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

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#
#                 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.
#
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#  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
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_0102

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H12 Cu3 N4 O19, 2(C4 H9 N O)'
_chemical_formula_sum            'C36 H30 Cu3 N6 O21'
_chemical_formula_weight         1073.28

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'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.418(2)
_cell_length_b                   34.135(5)
_cell_length_c                   10.1886(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.446(2)
_cell_angle_gamma                90.00
_cell_volume                     5168.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7403
_cell_measurement_theta_min      1.26
_cell_measurement_theta_max      27.04

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Blue'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2172
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8392
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35683
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8979
_reflns_number_gt                6331
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0899P)²+27.8849P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8979
_refine_ls_number_parameters     721
_refine_ls_number_restraints     229
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0836
_refine_ls_wR_factor_ref         0.2206
_refine_ls_wR_factor_gt          0.2082
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.081
_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 1.08564(5) 0.78123(2) 1.31863(8) 0.0236(2) Uani 1 1 d . . .
Cu2 Cu 0.93890(5) 0.72370(2) 1.33662(8) 0.0241(2) Uani 1 1 d . . .
Cu3 Cu 1.01653(5) 0.77986(2) 1.58449(8) 0.0248(2) Uani 1 1 d . . .
O1W O 1.0083(3) 0.69852(15) 1.5656(5) 0.0395(12) Uani 1 1 d . . .
H1WA H 1.0334 0.6816 1.5267 0.059 Uiso 1 1 d R . .
H1WB H 0.9710 0.6823 1.5831 0.059 Uiso 1 1 d R . .
O1 O 1.0497(3) 0.77368(12) 1.7776(4) 0.0216(9) Uani 1 1 d . . .
H1A H 1.0894 0.7901 1.8176 0.032 Uiso 1 1 d R . .
O2 O 0.9771(4) 0.66470(13) 1.1052(5) 0.0397(13) Uani 1 1 d . . .
O3 O 0.9138(3) 0.66874(13) 1.2785(5) 0.0331(11) Uani 1 1 d . . .
O4 O 0.1388(3) 0.76263(13) 1.5674(5) 0.0295(11) Uani 1 1 d . . .
O5 O 0.1894(3) 0.72334(13) 1.7483(5) 0.0311(11) Uani 1 1 d . . .
O6 O 0.9779(3) 0.77855(11) 1.3885(4) 0.0224(9) Uani 1 1 d . . .
H6A H 0.9383 0.7957 1.3543 0.034 Uiso 1 1 d R . .
O7 O 0.4419(13) 0.6380(6) 1.697(2) 0.105(6) Uani 0.50 1 d PU . .
O7A O 0.4664(15) 0.6548(7) 1.801(3) 0.125(7) Uani 0.50 1 d PU . .
O8 O 0.5643(11) 0.6832(5) 1.7804(18) 0.084(5) Uani 0.50 1 d PU . .
O8A O 0.5502(12) 0.6626(5) 1.706(2) 0.091(5) Uani 0.50 1 d PU . .
O9 O 0.4491(11) 0.6818(5) 1.3632(17) 0.082(4) Uani 0.50 1 d PU . .
O9A O 0.4768(14) 0.6584(6) 1.459(2) 0.115(6) Uani 0.50 1 d PU . .
O10 O 0.5700(14) 0.6431(6) 1.395(2) 0.108(6) Uani 0.50 1 d PU . .
O10A O 0.5467(12) 0.6611(5) 1.3068(19) 0.091(5) Uani 0.50 1 d PU . .
O11 O 0.7873(16) 0.4970(6) 1.310(2) 0.113(6) Uani 0.50 1 d PU . .
O11A O 0.846(2) 0.4974(8) 1.385(3) 0.142(9) Uani 0.50 1 d PU . .
O12 O 0.731(2) 0.5507(10) 1.310(3) 0.187(11) Uani 0.50 1 d PU . .
O12A O 0.924(2) 0.5379(10) 1.510(3) 0.199(12) Uani 0.50 1 d PDU . .
O13A O 0.692(3) 0.4760(11) 0.843(4) 0.234(16) Uani 0.50 1 d PDU . .
O13 O 1.102(3) 0.4422(10) 1.247(5) 0.27(2) Uani 0.50 1 d PDU . .
O14 O 1.076(2) 0.5012(9) 1.257(4) 0.218(14) Uani 0.50 1 d PDU . .
O14A O 0.728(3) 0.5192(13) 0.986(5) 0.28(2) Uani 0.50 1 d PDU . .
O15 O 0.8308(3) 0.72585(14) 1.3971(5) 0.0318(11) Uani 1 1 d . . .
O16 O 0.8812(3) 0.75969(13) 1.5911(5) 0.0293(11) Uani 1 1 d . . .
O17 O 0.7720(7) 0.3471(3) 1.0371(11) 0.121(3) Uani 1 1 d U . .
O18 O 0.9078(4) 0.33674(14) 1.1628(6) 0.0454(14) Uani 1 1 d . . .
O19 O 1.1378(4) 0.83083(17) 1.9404(6) 0.0564(16) Uani 1 1 d U . .
O20 O 0.8772(5) 0.82870(19) 1.2046(7) 0.0693(19) Uani 1 1 d . . .
C1 C 0.9396(5) 0.65066(19) 1.1871(7) 0.0302(15) Uani 1 1 d . . .
C2 C 0.9253(6) 0.6073(2) 1.1783(8) 0.0388(18) Uani 1 1 d . . .
C3A C 0.9248(15) 0.5879(4) 1.0592(16) 0.042(4) Uani 0.50 1 d P . .
