3) . . ?
C29 C30 S2 111.7(3) . . ?
C26 C30 S2 118.3(3) . . ?
H3W O1W H4W 108.4 . . ?
H5W O2W H6W 108.4 . . ?


loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 Cu1 O2 C19 -68.3(11) 4_585 . . . ?
N1 Cu1 O2 C19 115.1(11) . . . . ?
O1 Cu1 O2 C19 -149.3(10) 3_675 . . . ?
Cu1 O2 C19 C21 178.3(9) . . . . ?
Cu1 O5 C20 O4 -14.2(16) 3_575 . . . ?
Cu1 O5 C20 C24 165.3(6) 3_575 . . . ?
O3 C19 C21 C22 18.6(19) . . . . ?
O2 C19 C21 C22 -163.1(11) . . . . ?
O3 C19 C21 S1 -153.9(11) . . . . ?
O2 C19 C21 S1 24.3(17) . . . . ?
C24 S1 C21 C22 -1.5(6) . . . . ?
C24 S1 C21 C19 172.2(8) . . . . ?
C19 C21 C22 C23 -172.6(10) . . . . ?
S1 C21 C22 C23 0.5(9) . . . . ?
C19 C21 C22 O51W -12.1(13) . . . 3_575 ?
S1 C21 C22 O51W 161.0(7) . . . 3_575 ?
C19 C21 C22 O52W 36.9(13) . . . 3_575 ?
S1 C21 C22 O52W -149.9(7) . . . 3_575 ?
C21 C22 C23 C24 1.1(10) . . . . ?
O51W C22 C23 C24 -157.1(9) 3_575 . . . ?
O52W C22 C23 C24 141.4(11) 3_575 . . . ?
C22 C23 C24 C20 -178.9(7) . . . . ?
C22 C23 C24 S1 -2.2(9) . . . . ?
O4 C20 C24 C23 156.1(10) . . . . ?
O5 C20 C24 C23 -23.5(13) . . . . ?
O4 C20 C24 S1 -20.4(12) . . . . ?
O5 C20 C24 S1 160.0(8) . . . . ?
C21 S1 C24 C23 2.2(6) . . . . ?
C21 S1 C24 C20 179.2(6) . . . . ?
N4 Cu2 O1 Cu1 179.90(15) 2_655 . . . ?
N2 Cu2 O1 Cu1 20.40(14) . . . . ?
O10 Cu2 O1 Cu1 -69.57(14) . . . . ?
N4 Cu2 O1 Cu1 70.98(12) 2_655 . . 3_675 ?
N2 Cu2 O1 Cu1 -88.53(11) . . . 3_675 ?
O10 Cu2 O1 Cu1 -178.49(10) . . . 3_675 ?
O8 Cu1 O1 Cu2 159.01(13) 4_585 . . . ?
N1 Cu1 O1 Cu2 -22.58(14) . . . . ?
O1 Cu1 O1 Cu2 -117.47(16) 3_675 . . . ?
O2 Cu1 O1 Cu1 -177.7(12) . . . 3_675 ?
O8 Cu1 O1 Cu1 -83.52(10) 4_585 . . 3_675 ?
N1 Cu1 O1 Cu1 94.90(10) . . . 3_675 ?
O1 Cu1 O1 Cu1 0.0 3_675 . . 3_675 ?
N4 Cu2 O6 C25 78.0(3) 2_655 . . . ?
N2 Cu2 O6 C25 -122.3(3) . . . . ?
O10 Cu2 O6 C25 -32.3(3) . . . . ?
O1 Cu1 N1 C1 -165.7(3) . . . . ?
O2 Cu1 N1 C1 33.6(4) . . . . ?
O5 Cu1 N1 C1 17.6(4) 3_575 . . . ?
O1 Cu1 N1 C1 -80.5(3) 3_675 . . . ?
O1 Cu1 N1 N2 16.5(2) . . . . ?
O2 Cu1 N1 N2 -144.2(3) . . . . ?
O5 Cu1 N1 N2 -160.2(3) 3_575 . . . ?
O1 Cu1 N1 N2 101.7(2) 3_675 . . . ?
C1 N1 N2 C4 -1.2(5) . . . . ?
Cu1 N1 N2 C4 176.7(2) . . . . ?
C1 N1 N2 Cu2 175.8(3) . . . . ?
Cu1 N1 N2 Cu2 -6.3(3) . . . . ?
O1 Cu2 N2 C4 169.3(3) . . . . ?
O6 Cu2 N2 C4 -3.7(3) . . . . ?
N4 Cu2 N2 C4 78.0(4) 2_655 . . . ?
O10 Cu2 N2 C4 -97.0(3) . . . . ?
O1 Cu2 N2 N1 -7.5(2) . . . . ?
O6 Cu2 N2 N1 179.4(2) . . . . ?
N4 Cu2 N2 N1 -98.9(4) 2_655 . . . ?
O10 Cu2 N2 N1 86.2(2) . . . . ?
C5 N3 N4 C8 -0.9(6) . . . . ?
C5 N3 N4 Cu2 179.3(4) . . . 2_645 ?
N2 N1 C1 C2 1.9(7) . . . . ?
Cu1 N1 C1 C2 -175.9(4) . . . . ?
N1 C1 C2 C3 -1.0(7) . . . . ?
C1 C2 C3 C4 -0.6(6) . . . . ?
C1 C2 C3 C9 175.8(4) . . . . ?
N1 N2 C4 C3 -0.5(5) . . . . ?
Cu2 N2 C4 C3 -177.4(3) . . . . ?
C2 C3 C4 N2 1.4(5) . . . . ?
C9 C3 C4 N2 -175.1(3) . . . . ?
N4 N3 C5 C6 0.7(9) . . . . ?
N3 C5 C6 C7 0.0(10) . . . . ?
C5 C6 C7 C8 -0.5(7) . . . . ?
C5 C6 C7 C11 -177.3(5) . . . . ?
N3 N4 C8 C7 0.4(6) . . . . ?
Cu2 N4 C8 C7 -179.8(3) 2_645 . . . ?
C6 C7 C8 N4 0.3(6) . . . . ?
C11 C7 C8 N4 177.2(3) . . . . ?
C2 C3 C9 C10 166.2(4) . . . . ?
C4 C3 C9 C10 -17.8(5) . . . . ?
C2 C3 C9 C15 -73.4(5) . . . . ?
C4 C3 C9 C15 102.7(4) . . . . ?
C2 C3 C9 C14 45.3(5) . . . . ?
C4 C3 C9 C14 -138.6(3) . . . . ?
C3 C9 C10 C11 178.8(3) . . . . ?
C15 C9 C10 C11 58.5(4) . . . . ?
C14 C9 C10 C11 -58.9(4) . . . . ?
C6 C7 C11 C17 -18.7(6) . . . . ?
C8 C7 C11 C17 164.8(4) . . . . ?
C6 C7 C11 C12 -140.7(5) . . . . ?
C8 C7 C11 C12 42.8(5) . . . . ?
C6 C7 C11 C10 99.6(5) . . . . ?
C8 C7 C11 C10 -76.9(4) . . . . ?
C9 C10 C11 C7 -179.6(3) . . . . ?
C9 C10 C11 C17 -58.7(4) . . . . ?
C9 C10 C11 C12 59.1(4) . . . . ?
C7 C11 C12 C13 -178.3(3) . . . . ?
C17 C11 C12 C13 57.9(4) . . . . ?
C10 C11 C12 C13 -59.2(4) . . . . ?
C11 C12 C13 C18 -60.3(4) . . . . ?
C11 C12 C13 C14 60.6(4) . . . . ?
C18 C13 C14 C9 60.2(4) . . . . ?
C12 C13 C14 C9 -60.8(4) . . . . ?
C3 C9 C14 C13 -177.9(3) . . . . ?
C10 C9 C14 C13 59.6(4) . . . . ?
C15 C9 C14 C13 -58.6(4) . . . . ?
C3 C9 C15 C16 179.8(3) . . . . ?
C10 C9 C15 C16 -58.6(4) . . . . ?
C14 C9 C15 C16 59.2(4) . . . . ?
C9 C15 C16 C17 59.6(4) . . . . ?
C9 C15 C16 C18 -60.8(4) . . . . ?
C15 C16 C17 C11 -61.1(4) . . . . ?
C18 C16 C17 C11 58.7(4) . . . . ?
C7 C11 C17 C16 178.6(3) . . . . ?
C12 C11 C17 C16 -57.7(4) . . . . ?
C10 C11 C17 C16 60.1(4) . . . . ?
C14 C13 C18 C16 -60.4(4) . . . . ?
C12 C13 C18 C16 60.0(4) . . . . ?
C17 C16 C18 C13 -59.1(4) . . . . ?
C15 C16 C18 C13 60.4(4) . . . . ?
Cu2 O6 C25 O7 21.6(5) . . . . ?
Cu2 O6 C25 C27 -158.7(2) . . . . ?
Cu1 O8 C26 O9 -18.9(5) 4_686 . . . ?
Cu1 O8 C26 C30 161.6(2) 4_686 . . . ?
O7 C25 C27 C28 177.4(4) . . . . ?
O6 C25 C27 C28 -2.4(6) . . . . ?
O7 C25 C27 S2 -4.9(5) . . . . ?
O6 C25 C27 S2 175.4(2) . . . . ?
C30 S2 C27 C28 -0.2(3) . . . . ?
C30 S2 C27 C25 -178.3(3) . . . . ?
C25 C27 C28 C29 178.2(4) . . . . ?
S2 C27 C28 C29 0.3(4) . . . . ?
C27 C28 C29 C30 -0.3(5) . . . . ?
C28 C29 C30 C26 179.7(3) . . . . ?
C28 C29 C30 S2 0.2(4) . . . . ?
O9 C26 C30 C29 -7.0(6) . . . . ?
O8 C26 C30 C29 172.5(4) . . . . ?
O9 C26 C30 S2 172.4(3) . . . . ?
O8 C26 C30 S2 -8.1(4) . . . . ?
C27 S2 C30 C29 0.0(3) . . . . ?
C27 S2 C30 C26 -179.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.093


_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk2 in P2(1)/n
CELL  0.71073  13.3933   9.9035  23.7661   90.000   98.036   90.000
ZERR     2.00   0.0004   0.0003   0.0008    0.000    0.002    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    CU   S
UNIT  108  132  16   46   8    6
MERG   2
OMIT     0.00 180.00
OMIT     3   0   1
OMIT    -1   2   5
OMIT    -3   0   1
SHEL 0.78 5
SIMU 0.005 C19 C20 C21 C22 C23 C24
DELU 0.005 C21 C19 O2 O3
DELU 0.005 C24 C20 O4 O5
EQIV $1 -0.5+X, 2.5-Y, -0.5+Z
EQIV $2 1.5-X, 0.5+Y, 0.5-Z
EQIV $3 2-X, 2-Y, 1-Z
EQIV $4 1.5-X, -0.5+Y, 0.5-Z
RTAB H..O H1H O9_$1
RTAB H..O H1W O7
RTAB H..O H2W O1W_$2
RTAB H..O H3W O9
RTAB H..O H4W O9_$3
RTAB H..O H5W O3_$4
RTAB H..O H6W O1W
RTAB O..O O1 O9_$1
RTAB O..O O10 O7
RTAB O..O O10 O1W_$2
RTAB O..O O1W O9
RTAB O..O O1W O9_$3
RTAB O..O O2W O3_$4
RTAB O..O O2W O1W
RTAB XHY O1 H1H O9_$1
RTAB XHY O10 H1W O7
RTAB XHY O10 H2W O1W_$2
RTAB XHY O1W H3W O9
RTAB XHY O1W H4W O9_$3
RTAB XHY O2W H5W O3_$4
RTAB XHY O2W H6W O1W
FMAP   2
PLAN   12
SIZE     0.05   0.12   0.25
ACTA
BOND
BOND   $H
CONF
LIST   4
L.S.   6
TEMP  -100.00
WGHT    0.045400
FVAR       0.34654
CU1   5    0.390089    1.038594    0.010910    11.00000    0.01111    0.03446 =
         0.01177    0.00035   -0.00408    0.00151
CU2   5    0.570109    1.117533    0.117346    11.00000    0.02003    0.02392 =
         0.01288    0.00036   -0.00736   -0.00382
PART   -1
S1    6    0.029633    0.970277    0.002518    10.50000    0.01604    0.04094 =
         0.02142   -0.00587    0.00029   -0.00030
O2    4    0.246670    1.011135   -0.001361    10.50000    0.00701    0.05660 =
         0.02415   -0.00722    0.00178   -0.00428
O3    4    0.244488    1.231388    0.013542    10.50000    0.02438    0.06335 =
         0.05660   -0.03396    0.01408   -0.01599
O4    4   -0.182683    0.849968   -0.010686    10.50000    0.02389    0.04520 =
         0.05860   -0.01128    0.01548   -0.00090
O5    4   -0.255916    1.048495    0.003364    10.50000    0.01240    0.03793 =
         0.01698   -0.00281   -0.00247    0.00093
C19   1    0.204005    1.124837    0.001910    10.50000    0.01363    0.05024 =
         0.02034   -0.01150    0.00816   -0.00848
C20   1   -0.182071    0.971390   -0.005173    10.50000    0.01012    0.04985 =
         0.01615    0.00170   -0.00096    0.00236
C21   1    0.091450    1.117615   -0.008605    10.50000    0.01532    0.05013 =
         0.01849   -0.00664    0.00441   -0.00375
C22   1    0.024903    1.222228   -0.021487    10.50000    0.01980    0.04993 =
         0.02380   -0.00309   -0.00125   -0.00439
AFIX   3
H22   2    0.045863    1.312198   -0.029287    10.50000   -1.20000
AFIX   0
C23   1   -0.077100    1.182835   -0.021841    10.50000    0.01665    0.05007 =
         0.02469   -0.00222    0.00005   -0.00334
AFIX   3
H23   2   -0.133460    1.242725   -0.030741    10.50000   -1.20000
AFIX   0
C24   1   -0.086413    1.051896   -0.008455    10.50000    0.00992    0.05034 =
         0.02059    0.00098   -0.00248    0.00175
PART    0
S2    6    0.739164    1.286569    0.336322    11.00000    0.03001    0.02287 =
         0.01935   -0.00418   -0.01263    0.00200
O1    4    0.519503    1.115878    0.037712    11.00000    0.01927    0.01826 =
         0.01531   -0.00011   -0.00606   -0.00190
AFIX   3
H1H   2    0.526163    1.195088    0.024972    11.00000   -1.50000
AFIX   0
O6    4    0.630342    1.097128    0.197317    11.00000    0.02516    0.02390 =
         0.01544   -0.00235   -0.00726   -0.00487
O7    4    0.585988    1.292516    0.234979    11.00000    0.04790    0.03595 =
         0.03082   -0.01011   -0.02215    0.01447
O8    4    0.866870    1.368312    0.437835    11.00000    0.02699    0.02317 =
         0.02053   -0.00037   -0.01049   -0.00136
O9    4    0.949884    1.174457    0.457940    11.00000    0.03462    0.03034 =
         0.02037   -0.00033   -0.01396    0.00537
O10   4    0.457004    1.269358    0.137921    11.00000    0.03897    0.03225 =
         0.02532   -0.00397   -0.00904    0.00886
AFIX   3
H1W   2    0.486004    1.302927    0.168891    11.00000   -1.50000
H2W   2    0.449184    1.331497    0.113001    11.00000   -1.50000
AFIX   0
N1    3    0.403154    0.927678    0.084512    11.00000    0.01749    0.03878 =
         0.01367   -0.00400   -0.00205   -0.00931
N2    3    0.471056    0.963988    0.128191    11.00000    0.01840    0.01914 =
         0.01488   -0.00210   -0.00518   -0.00183
N3    3    0.811919    0.808917    0.435141    11.00000    0.03111    0.05611 =
         0.03706   -0.02459   -0.01610    0.01566
N4    3    0.802237    0.709994    0.396456    11.00000    0.02581    0.02568 =
         0.01506   -0.00026   -0.00947    0.00792
C1    1    0.344369    0.823360    0.091099    11.00000    0.04069    0.07694 =
         0.01824    0.00282   -0.00762   -0.03510
AFIX  43
H1    2    0.297405    0.795941    0.059461    11.00000   -1.20000
AFIX   0
C2    1    0.346986    0.752154    0.140858    11.00000    0.04502    0.05740 =
         0.02181    0.00350   -0.00343   -0.03595
AFIX  43
H2    2    0.302060    0.678791    0.143215    11.00000   -1.20000
AFIX   0
C3    1    0.414830    0.787633    0.187079    11.00000    0.01888    0.02945 =
         0.02015   -0.00327    0.00049   -0.00112
C4    1    0.476251    0.896759    0.176512    11.00000    0.02292    0.02674 =
         0.02097   -0.00070   -0.01062   -0.00275
AFIX  43
H4    2    0.525940    0.924796    0.206742    11.00000   -1.20000
AFIX   0
C5    1    0.728443    0.870447    0.443721    11.00000    0.04200    0.09166 =
         0.07774   -0.06411   -0.02244    0.02906
AFIX  43
H5    2    0.733899    0.941701    0.470739    11.00000   -1.20000
AFIX   0
C6    1    0.633321    0.839255    0.416382    11.00000    0.03612    0.08023 =
         0.06476   -0.04365   -0.01490    0.03193
AFIX  43
H6    2    0.576281    0.888337    0.424790    11.00000   -1.20000
AFIX   0
C7    1    0.621746    0.737962    0.377383    11.00000    0.02627    0.03640 =
         0.01855   -0.00407   -0.00260    0.00601
C8    1    0.712354    0.676036    0.369224    11.00000    0.02696    0.02683 =
         0.01791    0.00080   -0.00544   -0.00008
AFIX  43
H8    2    0.709457    0.604685    0.342328    11.00000   -1.20000
AFIX   0
C9    1    0.420041    0.723434    0.244623    11.00000    0.02027    0.02633 =
         0.01763    0.00088   -0.00190   -0.00195
C10   1    0.518726    0.760295    0.282675    11.00000    0.01385    0.03002 =
         0.01865   -0.00204    0.00024    0.00174
AFIX  23
H10A  2    0.523932    0.859701    0.286387    11.00000   -1.20000
H10B  2    0.576767    0.728035    0.264762    11.00000   -1.20000
AFIX   0
C11   1    0.522820    0.696383    0.342273    11.00000    0.02385    0.03110 =
         0.02100   -0.00117   -0.00505    0.00343
C12   1    0.514603    0.542287    0.335931    11.00000    0.03321    0.03686 =
         0.03005    0.00529   -0.00290    0.00341
AFIX  23
H12A  2    0.516956    0.500170    0.373872    11.00000   -1.20000
H12B  2    0.572272    0.507633    0.318312    11.00000   -1.20000
AFIX   0
C13   1    0.414918    0.504517    0.298604    11.00000    0.03260    0.02765 =
         0.04003    0.01106   -0.00606   -0.00265
AFIX  13
H13   2    0.410639    0.404065    0.294719    11.00000   -1.20000
AFIX   0
C14   1    0.413391    0.567670    0.239614    11.00000    0.02734    0.02622 =
         0.03385   -0.00419   -0.00233   -0.00663
AFIX  23
H14A  2    0.350391    0.541995    0.215032    11.00000   -1.20000
H14B  2    0.471030    0.533192    0.221922    11.00000   -1.20000
AFIX   0
C15   1    0.329985    0.772620    0.272984    11.00000    0.01720    0.03758 =
         0.02496    0.00465   -0.00325    0.00207
AFIX  23
H15A  2    0.332501    0.872168    0.276710    11.00000   -1.20000
H15B  2    0.266170    0.748193    0.248888    11.00000   -1.20000
AFIX   0
C16   1    0.332671    0.708577    0.331754    11.00000    0.01842    0.05501 =
         0.02737    0.00476    0.00135    0.00458
AFIX  13
H16   2    0.274436    0.742404    0.349876    11.00000   -1.20000
AFIX   0
C17   1    0.431378    0.748208    0.368292    11.00000    0.02941    0.04605 =
         0.01684    0.00341    0.00420    0.00733
AFIX  23
H17A  2    0.432842    0.710077    0.406905    11.00000   -1.20000
H17B  2    0.435102    0.847764    0.371723    11.00000   -1.20000
AFIX   0
C18   1    0.325882    0.554908    0.325686    11.00000    0.03954    0.05207 =
         0.03328    0.01586    0.00044   -0.01244
AFIX  23
H18A  2    0.326525    0.512876    0.363529    11.00000   -1.20000
H18B  2    0.262092    0.529742    0.301734    11.00000   -1.20000
AFIX   0
C25   1    0.637626    1.188731    0.235495    11.00000    0.02514    0.02647 =
         0.01923   -0.00212   -0.00388   -0.00658
C26   1    0.888194    1.247453    0.427326    11.00000    0.01844    0.02869 =
         0.01685    0.00261   -0.00489   -0.00602
C27   1    0.716558    1.164348    0.284917    11.00000    0.02504    0.02040 =
         0.01568   -0.00104   -0.00488   -0.00277
C28   1    0.779814    1.056921    0.296278    11.00000    0.03757    0.02312 =
         0.02368   -0.00674   -0.00645   -0.00157
AFIX  43
H28   2    0.778932    0.979558    0.272580    11.00000   -1.20000
AFIX   0
C29   1    0.846585    1.073487    0.347065    11.00000    0.02851    0.02947 =
         0.02529   -0.00256   -0.01127    0.00567
AFIX  43
H29   2    0.895446    1.008005    0.361397    11.00000   -1.20000
AFIX   0
C30   1    0.834116    1.191718    0.373276    11.00000    0.01881    0.02437 =
         0.01722    0.00305   -0.00397   -0.00118
O1W   4    1.082898    0.970189    0.443842    11.00000    0.05139    0.03358 =
         0.03079    0.00367   -0.00348    0.00898
AFIX   3
H3W   2    1.043538    1.037220    0.444792    11.00000   -1.50000
H4W   2    1.077868    0.920149    0.472362    11.00000   -1.50000
AFIX   0
O2W   4    1.283646    0.973029    0.430037    11.00000    0.07202    0.24110 =
         0.07968   -0.03626    0.00185    0.06965
AFIX   3
H5W   2    1.303705    0.904549    0.450037    11.00000   -1.50000
H6W   2    1.220876    0.983079    0.430987    11.00000   -1.50000
AFIX   0
O3W   4    0.426715    1.113835    0.285918    10.50000    0.06187    0.06494 =
         0.27802   -0.00172    0.02405    0.00160
O4W   4    1.395056    1.129135    0.391919    10.50000    0.10110    0.07566 =
         0.25948    0.05381    0.02714    0.02250
O51W  4   -0.071380    0.621510    0.013229    10.30000    0.07550
O52W  4   -0.084956    0.665382    0.067458    10.20000    0.07613
HKLF    4
 
