# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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 
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#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
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data_yyculg
_database_code_depnum_ccdc_archive 'CCDC 906058'
#TrackingRef 'YYCULG.CIF'
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.002 -0.014 -0.004 31876 6889 ' '
_platon_squeeze_details          
;
Approximately 74% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region. SQUEEZE estimated a total count of 6889 electrons
per unit cell, and thereby produced a set of solvent-free diffraction
intensities. The final formula was calculated from the TGA results combined
with elemental analysis data.
;
_refine_special_details          
;
The central phenyl ring and the three triazole moieties in the central core
of the hexacaboxylate ligand are equally disordered over two sets of positions.
The relevant atoms were refined isotropically.
;
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cu3 C36 H21 N9 O15, 10(C3 H7 N O), 10(H2 O)'
_chemical_formula_sum            'C66 H111 Cu3 N19 O35'
_chemical_formula_weight         1921.36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0108 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3483 1.2194 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 4/m'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
_cell_length_a                   30.926(5)
_cell_length_b                   30.926(5)
_cell_length_c                   45.103(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     43137(11)
_cell_formula_units_Z            16
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    56775
_cell_measurement_theta_min      0.9
_cell_measurement_theta_max      31.7
_exptl_crystal_description       'truncated octahedron'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             16112
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Diamond Beamline I19'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            53063
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.064
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         24.00
_reflns_number_total             18798
_reflns_number_gt                13280
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.126P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         18798
_refine_ls_number_parameters     553
_refine_ls_number_restraints     488
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.201
_refine_ls_wR_factor_gt          0.189
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_restrained_S_all      1.03
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.637837(14) 0.301075(14) 0.831079(10) 0.03727(14) Uani 1 1 d U . .
Cu2 Cu 0.601955(13) 0.352284(13) 0.871961(10) 0.03622(14) Uani 1 1 d U . .
Cu3 Cu 0.750576(18) 0.04306(2) 0.5000 0.03433(16) Uani 1 2 d SU . .
Cu4 Cu 0.665412(18) 0.05754(2) 0.5000 0.03611(17) Uani 1 2 d SU . .
O5 O 0.58044(8) 0.30183(9) 0.81251(6) 0.0506(7) Uani 1 1 d U . .
O6 O 0.55298(8) 0.34936(9) 0.84463(6) 0.0496(7) Uani 1 1 d U . .
O7 O 0.39857(8) 0.37287(9) 0.84802(6) 0.0506(7) Uani 1 1 d U . .
O8 O 0.35572(8) 0.34832(9) 0.81152(6) 0.0524(7) Uani 1 1 d U . .
O9 O 0.81056(8) 0.19121(9) 0.64381(6) 0.0512(7) Uani 1 1 d U . .
O10 O 0.84251(8) 0.15353(9) 0.60754(6) 0.0502(7) Uani 1 1 d U . .
O11 O 0.67111(13) 0.25940(13) 0.80086(8) 0.0935(12) Uani 1 1 d U . .
O12 O 0.56662(13) 0.38952(12) 0.90514(7) 0.0854(12) Uani 1 1 d U . .
O13 O 0.68120(8) 0.09916(9) 0.53078(6) 0.0509(7) Uani 1 1 d U . .
O14 O 0.75305(8) 0.08784(9) 0.53039(6) 0.0481(7) Uani 1 1 d U . .
O15 O 0.33757(8) -0.01189(10) 0.53024(6) 0.0531(7) Uani 1 1 d U . .
O16 O 0.26575(8) -0.00129(9) 0.53066(6) 0.0531(7) Uani 1 1 d U . .
O17 O 0.59809(14) 0.0731(2) 0.5000 0.0982(18) Uani 1 2 d SU . .
O18 O 0.81964(15) 0.02969(16) 0.5000 0.122(3) Uani 1 2 d SU . .
O19 O 0.24553(8) 0.11865(9) 0.64253(6) 0.0511(7) Uani 1 1 d U . .
O20 O 0.20268(8) 0.08299(9) 0.61062(6) 0.0532(7) Uani 1 1 d U . .
C1 C 0.55082(12) 0.32475(13) 0.82270(9) 0.0453(9) Uani 1 1 d U . .
C2 C 0.50758(13) 0.32311(14) 0.80715(9) 0.0510(10) Uani 1 1 d U . .
C3 C 0.50360(14) 0.30246(16) 0.77991(11) 0.0660(13) Uani 1 1 d U . .
H3A H 0.5282 0.2903 0.7704 0.079 Uiso 1 1 calc R . .
C4 C 0.46323(14) 0.29989(18) 0.76697(11) 0.0728(13) Uani 1 1 d U . .