C3 C 0.9793(17) 0.5845(7) 1.121(3) 0.065(6) Uani 0.50 1 d PU . .
C4A C 0.9151(16) 0.5476(4) 1.0483(18) 0.048(5) Uani 0.50 1 d P . .
C4 C 0.9681(18) 0.5446(7) 1.117(3) 0.074(7) Uani 0.50 1 d PU . .
C5 C 0.9005(7) 0.5260(2) 1.1575(10) 0.058(3) Uani 1 1 d . . .
C6 C 0.8556(15) 0.5483(4) 1.232(2) 0.045(4) Uani 0.50 1 d P . .
C6A C 0.9072(16) 0.5452(6) 1.278(2) 0.053(5) Uani 0.50 1 d PDU . .
C7 C 0.8610(17) 0.5898(7) 1.231(3) 0.057(6) Uani 0.50 1 d P . .
C7A C 0.9109(18) 0.5866(6) 1.283(2) 0.050(6) Uani 0.50 1 d P . .
C8 C 0.8886(8) 0.4828(2) 1.1431(11) 0.060(3) Uani 1 1 d . . .
C9 C 0.9500(8) 0.4573(3) 1.2058(13) 0.083(4) Uani 1 1 d D . .
C10 C 0.9392(7) 0.4168(3) 1.1891(12) 0.070(3) Uani 1 1 d . . .
H10A H 0.9854 0.4001 1.2330 0.083 Uiso 1 1 calc R . .
C11 C 0.8628(7) 0.4022(2) 1.1102(10) 0.059(2) Uani 1 1 d U . .
C12 C 0.7973(9) 0.4268(4) 1.0394(14) 0.094(4) Uani 1 1 d U . .
H12A H 0.7446 0.4170 0.9816 0.113 Uiso 1 1 calc R . .
C13 C 0.8111(10) 0.4673(3) 1.0554(17) 0.108(5) Uani 1 1 d D . .
C14 C 0.8467(8) 0.3577(3) 1.1011(11) 0.071(3) Uani 1 1 d . . .
C15 C 0.1973(4) 0.74200(19) 1.6462(7) 0.0257(14) Uani 1 1 d . . .
C16 C 0.2887(5) 0.7386(2) 1.6189(7) 0.0316(16) Uani 1 1 d . . .
C17 C 0.3437(5) 0.7079(2) 1.6727(9) 0.046(2) Uani 1 1 d . . .
H17A H 0.3230 0.6887 1.7214 0.055 Uiso 1 1 calc R . .
C18 C 0.4283(6) 0.7051(3) 1.6562(9) 0.056(2) Uani 1 1 d . . .
C19 C 0.4617(5) 0.7335(3) 1.5800(8) 0.045(2) Uani 1 1 d . . .
C20 C 0.4050(5) 0.7639(3) 1.5281(9) 0.048(2) Uani 1 1 d . . .
H20A H 0.4248 0.7831 1.4784 0.058 Uiso 1 1 calc R . .
C21 C 0.3191(5) 0.7673(2) 1.5462(8) 0.0378(17) Uani 1 1 d . . .
H21A H 0.2827 0.7885 1.5102 0.045 Uiso 1 1 calc R . .
C22 C 0.5547(5) 0.7332(3) 1.5593(8) 0.047(2) Uani 1 1 d . . .
C23 C 0.6132(6) 0.7633(3) 1.6185(9) 0.053(2) Uani 1 1 d . . .
H23A H 0.5936 0.7822 1.6700 0.063 Uiso 1 1 calc R . .
C24 C 0.6984(5) 0.7660(2) 1.6033(8) 0.0401(18) Uani 1 1 d . . .
H24A H 0.7362 0.7861 1.6458 0.048 Uiso 1 1 calc R . .
C25 C 0.7290(4) 0.7387(2) 1.5243(7) 0.0318(16) Uani 1 1 d . . .
C26 C 0.6716(5) 0.7093(2) 1.4621(9) 0.0439(19) Uani 1 1 d . . .
H26A H 0.6903 0.6910 1.4076 0.053 Uiso 1 1 calc R . .
C27 C 0.5873(6) 0.7069(3) 1.4804(9) 0.049(2) Uani 1 1 d . . .
C28 C 0.8220(4) 0.74153(19) 1.5057(7) 0.0266(15) Uani 1 1 d . . .
C29 C 0.8222(10) 0.8550(4) 1.1656(14) 0.110(5) Uani 1 1 d DU . .
C30 C 0.8136(11) 0.8794(5) 1.0372(16) 0.126(6) Uani 1 1 d D . .
H30A H 0.8561 0.8702 0.9904 0.189 Uiso 1 1 calc R . .
H30B H 0.8255 0.9064 1.0617 0.189 Uiso 1 1 calc R . .
H30C H 0.7537 0.8769 0.9787 0.189 Uiso 1 1 calc R . .
C31 C 0.7040(11) 0.8980(5) 1.2070(19) 0.141(6) Uani 1 1 d DU . .
H31A H 0.7125 0.9086 1.1241 0.211 Uiso 1 1 calc R . .
H31B H 0.7176 0.9177 1.2767 0.211 Uiso 1 1 calc R . .
H31C H 0.6427 0.8897 1.1924 0.211 Uiso 1 1 calc R . .
C32 C 0.7709(9) 0.8374(5) 1.3571(14) 0.110(5) Uani 1 1 d D . .
H32A H 0.7308 0.8450 1.4103 0.166 Uiso 1 1 calc R . .
H32B H 0.8316 0.8372 1.4138 0.166 Uiso 1 1 calc R . .
H32C H 0.7552 0.8117 1.3202 0.166 Uiso 1 1 calc R . .
C33 C 1.1935(10) 0.8536(4) 1.9023(15) 0.111(5) Uani 1 1 d D . .
C34 C 1.2352(11) 0.8408(5) 1.7882(17) 0.125(5) Uani 1 1 d DU . .
H34A H 1.2164 0.8146 1.7606 0.187 Uiso 1 1 calc R . .
H34B H 1.2996 0.8417 1.8208 0.187 Uiso 1 1 calc R . .
H34C H 1.2157 0.8582 1.7120 0.187 Uiso 1 1 calc R . .
C35 C 1.2789(18) 0.9119(8) 1.907(3) 0.247(13) Uani 1 1 d DU . .
H35A H 1.2888 0.9379 1.9438 0.371 Uiso 1 1 calc R . .
H35B H 1.2607 0.9133 1.8092 0.371 Uiso 1 1 calc R . .
H35C H 1.3335 0.8971 1.9358 0.371 Uiso 1 1 calc R . .
C36 C 1.1570(14) 0.8964(6) 2.057(2) 0.171(8) Uani 1 1 d DU . .
H36A H 1.1214 0.8733 2.0559 0.257 Uiso 1 1 calc R . .
H36B H 1.1181 0.9189 2.0358 0.257 Uiso 1 1 calc R . .
H36C H 1.1979 0.8997 2.1453 0.257 Uiso 1 1 calc R . .
N1 N 0.7884(18) 0.5312(8) 1.291(3) 0.106(7) Uani 0.50 1 d PU . .
N1A N 0.877(2) 0.5287(9) 1.394(3) 0.139(10) Uani 0.50 1 d PDU . .
N2 N 0.4850(7) 0.6739(3) 1.7221(12) 0.087(3) Uani 1 1 d U . .
N3 N 0.5293(6) 0.6762(3) 1.4070(11) 0.078(3) Uani 1 1 d U . .
N4 N 1.0472(14) 0.4675(11) 1.263(4) 0.174(13) Uani 0.50 1 d PDU . .
N4A N 0.743(2) 0.4865(12) 0.950(3) 0.187(14) Uani 0.50 1 d PDU . .
N5 N 1.2074(16) 0.8927(5) 1.956(2) 0.239(10) Uani 1 1 d DU . .
N6 N 0.7638(10) 0.8645(4) 1.2496(15) 0.142(5) Uani 1 1 d DU . .