REM  dk2 in P2(1)/n
REM R1 =  0.0494 for   4502 Fo > 4sig(Fo)  and  0.0961 for all   6862 data
REM    477 parameters refined using     42 restraints
 
END
 
WGHT      0.0454      0.0000
REM Highest difference peak  0.599,  deepest hole -0.507,  1-sigma level  0.093
Q1    1   0.5903  1.2038  0.1096  11.00000  0.05    0.60
Q2    1   1.3845  1.1177  0.3391  11.00000  0.05    0.57
Q3    1   0.6012  1.0385  0.1059  11.00000  0.05    0.55
Q4    1   0.4420  1.0762  0.2812  11.00000  0.05    0.49
Q5    1   0.5000  1.0000  0.0000  10.50000  0.05    0.48
Q6    1   0.5111  1.0381  0.1242  11.00000  0.05    0.43
Q7    1   0.4562  1.0969  0.0505  11.00000  0.05    0.41
Q8    1   0.4020  1.1249 -0.0004  11.00000  0.05    0.39
Q9    1   0.3083  1.0589  0.0069  11.00000  0.05    0.37
Q10   1   0.7837  1.2790  0.3593  11.00000  0.05    0.36
;
_database_code_depnum_ccdc_archive 'CCDC 967345'
#######################################################################
#
#                 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_(4a)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Poly[bis-[μ₄-[1,3-bis(pyridazin-4-yl)adamantane-κ⁴N1:N2:N3:N4)]]-
tetrakis-[μ₂-(1,3-benzenedicarboxylato)]-di(μ₂-hydroxido)-
diaquapentacopper(II)] pentahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H62 Cu5 N8 O20, 5(H2 O)'
_chemical_formula_sum            'C68 H72 Cu5 N8 O25'
_chemical_formula_weight         1719.04

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_space_group_name_Hall           '-P 2yn'
_symmetry_Int_Tables_number      14


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                   10.0517(7)
_cell_length_b                   18.4855(9)
_cell_length_c                   19.1143(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.721(5)
_cell_angle_gamma                90.00
_cell_volume                     3435.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.54

_exptl_crystal_description       prism
_exptl_crystal_colour            green-blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1762
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7282
_exptl_absorpt_correction_T_max  0.7601
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       'φ oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            28251
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         28.54
_reflns_number_total             8582
_reflns_number_gt                6087
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#


_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.

 The refinement of the framework portion (including coordinated water 
 molecules) was standard. The CH-hydrogen atoms were added geometrically, 
 with Uiso = 1.2Ueq(C) and OH-hydrogen atoms were located and included 
 with fixed d(O-H) = 0.85 A and Uiso = 1.5Ueq(O). The solvate water 
 molecules, however, are disordered. Two of them adopt pairs of closely 
 separated positions (O11W and O12W at 0.89 A; O21W and O22W at 0.72 A) 
 and the third one (occupancy 0.50) is at 1.97 A near O11W position. The 
 refined partial occupancy factors were 0.6 and 0.4 in the first two cases. 
 These disordered oxygen atoms (2.5 in assymmetric part, or 5 equivalents 
 per centrosymmetric pentanuclear unit) were refined anisotropically 
 giving reasonable thermal parameters (Ueq = 0.0329(8)-0.0476(16) A2), 
 but the hydrogen atoms were not added due to the disorder.
;

_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)+(0.0544P)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_number_reflns         8582
_refine_ls_number_parameters     502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_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 0.03385(10) Uani 1 2 d S . .
Cu2 Cu 0.70771(4) 0.413612(17) 0.428978(18) 0.04441(10) Uani 1 1 d . . .
Cu3 Cu 0.69635(3) 0.383357(16) 0.254732(17) 0.03557(8) Uani 1 1 d . . .
O1 O 0.60294(19) 0.49790(9) 0.42876(10) 0.0420(4) Uani 1 1 d . . .
H1H H 0.6347 0.5384 0.4188 0.063 Uiso 1 1 d R . .
O2 O 0.8324(2) 0.45887(11) 0.37453(12) 0.0535(5) Uani 1 1 d . . .
H1W H 0.7926 0.4927 0.3467 0.080 Uiso 1 1 d R . .
H2W H 0.9070 0.4485 0.3632 0.080 Uiso 1 1 d R . .
O3 O 0.8084(2) 0.32416(10) 0.43387(11) 0.0484(4) Uani 1 1 d . . .
O4 O 0.74672(19) 0.29708(10) 0.31613(11) 0.0471(4) Uani 1 1 d . . .
O5 O 0.7563(2) 0.04920(12) 0.23490(12) 0.0585(5) Uani 1 1 d . . .
O6 O 0.84936(19) -0.03679(10) 0.31464(11) 0.0484(4) Uani 1 1 d . . .
O7 O 0.50603(16) 0.37932(10) 0.26312(10) 0.0426(4) Uani 1 1 d . . .
O8 O 0.5175(2) 0.31059(13) 0.17053(12) 0.0595(5) Uani 1 1 d . . .
O9 O 0.0342(2) 0.38922(13) 0.33084(14) 0.0621(6) Uani 1 1 d . . .
O10 O -0.13221(18) 0.37531(14) 0.22963(12) 0.0629(6) Uani 1 1 d . . .
O11W O 0.6914(16) 0.2745(11) 0.0849(10) 0.113(7) Uani 0.40 1 d P . .
O12W O 0.6570(12) 0.2411(7) 0.0856(8) 0.103(3) Uani 0.60 1 d P . .
O21W O 0.7699(12) 0.1329(8) 0.1129(7) 0.104(4) Uani 0.40 1 d P . .
O22W O 0.8415(6) 0.1275(3) 0.1324(4) 0.0725(18) Uani 0.60 1 d P . .
O3W O 0.7770(8) 0.3847(4) 0.0818(3) 0.105(2) Uani 0.50 1 d P . .
N1 N 0.4292(2) 0.39128(12) 0.45669(12) 0.0419(5) Uani 1 1 d . . .
N2 N 0.5213(2) 0.35292(12) 0.43162(12) 0.0399(5) Uani 1 1 d . . .
N3 N 0.2802(2) 0.07989(12) 0.04887(12) 0.0425(5) Uani 1 1 d . . .
N4 N 0.1813(2) 0.05260(12) 0.07701(12) 0.0406(5) Uani 1 1 d . . .
C1 C 0.3107(3) 0.36046(16) 0.45686(16) 0.0483(6) Uani 1 1 d . . .
H1 H 0.2463 0.3879 0.4726 0.058 Uiso 1 1 calc R . .
C2 C 0.2762(3) 0.28974(17) 0.43507(16) 0.0487(6) Uani 1 1 d . . .
H2 H 0.1914 0.2706 0.4366 0.058 Uiso 1 1 calc R . .
C3 C 0.3699(3) 0.24850(15) 0.41117(14) 0.0395(5) Uani 1 1 d . . .
C4 C 0.4920(3) 0.28566(14) 0.40989(15) 0.0429(6) Uani 1 1 d . . .
H4 H 0.5570 0.2607 0.3923 0.052 Uiso 1 1 calc R . .
C5 C 0.3933(3) 0.10580(16) 0.09387(16) 0.0497(7) Uani 1 1 d . . .
H5 H 0.4630 0.1233 0.0745 0.060 Uiso 1 1 calc R . .
C6 C 0.4124(3) 0.10809(16) 0.16783(15) 0.0480(6) Uani 1 1 d . . .
H6 H 0.4938 0.1262 0.1973 0.058 Uiso 1 1 calc R . .
C7 C 0.3095(2) 0.08328(14) 0.19762(14) 0.0385(5) Uani 1 1 d . . .
C8 C 0.1953(3) 0.05422(15) 0.14756(14) 0.0409(5) Uani 1 1 d . . .
H8 H 0.1249 0.0348 0.1652 0.049 Uiso 1 1 calc R . .
C9 C 0.3496(2) 0.17030(14) 0.38691(14) 0.0394(5) Uani 1 1 d . . .
C10 C 0.3368(2) 0.16530(13) 0.30467(13) 0.0364(5) Uani 1 1 d . . .
H10A H 0.2588 0.1939 0.2789 0.044 Uiso 1 1 calc R . .
H10B H 0.4190 0.1852 0.2942 0.044 Uiso 1 1 calc R . .
C11 C 0.3178(2) 0.08605(14) 0.27806(14) 0.0380(5) Uani 1 1 d . . .
C12 C 0.4435(3) 0.04205(15) 0.31961(15) 0.0445(6) Uani 1 1 d . . .
H12A H 0.4341 -0.0079 0.3036 0.053 Uiso 1 1 calc R . .
H12B H 0.5266 0.0615 0.3098 0.053 Uiso 1 1 calc R . .
C13 C 0.4544(3) 0.04558(16) 0.40109(16) 0.0496(6) Uani 1 1 d . . .
H13 H 0.5340 0.0171 0.4269 0.060 Uiso 1 1 calc R . .
C14 C 0.4740(3) 0.12384(15) 0.42668(15) 0.0460(6) Uani 1 1 d . . .
H14A H 0.5576 0.1430 0.4173 0.055 Uiso 1 1 calc R . .
H14B H 0.4833 0.1259 0.4784 0.055 Uiso 1 1 calc R . .
C15 C 0.2182(3) 0.13750(17) 0.40196(15) 0.0472(6) Uani 1 1 d . . .
H15A H 0.2241 0.1399 0.4533 0.057 Uiso 1 1 calc R . .
H15B H 0.1386 0.1653 0.3767 0.057 Uiso 1 1 calc R . .
C16 C 0.2013(3) 0.05898(17) 0.37687(15) 0.0481(6) Uani 1 1 d . . .
H16 H 0.1178 0.0392 0.3871 0.058 Uiso 1 1 calc R . .
C17 C 0.1874(3) 0.05534(15) 0.29551(14) 0.0416(6) Uani 1 1 d . . .
H17A H 0.1077 0.0830 0.2701 0.050 Uiso 1 1 calc R . .
H17B H 0.1740 0.0055 0.2793 0.050 Uiso 1 1 calc R . .
C18 C 0.3246(3) 0.01406(17) 0.41654(17) 0.0558(7) Uani 1 1 d . . .
H18A H 0.3128 -0.0358 0.4002 0.067 Uiso 1 1 calc R . .
H18B H 0.3321 0.0149 0.4681 0.067 Uiso 1 1 calc R . .
C19 C 0.7960(2) 0.28176(13) 0.38106(14) 0.0374(5) Uani 1 1 d . . .
C20 C 0.8111(3) 0.02754(14) 0.29750(16) 0.0425(6) Uani 1 1 d . . .
C21 C 0.8331(2) 0.20435(13) 0.39889(14) 0.0372(5) Uani 1 1 d . . .
C22 C 0.8129(2) 0.15400(13) 0.34314(14) 0.0382(5) Uani 1 1 d . . .
H22 H 0.7846 0.1693 0.2953 0.046 Uiso 1 1 calc R . .
C23 C 0.8347(2) 0.08077(14) 0.35864(15) 0.0401(5) Uani 1 1 d . . .
C24 C 0.8759(3) 0.05863(15) 0.43029(16) 0.0482(6) Uani 1 1 d . . .
H24 H 0.8889 0.0097 0.4410 0.058 Uiso 1 1 calc R . .
C25 C 0.8977(3) 0.10855(16) 0.48576(16) 0.0518(7) Uani 1 1 d . . .
H25 H 0.9261 0.0932 0.5336 0.062 Uiso 1 1 calc R . .
C26 C 0.8772(3) 0.18158(14) 0.47004(15) 0.0442(6) Uani 1 1 d . . .
H26 H 0.8932 0.2153 0.5074 0.053 Uiso 1 1 calc R . .
C27 C 0.4515(3) 0.33818(14) 0.21060(15) 0.0413(6) Uani 1 1 d . . .
C28 C -0.0094(3) 0.36845(16) 0.26848(18) 0.0488(7) Uani 1 1 d . . .
C29 C 0.3008(2) 0.32168(14) 0.19693(14) 0.0388(5) Uani 1 1 d . . .
C30 C 0.2223(2) 0.35026(14) 0.24087(15) 0.0393(5) Uani 1 1 d . . .
H30 H 0.2626 0.3807 0.2792 0.047 Uiso 1 1 calc R . .
C31 C 0.0834(3) 0.33297(15) 0.22697(16) 0.0456(6) Uani 1 1 d . . .
C32 C 0.0272(3) 0.28452(19) 0.1722(2) 0.0634(9) Uani 1 1 d . . .
H32 H -0.0648 0.2715 0.1641 0.076 Uiso 1 1 calc R . .
C33 C 0.1051(3) 0.25518(19) 0.1295(2) 0.0641(9) Uani 1 1 d . . .
H33 H 0.0662 0.2224 0.0931 0.077 Uiso 1 1 calc R . .
C34 C 0.2412(3) 0.27497(16) 0.14111(17) 0.0500(6) Uani 1 1 d . . .
H34 H 0.2933 0.2568 0.1113 0.060 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 1.9086(16) . ?
Cu1 O1 1.9086(16) 3_666 ?
Cu1 N1 2.221(2) . ?
Cu1 N1 2.221(2) 3_666 ?
Cu1 N4 2.252(2) 2 ?
Cu1 N4 2.252(2) 4_666 ?
Cu2 O1 1.8800(16) . ?
Cu2 O3 1.9286(17) . ?
Cu2 O2 2.0040(18) . ?
Cu2 N2 2.195(2) . ?
Cu2 N3 2.224(2) 4_666 ?
Cu3 O10 1.9085(17) 1_655 ?
Cu3 O6 1.9593(19) 2_655 ?
Cu3 O7 1.9614(16) . ?
Cu3 O4 1.9685(18) . ?
Cu3 O8 2.482(2) . ?
Cu3 C27 2.532(3) . ?
Cu3 O2 2.733(2) . ?
O1 H1H 0.8538 . ?
O2 H1W 0.8525 . ?
O2 H2W 0.8536 . ?
O3 C19 1.259(3) . ?
O4 C19 1.246(3) . ?
O5 C20 1.249(4) . ?
O6 C20 1.267(3) . ?
O7 C27 1.268(3) . ?
O8 C27 1.243(3) . ?
O9 C28 1.222(4) . ?
O10 C28 1.275(3) . ?
N1 C1 1.321(3) . ?
N1 N2 1.347(3) . ?
N2 C4 1.320(3) . ?
N3 C5 1.328(4) . ?
N3 N4 1.343(3) . ?
N4 C8 1.320(3) . ?
C1 C2 1.389(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.412(3) . ?
C3 C9 1.516(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.378(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.380(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.401(4) . ?
C7 C11 1.519(4) . ?
C8 H8 0.9300 . ?
C9 C15 1.545(3) . ?
C9 C10 1.547(3) . ?
C9 C14 1.548(4) . ?
C10 C11 1.547(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C17 1.541(3) . ?
C11 C12 1.543(4) . ?
C12 C13 1.535(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.524(4) . ?
C13 C18 1.525(4) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.524(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C18 1.524(4) . ?
C16 C17 1.527(4) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C21 1.496(3) . ?
C20 C23 1.500(4) . ?
C21 C26 1.385(4) . ?
C21 C22 1.390(4) . ?
C22 C23 1.391(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.388(4) . ?
C24 C25 1.380(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.387(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C29 1.502(3) . ?
C28 C31 1.519(4) . ?
C29 C34 1.385(4) . ?
C29 C30 1.394(3) . ?
C30 C31 1.391(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.385(4) . ?
C32 C33 1.378(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.378(4) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?