C5 C 0.42668(14) 0.31728(17) 0.78082(11) 0.0701(13) Uani 1 1 d U . .
H5A H 0.3991 0.3153 0.7717 0.084 Uiso 1 1 calc R . .
C6 C 0.43124(13) 0.33736(14) 0.80791(9) 0.0520(10) Uani 1 1 d U . .
C7 C 0.47179(12) 0.34085(12) 0.82069(9) 0.0445(9) Uani 1 1 d U . .
H7A H 0.4750 0.3557 0.8390 0.053 Uiso 1 1 calc R . .
C10 C 0.4829(3) 0.2370(3) 0.66529(18) 0.0530(19) Uiso 0.50 1 d PDU A 1
C11 C 0.5266(3) 0.2420(3) 0.65761(18) 0.0538(19) Uiso 0.50 1 d PDU A 1
H11B H 0.5447 0.2609 0.6687 0.065 Uiso 0.50 1 calc PR A 1
C12 C 0.5433(3) 0.2188(2) 0.63338(18) 0.0498(18) Uiso 0.50 1 d PDU A 1
C13 C 0.5157(3) 0.1905(2) 0.61695(19) 0.0509(18) Uiso 0.50 1 d PDU A 1
H13A H 0.5269 0.1747 0.6006 0.061 Uiso 0.50 1 calc PR A 1
C14 C 0.4725(3) 0.1860(3) 0.62485(19) 0.0551(19) Uiso 0.50 1 d PDU A 1
C15 C 0.4565(3) 0.2100(3) 0.64956(19) 0.060(2) Uiso 0.50 1 d PDU A 1
H15A H 0.4270 0.2072 0.6551 0.071 Uiso 0.50 1 calc PR A 1
C10' C 0.4853(3) 0.2157(3) 0.67542(19) 0.0541(19) Uiso 0.50 1 d PDU A 2
C11' C 0.5281(3) 0.2214(3) 0.66763(19) 0.055(2) Uiso 0.50 1 d PDU A 2
H11C H 0.5460 0.2408 0.6785 0.066 Uiso 0.50 1 calc PR A 2
C12' C 0.5449(3) 0.1982(3) 0.64363(19) 0.0550(19) Uiso 0.50 1 d PDU A 2
C13' C 0.5178(3) 0.1696(3) 0.6277(2) 0.062(2) Uiso 0.50 1 d PDU A 2
H13B H 0.5291 0.1542 0.6113 0.074 Uiso 0.50 1 calc PR A 2
C14' C 0.4760(3) 0.1641(3) 0.6357(2) 0.063(2) Uiso 0.50 1 d PDU A 2
C15' C 0.4596(3) 0.1873(3) 0.6595(2) 0.064(2) Uiso 0.50 1 d PDU A 2
H15B H 0.4302 0.1837 0.6650 0.076 Uiso 0.50 1 calc PR A 2
C16 C 0.4431(3) 0.1600(3) 0.6075(2) 0.058(2) Uiso 0.50 1 d PDU A 1
C17 C 0.4035(3) 0.1451(2) 0.61390(19) 0.0462(18) Uiso 0.50 1 d PDU A 1
H17B H 0.3870 0.1522 0.6310 0.055 Uiso 0.50 1 calc PR A 1
N7 N 0.4544(3) 0.1419(3) 0.5810(2) 0.085(2) Uiso 0.50 1 d PDU A 1
N8 N 0.4224(3) 0.1165(3) 0.5711(2) 0.076(2) Uiso 0.50 1 d PDU A 1
N9 N 0.3910(2) 0.1181(2) 0.59180(16) 0.0508(15) Uiso 0.50 1 d PDU A 1
C16' C 0.4478(3) 0.1383(3) 0.6179(2) 0.060(2) Uiso 0.50 1 d PDU A 2
C17' C 0.4047(3) 0.1271(3) 0.62256(19) 0.053(2) Uiso 0.50 1 d PDU A 2
H17C H 0.3863 0.1382 0.6376 0.063 Uiso 0.50 1 calc PR A 2
N7' N 0.4627(3) 0.1155(3) 0.5944(2) 0.084(2) Uiso 0.50 1 d PDU A 2
N8' N 0.4302(3) 0.0899(3) 0.5840(2) 0.088(2) Uiso 0.50 1 d PDU A 2
N9' N 0.3942(2) 0.0979(2) 0.60193(17) 0.0600(17) Uiso 0.50 1 d PDU A 2
C8 C 0.4882(3) 0.2756(2) 0.71495(19) 0.0481(18) Uiso 0.50 1 d PDU A 1
H8A H 0.5186 0.2766 0.7175 0.058 Uiso 0.50 1 calc PR A 1