_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 O18 1.905(5) 2_757 ?
Cu1 O5 1.925(4) 4_675 ?
Cu1 O1 1.968(4) 4_575 ?
Cu1 O6 1.976(4) . ?
Cu1 Cu2 3.0379(11) . ?
Cu2 O15 1.925(4) . ?
Cu2 O1 1.958(4) 4_575 ?
Cu2 O3 1.974(4) . ?
Cu2 O6 1.994(4) . ?
Cu3 O1 1.908(4) . ?
Cu3 O6 1.926(4) . ?
Cu3 O2 2.016(5) 4_576 ?
Cu3 O4 2.026(4) 1_655 ?
Cu3 O16 2.215(4) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?
O1 Cu2 1.958(4) 4_576 ?
O1 Cu1 1.968(4) 4_576 ?
O1 H1A 0.8498 . ?
O2 C1 1.231(8) . ?
O2 Cu3 2.016(5) 4_575 ?
O3 C1 1.267(8) . ?
O4 C15 1.252(8) . ?
O4 Cu3 2.026(4) 1_455 ?
O5 C15 1.253(8) . ?
O5 Cu1 1.925(4) 4_476 ?
O6 H6A 0.8500 . ?
O7 O7A 1.18(3) . ?
O7 N2 1.38(2) . ?
O7A N2 1.13(2) . ?
O8 O8A 1.02(2) . ?
O8 N2 1.250(18) . ?
O8A N2 1.128(18) . ?
O9 N3 1.213(17) . ?
O9 O9A 1.25(2) . ?
O9A N3 1.24(2) . ?
O9A O10 1.81(3) . ?
O10 O10A 1.07(2) . ?
O10 N3 1.31(2) . ?
O10A N3 1.235(18) . ?
O11 O11A 1.01(3) . ?
O11 N1 1.19(3) . ?
O11 N1A 1.78(4) . ?
O11A N1A 1.16(3) . ?
O11A N1 1.61(4) . ?
O12 N1 1.16(3) . ?
O12A N1A 1.254(19) . ?
O13A N4A 1.222(19) . ?
O13 N4 1.245(19) . ?
O14 N4 1.240(18) . ?
O14A N4A 1.21(2) . ?
O15 C28 1.269(8) . ?
O16 C28 1.246(8) . ?
O17 C14 1.218(13) . ?
O18 C14 1.216(12) . ?
O18 Cu1 1.905(5) 2_747 ?
O19 C33 1.293(16) . ?
O20 C29 1.227(15) . ?
C1 C2 1.497(9) . ?
C2 C7A 1.34(2) . ?
C2 C3 1.38(2) . ?
C2 C3A 1.380(15) . ?
C2 C7 1.38(3) . ?
C3A C3 0.91(2) . ?
C3A C4A 1.38(2) . ?
C3A C4 1.66(3) . ?
C3 C4 1.37(3) . ?
C3 C4A 1.65(3) . ?
C4A C4 0.93(3) . ?
C4A C5 1.402(17) . ?
C4 C5 1.37(3) . ?
C5 C6A 1.37(2) . ?
C5 C6 1.39(2) . ?
C5 C8 1.489(11) . ?
C6 C6A 0.81(2) . ?
C6 C7 1.42(3) . ?
C6 N1 1.45(3) . ?
C6 C7A 1.57(3) . ?
C6 N1A 1.72(3) . ?
C6A C7A 1.41(3) . ?
C6A N1A 1.492(18) . ?
C6A C7 1.69(3) . ?
C6A N1 1.93(3) . ?
C7 C7A 0.82(3) . ?
C8 C9 1.318(15) . ?
C8 C13 1.393(17) . ?
C9 C10 1.397(14) . ?
C9 N4 1.496(18) . ?
C10 C11 1.334(14) . ?
C10 H10A 0.9300 . ?
C11 C12 1.364(15) . ?
C11 C14 1.536(12) . ?
C12 C13 1.399(16) . ?
C12 H12A 0.9300 . ?
C13 N4A 1.443(19) . ?
C15 C16 1.511(9) . ?
C16 C17 1.367(10) . ?
C16 C21 1.383(10) . ?
C17 C18 1.364(11) . ?
C17 H17A 0.9300 . ?
C18 C19 1.421(12) . ?
C18 N2 1.427(13) . ?
C19 C20 1.370(12) . ?
C19 C22 1.504(10) . ?
C20 C21 1.390(10) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C27 1.385(12) . ?
C22 C23 1.394(13) . ?
C23 C24 1.367(10) . ?
C23 H23A 0.9300 . ?
C24 C25 1.392(10) . ?
C24 H24A 0.9300 . ?
C25 C26 1.377(11) . ?
C25 C28 1.498(9) . ?
C26 C27 1.364(10) . ?
C26 H26A 0.9300 . ?
C27 N3 1.451(12) . ?
C29 N6 1.434(6) . ?
C29 C30 1.526(14) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N6 1.460(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 N6 1.414(14) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N5 1.436(6) . ?
C33 C34 1.534(15) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N5 1.480(17) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N5 1.449(6) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N1 N1A 1.49(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Cu1 O5 95.1(2) 2_757 4_675 ?
O18 Cu1 O1 166.8(2) 2_757 4_575 ?
O5 Cu1 O1 93.36(18) 4_675 4_575 ?
O18 Cu1 O6 92.2(2) 2_757 . ?
O5 Cu1 O6 172.67(18) 4_675 . ?
O1 Cu1 O6 79.42(17) 4_575 . ?
O18 Cu1 Cu2 131.16(16) 2_757 . ?
O5 Cu1 Cu2 132.54(14) 4_675 . ?
O1 Cu1 Cu2 39.19(12) 4_575 . ?
O6 Cu1 Cu2 40.30(12) . . ?
O15 Cu2 O1 175.15(18) . 4_575 ?
O15 Cu2 O3 90.85(19) . . ?
O1 Cu2 O3 93.94(18) 4_575 . ?
O15 Cu2 O6 96.03(18) . . ?
O1 Cu2 O6 79.19(17) 4_575 . ?
O3 Cu2 O6 173.11(18) . . ?
O15 Cu2 Cu1 135.76(14) . . ?
O1 Cu2 Cu1 39.42(12) 4_575 . ?
O3 Cu2 Cu1 133.30(13) . . ?
O6 Cu2 Cu1 39.85(11) . . ?
O1 Cu3 O6 171.99(17) . . ?
O1 Cu3 O2 90.08(19) . 4_576 ?
O6 Cu3 O2 96.42(19) . 4_576 ?
O1 Cu3 O4 93.24(18) . 1_655 ?
O6 Cu3 O4 86.67(18) . 1_655 ?
O2 Cu3 O4 126.5(2) 4_576 1_655 ?
O1 Cu3 O16 86.01(18) . . ?
O6 Cu3 O16 89.46(17) . . ?
O2 Cu3 O16 88.61(19) 4_576 . ?
O4 Cu3 O16 144.86(18) 1_655 . ?
H1WA O1W H1WB 94.3 . . ?
Cu3 O1 Cu2 107.2(2) . 4_576 ?
Cu3 O1 Cu1 107.91(19) . 4_576 ?
Cu2 O1 Cu1 101.39(18) 4_576 4_576 ?
Cu3 O1 H1A 112.5 . . ?
Cu2 O1 H1A 113.5 4_576 . ?
Cu1 O1 H1A 113.6 4_576 . ?
C1 O2 Cu3 130.2(4) . 4_575 ?
C1 O3 Cu2 127.5(4) . . ?
C15 O4 Cu3 129.5(4) . 1_455 ?
C15 O5 Cu1 128.6(4) . 4_476 ?
Cu3 O6 Cu1 108.4(2) . . ?
Cu3 O6 Cu2 106.54(19) . . ?
Cu1 O6 Cu2 99.85(18) . . ?
Cu3 O6 H6A 113.5 . . ?
Cu1 O6 H6A 113.7 . . ?
Cu2 O6 H6A 113.8 . . ?
O7A O7 N2 51.7(14) . . ?
N2 O7A O7 73.7(19) . . ?
O8A O8 N2 58.6(14) . . ?
O8 O8A N2 71.2(16) . . ?
N3 O9 O9A 60.5(13) . . ?
N3 O9A O9 58.3(13) . . ?
N3 O9A O10 46.6(11) . . ?
O9 O9A O10 92.2(16) . . ?
O10A O10 N3 61.6(15) . . ?
O10A O10 O9A 91.1(19) . . ?
N3 O10 O9A 43.3(10) . . ?
O10 O10A N3 69.1(16) . . ?
O11A O11 N1 93(3) . . ?
O11A O11 N1A 38(2) . . ?
N1 O11 N1A 55.7(18) . . ?
O11 O11A N1A 110(3) . . ?
O11 O11A N1 47.4(19) . . ?
N1A O11A N1 62(2) . . ?
C28 O15 Cu2 126.7(4) . . ?
C28 O16 Cu3 130.9(4) . . ?
C14 O18 Cu1 130.6(6) . 2_747 ?
O2 C1 O3 127.2(6) . . ?
O2 C1 C2 115.6(6) . . ?
O3 C1 C2 117.1(6) . . ?
C7A C2 C3 106.6(15) . . ?
C7A C2 C3A 118.8(12) . . ?
C3 C2 C3A 38.6(10) . . ?
C7A C2 C7 34.9(11) . . ?
C3 C2 C7 119.8(15) . . ?
C3A C2 C7 107.3(14) . . ?
C7A C2 C1 121.7(11) . . ?
C3 C2 C1 119.2(11) . . ?
C3A C2 C1 119.5(8) . . ?
C7 C2 C1 120.9(12) . . ?
C3 C3A C2 70.6(18) . . ?
C3 C3A C4A 89(2) . . ?
C2 C3A C4A 121.4(13) . . ?
C3 C3A C4 55.4(19) . . ?
C2 C3A C4 101.9(14) . . ?
C4A C3A C4 33.9(11) . . ?
C3A C3 C4 91(2) . . ?
C3A C3 C2 70.8(18) . . ?
C4 C3 C2 119(2) . . ?
C3A C3 C4A 57.2(18) . . ?
C4 C3 C4A 34.3(12) . . ?
C2 C3 C4A 105.3(16) . . ?
C4 C4A C3A 90(2) . . ?
C4 C4A C5 69(2) . . ?
C3A C4A C5 119.7(12) . . ?