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 O1 180.0 . 3_666 ?
O1 Cu1 N1 84.03(8) . . ?
O1 Cu1 N1 95.97(8) 3_666 . ?
O1 Cu1 N1 95.97(8) . 3_666 ?
O1 Cu1 N1 84.03(8) 3_666 3_666 ?
N1 Cu1 N1 180.0 . 3_666 ?
O1 Cu1 N4 92.17(8) . 2 ?
O1 Cu1 N4 87.83(8) 3_666 2 ?
N1 Cu1 N4 91.01(8) . 2 ?
N1 Cu1 N4 88.99(8) 3_666 2 ?
O1 Cu1 N4 87.83(8) . 4_666 ?
O1 Cu1 N4 92.17(8) 3_666 4_666 ?
N1 Cu1 N4 88.99(8) . 4_666 ?
N1 Cu1 N4 91.01(8) 3_666 4_666 ?
N4 Cu1 N4 180.00(10) 2 4_666 ?
O1 Cu2 O3 175.93(8) . . ?
O1 Cu2 O2 94.40(8) . . ?
O3 Cu2 O2 89.63(8) . . ?
O1 Cu2 N2 86.72(8) . . ?
O3 Cu2 N2 90.06(8) . . ?
O2 Cu2 N2 151.07(9) . . ?
O1 Cu2 N3 89.66(8) . 4_666 ?
O3 Cu2 N3 88.05(8) . 4_666 ?
O2 Cu2 N3 115.35(9) . 4_666 ?
N2 Cu2 N3 93.55(8) . 4_666 ?
O10 Cu3 O6 87.71(9) 1_655 2_655 ?
O10 Cu3 O7 168.34(10) 1_655 . ?
O6 Cu3 O7 91.04(8) 2_655 . ?
O10 Cu3 O4 88.56(9) 1_655 . ?
O6 Cu3 O4 173.94(9) 2_655 . ?
O7 Cu3 O4 91.65(8) . . ?
O10 Cu3 O8 110.26(9) 1_655 . ?
O6 Cu3 O8 87.87(8) 2_655 . ?
O7 Cu3 O8 58.10(7) . . ?
O4 Cu3 O8 88.95(8) . . ?
O10 Cu3 C27 138.92(10) 1_655 . ?
O6 Cu3 C27 88.97(8) 2_655 . ?
O7 Cu3 C27 29.43(8) . . ?
O4 Cu3 C27 90.71(8) . . ?
O8 Cu3 C27 28.67(7) . . ?
O10 Cu3 O2 87.65(9) 1_655 . ?
O6 Cu3 O2 99.42(7) 2_655 . ?
O7 Cu3 O2 103.98(7) . . ?
O4 Cu3 O2 85.19(7) . . ?
O8 Cu3 O2 161.03(6) . . ?
C27 Cu3 O2 133.20(7) . . ?
Cu2 O1 Cu1 114.85(9) . . ?
Cu2 O1 H1H 119.1 . . ?
Cu1 O1 H1H 116.3 . . ?
Cu2 O2 Cu3 88.63(8) . . ?
Cu2 O2 H1W 112.0 . . ?
Cu3 O2 H1W 78.2 . . ?
Cu2 O2 H2W 138.0 . . ?
Cu3 O2 H2W 87.5 . . ?
H1W O2 H2W 108.1 . . ?
C19 O3 Cu2 123.44(17) . . ?
C19 O4 Cu3 139.00(18) . . ?
C20 O6 Cu3 121.90(18) . 2_645 ?
C27 O7 Cu3 101.08(14) . . ?
C27 O8 Cu3 77.86(17) . . ?
C28 O10 Cu3 131.6(2) . 1_455 ?
C1 N1 N2 118.4(2) . . ?
C1 N1 Cu1 126.37(17) . . ?
N2 N1 Cu1 115.15(16) . . ?
C4 N2 N1 119.3(2) . . ?
C4 N2 Cu2 126.72(16) . . ?
N1 N2 Cu2 114.00(16) . . ?
C5 N3 N4 118.3(2) . . ?
C5 N3 Cu2 130.54(18) . 4_565 ?
N4 N3 Cu2 110.55(16) . 4_565 ?
C8 N4 N3 120.2(2) . . ?
C8 N4 Cu1 122.42(16) . 2_545 ?
N3 N4 Cu1 117.31(16) . 2_545 ?
N1 C1 C2 124.2(2) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C3 C2 C1 118.7(2) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 114.0(2) . . ?
C2 C3 C9 125.4(2) . . ?
C4 C3 C9 120.6(2) . . ?
N2 C4 C3 125.3(2) . . ?
N2 C4 H4 117.3 . . ?
C3 C4 H4 117.3 . . ?
N3 C5 C6 123.3(2) . . ?
N3 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C7 119.3(3) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C8 114.5(2) . . ?
C6 C7 C11 123.5(2) . . ?
C8 C7 C11 121.9(2) . . ?
N4 C8 C7 124.2(2) . . ?
N4 C8 H8 117.9 . . ?
C7 C8 H8 117.9 . . ?
C3 C9 C15 111.9(2) . . ?
C3 C9 C10 109.7(2) . . ?
C15 C9 C10 108.1(2) . . ?
C3 C9 C14 110.5(2) . . ?
C15 C9 C14 108.2(2) . . ?
C10 C9 C14 108.3(2) . . ?
C11 C10 C9 111.2(2) . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C7 C11 C17 112.1(2) . . ?
C7 C11 C12 109.3(2) . . ?
C17 C11 C12 109.0(2) . . ?
C7 C11 C10 109.6(2) . . ?
C17 C11 C10 108.6(2) . . ?
C12 C11 C10 108.3(2) . . ?
C13 C12 C11 109.7(2) . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C18 110.4(2) . . ?
C14 C13 C12 109.6(2) . . ?
C18 C13 C12 109.7(2) . . ?
C14 C13 H13 109.0 . . ?
C18 C13 H13 109.0 . . ?
C12 C13 H13 109.0 . . ?
C13 C14 C9 110.3(2) . . ?
C13 C14 H14A 109.6 . . ?
C9 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
C9 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C9 110.3(2) . . ?
C16 C15 H15A 109.6 . . ?
C9 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C9 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C18 C16 C15 110.5(2) . . ?
C18 C16 C17 109.6(2) . . ?
C15 C16 C17 109.6(2) . . ?
C18 C16 H16 109.0 . . ?
C15 C16 H16 109.0 . . ?
C17 C16 H16 109.0 . . ?
C16 C17 C11 110.0(2) . . ?
C16 C17 H17A 109.7 . . ?
C11 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
C11 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
C16 C18 C13 108.9(2) . . ?
C16 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 . . ?
C16 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O4 C19 O3 126.2(2) . . ?
O4 C19 C21 117.2(2) . . ?
O3 C19 C21 116.4(2) . . ?
O5 C20 O6 125.4(3) . . ?
O5 C20 C23 118.7(2) . . ?
O6 C20 C23 115.9(3) . . ?
C26 C21 C22 119.8(2) . . ?
C26 C21 C19 120.9(2) . . ?
C22 C21 C19 119.1(2) . . ?
C21 C22 C23 120.3(2) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 119.2(2) . . ?
C24 C23 C20 121.6(2) . . ?
C22 C23 C20 119.2(2) . . ?
C25 C24 C23 120.7(3) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 119.9(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C21 C26 C25 120.1(3) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
O8 C27 O7 122.9(2) . . ?
O8 C27 C29 118.8(3) . . ?
O7 C27 C29 118.3(2) . . ?
O8 C27 Cu3 73.46(15) . . ?
O7 C27 Cu3 49.49(11) . . ?
C29 C27 Cu3 167.72(19) . . ?
O9 C28 O10 126.2(3) . . ?
O9 C28 C31 122.0(2) . . ?
O10 C28 C31 111.8(3) . . ?
C34 C29 C30 120.0(2) . . ?
C34 C29 C27 118.7(2) . . ?
C30 C29 C27 121.2(2) . . ?
C31 C30 C29 119.5(3) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C32 C31 C30 119.3(2) . . ?
C32 C31 C28 119.2(2) . . ?
C30 C31 C28 121.4(3) . . ?
C33 C32 C31 121.3(3) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C32 C33 C34 119.3(3) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C33 C34 C29 120.5(3) . . ?
C33 C34 H34 119.8 . . ?
C29 C34 H34 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu2 O1 Cu1 -160.66(11) . . . . ?
N2 Cu2 O1 Cu1 48.31(11) . . . . ?
N3 Cu2 O1 Cu1 -45.26(11) 4_666 . . . ?
N1 Cu1 O1 Cu2 -50.07(11) . . . . ?
N1 Cu1 O1 Cu2 129.93(11) 3_666 . . . ?
N4 Cu1 O1 Cu2 -140.86(11) 2 . . . ?
N4 Cu1 O1 Cu2 39.14(11) 4_666 . . . ?
O1 Cu2 O2 Cu3 -105.27(7) . . . . ?
O3 Cu2 O2 Cu3 75.35(7) . . . . ?
N2 Cu2 O2 Cu3 -14.10(18) . . . . ?
N3 Cu2 O2 Cu3 163.01(6) 4_666 . . . ?
O10 Cu3 O2 Cu2 -145.26(9) 1_655 . . . ?
O6 Cu3 O2 Cu2 127.46(8) 2_655 . . . ?
O7 Cu3 O2 Cu2 34.00(9) . . . . ?
O4 Cu3 O2 Cu2 -56.50(8) . . . . ?
O8 Cu3 O2 Cu2 16.0(2) . . . . ?
C27 Cu3 O2 Cu2 29.94(12) . . . . ?
O2 Cu2 O3 C19 -75.8(2) . . . . ?
N2 Cu2 O3 C19 75.3(2) . . . . ?
N3 Cu2 O3 C19 168.9(2) 4_666 . . . ?
O10 Cu3 O4 C19 98.4(3) 1_655 . . . ?
O7 Cu3 O4 C19 -93.3(3) . . . . ?
O8 Cu3 O4 C19 -151.3(3) . . . . ?
C27 Cu3 O4 C19 -122.7(3) . . . . ?
O2 Cu3 O4 C19 10.6(2) . . . . ?
O10 Cu3 O7 C27 2.4(5) 1_655 . . . ?
O6 Cu3 O7 C27 86.06(16) 2_655 . . . ?
O4 Cu3 O7 C27 -88.52(16) . . . . ?
O8 Cu3 O7 C27 -0.78(15) . . . . ?
O2 Cu3 O7 C27 -173.97(15) . . . . ?
O10 Cu3 O8 C27 -178.52(16) 1_655 . . . ?
O6 Cu3 O8 C27 -91.76(17) 2_655 . . . ?
O7 Cu3 O8 C27 0.80(15) . . . . ?
O4 Cu3 O8 C27 93.40(17) . . . . ?
O2 Cu3 O8 C27 21.5(3) . . . . ?
O1 Cu1 N1 C1 -152.0(2) . . . . ?
O1 Cu1 N1 C1 28.0(2) 3_666 . . . ?
N4 Cu1 N1 C1 -59.9(2) 2 . . . ?
N4 Cu1 N1 C1 120.1(2) 4_666 . . . ?
O1 Cu1 N1 N2 31.65(17) . . . . ?
O1 Cu1 N1 N2 -148.35(17) 3_666 . . . ?
N4 Cu1 N1 N2 123.73(18) 2 . . . ?
N4 Cu1 N1 N2 -56.27(18) 4_666 . . . ?
C1 N1 N2 C4 -1.7(4) . . . . ?
Cu1 N1 N2 C4 174.95(19) . . . . ?
C1 N1 N2 Cu2 176.6(2) . . . . ?
Cu1 N1 N2 Cu2 -6.7(2) . . . . ?
O1 Cu2 N2 C4 156.5(2) . . . . ?
O3 Cu2 N2 C4 -26.0(2) . . . . ?
O2 Cu2 N2 C4 63.3(3) . . . . ?
N3 Cu2 N2 C4 -114.1(2) 4_666 . . . ?
O1 Cu2 N2 N1 -21.71(17) . . . . ?
O3 Cu2 N2 N1 155.79(18) . . . . ?
O2 Cu2 N2 N1 -114.9(2) . . . . ?
N3 Cu2 N2 N1 67.75(18) 4_666 . . . ?
C5 N3 N4 C8 2.4(4) . . . . ?
Cu2 N3 N4 C8 -169.8(2) 4_565 . . . ?
C5 N3 N4 Cu1 -174.5(2) . . . 2_545 ?
Cu2 N3 N4 Cu1 13.2(2) 4_565 . . 2_545 ?
N2 N1 C1 C2 2.3(4) . . . . ?
Cu1 N1 C1 C2 -173.9(2) . . . . ?
N1 C1 C2 C3 -0.4(5) . . . . ?
C1 C2 C3 C4 -1.8(4) . . . . ?
C1 C2 C3 C9 178.8(3) . . . . ?
N1 N2 C4 C3 -0.8(4) . . . . ?
Cu2 N2 C4 C3 -178.9(2) . . . . ?
C2 C3 C4 N2 2.5(4) . . . . ?
C9 C3 C4 N2 -178.1(3) . . . . ?
N4 N3 C5 C6 -2.1(4) . . . . ?
Cu2 N3 C5 C6 168.4(2) 4_565 . . . ?
N3 C5 C6 C7 -0.8(5) . . . . ?
C5 C6 C7 C8 3.0(4) . . . . ?
C5 C6 C7 C11 -177.5(3) . . . . ?
N3 N4 C8 C7 0.0(4) . . . . ?
Cu1 N4 C8 C7 176.8(2) 2_545 . . . ?
C6 C7 C8 N4 -2.8(4) . . . . ?
C11 C7 C8 N4 177.8(2) . . . . ?
C2 C3 C9 C15 -8.0(4) . . . . ?
C4 C3 C9 C15 172.6(2) . . . . ?
C2 C3 C9 C10 112.0(3) . . . . ?
C4 C3 C9 C10 -67.3(3) . . . . ?
C2 C3 C9 C14 -128.7(3) . . . . ?
C4 C3 C9 C14 52.0(3) . . . . ?
C3 C9 C10 C11 179.29(19) . . . . ?
C15 C9 C10 C11 -58.5(3) . . . . ?
C14 C9 C10 C11 58.6(3) . . . . ?
C6 C7 C11 C17 179.4(3) . . . . ?
C8 C7 C11 C17 -1.2(3) . . . . ?
C6 C7 C11 C12 -59.7(3) . . . . ?
C8 C7 C11 C12 119.7(3) . . . . ?
C6 C7 C11 C10 58.8(3) . . . . ?
C8 C7 C11 C10 -121.9(3) . . . . ?
C9 C10 C11 C7 -178.50(19) . . . . ?
C9 C10 C11 C17 58.8(3) . . . . ?
C9 C10 C11 C12 -59.4(2) . . . . ?
C7 C11 C12 C13 179.0(2) . . . . ?
C17 C11 C12 C13 -58.2(3) . . . . ?
C10 C11 C12 C13 59.7(3) . . . . ?
C11 C12 C13 C14 -61.3(3) . . . . ?
C11 C12 C13 C18 60.1(3) . . . . ?
C18 C13 C14 C9 -60.1(3) . . . . ?
C12 C13 C14 C9 60.8(3) . . . . ?
C3 C9 C14 C13 -178.9(2) . . . . ?
C15 C9 C14 C13 58.3(3) . . . . ?
C10 C9 C14 C13 -58.7(3) . . . . ?
C3 C9 C15 C16 180.0(2) . . . . ?
C10 C9 C15 C16 59.0(3) . . . . ?
C14 C9 C15 C16 -58.1(3) . . . . ?
C9 C15 C16 C18 59.9(3) . . . . ?
C9 C15 C16 C17 -61.0(3) . . . . ?
C18 C16 C17 C11 -60.6(3) . . . . ?
C15 C16 C17 C11 60.9(3) . . . . ?
C7 C11 C17 C16 179.7(2) . . . . ?
C12 C11 C17 C16 58.6(3) . . . . ?
C10 C11 C17 C16 -59.1(3) . . . . ?
C15 C16 C18 C13 -59.6(3) . . . . ?
C17 C16 C18 C13 61.4(3) . . . . ?
C14 C13 C18 C16 59.7(3) . . . . ?
C12 C13 C18 C16 -61.2(3) . . . . ?
Cu3 O4 C19 O3 14.1(4) . . . . ?
Cu3 O4 C19 C21 -171.52(17) . . . . ?
Cu2 O3 C19 O4 18.3(3) . . . . ?
Cu2 O3 C19 C21 -156.13(16) . . . . ?
Cu3 O6 C20 O5 -8.8(4) 2_645 . . . ?
Cu3 O6 C20 C23 171.00(15) 2_645 . . . ?
O4 C19 C21 C26 -174.4(2) . . . . ?
O3 C19 C21 C26 0.6(3) . . . . ?
O4 C19 C21 C22 0.8(3) . . . . ?
O3 C19 C21 C22 175.7(2) . . . . ?
C26 C21 C22 C23 1.0(4) . . . . ?
C19 C21 C22 C23 -174.2(2) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
C21 C22 C23 C20 179.6(2) . . . . ?
O5 C20 C23 C24 170.3(2) . . . . ?
O6 C20 C23 C24 -9.6(3) . . . . ?
O5 C20 C23 C22 -8.8(3) . . . . ?
O6 C20 C23 C22 171.4(2) . . . . ?
C22 C23 C24 C25 -1.3(4) . . . . ?
C20 C23 C24 C25 179.7(3) . . . . ?
C23 C24 C25 C26 0.6(4) . . . . ?
C22 C21 C26 C25 -1.7(4) . . . . ?
C19 C21 C26 C25 173.4(2) . . . . ?
C24 C25 C26 C21 0.9(4) . . . . ?
Cu3 O8 C27 O7 -1.3(2) . . . . ?
Cu3 O8 C27 C29 179.4(2) . . . . ?
Cu3 O7 C27 O8 1.6(3) . . . . ?
Cu3 O7 C27 C29 -179.06(18) . . . . ?
O10 Cu3 C27 O8 2.1(2) 1_655 . . . ?
O6 Cu3 C27 O8 87.43(17) 2_655 . . . ?
O7 Cu3 C27 O8 -178.6(3) . . . . ?
O4 Cu3 C27 O8 -86.52(17) . . . . ?
O2 Cu3 C27 O8 -170.58(14) . . . . ?
O10 Cu3 C27 O7 -179.27(16) 1_655 . . . ?
O6 Cu3 C27 O7 -93.95(16) 2_655 . . . ?
O4 Cu3 C27 O7 92.10(16) . . . . ?
O8 Cu3 C27 O7 178.6(3) . . . . ?
O2 Cu3 C27 O7 8.0(2) . . . . ?
O10 Cu3 C27 C29 -175.4(8) 1_655 . . . ?
O6 Cu3 C27 C29 -90.1(8) 2_655 . . . ?
O7 Cu3 C27 C29 3.9(8) . . . . ?
O4 Cu3 C27 C29 96.0(8) . . . . ?
O8 Cu3 C27 C29 -177.5(9) . . . . ?
O2 Cu3 C27 C29 11.9(9) . . . . ?
Cu3 O10 C28 O9 -26.7(5) 1_455 . . . ?
Cu3 O10 C28 C31 155.6(2) 1_455 . . . ?
O8 C27 C29 C34 1.4(4) . . . . ?
O7 C27 C29 C34 -178.0(2) . . . . ?
Cu3 C27 C29 C34 178.7(7) . . . . ?
O8 C27 C29 C30 179.0(2) . . . . ?
O7 C27 C29 C30 -0.4(4) . . . . ?
Cu3 C27 C29 C30 -3.7(10) . . . . ?
C34 C29 C30 C31 -1.7(4) . . . . ?
C27 C29 C30 C31 -179.2(2) . . . . ?
C29 C30 C31 C32 3.5(4) . . . . ?
C29 C30 C31 C28 -173.9(2) . . . . ?
O9 C28 C31 C32 152.8(3) . . . . ?
O10 C28 C31 C32 -29.5(4) . . . . ?
O9 C28 C31 C30 -29.8(4) . . . . ?
O10 C28 C31 C30 147.9(3) . . . . ?
C30 C31 C32 C33 -2.4(5) . . . . ?
C28 C31 C32 C33 175.0(3) . . . . ?
C31 C32 C33 C34 -0.6(6) . . . . ?
C32 C33 C34 C29 2.5(5) . . . . ?
C30 C29 C34 C33 -1.4(4) . . . . ?
C27 C29 C34 C33 176.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        28.54
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.642
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.065


_iucr_refine_instruction_details 
;
#---------------------------------------------------------

ITL IP2-1783 in P2(1)/n
CELL  0.71073  10.0517  18.4855  19.1143   90.000  104.721   90.000
ZERR     2.00   0.0007   0.0009   0.0013    0.000    0.005    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    CU
UNIT  136  144  16   50   10
MERG   2
OMIT     0.00 180.00
OMIT    -1   0   1
OMIT    12   9   1
BIND CU3 O2
BIND Cu3 O8
FMAP   2
PLAN   10
 