C9 C 0.4667(3) 0.2592(2) 0.69145(19) 0.0503(18) Uiso 0.50 1 d PDU A 1
N4 N 0.4240(3) 0.2643(2) 0.6966(2) 0.077(2) Uiso 0.50 1 d PDU A 1
N5 N 0.4182(3) 0.2840(2) 0.72316(19) 0.072(2) Uiso 0.50 1 d PDU A 1
N6 N 0.4581(2) 0.2905(2) 0.73415(16) 0.0506(15) Uiso 0.50 1 d PDU A 1
C8' C 0.4902(3) 0.2592(2) 0.72343(18) 0.0468(18) Uiso 0.50 1 d PDU A 2
H8'A H 0.5204 0.2648 0.7245 0.056 Uiso 0.50 1 calc PR A 2
C9' C 0.4681(3) 0.2380(3) 0.7015(2) 0.0569(19) Uiso 0.50 1 d PDU A 2
N4' N 0.4250(3) 0.2362(2) 0.70799(19) 0.073(2) Uiso 0.50 1 d PDU A 2
N5' N 0.4198(3) 0.2567(3) 0.7344(2) 0.079(2) Uiso 0.50 1 d PDU A 2
N6' N 0.4589(2) 0.2705(2) 0.74337(16) 0.0512(16) Uiso 0.50 1 d PDU A 2
C32 C 0.6131(2) 0.1916(3) 0.60928(16) 0.0415(17) Uiso 0.50 1 d PDU A 1
H32A H 0.6032 0.1662 0.5996 0.050 Uiso 0.50 1 calc PR A 1
C36 C 0.5888(3) 0.2208(3) 0.62557(17) 0.0490(18) Uiso 0.50 1 d PDU A 1
N1 N 0.6539(2) 0.2073(2) 0.61030(13) 0.0395(14) Uiso 0.50 1 d PDU A 1
N2 N 0.6550(2) 0.2441(2) 0.62630(14) 0.0442(15) Uiso 0.50 1 d PDU A 1
N3 N 0.6158(2) 0.2520(2) 0.63533(15) 0.0510(16) Uiso 0.50 1 d PDU A 1
C32' C 0.6151(3) 0.1754(3) 0.61783(16) 0.0443(18) Uiso 0.50 1 d PDU A 2
H32B H 0.6060 0.1507 0.6069 0.053 Uiso 0.50 1 calc PR A 2
C36' C 0.5899(3) 0.2020(3) 0.63606(19) 0.0557(19) Uiso 0.50 1 d PDU A 2
N1' N 0.6548(2) 0.1924(2) 0.61934(14) 0.0446(15) Uiso 0.50 1 d PDU A 2
N2' N 0.6566(2) 0.2281(2) 0.63719(16) 0.0578(18) Uiso 0.50 1 d PDU A 2
N3' N 0.6170(2) 0.2339(2) 0.64755(16) 0.0607(18) Uiso 0.50 1 d PDU A 2
C18 C 0.35268(15) 0.0877(2) 0.59110(12) 0.0792(14) Uani 1 1 d U . .
C19 C 0.31741(14) 0.10058(18) 0.60824(11) 0.0750(14) Uani 1 1 d U A .
H19A H 0.3207 0.1214 0.6236 0.090 Uiso 1 1 calc R . .
C20 C 0.27713(13) 0.08219(14) 0.60229(10) 0.0535(10) Uani 1 1 d U . .
C21 C 0.27266(13) 0.05254(14) 0.57929(10) 0.0527(10) Uani 1 1 d U A .
H21A H 0.2450 0.0411 0.5746 0.063 Uiso 1 1 calc R . .
C22 C 0.30908(13) 0.03951(16) 0.56308(11) 0.0615(11) Uani 1 1 d U . .
C23 C 0.34908(15) 0.05779(19) 0.56904(11) 0.0807(15) Uani 1 1 d U A .
H23A H 0.3738 0.0495 0.5578 0.097 Uiso 1 1 calc R . .
C24 C 0.23886(12) 0.09557(13) 0.61989(9) 0.0476(9) Uani 1 1 d U A .
C25 C 0.76457(12) 0.14188(13) 0.57873(9) 0.0456(9) Uani 1 1 d U A .
H25A H 0.7895 0.1285 0.5705 0.055 Uiso 1 1 calc R . .
C26 C 0.76822(12) 0.16764(13) 0.60404(9) 0.0476(9) Uani 1 1 d U . .
C27 C 0.73179(13) 0.18814(15) 0.61613(10) 0.0592(11) Uani 1 1 d U A .
H27A H 0.7342 0.2055 0.6334 0.071 Uiso 1 1 calc R . .