C4 C4A C3 56(2) . . ?
C3A C4A C3 33.6(10) . . ?
C5 C4A C3 104.5(14) . . ?
C4A C4 C3 89(2) . . ?
C4A C4 C5 72(2) . . ?
C3 C4 C5 123(2) . . ?
C4A C4 C3A 56.4(18) . . ?
C3 C4 C3A 33.3(11) . . ?
C5 C4 C3A 104.6(17) . . ?
C6A C5 C4 99.5(15) . . ?
C6A C5 C6 34.4(10) . . ?
C4 C5 C6 116.2(13) . . ?
C6A C5 C4A 118.0(12) . . ?
C4 C5 C4A 39.1(11) . . ?
C6 C5 C4A 110.9(11) . . ?
C6A C5 C8 122.7(11) . . ?
C4 C5 C8 120.8(13) . . ?
C6 C5 C8 122.1(10) . . ?
C4A C5 C8 119.0(9) . . ?
C6A C6 C5 72(2) . . ?
C6A C6 C7 95(2) . . ?
C5 C6 C7 120.2(16) . . ?
C6A C6 N1 114(3) . . ?
C5 C6 N1 121.4(16) . . ?
C7 C6 N1 117(2) . . ?
C6A C6 C7A 64(2) . . ?
C5 C6 C7A 109.2(16) . . ?
C7 C6 C7A 31.2(10) . . ?
N1 C6 C7A 125.9(18) . . ?
C6A C6 N1A 60(2) . . ?
C5 C6 N1A 108.4(16) . . ?
C7 C6 N1A 113.6(19) . . ?
N1 C6 N1A 55.0(15) . . ?
C7A C6 N1A 93.5(17) . . ?
C6 C6A C5 74(2) . . ?
C6 C6A C7A 85(2) . . ?
C5 C6A C7A 120.1(16) . . ?
C6 C6A N1A 92(3) . . ?
C5 C6A N1A 124(2) . . ?
C7A C6A N1A 111(2) . . ?
C6 C6A C7 57(2) . . ?
C5 C6A C7 104.5(16) . . ?
C7A C6A C7 28.7(11) . . ?
N1A C6A C7 111(2) . . ?
C6 C6A N1 43.1(19) . . ?
C5 C6A N1 95.5(15) . . ?
C7A C6A N1 106.0(19) . . ?
N1A C6A N1 49.4(15) . . ?
C7 C6A N1 84.6(15) . . ?
C7A C7 C2 70(3) . . ?
C7A C7 C6 85(3) . . ?
C2 C7 C6 119.1(19) . . ?
C7A C7 C6A 56(3) . . ?
C2 C7 C6A 101.9(17) . . ?
C6 C7 C6A 28.6(10) . . ?
C7 C7A C2 75(3) . . ?
C7 C7A C6A 95(3) . . ?
C2 C7A C6A 120.7(18) . . ?
C7 C7A C6 64(3) . . ?
C2 C7A C6 111.6(16) . . ?
C6A C7A C6 31.1(10) . . ?
C9 C8 C13 116.3(9) . . ?
C9 C8 C5 123.5(11) . . ?
C13 C8 C5 120.2(9) . . ?
C8 C9 C10 123.2(11) . . ?
C8 C9 N4 123.4(18) . . ?
C10 C9 N4 110.5(18) . . ?
C11 C10 C9 120.1(10) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 119.8(9) . . ?
C10 C11 C14 120.6(8) . . ?
C12 C11 C14 119.5(10) . . ?
C11 C12 C13 118.6(12) . . ?
C11 C12 H12A 120.7 . . ?
C13 C12 H12A 120.7 . . ?
C8 C13 C12 121.9(11) . . ?
C8 C13 N4A 129.4(19) . . ?
C12 C13 N4A 108(2) . . ?
O18 C14 O17 126.4(9) . . ?
O18 C14 C11 117.4(9) . . ?
O17 C14 C11 116.1(10) . . ?
O4 C15 O5 127.3(6) . . ?
O4 C15 C16 118.2(6) . . ?
O5 C15 C16 114.5(6) . . ?
C17 C16 C21 119.7(7) . . ?
C17 C16 C15 119.6(6) . . ?
C21 C16 C15 120.7(6) . . ?
C18 C17 C16 121.1(7) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 121.1(7) . . ?
C17 C18 N2 118.8(8) . . ?
C19 C18 N2 120.0(8) . . ?
C20 C19 C18 116.1(7) . . ?
C20 C19 C22 119.0(7) . . ?
C18 C19 C22 124.8(7) . . ?
C19 C20 C21 123.1(7) . . ?
C19 C20 H20A 118.5 . . ?
C21 C20 H20A 118.5 . . ?
C16 C21 C20 118.9(7) . . ?
C16 C21 H21A 120.6 . . ?
C20 C21 H21A 120.6 . . ?
C27 C22 C23 115.9(7) . . ?
C27 C22 C19 126.3(8) . . ?
C23 C22 C19 117.8(7) . . ?
C24 C23 C22 122.1(8) . . ?
C24 C23 H23A 119.0 . . ?
C22 C23 H23A 119.0 . . ?
C23 C24 C25 120.3(8) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
C26 C25 C24 118.7(6) . . ?
C26 C25 C28 120.5(6) . . ?
C24 C25 C28 120.9(6) . . ?
C27 C26 C25 119.9(7) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C22 123.2(8) . . ?
C26 C27 N3 116.8(8) . . ?
C22 C27 N3 120.0(8) . . ?
O16 C28 O15 126.1(6) . . ?
O16 C28 C25 119.5(6) . . ?
O15 C28 C25 114.3(6) . . ?
O20 C29 N6 117.4(12) . . ?
O20 C29 C30 124.9(13) . . ?
N6 C29 C30 117.7(13) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N6 C31 H31A 109.5 . . ?
N6 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N6 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N6 C32 H32A 109.5 . . ?
N6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O19 C33 N5 119.2(15) . . ?
O19 C33 C34 120.1(12) . . ?
N5 C33 C34 120.2(15) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 H35A 109.5 . . ?
N5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N5 C36 H36A 109.5 . . ?
N5 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N5 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O12 N1 O11 119(3) . . ?
O12 N1 C6 120(3) . . ?
O11 N1 C6 121(3) . . ?
O12 N1 N1A 121(3) . . ?
O11 N1 N1A 83(2) . . ?
C6 N1 N1A 72.0(17) . . ?
O12 N1 O11A 129(3) . . ?
O11 N1 O11A 39.1(16) . . ?
C6 N1 O11A 101(2) . . ?
N1A N1 O11A 44.0(14) . . ?
O12 N1 C6A 130(3) . . ?
O11 N1 C6A 108(2) . . ?
C6 N1 C6A 22.6(10) . . ?
N1A N1 C6A 49.7(11) . . ?
O11A N1 C6A 80.6(17) . . ?
O11A N1A O12A 115(3) . . ?
O11A N1A N1 74(3) . . ?
O12A N1A N1 148(3) . . ?
O11A N1A C6A 119(3) . . ?
O12A N1A C6A 116(3) . . ?
N1 N1A C6A 80.8(19) . . ?
O11A N1A C6 108(3) . . ?
O12A N1A C6 136(3) . . ?
N1 N1A C6 53.0(15) . . ?
C6A N1A C6 28.1(10) . . ?
O11A N1A O11 32.4(18) . . ?
O12A N1A O11 141(3) . . ?
N1 N1A O11 41.3(13) . . ?
C6A N1A O11 103(2) . . ?
C6 N1A O11 81.6(16) . . ?
O8A N2 O7A 108.2(17) . . ?
O8A N2 O8 50.2(11) . . ?
O7A N2 O8 102.1(18) . . ?
O8A N2 O7 94.2(15) . . ?
O7A N2 O7 54.6(14) . . ?
O8 N2 O7 132.4(14) . . ?
O8A N2 C18 130.1(13) . . ?
O7A N2 C18 121.7(15) . . ?
O8 N2 C18 115.6(12) . . ?
O7 N2 C18 111.7(12) . . ?
O9 N3 O10A 100.8(14) . . ?
O9 N3 O9A 61.2(12) . . ?
O10A N3 O9A 117.4(15) . . ?
O9 N3 O10 124.6(14) . . ?
O10A N3 O10 49.3(11) . . ?
O9A N3 O10 90.1(15) . . ?
O9 N3 C27 120.1(12) . . ?
O10A N3 C27 119.2(11) . . ?
O9A N3 C27 121.1(13) . . ?
O10 N3 C27 115.2(12) . . ?
O14 N4 O13 112(2) . . ?
O14 N4 C9 122(3) . . ?
O13 N4 C9 116(3) . . ?
O14A N4A O13A 114(4) . . ?
O14A N4A C13 111(4) . . ?
O13A N4A C13 135(4) . . ?
C33 N5 C36 107.4(17) . . ?
C33 N5 C35 109.4(19) . . ?
C36 N5 C35 142.0(19) . . ?
C32 N6 C29 112.6(12) . . ?
C32 N6 C31 130.8(14) . . ?
C29 N6 C31 116.5(13) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.127
_database_code_depnum_ccdc_archive 'CCDC 977429'
#######################################################################
#
#                 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_0421