EQIV $1 1.5-X, 0.5+Y, 0.5-Z
EQIV $2 1+X, Y, Z
 
RTAB XHY O2 H1W O5_$1
RTAB XHY O2 H2W O9_$2
RTAB XHY O1 H1H O21W_$1
RTAB XHY O1 H1H O22W_$1
 
RTAB H..O H1W O5_$1
RTAB H..O H2W O9_$2
RTAB H..O H1H O21W_$1
RTAB H..O H1H O22W_$1
 
RTAB O..O O2 O5_$1
RTAB O..O O2 O9_$2
RTAB O..O O1 O21W_$1
RTAB O..O O1 O22W_$1
 
SIZE     0.18   0.20   0.21
ACTA
BOND   $H
CONF
LIST   4
L.S.   4
TEMP    23.00
WGHT    0.054400
FVAR       1.01203
CU1   5    0.500000    0.500000    0.500000    10.50000    0.04105    0.03353 =
         0.02754   -0.00081    0.00978    0.00593
CU2   5    0.707709    0.413612    0.428978    11.00000    0.06206    0.03466 =
         0.04366    0.00458    0.02661    0.01341
CU3   5    0.696353    0.383357    0.254732    11.00000    0.02986    0.03685 =
         0.04081    0.00526    0.01046    0.00242
O1    4    0.602940    0.497899    0.428758    11.00000    0.05410    0.03599 =
         0.04161    0.00405    0.02278    0.00960
AFIX   3
H1H   2    0.634670    0.538379    0.418778    11.00000   -1.50000
AFIX   0
O2    4    0.832381    0.458870    0.374534    11.00000    0.05506    0.04772 =
         0.06668    0.01436    0.03222    0.01336
AFIX   3
H1W   2    0.792551    0.492690    0.346654    11.00000   -1.50000
H2W   2    0.906961    0.448460    0.363194    11.00000   -1.50000
AFIX   0
O3    4    0.808392    0.324156    0.433874    11.00000    0.06466    0.03667 =
         0.04618   -0.00023    0.01861    0.01467
O4    4    0.746721    0.297082    0.316131    11.00000    0.05282    0.03905 =
         0.04476    0.00701    0.00406    0.00571
O5    4    0.756326    0.049200    0.234903    11.00000    0.08126    0.04896 =
         0.04270   -0.00810    0.01107   -0.00372
O6    4    0.849355   -0.036789    0.314645    11.00000    0.04668    0.04051 =
         0.05446   -0.01138    0.00656    0.00435
O7    4    0.506027    0.379318    0.263125    11.00000    0.03173    0.04918 =
         0.04894    0.00049    0.01423    0.00039
O8    4    0.517465    0.310588    0.170526    11.00000    0.04486    0.07399 =
         0.06675   -0.01129    0.02706    0.00140
O9    4    0.034155    0.389217    0.330836    11.00000    0.04145    0.07670 =
         0.07016   -0.00978    0.01762    0.00907
O10   4   -0.132206    0.375308    0.229625    11.00000    0.03240    0.10260 =
         0.05764    0.02132    0.01855    0.01555
O11W  4    0.691381    0.274454    0.084878    10.40000    0.06346    0.22186 =
         0.05296    0.00034    0.01201    0.05266
O12W  4    0.656961    0.241102    0.085644    10.60000    0.08844    0.13839 =
         0.08852   -0.01956    0.03556    0.02423
O21W  4    0.769920    0.132908    0.112948    10.40000    0.13285    0.12014 =
         0.06938   -0.00762    0.04400   -0.02251
O22W  4    0.841513    0.127468    0.132351    10.60000    0.09893    0.04450 =
         0.08774   -0.00587    0.04912   -0.00073
O3W   4    0.776951    0.384658    0.081821    10.50000    0.17232    0.10645 =
         0.03948    0.00920    0.03052    0.05027
N1    3    0.429220    0.391284    0.456688    11.00000    0.04379    0.04466 =
         0.03754   -0.00303    0.01099    0.00691
N2    3    0.521328    0.352920    0.431617    11.00000    0.04231    0.04037 =
         0.03925   -0.00324    0.01460    0.00352
N3    3    0.280172    0.079890    0.048868    11.00000    0.05015    0.04159 =
         0.03787   -0.00080    0.01531   -0.00600
N4    3    0.181329    0.052604    0.077005    11.00000    0.04474    0.04439 =
         0.03252    0.00114    0.00948   -0.00671
C1    1    0.310725    0.360461    0.456856    11.00000    0.04360    0.05636 =
         0.04649   -0.00887    0.01413    0.00657
AFIX  43
H1    2    0.246298    0.387864    0.472562    11.00000   -1.20000
AFIX   0
C2    1    0.276217    0.289736    0.435073    11.00000    0.03795    0.06182 =
         0.04783   -0.01134    0.01341   -0.00228
AFIX  43
H2    2    0.191435    0.270602    0.436604    11.00000   -1.20000
AFIX   0
C3    1    0.369925    0.248503    0.411171    11.00000    0.03979    0.04853 =
         0.02943   -0.00025    0.00759    0.00077
C4    1    0.491975    0.285657    0.409889    11.00000    0.04288    0.04288 =
         0.04669   -0.00508    0.01808    0.00175
AFIX  43
H4    2    0.557031    0.260717    0.392302    11.00000   -1.20000
AFIX   0
C5    1    0.393258    0.105796    0.093873    11.00000    0.04921    0.05734 =
         0.04674   -0.00637    0.01964   -0.01319
AFIX  43
H5    2    0.463007    0.123263    0.074498    11.00000   -1.20000
AFIX   0
C6    1    0.412405    0.108088    0.167830    11.00000    0.04306    0.05980 =
         0.04134   -0.00688    0.01095   -0.01011
AFIX  43
H6    2    0.493813    0.126161    0.197347    11.00000   -1.20000
AFIX   0
C7    1    0.309496    0.083280    0.197620    11.00000    0.04092    0.03875 =
         0.03514    0.00148    0.00864    0.00112
C8    1    0.195346    0.054222    0.147563    11.00000    0.04222    0.04667 =
         0.03429    0.00222    0.01038   -0.00477
AFIX  43
H8    2    0.124879    0.034816    0.165174    11.00000   -1.20000
AFIX   0
C9    1    0.349620    0.170296    0.386913    11.00000    0.03699    0.04624 =
         0.03435    0.00066    0.00796   -0.00156
C10   1    0.336833    0.165300    0.304674    11.00000    0.03449    0.03980 =
         0.03415    0.00137    0.00727    0.00264
AFIX  23
H10A  2    0.258797    0.193869    0.278864    11.00000   -1.20000
H10B  2    0.418954    0.185198    0.294191    11.00000   -1.20000
AFIX   0
C11   1    0.317791    0.086054    0.278064    11.00000    0.03765    0.04182 =
         0.03358    0.00201    0.00728   -0.00051
C12   1    0.443537    0.042054    0.319609    11.00000    0.04102    0.04285 =
         0.04609   -0.00030    0.00479    0.00496
AFIX  23
H12A  2    0.434086   -0.007894    0.303552    11.00000   -1.20000
H12B  2    0.526571    0.061543    0.309814    11.00000   -1.20000
AFIX   0
C13   1    0.454372    0.045575    0.401089    11.00000    0.05246    0.04784 =
         0.03973    0.00674   -0.00457    0.00521
AFIX  13
H13   2    0.533955    0.017066    0.426894    11.00000   -1.20000
AFIX   0
C14   1    0.474025    0.123839    0.426683    11.00000    0.04403    0.05353 =
         0.03468    0.00297   -0.00063   -0.00124
AFIX  23
H14A  2    0.557595    0.143038    0.417262    11.00000   -1.20000
H14B  2    0.483329    0.125894    0.478414    11.00000   -1.20000
AFIX   0
C15   1    0.218206    0.137500    0.401956    11.00000    0.04659    0.06129 =
         0.03621   -0.00322    0.01491   -0.00788
AFIX  23
H15A  2    0.224110    0.139900    0.453350    11.00000   -1.20000
H15B  2    0.138616    0.165278    0.376659    11.00000   -1.20000
AFIX   0
C16   1    0.201287    0.058984    0.376874    11.00000    0.04848    0.05878 =
         0.03849    0.00302    0.01364   -0.01231
AFIX  13
H16   2    0.117820    0.039158    0.387141    11.00000   -1.20000
AFIX   0
C17   1    0.187358    0.055342    0.295508    11.00000    0.04001    0.04694 =
         0.03649    0.00121    0.00737   -0.00711
AFIX  23
H17A  2    0.107723    0.083037    0.270122    11.00000   -1.20000
H17B  2    0.174035    0.005525    0.279298    11.00000   -1.20000
AFIX   0
C18   1    0.324560    0.014061    0.416537    11.00000    0.07139    0.05216 =
         0.03753    0.01021    0.00229   -0.00970
AFIX  23
H18A  2    0.312841   -0.035771    0.400233    11.00000   -1.20000
H18B  2    0.332138    0.014935    0.468143    11.00000   -1.20000
AFIX   0
C19   1    0.795999    0.281756    0.381058    11.00000    0.03396    0.03643 =
         0.04442    0.00164    0.01491    0.00566
C20   1    0.811124    0.027544    0.297496    11.00000    0.03999    0.03962 =
         0.04874   -0.00921    0.01306   -0.00210
C21   1    0.833107    0.204355    0.398892    11.00000    0.03662    0.03489 =
         0.04028   -0.00106    0.01010    0.00481
C22   1    0.812875    0.154000    0.343140    11.00000    0.03910    0.03882 =
         0.03526    0.00169    0.00699    0.00549
AFIX  43
H22   2    0.784646    0.169333    0.295308    11.00000   -1.20000
AFIX   0
C23   1    0.834700    0.080767    0.358638    11.00000    0.03908    0.03756 =
         0.04390   -0.00384    0.01104    0.00279
C24   1    0.875865    0.058634    0.430289    11.00000    0.05864    0.03546 =
         0.04873    0.00412    0.01049    0.00926
AFIX  43
H24   2    0.888875    0.009671    0.441041    11.00000   -1.20000
AFIX   0
C25   1    0.897693    0.108552    0.485757    11.00000    0.07034    0.04466 =
         0.03614    0.00303    0.00577    0.01072
AFIX  43
H25   2    0.926077    0.093238    0.533590    11.00000   -1.20000
AFIX   0
C26   1    0.877229    0.181582    0.470042    11.00000    0.05366    0.04031 =
         0.03653   -0.00530    0.00754    0.00735
AFIX  43
H26   2    0.893169    0.215307    0.507354    11.00000   -1.20000
AFIX   0
C27   1    0.451536    0.338185    0.210596    11.00000    0.03713    0.04401 =
         0.04618    0.01133    0.01707    0.00693
C28   1   -0.009423    0.368452    0.268482    11.00000    0.03418    0.05193 =
         0.06443    0.01373    0.02013    0.00492
C29   1    0.300782    0.321676    0.196932    11.00000    0.03538    0.04041 =
         0.04020    0.00740    0.00889    0.00414
C30   1    0.222344    0.350260    0.240865    11.00000    0.03123    0.04136 =
         0.04513    0.00386    0.00917    0.00235
AFIX  43
H30   2    0.262589    0.380656    0.279170    11.00000   -1.20000
AFIX   0
C31   1    0.083392    0.332967    0.226972    11.00000    0.03468    0.04521 =
         0.05781    0.00463    0.01315    0.00223
C32   1    0.027218    0.284520    0.172186    11.00000    0.03475    0.06686 =
         0.08466   -0.01230    0.00801   -0.00673
AFIX  43
H32   2   -0.064835    0.271534    0.164070    11.00000   -1.20000
AFIX   0
C33   1    0.105055    0.255182    0.129467    11.00000    0.05224    0.06438 =
         0.06882   -0.01792    0.00270   -0.00385
AFIX  43
H33   2    0.066180    0.222363    0.093144    11.00000   -1.20000
AFIX   0
C34   1    0.241154    0.274970    0.141113    11.00000    0.04767    0.05301 =
         0.04925   -0.00321    0.01193    0.00461
AFIX  43
H34   2    0.293318    0.256824    0.111268    11.00000   -1.20000
 
HKLF    4
 
REM  IP2-1783 in P2(1)/n
REM R1 =  0.0362 for   6087 Fo > 4sig(Fo)  and  0.0566 for all   8582 data
REM    502 parameters refined using      0 restraints
 
END
 
WGHT      0.0543      0.0000
REM Highest difference peak  0.642,  deepest hole -1.098,  1-sigma level  0.065
Q1    1   0.7843  0.4334  0.4415  11.00000  0.05    0.64
Q2    1   0.5366  0.4830  0.4405  11.00000  0.05    0.38
Q3    1   0.5982  0.5002  0.4782  11.00000  0.05    0.36
Q4    1   0.6892  0.1830  0.1228  11.00000  0.05    0.34
Q5    1   0.8049  0.1159  0.1682  11.00000  0.05    0.33
Q6    1   0.6000  0.3804  0.4335  11.00000  0.05    0.32
Q7    1   0.6011  0.3811  0.2713  11.00000  0.05    0.32
Q8    1  -0.1953  0.3787  0.2367  11.00000  0.05    0.31
Q9    1   0.7222  0.4422  0.3735  11.00000  0.05    0.28
Q10   1   0.5895  0.2598  0.1023  11.00000  0.05    0.28
;
_database_code_depnum_ccdc_archive 'CCDC 967346'
#######################################################################
#
#                 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_(4b)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Poly[bis-[μ₄-[1,3-bis(pyridazin-4-yl)adamantane-κ⁴N1:N2:N3:N4)]]-
tetrakis-[μ₂-(1,3-benzenedicarboxylato)]-di(μ₂-hydroxido)-
diaquapentacopper(II)] pentahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H62 Cu5 N8 O20, 5(H2 O)'
_chemical_formula_sum            'C68 H72 Cu5 N8 O25'
_chemical_formula_weight         1719.04

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_space_group_name_Hall           '-P 2yn'
_symmetry_Int_Tables_number      14


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                   10.0322(6)
_cell_length_b                   18.4439(9)
_cell_length_c                   19.0354(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.897(5)
_cell_angle_gamma                90.00
_cell_volume                     3403.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      28.54

_exptl_crystal_description       prism
_exptl_crystal_colour            green-blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1762
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7262
_exptl_absorpt_correction_T_max  0.7583
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      105(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  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       'φ oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29554
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         28.54
_reflns_number_total             8508
_reflns_number_gt                6319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#


_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.

 Redetermination of this structure at 105K (compare with 4a CIF data)
 proved temperature dependency of Cu1-N bonds. This allows to attribute
 slightly unusual coordination environment of Cu1 ion (axially compressed
 octahedron) to dynamic disorder of Jahn-Teller axis, rather then to
 unusual d(z²) ground state of Cu. 

 The refinement of the framework portion (including coordinated water 
 molecules) was standard. The CH-hydrogen atoms were added geometrically, 
 with Uiso = 1.2Ueq(C) and OH-hydrogen atoms were located and included 
 with fixed d(O-H) = 0.85 A and Uiso = 1.5Ueq(O). The solvate water 
 molecules, however, are disordered. Two of them adopt pairs of closely 
 separated positions (O11W and O12W at 0.89 A; O21W and O22W at 0.72 A) 
 and the third one (occupancy 0.50) is at 1.97 A near O11W position. The 
 refined partial occupancy factors were 0.6 and 0.4 in the first two cases. 
 These disordered oxygen atoms (2.5 in assymmetric part, or 5 equivalents 
 per centrosymmetric pentanuclear unit) were refined anisotropically 
 giving reasonable thermal parameters, but the hydrogen atoms were not 
 added due to the disorder.
;

_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)+(0.0493P)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_number_reflns         8508
_refine_ls_number_parameters     502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.902
_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 0.01918(8) Uani 1 2 d S . .
Cu2 Cu 0.70003(3) 0.410473(15) 0.426112(15) 0.02206(7) Uani 1 1 d . . .
Cu3 Cu 0.69691(2) 0.380100(15) 0.254123(15) 0.02023(7) Uani 1 1 d . . .
O1 O 0.59573(15) 0.49525(8) 0.42504(8) 0.0220(3) Uani 1 1 d . . .
H1H H 0.6275 0.5357 0.4151 0.033 Uiso 1 1 d R . .
O2 O 0.82966(16) 0.45509(9) 0.37358(9) 0.0292(4) Uani 1 1 d . . .
H1W H 0.7898 0.4889 0.3457 0.044 Uiso 1 1 d R . .
H2W H 0.9042 0.4447 0.3622 0.044 Uiso 1 1 d R . .
O3 O 0.80430(15) 0.32189(8) 0.43446(8) 0.0237(3) Uani 1 1 d . . .
O4 O 0.74838(15) 0.29334(9) 0.31562(9) 0.0245(3) Uani 1 1 d . . .
O5 O 0.75309(17) 0.04497(9) 0.23703(9) 0.0292(4) Uani 1 1 d . . .
O6 O 0.85056(15) -0.04112(8) 0.31717(9) 0.0245(3) Uani 1 1 d . . .
O7 O 0.50646(14) 0.37624(9) 0.26292(9) 0.0231(3) Uani 1 1 d . . .
O8 O 0.51829(16) 0.30668(10) 0.16962(10) 0.0309(4) Uani 1 1 d . . .
O9 O 0.03425(17) 0.38254(10) 0.33392(11) 0.0343(4) Uani 1 1 d . . .
O10 O -0.13022(16) 0.37256(11) 0.22953(10) 0.0385(5) Uani 1 1 d . . .
O11W O 0.6980(5) 0.2784(4) 0.0868(3) 0.0389(12) Uani 0.40 1 d P . .
O12W O 0.6575(4) 0.2352(2) 0.08348(19) 0.0381(8) Uani 0.60 1 d P . .
O21W O 0.7688(8) 0.1304(4) 0.1140(4) 0.0475(16) Uani 0.40 1 d P . .
O22W O 0.8385(4) 0.1224(2) 0.1330(2) 0.0325(8) Uani 0.60 1 d P . .
O3W O 0.7700(4) 0.3770(2) 0.08232(17) 0.0329(8) Uani 0.50 1 d P . .
N1 N 0.42663(18) 0.38652(11) 0.45674(10) 0.0238(4) Uani 1 1 d . . .
N2 N 0.51858(18) 0.34861(10) 0.43032(10) 0.0224(4) Uani 1 1 d . . .
N3 N 0.27679(18) 0.07720(10) 0.04615(10) 0.0232(4) Uani 1 1 d . . .
N4 N 0.17881(18) 0.04879(10) 0.07429(10) 0.0225(4) Uani 1 1 d . . .
C1 C 0.3096(2) 0.35456(14) 0.45892(13) 0.0269(5) Uani 1 1 d . . .
H1 H 0.2445 0.3820 0.4763 0.032 Uiso 1 1 calc R . .
C2 C 0.2759(2) 0.28315(14) 0.43729(12) 0.0268(5) Uani 1 1 d . . .
H2 H 0.1909 0.2625 0.4405 0.032 Uiso 1 1 calc R . .
C3 C 0.3692(2) 0.24316(13) 0.41115(12) 0.0229(4) Uani 1 1 d . . .
C4 C 0.4901(2) 0.28125(12) 0.40833(12) 0.0238(4) Uani 1 1 d . . .
H4 H 0.5558 0.2564 0.3891 0.029 Uiso 1 1 calc R . .
C5 C 0.3915(2) 0.10241(13) 0.09148(13) 0.0265(5) Uani 1 1 d . . .
H5 H 0.4623 0.1207 0.0715 0.032 Uiso 1 1 calc R . .
C6 C 0.4128(2) 0.10328(13) 0.16675(13) 0.0261(5) Uani 1 1 d . . .
H6 H 0.4969 0.1208 0.1973 0.031 Uiso 1 1 calc R . .
C7 C 0.3085(2) 0.07799(12) 0.19595(12) 0.0222(4) Uani 1 1 d . . .
C8 C 0.1928(2) 0.04904(12) 0.14535(12) 0.0225(4) Uani 1 1 d . . .
H8 H 0.1210 0.0286 0.1632 0.027 Uiso 1 1 calc R . .
C9 C 0.3483(2) 0.16446(13) 0.38674(12) 0.0229(4) Uani 1 1 d . . .
C10 C 0.3362(2) 0.16007(12) 0.30397(12) 0.0219(4) Uani 1 1 d . . .
H10A H 0.4206 0.1803 0.2937 0.026 Uiso 1 1 calc R . .
H10B H 0.2567 0.1895 0.2774 0.026 Uiso 1 1 calc R . .
C11 C 0.3166(2) 0.08040(12) 0.27676(12) 0.0219(4) Uani 1 1 d . . .
C12 C 0.4419(2) 0.03562(13) 0.31892(12) 0.0253(5) Uani 1 1 d . . .
H12A H 0.4314 -0.0154 0.3023 0.030 Uiso 1 1 calc R . .
H12B H 0.5273 0.0551 0.3092 0.030 Uiso 1 1 calc R . .
C13 C 0.4528(2) 0.03889(13) 0.40079(13) 0.0280(5) Uani 1 1 d . . .
H13 H 0.5338 0.0094 0.4274 0.034 Uiso 1 1 calc R . .
C14 C 0.4725(2) 0.11763(13) 0.42720(13) 0.0259(5) Uani 1 1 d . . .
H14A H 0.5585 0.1373 0.4183 0.031 Uiso 1 1 calc R . .
H14B H 0.4810 0.1194 0.4802 0.031 Uiso 1 1 calc R . .
C15 C 0.2156(2) 0.13234(14) 0.40086(13) 0.0273(5) Uani 1 1 d . . .
H15A H 0.2209 0.1347 0.4535 0.033 Uiso 1 1 calc R . .
H15B H 0.1350 0.1612 0.3746 0.033 Uiso 1 1 calc R . .
C16 C 0.1974(2) 0.05361(14) 0.37526(13) 0.0279(5) Uani 1 1 d . . .
H16 H 0.1114 0.0337 0.3853 0.033 Uiso 1 1 calc R . .
C17 C 0.1845(2) 0.05012(13) 0.29353(12) 0.0241(4) Uani 1 1 d . . .
H17A H 0.1037 0.0788 0.2672 0.029 Uiso 1 1 calc R . .
H17B H 0.1703 -0.0008 0.2767 0.029 Uiso 1 1 calc R . .
C18 C 0.3208(3) 0.00787(14) 0.41574(13) 0.0317(5) Uani 1 1 d . . .
H18A H 0.3081 -0.0431 0.3990 0.038 Uiso 1 1 calc R . .
H18B H 0.3281 0.0088 0.4686 0.038 Uiso 1 1 calc R . .
C19 C 0.7953(2) 0.27889(12) 0.38179(12) 0.0212(4) Uani 1 1 d . . .
C20 C 0.8109(2) 0.02340(12) 0.30026(12) 0.0232(4) Uani 1 1 d . . .
C21 C 0.8334(2) 0.20144(12) 0.40044(12) 0.0219(4) Uani 1 1 d . . .
C22 C 0.8127(2) 0.15035(12) 0.34518(12) 0.0218(4) Uani 1 1 d . . .
H22 H 0.7836 0.1656 0.2959 0.026 Uiso 1 1 calc R . .
C23 C 0.8341(2) 0.07716(12) 0.36131(13) 0.0231(4) Uani 1 1 d . . .
C24 C 0.8761(2) 0.05559(13) 0.43398(13) 0.0270(5) Uani 1 1 d . . .
H24 H 0.8894 0.0056 0.4455 0.032 Uiso 1 1 calc R . .
C25 C 0.8986(2) 0.10623(13) 0.48939(13) 0.0282(5) Uani 1 1 d . . .
H25 H 0.9283 0.0910 0.5386 0.034 Uiso 1 1 calc R . .
C26 C 0.8778(2) 0.17956(13) 0.47285(12) 0.0236(4) Uani 1 1 d . . .
H26 H 0.8937 0.2146 0.5107 0.028 Uiso 1 1 calc R . .
C27 C 0.4521(2) 0.33401(12) 0.21043(12) 0.0234(4) Uani 1 1 d . . .
C28 C -0.0083(2) 0.36300(13) 0.27007(15) 0.0291(5) Uani 1 1 d . . .
C29 C 0.3019(2) 0.31638(12) 0.19796(12) 0.0224(4) Uani 1 1 d . . .
C30 C 0.2236(2) 0.34499(12) 0.24236(13) 0.0231(4) Uani 1 1 d . . .
H30 H 0.2648 0.3768 0.2811 0.028 Uiso 1 1 calc R . .
C31 C 0.0846(2) 0.32664(13) 0.22944(14) 0.0267(5) Uani 1 1 d . . .
C32 C 0.0279(2) 0.27613(14) 0.17552(15) 0.0334(6) Uani 1 1 d . . .
H32 H -0.0653 0.2614 0.1687 0.040 Uiso 1 1 calc R . .
C33 C 0.1054(2) 0.24726(14) 0.13187(15) 0.0340(6) Uani 1 1 d . . .
H33 H 0.0657 0.2131 0.0951 0.041 Uiso 1 1 calc R . .
C34 C 0.2413(2) 0.26844(13) 0.14225(13) 0.0279(5) Uani 1 1 d . . .
H34 H 0.2939 0.2502 0.1112 0.033 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 1.9160(14) . ?
Cu1 O1 1.9160(14) 3_666 ?
Cu1 N4 2.1732(18) 2 ?
Cu1 N4 2.1732(18) 4_666 ?
Cu1 N1 2.300(2) . ?
Cu1 N1 2.300(2) 3_666 ?
Cu2 O1 1.8785(15) . ?
Cu2 O3 1.9245(15) . ?
Cu2 O2 2.0093(16) . ?
Cu2 N2 2.1672(19) . ?
Cu2 N3 2.227(2) 4_666 ?
Cu3 O10 1.9141(16) 1_655 ?
Cu3 O6 1.9616(16) 2_655 ?
Cu3 O7 1.9617(14) . ?
Cu3 O4 1.9715(16) . ?
Cu3 O8 2.4799(18) . ?
Cu3 C27 2.529(2) . ?
Cu3 O2 2.7019(18) . ?
O1 H1H 0.8520 . ?
O2 H1W 0.8493 . ?
O2 H2W 0.8522 . ?
O3 C19 1.263(3) . ?
O4 C19 1.255(3) . ?
O5 C20 1.259(3) . ?
O6 C20 1.270(3) . ?
O7 C27 1.274(3) . ?
O8 C27 1.250(3) . ?
O9 C28 1.234(3) . ?
O10 C28 1.279(3) . ?
N1 C1 1.324(3) . ?
N1 N2 1.353(3) . ?
N2 C4 1.319(3) . ?
N3 C5 1.332(3) . ?
N3 N4 1.341(3) . ?
N4 C8 1.323(3) . ?
C1 C2 1.395(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.415(3) . ?
C3 C9 1.522(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.409(3) . ?
C7 C11 1.520(3) . ?
C8 H8 0.9500 . ?
C9 C15 1.543(3) . ?
C9 C14 1.549(3) . ?
C9 C10 1.551(3) . ?
C10 C11 1.554(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C17 1.545(3) . ?
C11 C12 1.545(3) . ?
C12 C13 1.535(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.533(3) . ?
C13 C18 1.535(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.528(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.529(3) . ?
C16 C18 1.533(4) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C21 1.498(3) . ?
C20 C23 1.499(3) . ?
C21 C22 1.388(3) . ?
C21 C26 1.395(3) . ?
C22 C23 1.389(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(3) . ?
C24 C25 1.383(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.392(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C29 1.500(3) . ?
C28 C31 1.513(3) . ?
C29 C34 1.394(3) . ?
C29 C30 1.397(3) . ?
C30 C31 1.394(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.395(4) . ?
C32 C33 1.383(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.382(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