C28 C 0.69200(13) 0.18247(16) 0.60221(10) 0.0604(11) Uani 1 1 d U . .
C29 C 0.68775(13) 0.15606(16) 0.57700(10) 0.0607(11) Uani 1 1 d U A .
H29A H 0.6603 0.1521 0.5679 0.073 Uiso 1 1 calc R . .
C30 C 0.72421(12) 0.13584(13) 0.56557(9) 0.0474(9) Uani 1 1 d U . .
C31 C 0.81054(12) 0.17154(12) 0.61970(9) 0.0443(9) Uani 1 1 d U . .
C33 C 0.71919(12) 0.10550(13) 0.54009(8) 0.0436(9) Uani 1 1 d U A .
C34 C 0.30344(13) 0.00557(14) 0.53898(9) 0.0495(9) Uani 1 1 d U A .
C35 C 0.39210(12) 0.35443(12) 0.82399(9) 0.0445(9) Uani 1 1 d U A .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0371(2) 0.0372(2) 0.0375(3) -0.00865(19) 0.01148(19) -0.00412(18)
Cu2 0.0351(2) 0.0364(2) 0.0371(3) -0.00703(19) 0.01075(18) -0.00427(17)
Cu3 0.0289(3) 0.0462(4) 0.0279(3) 0.000 0.000 0.0036(2)
Cu4 0.0285(3) 0.0511(4) 0.0287(3) 0.000 0.000 0.0054(3)
O5 0.0410(14) 0.0603(17) 0.0505(16) -0.0183(14) 0.0005(12) 0.0023(12)
O6 0.0378(14) 0.0583(16) 0.0527(17) -0.0195(14) 0.0001(12) -0.0008(12)
O7 0.0423(14) 0.0630(17) 0.0466(16) -0.0223(14) -0.0015(12) 0.0078(12)
O8 0.0456(15) 0.0648(17) 0.0468(16) -0.0241(14) -0.0013(13) 0.0100(13)
O9 0.0390(14) 0.0630(17) 0.0515(17) -0.0199(14) 0.0051(12) 0.0002(12)
O10 0.0379(14) 0.0668(18) 0.0459(16) -0.0168(14) 0.0036(12) 0.0033(13)
O11 0.100(3) 0.096(3) 0.085(3) -0.049(2) 0.035(2) 0.011(2)
O12 0.122(3) 0.089(2) 0.0458(19) -0.0022(18) 0.0182(19) 0.054(2)
O13 0.0420(14) 0.0651(18) 0.0456(16) -0.0190(13) 0.0006(12) 0.0087(13)
O14 0.0396(14) 0.0636(17) 0.0409(15) -0.0154(13) 0.0041(12) 0.0060(12)
O15 0.0413(14) 0.0723(19) 0.0458(16) -0.0209(14) -0.0019(12) 0.0006(13)
O16 0.0402(14) 0.0680(18) 0.0510(17) -0.0253(14) 0.0005(13) 0.0002(13)
O17 0.032(2) 0.121(5) 0.142(5) 0.000 0.000 0.009(3)
O18 0.037(2) 0.053(3) 0.276(9) 0.000 0.000 0.010(2)
O19 0.0395(14) 0.0591(17) 0.0547(17) -0.0218(14) -0.0034(13) 0.0033(12)
O20 0.0417(14) 0.0562(16) 0.0616(18) -0.0250(14) 0.0035(13) -0.0001(12)
C1 0.0416(19) 0.048(2) 0.046(2) -0.0148(18) 0.0065(17) -0.0057(16)
C2 0.0432(19) 0.057(2) 0.053(2) -0.0213(19) 0.0043(18) -0.0055(17)
C3 0.042(2) 0.088(3) 0.067(3) -0.041(2) 0.006(2) -0.006(2)
C4 0.046(2) 0.103(3) 0.069(3) -0.056(2) 0.004(2) -0.007(2)
C5 0.041(2) 0.101(3) 0.068(3) -0.045(3) 0.004(2) -0.004(2)
C6 0.046(2) 0.061(2) 0.050(2) -0.0219(19) 0.0030(18) -0.0010(18)
C7 0.046(2) 0.046(2) 0.042(2) -0.0097(17) 0.0075(17) -0.0028(16)
C18 0.046(2) 0.113(3) 0.078(3) -0.048(3) 0.003(2) -0.003(2)
C19 0.043(2) 0.108(4) 0.075(3) -0.053(3) 0.000(2) 0.000(2)