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C3 H6 O)'
_chemical_formula_sum            'C34 H26 Cu3 N4 O20'
_chemical_formula_weight         1001.21

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 '
_symmetry_space_group_name_Hall  '-P 2ybc    '

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

_cell_length_a                   15.331(9)
_cell_length_b                   32.500(19)
_cell_length_c                   10.050(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.451(8)
_cell_angle_gamma                90.00
_cell_volume                     4777(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5744
_cell_measurement_theta_min      1.26
_cell_measurement_theta_max      26.86

_exptl_crystal_description       Block
_exptl_crystal_colour            Light
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_T_max  0.8965
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'

_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  'Bruker Apex 2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33589
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8399
_reflns_number_gt                6002
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0839P)²+8.2636P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8399
_refine_ls_number_parameters     586
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1771
_refine_ls_wR_factor_gt          0.1639
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001

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
Cu3 Cu 0.41706(3) 0.716177(14) 0.73480(4) 0.02222(12) Uani 1 1 d . . .
Cu2 Cu 0.48896(3) 0.714368(14) 0.47274(5) 0.02311(12) Uani 1 1 d . . .
Cu1 Cu 0.34304(3) 0.773262(14) 0.49804(5) 0.02110(11) Uani 1 1 d . . .
O1 O 0.37873(16) 0.71549(7) 0.5310(2) 0.0202(6) Uani 1 1 d . . .
H1A H 0.3316 0.6953 0.4864 0.024 Uiso 1 1 calc R . .
O2 O 0.4682(2) 0.65718(9) 0.7356(3) 0.0373(8) Uani 1 1 d . . .
O3 O 0.53138(19) 0.66040(8) 0.5590(3) 0.0315(7) Uani 1 1 d . . .
O4 O 0.28992(18) 0.72606(9) 0.7447(3) 0.0294(7) Uani 1 1 d . . .
O5 O 0.23321(17) 0.76516(9) 0.5526(3) 0.0300(7) Uani 1 1 d . . .
O6 O 0.45313(16) 0.72600(7) 0.9334(2) 0.0207(6) Uani 1 1 d . . .
H6A H 0.5002 0.7068 0.9862 0.025 Uiso 1 1 calc R . .
O7 O -0.0339(4) 0.84460(19) 0.5316(8) 0.143(2) Uani 1 1 d U . .
O8 O -0.0970(8) 0.8447(4) 0.6681(13) 0.101(4) Uani 0.40 1 d PU . .
O8A O -0.1457(4) 0.8116(2) 0.5458(8) 0.088(2) Uani 0.60 1 d PDU . .
O9 O -0.0077(3) 0.81626(17) 0.9331(6) 0.1057(18) Uani 1 1 d . . .
O10 O -0.1175(3) 0.84809(18) 0.9689(7) 0.131(2) Uani 1 1 d U . .
O11 O 0.7742(9) 0.5051(4) 0.7174(14) 0.143(4) Uani 0.50 1 d PU . .
O11A O 0.7445(7) 0.4948(3) 0.6350(11) 0.095(2) Uani 0.50 1 d PDU . .
O12 O 0.6902(9) 0.5353(4) 0.4734(14) 0.146(4) Uani 0.50 1 d PU . .
O12A O 0.7580(9) 0.5526(4) 0.5704(16) 0.174(4) Uani 0.50 1 d PDU . .
O13 O 0.7269(4) 0.51624(19) 0.9980(7) 0.141(2) Uani 1 1 d U . .
O14 O 0.6777(5) 0.4723(2) 1.1387(8) 0.1224(19) Uani 0.75 1 d PU . .
O14A O 0.7651(11) 0.4712(7) 1.105(2) 0.133(2) Uani 0.25 1 d PDU . .
O15 O -0.40460(17) 0.78182(8) 0.9111(3) 0.0296(7) Uani 1 1 d . . .
O16 O -0.45846(17) 0.74079(8) 0.7225(3) 0.0274(7) Uani 1 1 d . . .
O17 O 0.6019(2) 0.31531(9) 0.7566(3) 0.0387(9) Uani 1 1 d . . .
O18 O 0.6642(2) 0.33136(8) 0.9820(3) 0.0338(8) Uani 1 1 d . . .
O19 O 0.2445(3) 0.65963(16) 0.4182(7) 0.124(2) Uani 1 1 d . . .
O20 O 0.5695(4) 0.66650(17) 1.0864(6) 0.137(2) Uani 1 1 d U . .
C1 C 0.5111(3) 0.64287(12) 0.6587(4) 0.0290(11) Uani 1 1 d . . .
C2 C 0.5416(3) 0.59885(12) 0.6853(4) 0.0339(11) Uani 1 1 d . . .
C3 C 0.5007(4) 0.57399(15) 0.7610(6) 0.0632(16) Uani 1 1 d . . .
H3A H 0.4562 0.5847 0.7967 0.076 Uiso 1 1 calc R . .
C4 C 0.5261(4) 0.53305(16) 0.7836(6) 0.0704(18) Uani 1 1 d . . .
H4A H 0.4952 0.5164 0.8298 0.084 Uiso 1 1 calc R . .
C5 C 0.5956(4) 0.51613(15) 0.7400(5) 0.0498(15) Uani 1 1 d . . .
C6 C 0.6329(4) 0.54145(15) 0.6652(6) 0.0551(15) Uani 1 1 d . . .
C7 C 0.6078(3) 0.58192(14) 0.6359(5) 0.0500(14) Uani 1 1 d . . .
H7A H 0.6356 0.5977 0.5828 0.060 Uiso 1 1 calc R . .
C8 C 0.6172(4) 0.47156(14) 0.7686(5) 0.0524(15) Uani 1 1 d . . .
C9 C 0.6580(5) 0.45538(15) 0.9009(6) 0.072(2) Uani 1 1 d . . .
C10 C 0.6640(4) 0.41353(15) 0.9284(6) 0.0621(18) Uani 1 1 d . . .
H10A H 0.6913 0.4040 1.0186 0.075 Uiso 1 1 calc R . .
C11 C 0.6296(3) 0.38620(13) 0.8217(5) 0.0358(12) Uani 1 1 d . . .
C12 C 0.5913(5) 0.40146(15) 0.6899(6) 0.069(2) Uani 1 1 d . . .
H12A H 0.5695 0.3833 0.6158 0.082 Uiso 1 1 calc R . .
C13 C 0.5844(5) 0.44351(16) 0.6655(6) 0.076(2) Uani 1 1 d . . .
H13A H 0.5564 0.4528 0.5753 0.091 Uiso 1 1 calc R . .
C14 C 0.6317(3) 0.34080(12) 0.8522(4) 0.0311(11) Uani 1 1 d . . .
C15 C 0.2261(3) 0.74637(13) 0.6589(4) 0.0271(10) Uani 1 1 d . . .
C16 C 0.1361(3) 0.74888(14) 0.6855(4) 0.0321(11) Uani 1 1 d . . .
C17 C 0.0790(3) 0.78216(16) 0.6331(5) 0.0437(13) Uani 1 1 d . . .
H17A H 0.0973 0.8024 0.5818 0.052 Uiso 1 1 calc R . .
C18 C -0.0034(3) 0.78515(17) 0.6569(5) 0.0514(15) Uani 1 1 d . . .
C19 C -0.0357(3) 0.75626(18) 0.7331(5) 0.0461(14) Uani 1 1 d . . .
C20 C 0.0212(3) 0.72226(16) 0.7805(5) 0.0444(14) Uani 1 1 d . . .
H20A H 0.0018 0.7015 0.8287 0.053 Uiso 1 1 calc R . .
C21 C 0.1061(3) 0.71862(15) 0.7574(5) 0.0402(13) Uani 1 1 d . . .
H21A H 0.1426 0.6957 0.7906 0.048 Uiso 1 1 calc R . .
C22 C -0.1257(3) 0.75767(17) 0.7625(5) 0.0432(14) Uani 1 1 d . . .
C23 C -0.1875(3) 0.72680(18) 0.7110(5) 0.0519(15) Uani 1 1 d . . .
H23A H -0.1698 0.7048 0.6658 0.062 Uiso 1 1 calc R . .
C24 C -0.2756(3) 0.72701(16) 0.7233(4) 0.0427(13) Uani 1 1 d . . .
H24A H -0.3165 0.7061 0.6839 0.051 Uiso 1 1 calc R . .
C25 C -0.3013(3) 0.75867(14) 0.7947(4) 0.0302(11) Uani 1 1 d . . .
C26 C -0.2388(3) 0.78924(15) 0.8564(4) 0.0382(12) Uani 1 1 d . . .
H26A H -0.2550 0.8102 0.9075 0.046 Uiso 1 1 calc R . .
C27 C -0.1525(3) 0.78816(16) 0.8409(5) 0.0432(13) Uani 1 1 d . . .
C28 C -0.3965(2) 0.76052(12) 0.8091(4) 0.0231(9) Uani 1 1 d . . .
C29 C 0.2270(8) 0.6187(4) 0.6006(14) 0.207(6) Uani 1 1 d . . .
H29A H 0.2703 0.6378 0.6573 0.311 Uiso 1 1 calc R . .
H29B H 0.2514 0.5913 0.6167 0.311 Uiso 1 1 calc R . .
H29C H 0.1709 0.6201 0.6244 0.311 Uiso 1 1 calc R . .
C30 C 0.2089(6) 0.6297(3) 0.4484(9) 0.105(3) Uani 1 1 d U . .
C31 C 0.1450(7) 0.6039(3) 0.3361(14) 0.205(7) Uani 1 1 d . . .
H31A H 0.1430 0.6146 0.2463 0.307 Uiso 1 1 calc R . .
H31B H 0.0848 0.6047 0.3466 0.307 Uiso 1 1 calc R . .
H31C H 0.1664 0.5760 0.3440 0.307 Uiso 1 1 calc R . .
C32 C 0.6355(10) 0.6111(4) 1.2153(17) 0.276(9) Uani 1 1 d . . .
H32A H 0.5908 0.6160 1.2629 0.415 Uiso 1 1 calc R . .
H32B H 0.6957 0.6142 1.2796 0.415 Uiso 1 1 calc R . .
H32C H 0.6286 0.5836 1.1785 0.415 Uiso 1 1 calc R . .
C33 C 0.6226(5) 0.6408(2) 1.1000(9) 0.104(3) Uani 1 1 d U . .
C34 C 0.6873(9) 0.6324(4) 1.0223(14) 0.208(5) Uani 1 1 d U . .
H34A H 0.6798 0.6526 0.9498 0.312 Uiso 1 1 calc R . .
H34B H 0.6760 0.6055 0.9817 0.312 Uiso 1 1 calc R . .
H34C H 0.7485 0.6338 1.0844 0.312 Uiso 1 1 calc R . .
N1 N 0.7079(6) 0.5272(2) 0.6128(9) 0.143(3) Uani 1 1 d DU . .
N2 N -0.0621(4) 0.82003(19) 0.5919(6) 0.0823(14) Uani 1 1 d DU . .
N3 N -0.0882(3) 0.82016(16) 0.9118(6) 0.0722(16) Uani 1 1 d . . .
N4 N 0.6905(5) 0.4834(2) 1.0224(7) 0.115(2) Uani 1 1 d DU . .