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 O1 180.000(1) . 3_666 ?
O1 Cu1 N4 91.28(7) . 2 ?
O1 Cu1 N4 88.72(7) 3_666 2 ?
O1 Cu1 N4 88.72(7) . 4_666 ?
O1 Cu1 N4 91.28(7) 3_666 4_666 ?
N4 Cu1 N4 180.00(9) 2 4_666 ?
O1 Cu1 N1 82.37(7) . . ?
O1 Cu1 N1 97.63(7) 3_666 . ?
N4 Cu1 N1 90.53(7) 2 . ?
N4 Cu1 N1 89.47(7) 4_666 . ?
O1 Cu1 N1 97.63(7) . 3_666 ?
O1 Cu1 N1 82.37(7) 3_666 3_666 ?
N4 Cu1 N1 89.47(7) 2 3_666 ?
N4 Cu1 N1 90.53(7) 4_666 3_666 ?
N1 Cu1 N1 180.0 . 3_666 ?
O1 Cu2 O3 175.53(7) . . ?
O1 Cu2 O2 94.80(7) . . ?
O3 Cu2 O2 88.92(7) . . ?
O1 Cu2 N2 88.16(7) . . ?
O3 Cu2 N2 89.65(7) . . ?
O2 Cu2 N2 153.04(7) . . ?
O1 Cu2 N3 88.33(7) . 4_666 ?
O3 Cu2 N3 87.98(7) . 4_666 ?
O2 Cu2 N3 111.80(7) . 4_666 ?
N2 Cu2 N3 95.05(7) . 4_666 ?
O10 Cu3 O6 87.63(7) 1_655 2_655 ?
O10 Cu3 O7 169.07(8) 1_655 . ?
O6 Cu3 O7 91.00(6) 2_655 . ?
O10 Cu3 O4 88.33(7) 1_655 . ?
O6 Cu3 O4 172.75(7) 2_655 . ?
O7 Cu3 O4 91.84(6) . . ?
O10 Cu3 O8 110.53(7) 1_655 . ?
O6 Cu3 O8 87.10(6) 2_655 . ?
O7 Cu3 O8 58.56(6) . . ?
O4 Cu3 O8 88.69(6) . . ?
O10 Cu3 C27 139.42(8) 1_655 . ?
O6 Cu3 C27 88.79(7) 2_655 . ?
O7 Cu3 C27 29.67(7) . . ?
O4 Cu3 C27 90.37(7) . . ?
O8 Cu3 C27 28.89(6) . . ?
O10 Cu3 O2 87.79(7) 1_655 . ?
O6 Cu3 O2 100.52(6) 2_655 . ?
O7 Cu3 O2 103.12(6) . . ?
O4 Cu3 O2 85.33(6) . . ?
O8 Cu3 O2 160.57(5) . . ?
C27 Cu3 O2 132.51(6) . . ?
Cu2 O1 Cu1 114.48(8) . . ?
Cu2 O1 H1H 119.5 . . ?
Cu1 O1 H1H 114.4 . . ?
Cu2 O2 Cu3 88.11(6) . . ?
Cu2 O2 H1W 110.5 . . ?
Cu3 O2 H1W 78.4 . . ?
Cu2 O2 H2W 139.2 . . ?
Cu3 O2 H2W 86.9 . . ?
H1W O2 H2W 108.0 . . ?
C19 O3 Cu2 122.75(14) . . ?
C19 O4 Cu3 137.89(15) . . ?
C20 O6 Cu3 120.96(15) . 2_645 ?
C27 O7 Cu3 100.67(13) . . ?
C27 O8 Cu3 77.73(13) . . ?
C28 O10 Cu3 130.40(17) . 1_455 ?
C1 N1 N2 118.4(2) . . ?
C1 N1 Cu1 126.79(16) . . ?
N2 N1 Cu1 114.67(13) . . ?
C4 N2 N1 119.48(18) . . ?
C4 N2 Cu2 126.84(14) . . ?
N1 N2 Cu2 113.64(14) . . ?
C5 N3 N4 118.52(19) . . ?
C5 N3 Cu2 129.95(15) . 4_565 ?
N4 N3 Cu2 110.73(13) . 4_565 ?
C8 N4 N3 120.70(18) . . ?
C8 N4 Cu1 121.31(14) . 2_545 ?
N3 N4 Cu1 117.97(14) . 2_545 ?
N1 C1 C2 124.1(2) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 118.4(2) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 114.5(2) . . ?
C2 C3 C9 124.5(2) . . ?
C4 C3 C9 120.96(19) . . ?
N2 C4 C3 125.0(2) . . ?
N2 C4 H4 117.5 . . ?
C3 C4 H4 117.5 . . ?
N3 C5 C6 123.3(2) . . ?
N3 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C7 C6 C5 118.5(2) . . ?
C7 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
C6 C7 C8 115.3(2) . . ?
C6 C7 C11 123.14(19) . . ?
C8 C7 C11 121.56(19) . . ?
N4 C8 C7 123.6(2) . . ?
N4 C8 H8 118.2 . . ?
C7 C8 H8 118.2 . . ?
C3 C9 C15 111.75(18) . . ?
C3 C9 C14 110.48(17) . . ?
C15 C9 C14 108.62(19) . . ?
C3 C9 C10 109.18(18) . . ?
C15 C9 C10 108.14(17) . . ?
C14 C9 C10 108.60(18) . . ?
C9 C10 C11 110.99(18) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C7 C11 C17 111.90(17) . . ?
C7 C11 C12 109.54(17) . . ?
C17 C11 C12 109.02(18) . . ?
C7 C11 C10 109.53(18) . . ?
C17 C11 C10 108.35(18) . . ?
C12 C11 C10 108.42(17) . . ?
C13 C12 C11 110.03(18) . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C18 109.7(2) . . ?
C14 C13 C12 109.9(2) . . ?
C18 C13 C12 109.49(19) . . ?
C14 C13 H13 109.3 . . ?
C18 C13 H13 109.3 . . ?
C12 C13 H13 109.3 . . ?
C13 C14 C9 110.24(18) . . ?
C13 C14 H14A 109.6 . . ?
C9 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
C9 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C9 110.31(19) . . ?
C16 C15 H15A 109.6 . . ?
C9 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C9 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C15 C16 C17 109.67(19) . . ?
C15 C16 C18 110.36(19) . . ?
C17 C16 C18 109.5(2) . . ?
C15 C16 H16 109.1 . . ?
C17 C16 H16 109.1 . . ?
C18 C16 H16 109.1 . . ?
C16 C17 C11 110.03(18) . . ?
C16 C17 H17A 109.7 . . ?
C11 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
C11 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
C16 C18 C13 109.01(19) . . ?
C16 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 . . ?
C16 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O4 C19 O3 126.5(2) . . ?
O4 C19 C21 116.6(2) . . ?
O3 C19 C21 116.67(19) . . ?
O5 C20 O6 125.2(2) . . ?
O5 C20 C23 118.3(2) . . ?
O6 C20 C23 116.6(2) . . ?
C22 C21 C26 120.0(2) . . ?
C22 C21 C19 119.3(2) . . ?
C26 C21 C19 120.5(2) . . ?
C21 C22 C23 120.5(2) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 119.1(2) . . ?
C22 C23 C20 119.1(2) . . ?
C24 C23 C20 121.8(2) . . ?
C25 C24 C23 120.8(2) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 119.9(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 119.7(2) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
O8 C27 O7 123.0(2) . . ?
O8 C27 C29 119.1(2) . . ?
O7 C27 C29 117.82(19) . . ?
O8 C27 Cu3 73.38(12) . . ?
O7 C27 Cu3 49.67(10) . . ?
C29 C27 Cu3 167.49(17) . . ?
O9 C28 O10 126.1(2) . . ?
O9 C28 C31 122.0(2) . . ?
O10 C28 C31 111.8(2) . . ?
C34 C29 C30 119.8(2) . . ?
C34 C29 C27 118.8(2) . . ?
C30 C29 C27 121.4(2) . . ?
C31 C30 C29 119.6(2) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C30 C31 C32 119.5(2) . . ?
C30 C31 C28 121.5(2) . . ?
C32 C31 C28 118.9(2) . . ?
C33 C32 C31 120.9(2) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C34 C33 C32 119.5(2) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C29 120.6(2) . . ?
C33 C34 H34 119.7 . . ?
C29 C34 H34 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu2 O1 Cu1 -156.20(9) . . . . ?
N2 Cu2 O1 Cu1 50.65(9) . . . . ?
N3 Cu2 O1 Cu1 -44.46(9) 4_666 . . . ?
N4 Cu1 O1 Cu2 -140.96(9) 2 . . . ?
N4 Cu1 O1 Cu2 39.04(9) 4_666 . . . ?
N1 Cu1 O1 Cu2 -50.60(8) . . . . ?
N1 Cu1 O1 Cu2 129.40(8) 3_666 . . . ?
O1 Cu2 O2 Cu3 -105.55(6) . . . . ?
O3 Cu2 O2 Cu3 76.93(6) . . . . ?
N2 Cu2 O2 Cu3 -10.16(16) . . . . ?
N3 Cu2 O2 Cu3 164.33(5) 4_666 . . . ?
O10 Cu3 O2 Cu2 -146.60(7) 1_655 . . . ?
O6 Cu3 O2 Cu2 126.22(6) 2_655 . . . ?
O7 Cu3 O2 Cu2 32.70(7) . . . . ?
O4 Cu3 O2 Cu2 -58.10(6) . . . . ?
O8 Cu3 O2 Cu2 14.42(19) . . . . ?
C27 Cu3 O2 Cu2 28.10(10) . . . . ?
O2 Cu2 O3 C19 -75.96(16) . . . . ?
N2 Cu2 O3 C19 77.12(16) . . . . ?
N3 Cu2 O3 C19 172.18(16) 4_666 . . . ?
O10 Cu3 O4 C19 100.5(2) 1_655 . . . ?
O7 Cu3 O4 C19 -90.4(2) . . . . ?
O8 Cu3 O4 C19 -148.9(2) . . . . ?
C27 Cu3 O4 C19 -120.0(2) . . . . ?
O2 Cu3 O4 C19 12.6(2) . . . . ?
O10 Cu3 O7 C27 3.2(5) 1_655 . . . ?
O6 Cu3 O7 C27 85.81(14) 2_655 . . . ?
O4 Cu3 O7 C27 -87.52(14) . . . . ?
O8 Cu3 O7 C27 -0.17(12) . . . . ?
O2 Cu3 O7 C27 -173.15(13) . . . . ?
O10 Cu3 O8 C27 -179.15(13) 1_655 . . . ?
O6 Cu3 O8 C27 -92.77(14) 2_655 . . . ?
O7 Cu3 O8 C27 0.18(13) . . . . ?
O4 Cu3 O8 C27 93.13(14) . . . . ?
O2 Cu3 O8 C27 21.2(2) . . . . ?
O1 Cu1 N1 C1 -152.0(2) . . . . ?
O1 Cu1 N1 C1 28.0(2) 3_666 . . . ?
N4 Cu1 N1 C1 -60.77(19) 2 . . . ?
N4 Cu1 N1 C1 119.23(19) 4_666 . . . ?
O1 Cu1 N1 N2 31.85(14) . . . . ?
O1 Cu1 N1 N2 -148.15(14) 3_666 . . . ?
N4 Cu1 N1 N2 123.06(15) 2 . . . ?
N4 Cu1 N1 N2 -56.94(15) 4_666 . . . ?
C1 N1 N2 C4 -0.7(3) . . . . ?
Cu1 N1 N2 C4 175.85(16) . . . . ?
C1 N1 N2 Cu2 177.40(16) . . . . ?
Cu1 N1 N2 Cu2 -6.10(17) . . . . ?
O1 Cu2 N2 C4 155.09(19) . . . . ?
O3 Cu2 N2 C4 -28.80(19) . . . . ?
O2 Cu2 N2 C4 58.1(3) . . . . ?
N3 Cu2 N2 C4 -116.74(19) 4_666 . . . ?
O1 Cu2 N2 N1 -22.80(14) . . . . ?
O3 Cu2 N2 N1 153.31(15) . . . . ?
O2 Cu2 N2 N1 -119.77(17) . . . . ?
N3 Cu2 N2 N1 65.37(15) 4_666 . . . ?
C5 N3 N4 C8 3.3(3) . . . . ?
Cu2 N3 N4 C8 -167.55(16) 4_565 . . . ?
C5 N3 N4 Cu1 -175.09(16) . . . 2_545 ?
Cu2 N3 N4 Cu1 14.08(18) 4_565 . . 2_545 ?
N2 N1 C1 C2 1.7(3) . . . . ?
Cu1 N1 C1 C2 -174.35(17) . . . . ?
N1 C1 C2 C3 -0.8(4) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
C1 C2 C3 C9 178.9(2) . . . . ?
N1 N2 C4 C3 -1.3(3) . . . . ?
Cu2 N2 C4 C3 -179.07(16) . . . . ?
C2 C3 C4 N2 2.1(3) . . . . ?
C9 C3 C4 N2 -177.9(2) . . . . ?
N4 N3 C5 C6 -2.5(3) . . . . ?
Cu2 N3 C5 C6 166.27(18) 4_565 . . . ?
N3 C5 C6 C7 -1.3(4) . . . . ?
C5 C6 C7 C8 4.0(3) . . . . ?
C5 C6 C7 C11 -176.3(2) . . . . ?
N3 N4 C8 C7 -0.3(3) . . . . ?
Cu1 N4 C8 C7 178.05(16) 2_545 . . . ?
C6 C7 C8 N4 -3.4(3) . . . . ?
C11 C7 C8 N4 176.9(2) . . . . ?
C2 C3 C9 C15 -4.9(3) . . . . ?
C4 C3 C9 C15 175.1(2) . . . . ?
C2 C3 C9 C14 -126.0(2) . . . . ?
C4 C3 C9 C14 54.0(3) . . . . ?
C2 C3 C9 C10 114.6(2) . . . . ?
C4 C3 C9 C10 -65.4(2) . . . . ?
C3 C9 C10 C11 179.26(16) . . . . ?
C15 C9 C10 C11 -59.0(2) . . . . ?
C14 C9 C10 C11 58.7(2) . . . . ?
C6 C7 C11 C17 178.8(2) . . . . ?
C8 C7 C11 C17 -1.6(3) . . . . ?
C6 C7 C11 C12 -60.2(3) . . . . ?
C8 C7 C11 C12 119.4(2) . . . . ?
C6 C7 C11 C10 58.6(3) . . . . ?
C8 C7 C11 C10 -121.8(2) . . . . ?
C9 C10 C11 C7 -178.68(16) . . . . ?
C9 C10 C11 C17 59.0(2) . . . . ?
C9 C10 C11 C12 -59.2(2) . . . . ?
C7 C11 C12 C13 178.88(18) . . . . ?
C17 C11 C12 C13 -58.4(2) . . . . ?
C10 C11 C12 C13 59.4(2) . . . . ?
C11 C12 C13 C14 -60.6(2) . . . . ?
C11 C12 C13 C18 59.9(3) . . . . ?
C18 C13 C14 C9 -60.2(2) . . . . ?
C12 C13 C14 C9 60.2(2) . . . . ?
C3 C9 C14 C13 -178.35(18) . . . . ?
C15 C9 C14 C13 58.8(2) . . . . ?
C10 C9 C14 C13 -58.6(2) . . . . ?
C3 C9 C15 C16 179.60(18) . . . . ?
C14 C9 C15 C16 -58.3(2) . . . . ?
C10 C9 C15 C16 59.4(2) . . . . ?
C9 C15 C16 C17 -61.1(2) . . . . ?
C9 C15 C16 C18 59.7(2) . . . . ?
C15 C16 C17 C11 60.8(2) . . . . ?
C18 C16 C17 C11 -60.5(2) . . . . ?
C7 C11 C17 C16 179.98(18) . . . . ?
C12 C11 C17 C16 58.7(2) . . . . ?
C10 C11 C17 C16 -59.2(2) . . . . ?
C15 C16 C18 C13 -59.7(3) . . . . ?
C17 C16 C18 C13 61.1(3) . . . . ?
C14 C13 C18 C16 59.9(2) . . . . ?
C12 C13 C18 C16 -60.8(3) . . . . ?
Cu3 O4 C19 O3 12.7(3) . . . . ?
Cu3 O4 C19 C21 -172.72(14) . . . . ?
Cu2 O3 C19 O4 18.5(3) . . . . ?
Cu2 O3 C19 C21 -156.06(13) . . . . ?
Cu3 O6 C20 O5 -8.2(3) 2_645 . . . ?
Cu3 O6 C20 C23 171.04(13) 2_645 . . . ?
O4 C19 C21 C22 -1.4(3) . . . . ?
O3 C19 C21 C22 173.71(18) . . . . ?
O4 C19 C21 C26 -175.77(19) . . . . ?
O3 C19 C21 C26 -0.6(3) . . . . ?
C26 C21 C22 C23 0.8(3) . . . . ?
C19 C21 C22 C23 -173.57(18) . . . . ?
C21 C22 C23 C24 0.4(3) . . . . ?
C21 C22 C23 C20 -179.93(18) . . . . ?
O5 C20 C23 C22 -10.5(3) . . . . ?
O6 C20 C23 C22 170.23(19) . . . . ?
O5 C20 C23 C24 169.2(2) . . . . ?
O6 C20 C23 C24 -10.1(3) . . . . ?
C22 C23 C24 C25 -1.2(3) . . . . ?
C20 C23 C24 C25 179.1(2) . . . . ?
C23 C24 C25 C26 0.8(3) . . . . ?
C24 C25 C26 C21 0.4(3) . . . . ?
C22 C21 C26 C25 -1.2(3) . . . . ?
C19 C21 C26 C25 173.11(19) . . . . ?
Cu3 O8 C27 O7 -0.3(2) . . . . ?
Cu3 O8 C27 C29 -179.9(2) . . . . ?
Cu3 O7 C27 O8 0.4(3) . . . . ?
Cu3 O7 C27 C29 179.96(16) . . . . ?
O10 Cu3 C27 O8 1.23(19) 1_655 . . . ?
O6 Cu3 C27 O8 86.17(13) 2_655 . . . ?
O7 Cu3 C27 O8 -179.7(2) . . . . ?
O4 Cu3 C27 O8 -86.63(13) . . . . ?
O2 Cu3 C27 O8 -170.62(11) . . . . ?
O10 Cu3 C27 O7 -179.08(13) 1_655 . . . ?
O6 Cu3 C27 O7 -94.13(14) 2_655 . . . ?
O4 Cu3 C27 O7 93.07(14) . . . . ?
O8 Cu3 C27 O7 179.7(2) . . . . ?
O2 Cu3 C27 O7 9.07(17) . . . . ?
Cu3 O10 C28 O9 -29.1(4) 1_455 . . . ?
Cu3 O10 C28 C31 153.48(18) 1_455 . . . ?
O8 C27 C29 C34 1.6(3) . . . . ?
O7 C27 C29 C34 -178.0(2) . . . . ?
Cu3 C27 C29 C34 -177.8(6) . . . . ?
O8 C27 C29 C30 179.5(2) . . . . ?
O7 C27 C29 C30 -0.2(3) . . . . ?
Cu3 C27 C29 C30 0.0(9) . . . . ?
C34 C29 C30 C31 -1.5(3) . . . . ?
C27 C29 C30 C31 -179.3(2) . . . . ?
C29 C30 C31 C32 4.3(3) . . . . ?
C29 C30 C31 C28 -172.6(2) . . . . ?
O9 C28 C31 C30 -34.1(4) . . . . ?
O10 C28 C31 C30 143.5(2) . . . . ?
O9 C28 C31 C32 149.0(2) . . . . ?
O10 C28 C31 C32 -33.4(3) . . . . ?
C30 C31 C32 C33 -3.9(4) . . . . ?
C28 C31 C32 C33 173.2(2) . . . . ?
C31 C32 C33 C34 0.5(4) . . . . ?
C32 C33 C34 C29 2.4(4) . . . . ?
C30 C29 C34 C33 -1.9(3) . . . . ?
C27 C29 C34 C33 175.9(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.54
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.077