C20 0.0415(19) 0.064(2) 0.055(2) -0.016(2) -0.0011(18) -0.0013(18)
C21 0.044(2) 0.058(2) 0.056(2) -0.022(2) -0.0007(18) -0.0032(18)
C22 0.045(2) 0.079(3) 0.061(3) -0.031(2) -0.0045(19) 0.001(2)
C23 0.045(2) 0.126(4) 0.071(3) -0.054(3) 0.005(2) -0.003(2)
C24 0.0412(19) 0.047(2) 0.055(2) -0.0121(18) -0.0037(18) 0.0045(16)
C25 0.0410(19) 0.055(2) 0.041(2) -0.0070(17) 0.0056(17) 0.0007(17)
C26 0.0384(18) 0.055(2) 0.049(2) -0.0108(18) 0.0093(17) -0.0015(17)
C27 0.041(2) 0.075(3) 0.062(3) -0.030(2) 0.0042(19) -0.0053(19)
C28 0.0375(19) 0.080(3) 0.064(3) -0.027(2) 0.0067(18) 0.0022(19)
C29 0.040(2) 0.078(3) 0.064(3) -0.024(2) 0.001(2) 0.004(2)
C30 0.0389(19) 0.059(2) 0.044(2) -0.0104(18) 0.0048(16) 0.0043(17)
C31 0.0376(18) 0.046(2) 0.049(2) -0.0061(18) 0.0036(17) -0.0021(16)
C33 0.0408(19) 0.057(2) 0.0328(19) -0.0043(17) -0.0011(16) 0.0074(17)
C34 0.046(2) 0.064(2) 0.038(2) -0.0108(18) 0.0018(17) -0.0001(18)
C35 0.0428(19) 0.047(2) 0.044(2) -0.0135(17) -0.0029(17) 0.0064(16)
_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 O8 1.954(3) 2_655 ?
Cu1 O19 1.961(3) 14_556 ?
Cu1 O5 1.963(3) . ?
Cu1 O9 1.971(3) 13_656 ?
Cu1 O11 2.140(3) . ?
Cu1 Cu2 2.6720(6) . ?
Cu2 O7 1.955(3) 2_655 ?
Cu2 O6 1.955(3) . ?
Cu2 O10 1.959(3) 13_656 ?
Cu2 O20 1.962(3) 14_556 ?
Cu2 O12 2.182(3) . ?
Cu3 O14 1.950(3) . ?
Cu3 O14 1.950(3) 11_556 ?
Cu3 O16 1.958(3) 9_656 ?
Cu3 O16 1.958(3) 3_655 ?
Cu3 O18 2.176(4) . ?
Cu3 Cu4 2.6716(9) . ?
Cu4 O13 1.955(3) . ?
Cu4 O13 1.955(3) 11_556 ?
Cu4 O15 1.965(3) 9_656 ?
Cu4 O15 1.965(3) 3_655 ?
Cu4 O17 2.137(4) . ?
O5 C1 1.247(4) . ?
O6 C1 1.249(4) . ?
O7 C35 1.241(4) . ?
O7 Cu2 1.955(3) 4_565 ?
O8 C35 1.272(4) . ?
O8 Cu1 1.954(3) 4_565 ?
O9 C31 1.246(5) . ?
O9 Cu1 1.971(3) 13_656 ?
O10 C31 1.260(4) . ?
O10 Cu2 1.959(3) 13_656 ?
O13 C33 1.263(4) . ?
O14 C33 1.260(4) . ?
O15 C34 1.250(5) . ?
O15 Cu4 1.965(3) 9_656 ?
O16 C34 1.243(5) . ?
O16 Cu3 1.958(3) 9_656 ?
O19 C24 1.263(5) . ?
O19 Cu1 1.961(3) 16_546 ?
O20 C24 1.256(5) . ?
O20 Cu2 1.962(3) 16_546 ?
C1 C2 1.511(5) . ?
C2 C7 1.378(5) . ?
C2 C3 1.390(6) . ?
C3 C4 1.381(6) . ?
C4 C5 1.399(6) . ?
C4 N6' 1.406(8) . ?
C4 N6 1.517(8) . ?
C5 C6 1.378(6) . ?
C6 C7 1.384(6) . ?
C6 C35 1.507(5) . ?
C10 C15 1.366(12) . ?
C10 C11 1.406(12) . ?
C10 C9 1.452(12) . ?
C11 C12 1.406(12) . ?
C12 C13 1.430(12) . ?
C12 C36 1.452(12) . ?
C13 C14 1.388(12) . ?
C14 C15 1.428(13) . ?
C14 C16 1.442(13) . ?
C10' C11' 1.381(12) . ?
C10' C15' 1.384(13) . ?
C10' C9' 1.464(13) . ?
C11' C12' 1.399(12) . ?
C12' C13' 1.412(13) . ?