_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
Cu3 O6 1.931(3) . ?
Cu3 O1 1.954(3) . ?
Cu3 O4 2.007(3) . ?
Cu3 O2 2.071(3) . ?
Cu3 O16 2.107(3) 1_655 ?
Cu3 Cu1 2.9618(13) . ?
Cu2 O15 1.915(3) 4_675 ?
Cu2 O1 1.948(3) . ?
Cu2 O3 1.978(3) . ?
Cu2 O6 2.021(3) 4_575 ?
Cu2 Cu1 3.0123(14) . ?
Cu1 O18 1.905(3) 2_656 ?
Cu1 O5 1.939(3) . ?
Cu1 O1 1.956(3) . ?
Cu1 O6 1.982(3) 4_575 ?
Cu1 O4 2.430(3) 4_575 ?
O1 H1A 0.9800 . ?
O2 C1 1.245(5) . ?
O3 C1 1.270(5) . ?
O4 C15 1.277(4) . ?
O4 Cu1 2.430(3) 4_576 ?
O5 C15 1.263(5) . ?
O6 Cu1 1.982(3) 4_576 ?
O6 Cu2 2.021(3) 4_576 ?
O6 H6A 0.9800 . ?
O7 N2 1.161(8) . ?
O8 N2 1.327(13) . ?
O8 O8A 1.635(15) . ?
O8A N2 1.256(8) . ?
O9 N3 1.195(6) . ?
O10 N3 1.228(7) . ?
O11 O11A 0.884(16) . ?
O11 N1 1.420(14) . ?
O11A N1 1.184(10) . ?
O12 O12A 1.319(18) . ?
O12 N1 1.370(15) . ?
O12A N1 1.284(13) . ?
O13 N4 1.261(9) . ?
O13 O14A 1.81(2) . ?
O14 N4 1.294(10) . ?
O14 O14A 1.48(2) . ?
O14A N4 1.260(15) . ?
O15 C28 1.273(5) . ?
O15 Cu2 1.915(3) 4_476 ?
O16 C28 1.255(4) . ?
O16 Cu3 2.107(3) 1_455 ?
O17 C14 1.247(5) . ?
O18 C14 1.286(5) . ?
O18 Cu1 1.905(3) 2_646 ?
O19 C30 1.199(10) . ?
O20 C33 1.144(9) . ?
C1 C2 1.504(6) . ?
C2 C7 1.372(7) . ?
C2 C3 1.382(7) . ?
C3 C4 1.385(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.382(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.353(8) . ?
C5 C8 1.494(7) . ?
C6 C7 1.377(7) . ?
C6 N1 1.475(10) . ?
C7 H7A 0.9300 . ?
C8 C13 1.358(7) . ?
C8 C9 1.392(7) . ?
C9 C10 1.386(7) . ?
C9 N4 1.485(9) . ?
C10 C11 1.370(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.371(7) . ?
C11 C14 1.505(6) . ?
C12 C13 1.387(7) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.485(6) . ?
C16 C21 1.378(6) . ?
C16 C17 1.391(6) . ?
C17 C18 1.357(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.393(7) . ?
C18 N2 1.472(7) . ?
C19 C20 1.400(7) . ?
C19 C22 1.497(6) . ?
C20 C21 1.395(6) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.370(7) . ?
C22 C27 1.401(7) . ?
C23 C24 1.394(6) . ?
C23 H23A 0.9300 . ?
C24 C25 1.378(6) . ?
C24 H24A 0.9300 . ?
C25 C26 1.391(6) . ?
C25 C28 1.510(5) . ?
C26 C27 1.378(6) . ?
C26 H26A 0.9300 . ?
C27 N3 1.463(7) . ?
C29 C30 1.513(15) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.507(12) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.477(16) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.460(15) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Cu3 O1 171.12(10) . . ?
O6 Cu3 O4 84.47(11) . . ?
O1 Cu3 O4 93.58(11) . . ?
O6 Cu3 O2 99.12(11) . . ?
O1 Cu3 O2 89.30(11) . . ?
O4 Cu3 O2 121.36(12) . . ?
O6 Cu3 O16 90.82(10) . 1_655 ?
O1 Cu3 O16 86.31(10) . 1_655 ?
O4 Cu3 O16 148.47(12) . 1_655 ?
O2 Cu3 O16 90.17(12) . 1_655 ?
O6 Cu3 Cu1 130.45(8) . . ?
O1 Cu3 Cu1 40.78(7) . . ?
O4 Cu3 Cu1 78.22(8) . . ?
O2 Cu3 Cu1 129.52(8) . . ?
O16 Cu3 Cu1 81.40(8) 1_655 . ?
O15 Cu2 O1 175.03(11) 4_675 . ?
O15 Cu2 O3 89.94(12) 4_675 . ?
O1 Cu2 O3 94.92(11) . . ?
O15 Cu2 O6 94.74(11) 4_675 4_575 ?
O1 Cu2 O6 80.29(10) . 4_575 ?
O3 Cu2 O6 166.05(11) . 4_575 ?
O15 Cu2 Cu1 135.44(9) 4_675 . ?
O1 Cu2 Cu1 39.60(7) . . ?
O3 Cu2 Cu1 132.95(9) . . ?
O6 Cu2 Cu1 40.71(8) 4_575 . ?
O18 Cu1 O5 91.27(13) 2_656 . ?
O18 Cu1 O1 162.83(11) 2_656 . ?
O5 Cu1 O1 92.53(11) . . ?
O18 Cu1 O6 96.00(12) 2_656 4_575 ?
O5 Cu1 O6 172.49(11) . 4_575 ?
O1 Cu1 O6 81.07(10) . 4_575 ?
O18 Cu1 O4 95.14(11) 2_656 4_575 ?
O5 Cu1 O4 104.54(10) . 4_575 ?
O1 Cu1 O4 100.08(10) . 4_575 ?
O6 Cu1 O4 72.97(10) 4_575 4_575 ?
O18 Cu1 Cu3 123.81(9) 2_656 . ?
O5 Cu1 Cu3 81.00(8) . . ?
O1 Cu1 Cu3 40.74(7) . . ?
O6 Cu1 Cu3 96.44(8) 4_575 . ?
O4 Cu1 Cu3 140.79(7) 4_575 . ?
O18 Cu1 Cu2 134.95(10) 2_656 . ?
O5 Cu1 Cu2 131.87(9) . . ?
O1 Cu1 Cu2 39.40(8) . . ?
O6 Cu1 Cu2 41.68(7) 4_575 . ?
O4 Cu1 Cu2 86.63(7) 4_575 . ?
Cu3 Cu1 Cu2 63.55(3) . . ?
Cu2 O1 Cu3 107.46(11) . . ?
Cu2 O1 Cu1 101.00(11) . . ?
Cu3 O1 Cu1 98.48(11) . . ?
Cu2 O1 H1A 115.9 . . ?
Cu3 O1 H1A 115.9 . . ?
Cu1 O1 H1A 115.9 . . ?
C1 O2 Cu3 127.8(3) . . ?
C1 O3 Cu2 128.1(3) . . ?