_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL IP2-1780 in P2(1)/n
CELL  0.71073  10.0322  18.4439  19.0354   90.000  104.897   90.000
ZERR     2.00   0.0006   0.0009   0.0012    0.000    0.005    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    CU
UNIT  136  144  16   50   10
MERG   2
OMIT     0.00 180.00
OMIT   -11  14   8
OMIT     6  18  10
OMIT    12   8   2
OMIT    -1   0   1
BIND CU3 O2
BIND Cu3 O8
EQIV $1 1.5-X, 0.5+Y, 0.5-Z
EQIV $2 1+X, Y, Z
RTAB XHY O2 H1W O5_$1
RTAB XHY O2 H2W O9_$2
RTAB XHY O1 H1H O21W_$1
RTAB XHY O1 H1H O22W_$1
RTAB H..O H1W O5_$1
RTAB H..O H2W O9_$2
RTAB H..O H1H O21W_$1
RTAB H..O H1H O22W_$1
RTAB O..O O2 O5_$1
RTAB O..O O2 O9_$2
RTAB O..O O1 O21W_$1
RTAB O..O O1 O22W_$1
FMAP   2
PLAN   10
SIZE     0.18   0.20   0.21
ACTA
BOND   $H
CONF
LIST   4
L.S.   4
TEMP  -168.00
WGHT    0.049300
FVAR       1.00002
CU1   5    0.500000    0.500000    0.500000    10.50000    0.02086    0.02005 =
         0.01663    0.00001    0.00483    0.00309
CU2   5    0.700025    0.410473    0.426112    11.00000    0.02615    0.01929 =
         0.02275    0.00178    0.00994    0.00464
CU3   5    0.696905    0.380100    0.254123    11.00000    0.01685    0.02107 =
         0.02305    0.00345    0.00561    0.00135
O1    4    0.595734    0.495247    0.425037    11.00000    0.02612    0.01938 =
         0.02247    0.00078    0.00992    0.00411
AFIX   3
H1H   2    0.627464    0.535727    0.415056    11.00000   -1.50000
AFIX   0
O2    4    0.829663    0.455091    0.373582    11.00000    0.02640    0.02839 =
         0.03697    0.01055    0.01555    0.00653
AFIX   3
H1W   2    0.789833    0.488911    0.345702    11.00000   -1.50000
H2W   2    0.904243    0.444681    0.362242    11.00000   -1.50000
AFIX   0
O3    4    0.804296    0.321886    0.434456    11.00000    0.02690    0.01992 =
         0.02493   -0.00050    0.00798    0.00415
O4    4    0.748384    0.293341    0.315623    11.00000    0.02662    0.02204 =
         0.02320    0.00423    0.00352    0.00228
O5    4    0.753087    0.044967    0.237027    11.00000    0.03671    0.02569 =
         0.02328   -0.00196    0.00443   -0.00060
O6    4    0.850564   -0.041118    0.317174    11.00000    0.02296    0.02113 =
         0.02768   -0.00476    0.00355    0.00227
O7    4    0.506457    0.376242    0.262921    11.00000    0.01851    0.02457 =
         0.02725    0.00059    0.00750    0.00021
O8    4    0.518285    0.306678    0.169624    11.00000    0.02615    0.03581 =
         0.03396   -0.00204    0.01370    0.00186
O9    4    0.034249    0.382544    0.333920    11.00000    0.02572    0.03572 =
         0.04334   -0.00133    0.01211    0.00477
O10   4   -0.130225    0.372562    0.229530    11.00000    0.02049    0.06022 =
         0.03825    0.01919    0.01381    0.01217
O11W  4    0.698013    0.278420    0.086756    10.40000    0.03216    0.05731 =
         0.02683   -0.00271    0.00671    0.01459
O12W  4    0.657479    0.235183    0.083483    10.60000    0.03813    0.04314 =
         0.03258   -0.00809    0.00825    0.01000
O21W  4    0.768816    0.130359    0.114021    10.40000    0.06957    0.04604 =
         0.03267   -0.00269    0.02371   -0.00063
O22W  4    0.838548    0.122396    0.132984    10.60000    0.04189    0.02137 =
         0.03784   -0.00136    0.01651    0.00215
O3W   4    0.769959    0.376960    0.082319    10.50000    0.05212    0.03381 =
         0.01246    0.00076    0.00770    0.01697
N1    3    0.426634    0.386522    0.456745    11.00000    0.02192    0.02894 =
         0.02024   -0.00033    0.00463    0.00275
N2    3    0.518580    0.348610    0.430324    11.00000    0.02365    0.02456 =
         0.02004    0.00159    0.00730    0.00327
N3    3    0.276790    0.077199    0.046147    11.00000    0.02568    0.02207 =
         0.02307   -0.00024    0.00851   -0.00366
N4    3    0.178805    0.048786    0.074288    11.00000    0.02366    0.02198 =
         0.02208    0.00126    0.00610   -0.00099
C1    1    0.309628    0.354562    0.458922    11.00000    0.02444    0.03294 =
         0.02327   -0.00197    0.00630    0.00472
AFIX  43
H1    2    0.244514    0.381957    0.476297    11.00000   -1.20000
AFIX   0
C2    1    0.275945    0.283153    0.437292    11.00000    0.02187    0.03572 =
         0.02283   -0.00334    0.00597   -0.00237
AFIX  43
H2    2    0.190906    0.262547    0.440473    11.00000   -1.20000
AFIX   0
C3    1    0.369221    0.243160    0.411148    11.00000    0.02090    0.02952 =
         0.01722    0.00061    0.00271    0.00121
C4    1    0.490116    0.281255    0.408326    11.00000    0.02369    0.02602 =
         0.02204   -0.00055    0.00646    0.00246
AFIX  43
H4    2    0.555835    0.256408    0.389110    11.00000   -1.20000
AFIX   0
C5    1    0.391512    0.102406    0.091479    11.00000    0.02615    0.02814 =
         0.02789   -0.00184    0.01164   -0.00267
AFIX  43
H5    2    0.462338    0.120698    0.071489    11.00000   -1.20000
AFIX   0
C6    1    0.412806    0.103280    0.166747    11.00000    0.02345    0.02975 =
         0.02481   -0.00193    0.00569   -0.00328
AFIX  43
H6    2    0.496880    0.120805    0.197342    11.00000   -1.20000
AFIX   0
C7    1    0.308488    0.077988    0.195951    11.00000    0.02158    0.02123 =
         0.02249   -0.00068    0.00341    0.00220
C8    1    0.192844    0.049043    0.145348    11.00000    0.02231    0.02241 =
         0.02321    0.00170    0.00671   -0.00089
AFIX  43
H8    2    0.121033    0.028597    0.163197    11.00000   -1.20000
AFIX   0
C9    1    0.348298    0.164458    0.386740    11.00000    0.01999    0.02781 =
         0.02079    0.00000    0.00485   -0.00248
C10   1    0.336185    0.160067    0.303968    11.00000    0.02051    0.02424 =
         0.02078    0.00068    0.00522    0.00051
AFIX  23
H10A  2    0.420616    0.180331    0.293724    11.00000   -1.20000
H10B  2    0.256692    0.189548    0.277395    11.00000   -1.20000
AFIX   0
C11   1    0.316578    0.080401    0.276764    11.00000    0.02148    0.02360 =
         0.02029    0.00130    0.00452    0.00011
C12   1    0.441896    0.035618    0.318920    11.00000    0.02346    0.02441 =
         0.02528    0.00148    0.00139    0.00246
AFIX  23
H12A  2    0.431381   -0.015408    0.302269    11.00000   -1.20000
H12B  2    0.527325    0.055129    0.309180    11.00000   -1.20000
AFIX   0
C13   1    0.452847    0.038892    0.400787    11.00000    0.02727    0.02745 =
         0.02497    0.00376   -0.00110    0.00088
AFIX  13
H13   2    0.533754    0.009397    0.427403    11.00000   -1.20000
AFIX   0
C14   1    0.472521    0.117627    0.427204    11.00000    0.02517    0.02800 =
         0.02148    0.00102    0.00027   -0.00142
AFIX  23
H14A  2    0.558523    0.137309    0.418300    11.00000   -1.20000
H14B  2    0.481035    0.119410    0.480156    11.00000   -1.20000
AFIX   0
C15   1    0.215603    0.132342    0.400863    11.00000    0.02492    0.03494 =
         0.02277   -0.00175    0.00756   -0.00593
AFIX  23
H15A  2    0.220879    0.134696    0.453466    11.00000   -1.20000
H15B  2    0.134961    0.161226    0.374617    11.00000   -1.20000
AFIX   0
C16   1    0.197396    0.053612    0.375256    11.00000    0.02721    0.03512 =
         0.02128    0.00138    0.00604   -0.00914
AFIX  13
H16   2    0.111410    0.033678    0.385258    11.00000   -1.20000
AFIX   0
C17   1    0.184538    0.050125    0.293534    11.00000    0.02333    0.02773 =
         0.01940    0.00159    0.00225   -0.00178
AFIX  23
H17A  2    0.103712    0.078837    0.267211    11.00000   -1.20000
H17B  2    0.170253   -0.000754    0.276710    11.00000   -1.20000
AFIX   0
C18   1    0.320839    0.007870    0.415740    11.00000    0.03919    0.02998 =
         0.02272    0.00416    0.00229   -0.00796
AFIX  23
H18A  2    0.308121   -0.043082    0.398995    11.00000   -1.20000
H18B  2    0.328113    0.008831    0.468593    11.00000   -1.20000
AFIX   0
C19   1    0.795255    0.278893    0.381793    11.00000    0.01798    0.02151 =
         0.02518    0.00095    0.00752    0.00157
C20   1    0.810931    0.023403    0.300264    11.00000    0.01993    0.02422 =
         0.02571   -0.00200    0.00624   -0.00054
C21   1    0.833438    0.201443    0.400437    11.00000    0.01887    0.02273 =
         0.02405    0.00037    0.00555    0.00134
C22   1    0.812708    0.150349    0.345176    11.00000    0.01982    0.02369 =
         0.02140    0.00056    0.00438    0.00060
AFIX  43
H22   2    0.783624    0.165554    0.295912    11.00000   -1.20000
AFIX   0
C23   1    0.834136    0.077163    0.361306    11.00000    0.02135    0.02262 =
         0.02524   -0.00114    0.00595    0.00090
C24   1    0.876112    0.055588    0.433985    11.00000    0.03039    0.02143 =
         0.02817    0.00175    0.00579    0.00601
AFIX  43
H24   2    0.889352    0.005551    0.445508    11.00000   -1.20000
AFIX   0
C25   1    0.898635    0.106233    0.489392    11.00000    0.03394    0.02612 =
         0.02307    0.00173    0.00481    0.00569
AFIX  43
H25   2    0.928274    0.091008    0.538632    11.00000   -1.20000
AFIX   0
C26   1    0.877781    0.179563    0.472851    11.00000    0.02391    0.02367 =
         0.02231   -0.00268    0.00423    0.00271
AFIX  43
H26   2    0.893685    0.214551    0.510725    11.00000   -1.20000
AFIX   0
C27   1    0.452112    0.334009    0.210428    11.00000    0.02286    0.02410 =
         0.02482    0.00666    0.00883    0.00420
C28   1   -0.008336    0.363005    0.270067    11.00000    0.01909    0.02841 =
         0.04148    0.01110    0.01064    0.00284
C29   1    0.301855    0.316381    0.197963    11.00000    0.02180    0.02169 =
         0.02354    0.00559    0.00526    0.00238
C30   1    0.223585    0.344992    0.242361    11.00000    0.02052    0.02080 =
         0.02726    0.00395    0.00463    0.00055
AFIX  43
H30   2    0.264821    0.376772    0.281135    11.00000   -1.20000
AFIX   0
C31   1    0.084601    0.326638    0.229439    11.00000    0.01939    0.02677 =
         0.03380    0.00712    0.00646    0.00302
C32   1    0.027876    0.276127    0.175520    11.00000    0.02041    0.03469 =
         0.04175    0.00440    0.00168   -0.00208
AFIX  43
H32   2   -0.065306    0.261358    0.168687    11.00000   -1.20000
AFIX   0
C33   1    0.105439    0.247256    0.131874    11.00000    0.03166    0.02993 =
         0.03383   -0.00024   -0.00340   -0.00216
AFIX  43
H33   2    0.065689    0.213141    0.095053    11.00000   -1.20000
AFIX   0
C34   1    0.241297    0.268438    0.142252    11.00000    0.02997    0.02589 =
         0.02626    0.00009    0.00446    0.00210
AFIX  43
H34   2    0.293866    0.250172    0.111157    11.00000   -1.20000
HKLF    4
 
REM  IP2-1780 in P2(1)/n
REM R1 =  0.0319 for   6319 Fo > 4sig(Fo)  and  0.0487 for all   8508 data
REM    502 parameters refined using      0 restraints
 
END
 
WGHT      0.0493      0.0000
REM Highest difference peak  0.534,  deepest hole -0.553,  1-sigma level  0.077
Q1    1   0.8015  0.3791  0.1098  11.00000  0.05    0.53
Q2    1   0.8045  0.3957  0.0818  11.00000  0.05    0.52
Q3    1   0.6241  0.2600  0.1117  11.00000  0.05    0.50
Q4    1   0.8121  0.1128  0.1704  11.00000  0.05    0.47
Q5    1   0.7731  0.3668  0.0693  11.00000  0.05    0.46
Q6    1   0.7253  0.3917  0.0824  11.00000  0.05    0.45
Q7    1   0.8397  0.1591  0.1381  11.00000  0.05    0.41
Q8    1   0.5497  0.4932  0.4375  11.00000  0.05    0.38
Q9    1   0.5834  0.3801  0.2719  11.00000  0.05    0.36
Q10   1   0.7586  0.1783  0.1066  11.00000  0.05    0.35
;
_database_code_depnum_ccdc_archive 'CCDC 967347'
#######################################################################
#
#                 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_(5)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Poly[bis-[μ₄-[1,3-bis(pyridazin-4-yl)adamantane-κ⁴N1:N2:N3:N4)]]-
tetrakis-[μ₂-(5-hydroxy-1,3-benzenedicarboxylato)]-di(μ₂-hydroxido)-
diaquapentacopper(II)] hexahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H62 Cu5 N8 O24, 6(H2 O)'
_chemical_formula_sum            'C68 H74 Cu5 N8 O30'
_chemical_formula_weight         1801.05

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_symmetry_Int_Tables_number      14


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

_cell_length_a                   10.0552(5)
_cell_length_b                   18.7840(8)
_cell_length_c                   19.1757(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.829(2)
_cell_angle_gamma                90.00
_cell_volume                     3501.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    31226
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            green-blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1846
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_T_max  0.8320
_exptl_absorpt_process_details   'face indexed (SADABS; Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(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 APEX2 area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31226
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_sigmaI/netI    0.0982
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8020
_reflns_number_gt                5132
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 The refinement was standard and no disordered moieties were found in the 
 structure. The CH-hydrogen atoms were added geometrically, with Uiso = 
 1.2Ueq(C) and OH-hydrogen atoms were located and included with 
 fixed d(O-H) = 0.85 A and Uiso = 1.5Ueq(O). 
;