C12' C36' 1.436(12) . ?
C13' C14' 1.354(13) . ?
C14' C15' 1.390(13) . ?
C14' C16' 1.427(13) . ?
C16 C17 1.340(12) . ?
C16 N7 1.367(13) . ?
C17 N9 1.357(11) . ?
N7 N8 1.339(12) . ?
N8 N9 1.348(11) . ?
N9 C18 1.511(8) . ?
C16' N7' 1.353(13) . ?
C16' C17' 1.393(12) . ?
C17' N9' 1.337(11) . ?
N7' N8' 1.362(12) . ?
N8' N9' 1.398(12) . ?
N9' C18 1.409(9) . ?
C8 C9 1.350(12) . ?
C8 N6 1.352(11) . ?
C9 N4 1.352(12) . ?
N4 N5 1.354(12) . ?
N5 N6 1.343(11) . ?
C8' N6' 1.367(11) . ?
C8' C9' 1.369(12) . ?
C9' N4' 1.366(12) . ?
N4' N5' 1.360(12) . ?
N5' N6' 1.343(11) . ?
C32 N1 1.352(10) . ?
C32 C36 1.385(11) . ?
C36 N3 1.349(11) . ?
N1 N2 1.349(9) . ?
N1 C28 1.453(7) . ?
N2 N3 1.301(9) . ?
C32' N1' 1.340(10) . ?
C32' C36' 1.401(12) . ?
C36' N3' 1.395(11) . ?
N1' N2' 1.367(10) . ?
N1' C28 1.419(8) . ?
N2' N3' 1.324(10) . ?
C18 C23 1.363(6) . ?
C18 C19 1.395(6) . ?
C19 C20 1.395(6) . ?
C20 C21 1.391(6) . ?
C20 C24 1.484(6) . ?
C21 C22 1.402(6) . ?
C22 C23 1.386(6) . ?
C22 C34 1.521(6) . ?
C25 C30 1.395(5) . ?
C25 C26 1.397(5) . ?
C26 C27 1.403(5) . ?
C26 C31 1.492(5) . ?
C27 C28 1.393(6) . ?
C28 C29 1.406(6) . ?
C29 C30 1.389(5) . ?
C30 C33 1.492(5) . ?
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
O8 Cu1 O19 167.42(11) 2_655 14_556 ?
O8 Cu1 O5 89.72(12) 2_655 . ?
O19 Cu1 O5 89.67(12) 14_556 . ?
O8 Cu1 O9 88.71(13) 2_655 13_656 ?
O19 Cu1 O9 89.15(12) 14_556 13_656 ?
O5 Cu1 O9 167.36(11) . 13_656 ?
O8 Cu1 O11 97.35(14) 2_655 . ?
O19 Cu1 O11 95.13(14) 14_556 . ?
O5 Cu1 O11 99.80(14) . . ?
O9 Cu1 O11 92.84(14) 13_656 . ?
O8 Cu1 Cu2 83.68(8) 2_655 . ?
O19 Cu1 Cu2 83.75(8) 14_556 . ?
O5 Cu1 Cu2 84.95(8) . . ?
O9 Cu1 Cu2 82.42(8) 13_656 . ?
O11 Cu1 Cu2 175.13(12) . . ?
O7 Cu2 O6 89.66(13) 2_655 . ?
O7 Cu2 O10 88.78(12) 2_655 13_656 ?
O6 Cu2 O10 166.57(11) . 13_656 ?
O7 Cu2 O20 167.04(11) 2_655 14_556 ?
O6 Cu2 O20 88.91(12) . 14_556 ?
O10 Cu2 O20 89.63(13) 13_656 14_556 ?
O7 Cu2 O12 101.07(13) 2_655 . ?
O6 Cu2 O12 93.95(13) . . ?
O10 Cu2 O12 99.44(13) 13_656 . ?
O20 Cu2 O12 91.88(13) 14_556 . ?
O7 Cu2 Cu1 83.53(8) 2_655 . ?
O6 Cu2 Cu1 81.90(8) . . ?
O10 Cu2 Cu1 84.67(8) 13_656 . ?
O20 Cu2 Cu1 83.51(8) 14_556 . ?
O12 Cu2 Cu1 173.83(12) . . ?
O14 Cu3 O14 89.33(17) . 11_556 ?
O14 Cu3 O16 167.12(11) . 9_656 ?
O14 Cu3 O16 88.98(12) 11_556 9_656 ?
O14 Cu3 O16 88.98(12) . 3_655 ?
O14 Cu3 O16 167.12(11) 11_556 3_655 ?
O16 Cu3 O16 89.82(18) 9_656 3_655 ?