C15 O4 Cu3 127.4(3) . . ?
C15 O4 Cu1 130.6(3) . 4_576 ?
Cu3 O4 Cu1 91.61(10) . 4_576 ?
C15 O5 Cu1 127.4(2) . . ?
Cu3 O6 Cu1 109.44(11) . 4_576 ?
Cu3 O6 Cu2 109.72(12) . 4_576 ?
Cu1 O6 Cu2 97.61(11) 4_576 4_576 ?
Cu3 O6 H6A 113.0 . . ?
Cu1 O6 H6A 113.0 4_576 . ?
Cu2 O6 H6A 113.0 4_576 . ?
N2 O8 O8A 48.8(5) . . ?
N2 O8A O8 52.7(6) . . ?
O11A O11 N1 56.2(10) . . ?
O11 O11A N1 85.4(13) . . ?
O12A O12 N1 57.0(8) . . ?
N1 O12A O12 63.5(9) . . ?
N4 O13 O14A 44.2(7) . . ?
N4 O14 O14A 53.5(8) . . ?
N4 O14A O14 55.7(9) . . ?
N4 O14A O13 44.3(8) . . ?
O14 O14A O13 87.8(10) . . ?
C28 O15 Cu2 126.4(2) . 4_476 ?
C28 O16 Cu3 131.6(3) . 1_455 ?
C14 O18 Cu1 109.0(2) . 2_646 ?
O2 C1 O3 128.5(4) . . ?
O2 C1 C2 116.0(4) . . ?
O3 C1 C2 115.5(4) . . ?
C7 C2 C3 118.2(4) . . ?
C7 C2 C1 122.8(4) . . ?
C3 C2 C1 119.1(4) . . ?
C2 C3 C4 120.0(5) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C5 C4 C3 122.4(5) . . ?
C5 C4 H4A 118.8 . . ?
C3 C4 H4A 118.8 . . ?
C6 C5 C4 115.4(5) . . ?
C6 C5 C8 126.2(5) . . ?
C4 C5 C8 118.2(5) . . ?
C5 C6 C7 124.2(5) . . ?
C5 C6 N1 120.9(5) . . ?
C7 C6 N1 114.9(5) . . ?
C2 C7 C6 119.7(5) . . ?
C2 C7 H7A 120.2 . . ?
C6 C7 H7A 120.2 . . ?
C13 C8 C9 115.6(5) . . ?
C13 C8 C5 119.6(5) . . ?
C9 C8 C5 124.1(5) . . ?
C10 C9 C8 123.1(5) . . ?
C10 C9 N4 116.9(5) . . ?
C8 C9 N4 119.8(5) . . ?
C11 C10 C9 119.6(5) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C10 C11 C12 118.3(4) . . ?
C10 C11 C14 119.8(4) . . ?
C12 C11 C14 121.9(4) . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C8 C13 C12 122.3(5) . . ?
C8 C13 H13A 118.8 . . ?
C12 C13 H13A 118.8 . . ?
O17 C14 O18 124.3(4) . . ?
O17 C14 C11 120.9(4) . . ?
O18 C14 C11 114.7(4) . . ?
O5 C15 O4 125.3(4) . . ?
O5 C15 C16 116.5(3) . . ?
O4 C15 C16 118.2(4) . . ?
C21 C16 C17 118.8(4) . . ?
C21 C16 C15 121.9(4) . . ?
C17 C16 C15 119.2(4) . . ?
C18 C17 C16 120.1(5) . . ?
C18 C17 H17A 119.9 . . ?
C16 C17 H17A 119.9 . . ?
C17 C18 C19 123.4(5) . . ?
C17 C18 N2 117.0(5) . . ?
C19 C18 N2 119.5(5) . . ?
C18 C19 C20 115.6(4) . . ?
C18 C19 C22 126.1(5) . . ?
C20 C19 C22 118.3(5) . . ?
C21 C20 C19 121.9(5) . . ?
C21 C20 H20A 119.1 . . ?
C19 C20 H20A 119.1 . . ?
C16 C21 C20 120.1(4) . . ?
C16 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
C23 C22 C27 116.4(4) . . ?
C23 C22 C19 118.4(5) . . ?
C27 C22 C19 125.1(4) . . ?
C22 C23 C24 122.8(5) . . ?
C22 C23 H23A 118.6 . . ?
C24 C23 H23A 118.6 . . ?
C25 C24 C23 119.1(4) . . ?
C25 C24 H24A 120.4 . . ?
C23 C24 H24A 120.4 . . ?
C24 C25 C26 119.9(4) . . ?
C24 C25 C28 121.0(4) . . ?
C26 C25 C28 119.0(4) . . ?
C27 C26 C25 119.2(4) . . ?
C27 C26 H26A 120.4 . . ?
C25 C26 H26A 120.4 . . ?
C26 C27 C22 122.3(4) . . ?
C26 C27 N3 117.1(5) . . ?
C22 C27 N3 120.6(4) . . ?
O16 C28 O15 126.9(4) . . ?
O16 C28 C25 117.7(3) . . ?
O15 C28 C25 115.4(3) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C31 120.3(9) . . ?
O19 C30 C29 119.2(8) . . ?
C31 C30 C29 120.5(9) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O20 C33 C34 130.1(10) . . ?
O20 C33 C32 119.7(11) . . ?
C34 C33 C32 110.1(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O11A N1 O12A 109.8(11) . . ?
O11A N1 O12 107.4(10) . . ?
O12A N1 O12 59.5(9) . . ?
O11A N1 O11 38.3(7) . . ?
O12A N1 O11 101.8(10) . . ?
O12 N1 O11 137.1(11) . . ?
O11A N1 C6 126.0(9) . . ?
O12A N1 C6 121.6(9) . . ?
O12 N1 C6 111.7(8) . . ?
O11 N1 C6 110.8(9) . . ?
O7 N2 O8A 117.1(7) . . ?
O7 N2 O8 99.4(8) . . ?
O8A N2 O8 78.5(7) . . ?
O7 N2 C18 119.2(6) . . ?
O8A N2 C18 114.6(6) . . ?
O8 N2 C18 120.5(7) . . ?
O9 N3 O10 119.8(5) . . ?
O9 N3 C27 121.4(5) . . ?
O10 N3 C27 117.8(5) . . ?
O14A N4 O14 70.9(12) . . ?
O14A N4 O13 91.6(13) . . ?
O14 N4 O13 127.5(8) . . ?
O14A N4 C9 111.1(13) . . ?
O14 N4 C9 117.8(7) . . ?
O13 N4 C9 114.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.139
_database_code_depnum_ccdc_archive 'CCDC 977430'
#######################################################################
#
#                 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_405