_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)+(0.0308P)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_number_reflns         8020
_refine_ls_number_parameters     502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1045
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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 0.5000 0.0000 0.5000 0.01822(15) Uani 1 2 d S . .
Cu2 Cu 0.21873(5) 0.08099(2) 0.43059(2) 0.02391(13) Uani 1 1 d . . .
Cu3 Cu 0.05983(4) 0.10230(2) 0.25926(2) 0.01637(11) Uani 1 1 d . . .
O1 O 0.3257(2) -0.00139(11) 0.43162(13) 0.0241(6) Uani 1 1 d . . .
H1H H 0.2795 -0.0398 0.4261 0.036 Uiso 1 1 d R . .
O2 O 0.0450(3) 0.03238(12) 0.37806(14) 0.0326(7) Uani 1 1 d . . .
H1W H 0.0341 -0.0092 0.3600 0.049 Uiso 1 1 d R . .
H2W H -0.0318 0.0466 0.3838 0.049 Uiso 1 1 d R . .
O3 O 0.1177(3) 0.16852(12) 0.43058(13) 0.0256(6) Uani 1 1 d . . .
O4 O 0.0640(3) 0.19148(12) 0.31173(13) 0.0263(6) Uani 1 1 d . . .
O5 O -0.0418(3) 0.43591(13) 0.22390(14) 0.0336(7) Uani 1 1 d . . .
O6 O -0.0437(3) 0.52145(12) 0.30425(13) 0.0257(6) Uani 1 1 d . . .
O7 O 0.0879(3) 0.40936(13) 0.54313(14) 0.0399(8) Uani 1 1 d . . .
H1O H 0.1092 0.3779 0.5759 0.060 Uiso 1 1 d R . .
O8 O -0.1369(3) 0.10740(14) 0.23472(14) 0.0287(6) Uani 1 1 d . . .
O9 O -0.2008(3) 0.09745(15) 0.33722(15) 0.0357(7) Uani 1 1 d . . .
O10 O -0.7417(2) 0.10886(12) 0.26777(13) 0.0227(6) Uani 1 1 d . . .
O11 O -0.8416(3) 0.16752(13) 0.16774(13) 0.0267(6) Uani 1 1 d . . .
O12 O -0.4623(3) 0.29050(14) 0.09474(15) 0.0397(8) Uani 1 1 d . . .
H2O H -0.3834 0.3100 0.1040 0.060 Uiso 1 1 d R . .
N1 N 0.5205(3) 0.10246(14) 0.45529(16) 0.0216(7) Uani 1 1 d . . .
N2 N 0.4039(3) 0.13957(14) 0.43274(16) 0.0220(7) Uani 1 1 d . . .
N3 N 0.2643(3) 0.41901(15) 0.05066(16) 0.0247(7) Uani 1 1 d . . .
N4 N 0.3883(3) 0.44646(15) 0.07985(15) 0.0219(7) Uani 1 1 d . . .
C1 C 0.6375(4) 0.13259(19) 0.4528(2) 0.0251(9) Uani 1 1 d . . .
H1 H 0.7172 0.1054 0.4664 0.030 Uiso 1 1 calc R . .
C2 C 0.6497(4) 0.2028(2) 0.43106(19) 0.0264(9) Uani 1 1 d . . .
H2 H 0.7350 0.2219 0.4308 0.032 Uiso 1 1 calc R . .
C3 C 0.5314(4) 0.24282(18) 0.41003(18) 0.0206(8) Uani 1 1 d . . .
C4 C 0.4104(4) 0.20620(18) 0.41103(19) 0.0244(9) Uani 1 1 d . . .
H4 H 0.3277 0.2307 0.3952 0.029 Uiso 1 1 calc R . .
C5 C 0.1984(4) 0.3876(2) 0.0941(2) 0.0287(9) Uani 1 1 d . . .
H5 H 0.1118 0.3685 0.0739 0.034 Uiso 1 1 calc R . .
C6 C 0.2518(4) 0.3819(2) 0.1682(2) 0.0301(10) Uani 1 1 d . . .
H6 H 0.2010 0.3605 0.1967 0.036 Uiso 1 1 calc R . .
C7 C 0.3813(4) 0.40843(17) 0.19887(19) 0.0194(8) Uani 1 1 d . . .
C8 C 0.4446(4) 0.44147(18) 0.14994(19) 0.0222(8) Uani 1 1 d . . .
H8 H 0.5315 0.4610 0.1680 0.027 Uiso 1 1 calc R . .
C9 C 0.5268(4) 0.32021(18) 0.38663(18) 0.0197(8) Uani 1 1 d . . .
C10 C 0.4600(4) 0.32536(17) 0.30475(17) 0.0187(8) Uani 1 1 d . . .
H10A H 0.3686 0.3048 0.2940 0.022 Uiso 1 1 calc R . .
H10B H 0.5143 0.2983 0.2789 0.022 Uiso 1 1 calc R . .
C11 C 0.4503(4) 0.40424(17) 0.27883(19) 0.0212(8) Uani 1 1 d . . .
C12 C 0.3624(4) 0.44557(19) 0.32090(19) 0.0262(9) Uani 1 1 d . . .
H12A H 0.3545 0.4949 0.3055 0.031 Uiso 1 1 calc R . .
H12B H 0.2707 0.4254 0.3104 0.031 Uiso 1 1 calc R . .
C13 C 0.4278(4) 0.44175(19) 0.4014(2) 0.0318(10) Uani 1 1 d . . .
H13 H 0.3715 0.4688 0.4269 0.038 Uiso 1 1 calc R . .
C14 C 0.4368(4) 0.36378(18) 0.4269(2) 0.0279(9) Uani 1 1 d . . .
H14A H 0.3452 0.3434 0.4171 0.033 Uiso 1 1 calc R . .
H14B H 0.4773 0.3617 0.4786 0.033 Uiso 1 1 calc R . .
C15 C 0.6699(4) 0.35407(18) 0.4030(2) 0.0267(9) Uani 1 1 d . . .
H15A H 0.7271 0.3281 0.3780 0.032 Uiso 1 1 calc R . .
H15B H 0.7126 0.3513 0.4544 0.032 Uiso 1 1 calc R . .
C16 C 0.6596(4) 0.43229(19) 0.3789(2) 0.0275(9) Uani 1 1 d . . .
H16 H 0.7522 0.4528 0.3899 0.033 Uiso 1 1 calc R . .
C17 C 0.5967(4) 0.43609(19) 0.29795(19) 0.0245(9) Uani 1 1 d . . .
H17A H 0.6538 0.4099 0.2730 0.029 Uiso 1 1 calc R . .
H17B H 0.5928 0.4853 0.2822 0.029 Uiso 1 1 calc R . .
C18 C 0.5733(5) 0.4738(2) 0.4188(2) 0.0356(11) Uani 1 1 d . . .
H18A H 0.5686 0.5233 0.4041 0.043 Uiso 1 1 calc R . .
H18B H 0.6147 0.4715 0.4703 0.043 Uiso 1 1 calc R . .
C19 C 0.0777(3) 0.20883(17) 0.3761(2) 0.0186(8) Uani 1 1 d . . .
C20 C -0.0311(4) 0.45722(18) 0.2869(2) 0.0211(8) Uani 1 1 d . . .
C21 C 0.0532(4) 0.28537(17) 0.39120(18) 0.0180(8) Uani 1 1 d . . .
C22 C 0.0162(4) 0.33311(17) 0.33418(19) 0.0190(8) Uani 1 1 d . . .
H22 H -0.0007 0.3168 0.2869 0.023 Uiso 1 1 calc R . .
C23 C 0.0044(4) 0.40493(17) 0.34777(19) 0.0188(8) Uani 1 1 d . . .
C24 C 0.0291(4) 0.42867(18) 0.41819(19) 0.0228(9) Uani 1 1 d . . .
H24 H 0.0210 0.4769 0.4273 0.027 Uiso 1 1 calc R . .
C25 C 0.0660(4) 0.38087(18) 0.47575(19) 0.0235(9) Uani 1 1 d . . .
C26 C 0.0789(4) 0.30937(17) 0.46236(19) 0.0202(8) Uani 1 1 d . . .
H26 H 0.1045 0.2774 0.5005 0.024 Uiso 1 1 calc R . .
C27 C -0.2201(4) 0.11659(18) 0.2738(2) 0.0235(9) Uani 1 1 d . . .
C28 C -0.7354(4) 0.14572(18) 0.2130(2) 0.0211(8) Uani 1 1 d . . .
C29 C -0.3514(4) 0.15395(18) 0.2356(2) 0.0219(8) Uani 1 1 d . . .
C30 C -0.4774(4) 0.13524(18) 0.24645(19) 0.0202(8) Uani 1 1 d . . .
H30 H -0.4823 0.1031 0.2826 0.024 Uiso 1 1 calc R . .
C31 C -0.5972(4) 0.16474(17) 0.20296(19) 0.0185(8) Uani 1 1 d . . .
C32 C -0.5902(4) 0.21430(18) 0.1506(2) 0.0241(9) Uani 1 1 d . . .
H32 H -0.6708 0.2319 0.1202 0.029 Uiso 1 1 calc R . .
C33 C -0.4638(4) 0.23785(19) 0.1433(2) 0.0263(9) Uani 1 1 d . . .
C34 C -0.3450(4) 0.20596(19) 0.1846(2) 0.0266(9) Uani 1 1 d . . .
H34 H -0.2599 0.2195 0.1782 0.032 Uiso 1 1 calc R . .
O1W O 0.2150(3) 0.85780(13) 0.38149(15) 0.0399(8) Uani 1 1 d . . .
H3W H 0.1778 0.8807 0.3432 0.060 Uiso 1 1 d R . .
H4W H 0.1622 0.8236 0.3856 0.060 Uiso 1 1 d R . .
O2W O 0.0684(3) 0.74657(17) 0.40751(18) 0.0621(10) Uani 1 1 d . . .
H5W H 0.1153 0.7085 0.4176 0.093 Uiso 1 1 d R . .
H6W H -0.0120 0.7357 0.3830 0.093 Uiso 1 1 d R . .
O3W O 0.1912(4) 0.61019(17) 0.41742(16) 0.0650(10) Uani 1 1 d . . .
H7W H 0.1222 0.5903 0.4271 0.097 Uiso 1 1 d R . .
H8W H 0.1842 0.6056 0.3725 0.097 Uiso 1 1 d 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 1.901(2) . ?
Cu1 O1 1.901(2) 3_656 ?
Cu1 N1 2.138(3) . ?
Cu1 N1 2.138(3) 3_656 ?
Cu1 N4 2.344(3) 4_566 ?
Cu1 N4 2.344(3) 2_645 ?
Cu2 O1 1.882(2) . ?
Cu2 O3 1.933(2) . ?
Cu2 O2 2.000(3) . ?
Cu2 N2 2.154(3) . ?
Cu2 N3 2.230(3) 4_566 ?
Cu3 O8 1.915(2) . ?
Cu3 O6 1.927(2) 2_545 ?
Cu3 O4 1.949(2) . ?
Cu3 O10 1.964(2) 1_655 ?
Cu3 O11 2.541(3) 1_655 ?
Cu3 O2 2.667(3) . ?
O1 H1H 0.8500 . ?
O2 H1W 0.8500 . ?
O2 H2W 0.8500 . ?
O3 C19 1.270(4) . ?
O4 C19 1.249(4) . ?
O5 C20 1.251(4) . ?
O6 C20 1.266(4) . ?
O6 Cu3 1.927(2) 2 ?
O7 C25 1.364(4) . ?
O7 H1O 0.8499 . ?
O8 C27 1.270(4) . ?
O9 C27 1.235(4) . ?
O10 C28 1.273(4) . ?
O10 Cu3 1.964(2) 1_455 ?
O11 C28 1.259(4) . ?
O12 C33 1.361(4) . ?
O12 H2O 0.8500 . ?
N1 C1 1.317(4) . ?
N1 N2 1.337(4) . ?
N2 C4 1.326(4) . ?
N3 C5 1.328(5) . ?
N3 N4 1.334(4) . ?
N3 Cu2 2.230(3) 4_565 ?
N4 C8 1.321(4) . ?
N4 Cu1 2.344(3) 2_655 ?
C1 C2 1.398(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.403(5) . ?
C3 C9 1.518(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.377(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.406(5) . ?
C7 C11 1.515(5) . ?
C8 H8 0.9300 . ?
C9 C15 1.531(5) . ?
C9 C10 1.544(4) . ?
C9 C14 1.564(5) . ?
C10 C11 1.558(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C17 1.544(5) . ?
C11 C12 1.549(5) . ?
C12 C13 1.517(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C18 1.537(6) . ?
C13 C14 1.540(5) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.536(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C18 1.511(6) . ?
C16 C17 1.521(5) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C21 1.499(4) . ?
C20 C23 1.497(5) . ?
C21 C22 1.389(4) . ?
C21 C26 1.397(5) . ?
C22 C23 1.385(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.383(5) . ?
C24 C25 1.397(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.380(4) . ?
C26 H26 0.9300 . ?
C27 C29 1.509(5) . ?
C28 C31 1.495(5) . ?
C29 C30 1.381(5) . ?
C29 C34 1.395(5) . ?
C30 C31 1.392(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.384(5) . ?
C32 C33 1.387(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.389(5) . ?
C34 H34 0.9300 . ?
O1W H3W 0.8500 . ?
O1W H4W 0.8500 . ?
O2W H5W 0.8502 . ?
O2W H6W 0.8500 . ?
O3W H7W 0.8500 . ?
O3W H8W 0.8500 . ?

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 O1 180.0 . 3_656 ?
O1 Cu1 N1 84.39(11) . . ?
O1 Cu1 N1 95.61(11) 3_656 . ?
O1 Cu1 N1 95.61(11) . 3_656 ?
O1 Cu1 N1 84.39(11) 3_656 3_656 ?
N1 Cu1 N1 180.00(6) . 3_656 ?
O1 Cu1 N4 86.86(10) . 4_566 ?
O1 Cu1 N4 93.14(10) 3_656 4_566 ?
N1 Cu1 N4 89.27(11) . 4_566 ?
N1 Cu1 N4 90.73(11) 3_656 4_566 ?
O1 Cu1 N4 93.14(10) . 2_645 ?
O1 Cu1 N4 86.86(10) 3_656 2_645 ?
N1 Cu1 N4 90.73(11) . 2_645 ?
N1 Cu1 N4 89.27(11) 3_656 2_645 ?
N4 Cu1 N4 180.00(9) 4_566 2_645 ?
O1 Cu2 O3 176.97(11) . . ?
O1 Cu2 O2 93.04(10) . . ?
O3 Cu2 O2 89.83(10) . . ?
O1 Cu2 N2 86.03(10) . . ?
O3 Cu2 N2 90.99(11) . . ?
O2 Cu2 N2 151.91(12) . . ?
O1 Cu2 N3 91.34(10) . 4_566 ?
O3 Cu2 N3 88.24(10) . 4_566 ?
O2 Cu2 N3 116.24(12) . 4_566 ?
N2 Cu2 N3 91.85(11) . 4_566 ?
O8 Cu3 O6 88.25(11) . 2_545 ?
O8 Cu3 O4 88.18(11) . . ?
O6 Cu3 O4 172.16(11) 2_545 . ?
O8 Cu3 O10 168.81(11) . 1_655 ?
O6 Cu3 O10 91.23(10) 2_545 1_655 ?
O4 Cu3 O10 90.91(10) . 1_655 ?
O8 Cu3 O11 111.55(10) . 1_655 ?
O6 Cu3 O11 85.88(9) 2_545 1_655 ?
O4 Cu3 O11 88.94(9) . 1_655 ?
O10 Cu3 O11 57.27(9) 1_655 1_655 ?
O8 Cu3 O2 87.39(10) . . ?
O6 Cu3 O2 97.91(9) 2_545 . ?
O4 Cu3 O2 88.90(9) . . ?
O10 Cu3 O2 103.75(9) 1_655 . ?
O11 Cu3 O2 160.85(8) 1_655 . ?
Cu2 O1 Cu1 114.80(12) . . ?
Cu2 O1 H1H 113.8 . . ?
Cu1 O1 H1H 118.4 . . ?
Cu2 O2 Cu3 88.44(10) . . ?
Cu2 O2 H1W 129.0 . . ?
Cu3 O2 H1W 97.7 . . ?
Cu2 O2 H2W 119.7 . . ?
Cu3 O2 H2W 102.0 . . ?
H1W O2 H2W 108.4 . . ?
C19 O3 Cu2 124.3(2) . . ?
C19 O4 Cu3 135.8(2) . . ?
C20 O6 Cu3 125.6(2) . 2 ?
C25 O7 H1O 112.2 . . ?
C27 O8 Cu3 131.1(3) . . ?
C28 O10 Cu3 103.3(2) . 1_455 ?
C33 O12 H2O 110.0 . . ?
C1 N1 N2 118.8(3) . . ?
C1 N1 Cu1 125.4(2) . . ?
N2 N1 Cu1 115.6(2) . . ?
C4 N2 N1 119.0(3) . . ?
C4 N2 Cu2 126.0(3) . . ?
N1 N2 Cu2 114.9(2) . . ?
C5 N3 N4 118.1(3) . . ?
C5 N3 Cu2 130.1(3) . 4_565 ?
N4 N3 Cu2 110.9(2) . 4_565 ?
C8 N4 N3 120.7(3) . . ?
C8 N4 Cu1 122.9(2) . 2_655 ?
N3 N4 Cu1 116.4(2) . 2_655 ?
N1 C1 C2 124.3(3) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C3 C2 C1 117.8(4) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 114.6(3) . . ?
C2 C3 C9 124.6(3) . . ?
C4 C3 C9 120.8(3) . . ?
N2 C4 C3 125.4(3) . . ?
N2 C4 H4 117.3 . . ?
C3 C4 H4 117.3 . . ?
N3 C5 C6 123.5(4) . . ?
N3 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C7 C6 C5 119.0(4) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C6 C7 C8 114.5(3) . . ?
C6 C7 C11 123.5(3) . . ?
C8 C7 C11 122.0(3) . . ?
N4 C8 C7 124.2(3) . . ?
N4 C8 H8 117.9 . . ?
C7 C8 H8 117.9 . . ?
C3 C9 C15 112.4(3) . . ?
C3 C9 C10 109.4(3) . . ?
C15 C9 C10 108.9(3) . . ?
C3 C9 C14 109.5(3) . . ?
C15 C9 C14 108.3(3) . . ?
C10 C9 C14 108.3(3) . . ?
C9 C10 C11 111.1(3) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C7 C11 C17 112.5(3) . . ?
C7 C11 C12 109.1(3) . . ?
C17 C11 C12 108.6(3) . . ?
C7 C11 C10 110.3(3) . . ?
C17 C11 C10 108.3(3) . . ?
C12 C11 C10 108.0(3) . . ?
C13 C12 C11 110.5(3) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 C18 110.0(3) . . ?
C12 C13 C14 110.1(3) . . ?
C18 C13 C14 109.2(3) . . ?
C12 C13 H13 109.2 . . ?
C18 C13 H13 109.2 . . ?
C14 C13 H13 109.2 . . ?
C13 C14 C9 109.6(3) . . ?
C13 C14 H14A 109.8 . . ?
C9 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C9 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
C9 C15 C16 110.4(3) . . ?
C9 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
C9 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C18 C16 C17 110.5(3) . . ?
C18 C16 C15 110.1(3) . . ?
C17 C16 C15 109.3(3) . . ?
C18 C16 H16 109.0 . . ?
C17 C16 H16 109.0 . . ?
C15 C16 H16 109.0 . . ?
C16 C17 C11 110.3(3) . . ?
C16 C17 H17A 109.6 . . ?
C11 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C11 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C16 C18 C13 109.0(3) . . ?
C16 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 . . ?
C16 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O4 C19 O3 126.1(3) . . ?
O4 C19 C21 117.3(3) . . ?
O3 C19 C21 116.5(3) . . ?
O5 C20 O6 124.7(3) . . ?
O5 C20 C23 119.2(3) . . ?
O6 C20 C23 116.1(3) . . ?
C22 C21 C26 120.4(3) . . ?
C22 C21 C19 119.4(3) . . ?
C26 C21 C19 120.0(3) . . ?
C23 C22 C21 120.0(3) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 119.7(3) . . ?
C24 C23 C20 119.8(3) . . ?
C22 C23 C20 120.5(3) . . ?
C23 C24 C25 120.6(3) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
O7 C25 C26 123.9(3) . . ?
O7 C25 C24 116.2(3) . . ?
C26 C25 C24 119.8(3) . . ?
C25 C26 C21 119.5(3) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
O9 C27 O8 125.5(4) . . ?
O9 C27 C29 120.7(3) . . ?
O8 C27 C29 113.8(3) . . ?
O11 C28 O10 122.2(3) . . ?
O11 C28 C31 119.0(3) . . ?
O10 C28 C31 118.7(3) . . ?
C30 C29 C34 119.5(3) . . ?
C30 C29 C27 122.1(3) . . ?
C34 C29 C27 118.3(3) . . ?
C29 C30 C31 119.6(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C32 C31 C30 120.4(3) . . ?
C32 C31 C28 118.4(3) . . ?
C30 C31 C28 121.2(3) . . ?
C31 C32 C33 120.4(3) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
O12 C33 C32 118.2(3) . . ?
O12 C33 C34 123.0(3) . . ?
C32 C33 C34 118.8(3) . . ?
C33 C34 C29 121.0(3) . . ?
C33 C34 H34 119.5 . . ?
C29 C34 H34 119.5 . . ?
H3W O1W H4W 108.4 . . ?
H5W O2W H6W 108.5 . . ?
H7W O3W H8W 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu2 O1 Cu1 -162.29(14) . . . . ?
N2 Cu2 O1 Cu1 45.84(14) . . . . ?
N3 Cu2 O1 Cu1 -45.92(15) 4_566 . . . ?
N1 Cu1 O1 Cu2 -49.24(14) . . . . ?
N1 Cu1 O1 Cu2 130.76(14) 3_656 . . . ?
N4 Cu1 O1 Cu2 40.34(14) 4_566 . . . ?
N4 Cu1 O1 Cu2 -139.66(14) 2_645 . . . ?
O1 Cu2 O2 Cu3 -105.02(9) . . . . ?
O3 Cu2 O2 Cu3 74.04(9) . . . . ?
N2 Cu2 O2 Cu3 -17.7(2) . . . . ?
N3 Cu2 O2 Cu3 161.99(9) 4_566 . . . ?
O8 Cu3 O2 Cu2 -144.59(11) . . . . ?
O6 Cu3 O2 Cu2 127.54(10) 2_545 . . . ?
O4 Cu3 O2 Cu2 -56.36(10) . . . . ?
O10 Cu3 O2 Cu2 34.31(11) 1_655 . . . ?
O11 Cu3 O2 Cu2 27.2(3) 1_655 . . . ?
O2 Cu2 O3 C19 -76.5(3) . . . . ?
N2 Cu2 O3 C19 75.4(3) . . . . ?
N3 Cu2 O3 C19 167.2(3) 4_566 . . . ?
O8 Cu3 O4 C19 98.1(4) . . . . ?
O10 Cu3 O4 C19 -93.1(3) 1_655 . . . ?
O11 Cu3 O4 C19 -150.3(3) 1_655 . . . ?
O2 Cu3 O4 C19 10.7(3) . . . . ?
O6 Cu3 O8 C27 135.6(3) 2_545 . . . ?
O4 Cu3 O8 C27 -51.4(3) . . . . ?
O10 Cu3 O8 C27 -136.9(5) 1_655 . . . ?
O11 Cu3 O8 C27 -139.5(3) 1_655 . . . ?
O2 Cu3 O8 C27 37.6(3) . . . . ?
O1 Cu1 N1 C1 -151.4(3) . . . . ?
O1 Cu1 N1 C1 28.6(3) 3_656 . . . ?
N4 Cu1 N1 C1 121.7(3) 4_566 . . . ?
N4 Cu1 N1 C1 -58.3(3) 2_645 . . . ?
O1 Cu1 N1 N2 33.2(2) . . . . ?
O1 Cu1 N1 N2 -146.8(2) 3_656 . . . ?
N4 Cu1 N1 N2 -53.7(2) 4_566 . . . ?
N4 Cu1 N1 N2 126.3(2) 2_645 . . . ?
C1 N1 N2 C4 -2.3(5) . . . . ?
Cu1 N1 N2 C4 173.4(3) . . . . ?
C1 N1 N2 Cu2 174.7(3) . . . . ?
Cu1 N1 N2 Cu2 -9.6(3) . . . . ?
O1 Cu2 N2 C4 157.6(3) . . . . ?
O3 Cu2 N2 C4 -22.9(3) . . . . ?
O2 Cu2 N2 C4 68.6(4) . . . . ?
N3 Cu2 N2 C4 -111.1(3) 4_566 . . . ?
O1 Cu2 N2 N1 -19.1(2) . . . . ?
O3 Cu2 N2 N1 160.3(2) . . . . ?
O2 Cu2 N2 N1 -108.2(3) . . . . ?
N3 Cu2 N2 N1 72.1(2) 4_566 . . . ?
C5 N3 N4 C8 1.0(5) . . . . ?
Cu2 N3 N4 C8 -169.4(3) 4_565 . . . ?
C5 N3 N4 Cu1 179.4(3) . . . 2_655 ?
Cu2 N3 N4 Cu1 8.9(3) 4_565 . . 2_655 ?
N2 N1 C1 C2 3.1(5) . . . . ?
Cu1 N1 C1 C2 -172.2(3) . . . . ?
N1 C1 C2 C3 -0.8(6) . . . . ?
C1 C2 C3 C4 -2.0(5) . . . . ?
C1 C2 C3 C9 178.5(3) . . . . ?
N1 N2 C4 C3 -0.6(5) . . . . ?
Cu2 N2 C4 C3 -177.3(3) . . . . ?
C2 C3 C4 N2 2.8(5) . . . . ?
C9 C3 C4 N2 -177.7(3) . . . . ?
N4 N3 C5 C6 0.0(6) . . . . ?
Cu2 N3 C5 C6 168.3(3) 4_565 . . . ?
N3 C5 C6 C7 -1.6(6) . . . . ?
C5 C6 C7 C8 2.1(5) . . . . ?
C5 C6 C7 C11 -179.2(3) . . . . ?
N3 N4 C8 C7 -0.4(5) . . . . ?
Cu1 N4 C8 C7 -178.7(3) 2_655 . . . ?
C6 C7 C8 N4 -1.2(5) . . . . ?
C11 C7 C8 N4 -179.9(3) . . . . ?
C2 C3 C9 C15 -11.5(5) . . . . ?
C4 C3 C9 C15 169.0(3) . . . . ?
C2 C3 C9 C10 109.6(4) . . . . ?
C4 C3 C9 C10 -69.9(4) . . . . ?
C2 C3 C9 C14 -131.8(4) . . . . ?
C4 C3 C9 C14 48.7(4) . . . . ?
C3 C9 C10 C11 178.7(3) . . . . ?
C15 C9 C10 C11 -58.1(4) . . . . ?
C14 C9 C10 C11 59.5(4) . . . . ?
C6 C7 C11 C17 178.3(3) . . . . ?
C8 C7 C11 C17 -3.1(5) . . . . ?
C6 C7 C11 C12 -61.2(4) . . . . ?
C8 C7 C11 C12 117.4(4) . . . . ?
C6 C7 C11 C10 57.2(5) . . . . ?
C8 C7 C11 C10 -124.1(4) . . . . ?
C9 C10 C11 C7 -178.5(3) . . . . ?
C9 C10 C11 C17 58.0(4) . . . . ?
C9 C10 C11 C12 -59.4(4) . . . . ?
C7 C11 C12 C13 179.3(3) . . . . ?
C17 C11 C12 C13 -57.8(4) . . . . ?
C10 C11 C12 C13 59.4(4) . . . . ?
C11 C12 C13 C18 59.3(4) . . . . ?
C11 C12 C13 C14 -61.0(4) . . . . ?
C12 C13 C14 C9 60.3(4) . . . . ?
C18 C13 C14 C9 -60.6(4) . . . . ?
C3 C9 C14 C13 -178.1(3) . . . . ?
C15 C9 C14 C13 59.1(4) . . . . ?
C10 C9 C14 C13 -58.8(4) . . . . ?
C3 C9 C15 C16 -179.6(3) . . . . ?
C10 C9 C15 C16 59.0(4) . . . . ?
C14 C9 C15 C16 -58.6(4) . . . . ?
C9 C15 C16 C18 60.5(4) . . . . ?
C9 C15 C16 C17 -61.0(4) . . . . ?
C18 C16 C17 C11 -60.2(4) . . . . ?
C15 C16 C17 C11 61.2(4) . . . . ?
C7 C11 C17 C16 178.5(3) . . . . ?
C12 C11 C17 C16 57.7(4) . . . . ?
C10 C11 C17 C16 -59.3(4) . . . . ?
C17 C16 C18 C13 60.1(4) . . . . ?
C15 C16 C18 C13 -60.7(4) . . . . ?
C12 C13 C18 C16 -59.8(4) . . . . ?
C14 C13 C18 C16 61.1(4) . . . . ?
Cu3 O4 C19 O3 13.0(6) . . . . ?
Cu3 O4 C19 C21 -171.0(2) . . . . ?
Cu2 O3 C19 O4 19.8(5) . . . . ?
Cu2 O3 C19 C21 -156.2(2) . . . . ?
Cu3 O6 C20 O5 -7.9(5) 2 . . . ?
Cu3 O6 C20 C23 169.6(2) 2 . . . ?
O4 C19 C21 C22 0.4(5) . . . . ?
O3 C19 C21 C22 176.7(3) . . . . ?
O4 C19 C21 C26 -174.3(3) . . . . ?
O3 C19 C21 C26 2.1(5) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
C19 C21 C22 C23 -174.7(3) . . . . ?
C21 C22 C23 C24 -0.3(5) . . . . ?
C21 C22 C23 C20 178.1(3) . . . . ?
O5 C20 C23 C24 174.1(4) . . . . ?
O6 C20 C23 C24 -3.6(5) . . . . ?
O5 C20 C23 C22 -4.3(5) . . . . ?
O6 C20 C23 C22 178.0(3) . . . . ?
C22 C23 C24 C25 0.1(6) . . . . ?
C20 C23 C24 C25 -178.3(3) . . . . ?
C23 C24 C25 O7 -179.9(3) . . . . ?
C23 C24 C25 C26 0.4(6) . . . . ?
O7 C25 C26 C21 179.6(4) . . . . ?
C24 C25 C26 C21 -0.8(6) . . . . ?
C22 C21 C26 C25 0.6(5) . . . . ?
C19 C21 C26 C25 175.2(3) . . . . ?
Cu3 O8 C27 O9 -30.3(6) . . . . ?
Cu3 O8 C27 C29 150.1(2) . . . . ?
Cu3 O10 C28 O11 -1.5(4) 1_455 . . . ?
Cu3 O10 C28 C31 177.4(2) 1_455 . . . ?
O9 C27 C29 C30 -37.9(5) . . . . ?
O8 C27 C29 C30 141.7(4) . . . . ?
O9 C27 C29 C34 146.0(4) . . . . ?
O8 C27 C29 C34 -34.3(5) . . . . ?
C34 C29 C30 C31 4.6(5) . . . . ?
C27 C29 C30 C31 -171.5(3) . . . . ?
C29 C30 C31 C32 -2.1(5) . . . . ?
C29 C30 C31 C28 179.9(3) . . . . ?
O11 C28 C31 C32 9.6(5) . . . . ?
O10 C28 C31 C32 -169.4(3) . . . . ?
O11 C28 C31 C30 -172.4(3) . . . . ?
O10 C28 C31 C30 8.6(5) . . . . ?
C30 C31 C32 C33 -3.3(5) . . . . ?
C28 C31 C32 C33 174.8(3) . . . . ?
C31 C32 C33 O12 -175.1(3) . . . . ?
C31 C32 C33 C34 6.1(6) . . . . ?
O12 C33 C34 C29 177.7(3) . . . . ?
C32 C33 C34 C29 -3.6(6) . . . . ?
C30 C29 C34 C33 -1.7(6) . . . . ?
C27 C29 C34 C33 174.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.104