O14 Cu3 O18 95.53(12) . . ?
O14 Cu3 O18 95.53(12) 11_556 . ?
O16 Cu3 O18 97.33(12) 9_656 . ?
O16 Cu3 O18 97.33(12) 3_655 . ?
O14 Cu3 Cu4 85.39(8) . . ?
O14 Cu3 Cu4 85.39(8) 11_556 . ?
O16 Cu3 Cu4 81.75(8) 9_656 . ?
O16 Cu3 Cu4 81.75(8) 3_655 . ?
O18 Cu3 Cu4 178.69(13) . . ?
O13 Cu4 O13 90.48(18) . 11_556 ?
O13 Cu4 O15 167.83(11) . 9_656 ?
O13 Cu4 O15 89.54(13) 11_556 9_656 ?
O13 Cu4 O15 89.54(13) . 3_655 ?
O13 Cu4 O15 167.83(11) 11_556 3_655 ?
O15 Cu4 O15 87.90(18) 9_656 3_655 ?
O13 Cu4 O17 95.46(14) . . ?
O13 Cu4 O17 95.46(14) 11_556 . ?
O15 Cu4 O17 96.66(14) 9_656 . ?
O15 Cu4 O17 96.66(14) 3_655 . ?
O13 Cu4 Cu3 82.19(8) . . ?
O13 Cu4 Cu3 82.19(8) 11_556 . ?
O15 Cu4 Cu3 85.75(8) 9_656 . ?
O15 Cu4 Cu3 85.75(8) 3_655 . ?
O17 Cu4 Cu3 176.64(17) . . ?
C1 O5 Cu1 120.9(2) . . ?
C1 O6 Cu2 124.7(3) . . ?
C35 O7 Cu2 123.2(2) . 4_565 ?
C35 O8 Cu1 122.2(2) . 4_565 ?
C31 O9 Cu1 124.1(2) . 13_656 ?
C31 O10 Cu2 121.5(3) . 13_656 ?
C33 O13 Cu4 124.8(2) . . ?
C33 O14 Cu3 121.3(2) . . ?
C34 O15 Cu4 119.3(3) . 9_656 ?
C34 O16 Cu3 124.6(3) . 9_656 ?
C24 O19 Cu1 122.8(2) . 16_546 ?
C24 O20 Cu2 123.1(2) . 16_546 ?
O5 C1 O6 126.8(4) . . ?
O5 C1 C2 117.4(3) . . ?
O6 C1 C2 115.8(3) . . ?
C7 C2 C3 120.2(4) . . ?
C7 C2 C1 119.5(3) . . ?
C3 C2 C1 120.3(4) . . ?
C4 C3 C2 118.7(4) . . ?
C3 C4 C5 121.3(4) . . ?
C3 C4 N6' 116.3(5) . . ?
C5 C4 N6' 120.7(5) . . ?
C3 C4 N6 121.3(5) . . ?
C5 C4 N6 115.1(5) . . ?
C6 C5 C4 119.1(4) . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 C35 120.2(4) . . ?
C7 C6 C35 120.0(3) . . ?
C2 C7 C6 120.8(4) . . ?
C15 C10 C11 120.9(9) . . ?
C15 C10 C9 120.3(8) . . ?
C11 C10 C9 118.6(8) . . ?
C10 C11 C12 119.2(8) . . ?
C11 C12 C13 119.8(8) . . ?
C11 C12 C36 121.4(8) . . ?
C13 C12 C36 118.7(8) . . ?
C14 C13 C12 120.2(8) . . ?
C13 C14 C15 118.8(8) . . ?
C13 C14 C16 121.5(8) . . ?
C15 C14 C16 119.6(8) . . ?
C10 C15 C14 121.1(9) . . ?
C11' C10' C15' 120.0(9) . . ?
C11' C10' C9' 119.5(8) . . ?
C15' C10' C9' 120.4(8) . . ?
C10' C11' C12' 119.2(9) . . ?
C11' C12' C13' 119.5(8) . . ?
C11' C12' C36' 120.0(8) . . ?
C13' C12' C36' 120.4(8) . . ?
C14' C13' C12' 120.9(9) . . ?
C13' C14' C15' 119.1(9) . . ?
C13' C14' C16' 120.4(9) . . ?
C15' C14' C16' 120.2(9) . . ?
C10' C15' C14' 121.4(9) . . ?
C17 C16 N7 106.1(8) . . ?
C17 C16 C14 130.7(9) . . ?
N7 C16 C14 122.9(9) . . ?
C16 C17 N9 108.5(8) . . ?
N8 N7 C16 110.2(9) . . ?
N7 N8 N9 106.3(8) . . ?
N8 N9 C17 108.9(7) . . ?
N8 N9 C18 121.9(7) . . ?
C17 N9 C18 128.5(7) . . ?
N7' C16' C17' 108.4(9) . . ?
N7' C16' C14' 121.5(9) . . ?
C17' C16' C14' 129.6(9) . . ?
N9' C17' C16' 107.2(8) . . ?
C16' N7' N8' 108.6(9) . . ?
N7' N8' N9' 106.8(9) . . ?
C17' N9' N8' 109.1(8) . . ?
C17' N9' C18 128.0(7) . . ?
N8' N9' C18 119.1(7) . . ?
C9 C8 N6 107.0(8) . . ?
C8 C9 N4 107.4(8) . . ?
C8 C9 C10 130.3(8) . . ?
N4 C9 C10 122.2(8) . . ?
C9 N4 N5 109.5(8) . . ?
N6 N5 N4 105.8(8) . . ?
N5 N6 C8 110.2(7) . . ?
N5 N6 C4 119.0(6) . . ?
C8 N6 C4 128.2(6) . . ?
N6' C8' C9' 104.1(8) . . ?
N4' C9' C8' 110.6(8) . . ?
N4' C9' C10' 120.5(8) . . ?
C8' C9' C10' 128.7(8) . . ?
N5' N4' C9' 106.5(8) . . ?
N6' N5' N4' 107.7(8) . . ?
N5' N6' C8' 111.0(7) . . ?
N5' N6' C4 121.2(7) . . ?
C8' N6' C4 126.6(7) . . ?
N1 C32 C36 104.7(7) . . ?
N3 C36 C32 107.7(7) . . ?
N3 C36 C12 123.5(8) . . ?
C32 C36 C12 128.7(8) . . ?
N2 N1 C32 110.2(6) . . ?
N2 N1 C28 124.0(6) . . ?
C32 N1 C28 124.0(6) . . ?
N3 N2 N1 107.5(6) . . ?
N2 N3 C36 109.9(7) . . ?
N1' C32' C36' 104.4(7) . . ?
N3' C36' C32' 107.4(8) . . ?
N3' C36' C12' 123.5(8) . . ?
C32' C36' C12' 129.0(8) . . ?
C32' N1' N2' 112.7(7) . . ?
C32' N1' C28 129.1(6) . . ?
N2' N1' C28 117.5(6) . . ?
N3' N2' N1' 106.2(7) . . ?
N2' N3' C36' 109.2(7) . . ?
C23 C18 C19 122.3(4) . . ?
C23 C18 N9' 118.7(5) . . ?
C19 C18 N9' 117.1(5) . . ?
C23 C18 N9 120.1(5) . . ?
C19 C18 N9 115.0(5) . . ?
C18 C19 C20 118.4(4) . . ?
C21 C20 C19 120.1(4) . . ?
C21 C20 C24 120.2(4) . . ?
C19 C20 C24 119.7(4) . . ?
C20 C21 C22 119.9(4) . . ?
C23 C22 C21 119.9(4) . . ?
C23 C22 C34 121.5(4) . . ?
C21 C22 C34 118.6(4) . . ?
C18 C23 C22 119.4(4) . . ?
O20 C24 O19 126.1(4) . . ?
O20 C24 C20 116.5(3) . . ?
O19 C24 C20 117.4(3) . . ?
C30 C25 C26 119.8(4) . . ?
C25 C26 C27 120.7(4) . . ?
C25 C26 C31 120.3(3) . . ?
C27 C26 C31 118.9(4) . . ?
C28 C27 C26 118.5(4) . . ?
C27 C28 C29 121.4(4) . . ?
C27 C28 N1' 116.3(4) . . ?
C29 C28 N1' 119.4(4) . . ?
C27 C28 N1 122.5(4) . . ?
C29 C28 N1 115.7(4) . . ?
C30 C29 C28 119.1(4) . . ?
C29 C30 C25 120.6(4) . . ?
C29 C30 C33 119.0(4) . . ?
C25 C30 C33 120.3(3) . . ?
O9 C31 O10 126.5(4) . . ?
O9 C31 C26 116.9(3) . . ?
O10 C31 C26 116.5(3) . . ?
O14 C33 O13 126.2(4) . . ?
O14 C33 C30 117.0(3) . . ?
O13 C33 C30 116.8(3) . . ?
O16 C34 O15 128.5(4) . . ?
O16 C34 C22 116.2(4) . . ?
O15 C34 C22 115.3(4) . . ?
O7 C35 O8 126.7(3) . . ?
O7 C35 C6 116.9(3) . . ?
O8 C35 C6 116.5(3) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.07
#=== END of CIF