_iucr_refine_instruction_details 
;
#---------------------------------------------------------
TITL dk23 in P2(1)/c
CELL  0.71073  10.0552  18.7840  19.1757   90.000  104.829   90.000
ZERR     2.00   0.0005   0.0008   0.0009    0.000    0.002    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    CU
UNIT  136  148  16   60   10
MERG   2
SHEL 0.77 8
FMAP   2
PLAN   20
SIZE     0.12   0.14   0.25
 
EQIV $1 1+X, Y, Z
 
BIND Cu3 O2
BIND Cu3 O11_$1
 
EQIV $2 X, -1+Y, Z
EQIV $3 -X, -0.5+Y, 0.5-Z
EQIV $4 1+X, 0.5-Y, 0.5+Z
EQIV $5 -X, 0.5+Y, 0.5-Z
EQIV $6 -1-X, 0.5+Y, 0.5-Z
EQIV $7 -X, 1-Y, 1-Z
 
RTAB H..O H1H O1W_$2
RTAB H..O H1W O5_$3
RTAB H..O H2W O9
RTAB H..O H1O O11_$4
RTAB H..O H2O O1W_$3
RTAB H..O H3W O5_$5
RTAB H..O H4W O2W
RTAB H..O H5W O3W
RTAB H..O H6W O11_$6
RTAB H..O H7W O7_$7
RTAB H..O H8W O8_$5
 
RTAB O..O O1 O1W_$2
RTAB O..O O2 O5_$3
RTAB O..O O2 O9
RTAB O..O O7 O11_$4
RTAB O..O O12 O1W_$3
RTAB O..O O1W O5_$5
RTAB O..O O1W O2W
RTAB O..O O2W O3W
RTAB O..O O2W O11_$6
RTAB O..O O3W O7_$7
RTAB O..O O3W O8_$5
 
RTAB XHY O1 H1H O1W_$2
RTAB XHY O2 H1W O5_$3
RTAB XHY O2 H2W O9
RTAB XHY O7 H1O O11_$4
RTAB XHY O12 H2O O1W_$3
RTAB XHY O1W H3W O5_$5
RTAB XHY O1W H4W O2W
RTAB XHY O2W H5W O3W
RTAB XHY O2W H6W O11_$6
RTAB XHY O3W H7W O7_$7
RTAB XHY O3W H8W O8_$5
 
ACTA
BOND
BOND $H
CONF
L.S.   4
TEMP    -100.00
WGHT    0.030800
FVAR       0.29282
CU1   5    0.500000    0.000000    0.500000    10.50000    0.02145    0.01555 =
         0.01441    0.00103   -0.00136    0.00414
CU2   5    0.218726    0.080994    0.430592    11.00000    0.02680    0.01440 =
         0.02372   -0.00245   -0.00597    0.00703
CU3   5    0.059828    0.102300    0.259259    11.00000    0.01585    0.01589 =
         0.01728   -0.00290    0.00410   -0.00016
O1    4    0.325708   -0.001394    0.431621    11.00000    0.02309    0.01388 =
         0.02956   -0.00149   -0.00405    0.00297
AFIX   3
H1H   2    0.279515   -0.039810    0.426087    11.00000   -1.50000
AFIX   0
O2    4    0.044995    0.032378    0.378055    11.00000    0.02460    0.02255 =
         0.04515   -0.01392   -0.00112    0.00397
AFIX   3
H1W   2    0.034112   -0.009200    0.359987    11.00000   -1.50000
H2W   2   -0.031751    0.046614    0.383832    11.00000   -1.50000
AFIX   0
O3    4    0.117707    0.168524    0.430578    11.00000    0.03395    0.01619 =
         0.02183    0.00303   -0.00174    0.00833
O4    4    0.064018    0.191477    0.311731    11.00000    0.04133    0.01802 =
         0.02079   -0.00323    0.01038   -0.00004
O5    4   -0.041791    0.435908    0.223905    11.00000    0.05473    0.02736 =
         0.01754    0.00414    0.00721   -0.00174
O6    4   -0.043675    0.521450    0.304247    11.00000    0.03564    0.01868 =
         0.02559    0.00639    0.01295    0.00510
O7    4    0.087856    0.409363    0.543135    11.00000    0.07914    0.02219 =
         0.01587   -0.00327    0.00761    0.00950
AFIX   3
H1O   2    0.109165    0.377873    0.575934    11.00000   -1.50000
AFIX   0
O8    4   -0.136913    0.107404    0.234719    11.00000    0.01434    0.04693 =
         0.02513   -0.00302    0.00537    0.00459
O9    4   -0.200770    0.097449    0.337221    11.00000    0.02409    0.05589 =
         0.02808    0.01416    0.00842    0.01459
O10   4   -0.741727    0.108860    0.267775    11.00000    0.01492    0.03103 =
         0.02152    0.00299    0.00345   -0.00028
O11   4   -0.841551    0.167518    0.167738    11.00000    0.01545    0.03663 =
         0.02441   -0.00130   -0.00130    0.00225
O12   4   -0.462290    0.290501    0.094742    11.00000    0.03723    0.04030 =
         0.04220    0.02043    0.01112   -0.00167
AFIX   3
H2O   2   -0.383390    0.309971    0.104022    11.00000   -1.50000
AFIX   0
N1    3    0.520487    0.102456    0.455289    11.00000    0.02601    0.01804 =
         0.01790    0.00091    0.00021    0.00905
N2    3    0.403920    0.139572    0.432737    11.00000    0.02714    0.01577 =
         0.02083    0.00147    0.00185    0.00277
N3    3    0.264251    0.419015    0.050662    11.00000    0.02637    0.02127 =
         0.02356   -0.00077    0.00086   -0.00610
N4    3    0.388330    0.446465    0.079849    11.00000    0.02380    0.02273 =
         0.01583    0.00062   -0.00104   -0.00600
C1    1    0.637467    0.132595    0.452805    11.00000    0.01902    0.03147 =
         0.02347    0.00431    0.00283    0.01071
AFIX  43
H1    2    0.717172    0.105369    0.466414    11.00000   -1.20000
AFIX   0
C2    1    0.649743    0.202817    0.431060    11.00000    0.02433    0.03367 =
         0.02091    0.00527    0.00540    0.00410
AFIX  43
H2    2    0.734978    0.221879    0.430806    11.00000   -1.20000
AFIX   0
C3    1    0.531418    0.242822    0.410030    11.00000    0.02557    0.02401 =
         0.01037    0.00231    0.00110    0.00151
C4    1    0.410355    0.206203    0.411034    11.00000    0.02737    0.01894 =
         0.02387    0.00088    0.00099    0.00379
AFIX  43
H4    2    0.327744    0.230695    0.395159    11.00000   -1.20000
AFIX   0
C5    1    0.198351    0.387648    0.094118    11.00000    0.02118    0.03847 =
         0.02207    0.00369   -0.00257   -0.00828
AFIX  43
H5    2    0.111795    0.368486    0.073858    11.00000   -1.20000
AFIX   0
C6    1    0.251845    0.381944    0.168223    11.00000    0.03079    0.03777 =
         0.02193    0.00741    0.00691   -0.00608
AFIX  43
H6    2    0.200977    0.360546    0.196721    11.00000   -1.20000
AFIX   0
C7    1    0.381272    0.408429    0.198871    11.00000    0.02035    0.01894 =
         0.01713   -0.00007    0.00134    0.00171
C8    1    0.444551    0.441467    0.149936    11.00000    0.02237    0.02570 =
         0.01693   -0.00043    0.00229   -0.00351
AFIX  43
H8    2    0.531503    0.461048    0.168044    11.00000   -1.20000
AFIX   0
C9    1    0.526753    0.320208    0.386627    11.00000    0.02240    0.02090 =
         0.01298    0.00109   -0.00052   -0.00514
C10   1    0.460033    0.325360    0.304753    11.00000    0.02054    0.02066 =
         0.01366   -0.00002    0.00209    0.00022
AFIX  23
H10A  2    0.368565    0.304772    0.294007    11.00000   -1.20000
H10B  2    0.514298    0.298314    0.278865    11.00000   -1.20000
AFIX   0
C11   1    0.450276    0.404242    0.278829    11.00000    0.02592    0.01806 =
         0.01915   -0.00065    0.00501   -0.00225
C12   1    0.362434    0.445572    0.320898    11.00000    0.03546    0.01934 =
         0.02353   -0.00302    0.00711    0.00387
AFIX  23
H12A  2    0.354504    0.494938    0.305544    11.00000   -1.20000
H12B  2    0.270656    0.425380    0.310371    11.00000   -1.20000
AFIX   0
C13   1    0.427796    0.441752    0.401392    11.00000    0.05287    0.02062 =
         0.02515   -0.00562    0.01598    0.00459
AFIX  13
H13   2    0.371460    0.468798    0.426914    11.00000   -1.20000
AFIX   0
C14   1    0.436754    0.363783    0.426945    11.00000    0.03929    0.02578 =
         0.02014   -0.00008    0.01062    0.00076
AFIX  23
H14A  2    0.345184    0.343411    0.417113    11.00000   -1.20000
H14B  2    0.477312    0.361705    0.478562    11.00000   -1.20000
AFIX   0
C15   1    0.669862    0.354074    0.403035    11.00000    0.02885    0.02837 =
         0.01953    0.00102   -0.00014   -0.00197
AFIX  23
H15A  2    0.727113    0.328104    0.378016    11.00000   -1.20000
H15B  2    0.712561    0.351315    0.454405    11.00000   -1.20000
AFIX   0
C16   1    0.659564    0.432287    0.378925    11.00000    0.02774    0.02921 =
         0.02137   -0.00047   -0.00161   -0.01123
AFIX  13
H16   2    0.752182    0.452847    0.389918    11.00000   -1.20000
AFIX   0
C17   1    0.596659    0.436085    0.297947    11.00000    0.02526    0.02688 =
         0.02013    0.00180    0.00377   -0.00149
AFIX  23
H17A  2    0.653783    0.409910    0.273011    11.00000   -1.20000
H17B  2    0.592792    0.485290    0.282204    11.00000   -1.20000
AFIX   0
C18   1    0.573255    0.473777    0.418772    11.00000    0.05492    0.02395 =
         0.02323   -0.00722    0.00119   -0.00370
AFIX  23
H18A  2    0.568587    0.523334    0.404121    11.00000   -1.20000
H18B  2    0.614651    0.471490    0.470300    11.00000   -1.20000
AFIX   0
C19   1    0.077717    0.208834    0.376087    11.00000    0.01265    0.01473 =
         0.02700   -0.00072    0.00266    0.00200
C20   1   -0.031098    0.457223    0.286885    11.00000    0.01895    0.02033 =
         0.02410    0.00559    0.00549    0.00066
C21   1    0.053237    0.285373    0.391203    11.00000    0.01957    0.01785 =
         0.01557    0.00124    0.00243    0.00280
C22   1    0.016209    0.333111    0.334182    11.00000    0.02452    0.01775 =
         0.01462   -0.00024    0.00463    0.00368
AFIX  43
H22   2   -0.000661    0.316846    0.286916    11.00000   -1.20000
AFIX   0
C23   1    0.004435    0.404928    0.347767    11.00000    0.02108    0.01604 =
         0.01861    0.00369    0.00402    0.00344
C24   1    0.029059    0.428674    0.418191    11.00000    0.03633    0.01312 =
         0.01958    0.00022    0.00809    0.00572
AFIX  43
H24   2    0.020989    0.476893    0.427323    11.00000   -1.20000
AFIX   0
C25   1    0.065955    0.380868    0.475746    11.00000    0.03421    0.01917 =
         0.01659    0.00024    0.00568    0.00701
C26   1    0.078895    0.309369    0.462364    11.00000    0.02702    0.01537 =
         0.01812    0.00376    0.00573    0.00532
AFIX  43
H26   2    0.104523    0.277370    0.500456    11.00000   -1.20000
AFIX   0
C27   1   -0.220105    0.116591    0.273790    11.00000    0.02004    0.02224 =
         0.02808   -0.00428    0.00567   -0.00285
C28   1   -0.735437    0.145723    0.213015    11.00000    0.02000    0.01955 =
         0.02231   -0.01326    0.00274   -0.00079
C29   1   -0.351432    0.153950    0.235584    11.00000    0.01540    0.02429 =
         0.02598   -0.00262    0.00513    0.00403
C30   1   -0.477422    0.135243    0.246455    11.00000    0.01741    0.02087 =
         0.02213   -0.00112    0.00444    0.00164
AFIX  43
H30   2   -0.482259    0.103117    0.282627    11.00000   -1.20000
AFIX   0
C31   1   -0.597157    0.164744    0.202961    11.00000    0.01370    0.01953 =
         0.02139   -0.00191    0.00310    0.00001
C32   1   -0.590224    0.214303    0.150607    11.00000    0.01891    0.02886 =
         0.02259    0.00031    0.00159    0.00394
AFIX  43
H32   2   -0.670817    0.231913    0.120154    11.00000   -1.20000
AFIX   0
C33   1   -0.463787    0.237852    0.143299    11.00000    0.02988    0.02624 =
         0.02420    0.00518    0.00965    0.00189
C34   1   -0.344978    0.205956    0.184634    11.00000    0.01971    0.03131 =
         0.03168    0.00075    0.01179   -0.00495
AFIX  43
H34   2   -0.259905    0.219473    0.178244    11.00000   -1.20000
AFIX   0
O1W   4    0.214956    0.857799    0.381493    11.00000    0.03920    0.02927 =
         0.04444    0.00222   -0.00147   -0.00109
AFIX   3
H3W   2    0.177816    0.880678    0.343222    11.00000   -1.50000
H4W   2    0.162189    0.823559    0.385562    11.00000   -1.50000
AFIX   0
O2W   4    0.068431    0.746574    0.407505    11.00000    0.05626    0.06151 =
         0.06625   -0.00464    0.01171   -0.02251
AFIX   3
H5W   2    0.115270    0.708545    0.417589    11.00000   -1.50000
H6W   2   -0.012027    0.735659    0.383018    11.00000   -1.50000
AFIX   0
O3W   4    0.191213    0.610189    0.417419    11.00000    0.07847    0.08251 =
         0.02791   -0.00088    0.00248   -0.01815
AFIX   3
H7W   2    0.122196    0.590259    0.427130    11.00000   -1.50000
H8W   2    0.184219    0.605606    0.372531    11.00000   -1.50000
HKLF    4
 
REM  dk23 in P2(1)/c
REM R1 =  0.0471 for   5132 Fo > 4sig(Fo)  and  0.0941 for all   8020 data
REM    502 parameters refined using      0 restraints
 
END
 
WGHT      0.0312      0.0000
REM Highest difference peak  0.474,  deepest hole -0.534,  1-sigma level  0.104
Q1    1   0.2858  0.1563  0.4597  11.00000  0.05    0.47
Q2    1   0.2692  0.0351  0.3885  11.00000  0.05    0.46
Q3    1   0.5557 -0.0544  0.4788  11.00000  0.05    0.45
Q4    1   0.0877  0.7817  0.4700  11.00000  0.05    0.45
Q5    1   0.2407  0.4286  0.0078  11.00000  0.05    0.44
Q6    1   0.2983 -0.0261  0.4192  11.00000  0.05    0.44
Q7    1   0.1624  0.0734  0.3603  11.00000  0.05    0.43
Q8    1   0.1000  0.1902  0.3365  11.00000  0.05    0.43
Q9    1   0.0335  0.1611  0.3004  11.00000  0.05    0.43
Q10   1   0.3875  0.0034  0.4517  11.00000  0.05    0.43
;

#   -------------  END of CIF  -----------------#

_database_code_depnum_ccdc_archive 'CCDC 967348'