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C3 H8 O)'
_chemical_formula_sum            'C34 H30 Cu3 N4 O20'
_chemical_formula_weight         1005.24

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   'P2(1)/c  '
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.286(3)
_cell_length_b                   32.626(7)
_cell_length_c                   10.053(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.200(3)
_cell_angle_gamma                90.00
_cell_volume                     4789.4(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7120
_cell_measurement_theta_min      1.20
_cell_measurement_theta_max      26.09

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2036
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.7876
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31866
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8232
_reflns_number_gt                5748
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0735P)²+27.2151P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8232
_refine_ls_number_parameters     551
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0875
_refine_ls_wR_factor_ref         0.2098
_refine_ls_wR_factor_gt          0.1964
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu3 Cu 0.40849(5) 0.71624(2) 0.26962(7) 0.02349(16) Uani 1 1 d . . .
Cu2 Cu 0.48204(4) 0.71743(2) 0.01209(8) 0.02590(17) Uani 1 1 d . . .
Cu1 Cu 0.33414(4) 0.774765(19) 0.03323(7) 0.02243(16) Uani 1 1 d . . .
O1 O 0.3709(2) 0.71792(10) 0.0689(4) 0.0225(9) Uani 1 1 d . . .
H1 H 0.3307 0.7004 0.0288 0.027 Uiso 1 1 d R . .
O2 O 0.4564(3) 0.65713(12) 0.2603(5) 0.0406(11) Uani 1 1 d . . .
O3 O 0.5183(3) 0.66253(12) 0.0816(4) 0.0333(10) Uani 1 1 d . . .
O4 O 0.2833(3) 0.72763(13) 0.2818(4) 0.0319(10) Uani 1 1 d . . .
O5 O 0.2253(3) 0.76676(13) 0.0923(4) 0.0323(10) Uani 1 1 d . . .
O6 O 0.4448(2) 0.72434(11) 0.4679(4) 0.0224(9) Uani 1 1 d . . .
H6 H 0.4850 0.7073 0.5119 0.027 Uiso 1 1 d R . .
O7A O -0.0349(8) 0.8479(3) 0.1168(17) 0.093(4) Uani 0.50 1 d PDU A 1
O7B O -0.0548(8) 0.8381(3) 0.0424(11) 0.072(3) Uani 0.50 1 d PDU A 2
O8A O -0.1569(5) 0.8083(4) 0.0918(14) 0.083(3) Uani 0.50 1 d PDU A 1
O8B O -0.1294(7) 0.8332(4) 0.1756(13) 0.083(3) Uani 0.50 1 d PDU A 2
O9 O -0.0144(3) 0.8117(2) 0.4699(7) 0.089(2) Uani 1 1 d D . .
O10 O -0.1222(4) 0.8421(2) 0.5164(8) 0.095(2) Uani 1 1 d . . .
O11A O 0.7598(9) 0.5091(4) 0.2074(15) 0.108(5) Uani 0.50 1 d PDU B 1
O11B O 0.7314(11) 0.4993(3) 0.121(2) 0.116(5) Uani 0.50 1 d PDU B 2
O12A O 0.7484(9) 0.5609(4) 0.0820(17) 0.112(5) Uani 0.50 1 d PDU B 1
O12B O 0.6910(15) 0.5430(6) 0.0072(11) 0.144(6) Uani 0.50 1 d PDU B 2
O13A O 0.7323(9) 0.5131(4) 0.4836(17) 0.112(4) Uani 0.50 1 d PDU C 1
O13B O 0.6943(12) 0.5207(3) 0.5035(19) 0.112(4) Uani 0.50 1 d PDU C 2
O14A O 0.7203(12) 0.4698(5) 0.6356(11) 0.111(3) Uani 0.50 1 d PDU C 1
O14B O 0.6689(10) 0.4725(5) 0.6192(12) 0.111(3) Uani 0.50 1 d PDU C 2
O15 O -0.4120(3) 0.77811(13) 0.4495(5) 0.0348(11) Uani 1 1 d . . .
O16 O -0.4657(2) 0.73909(13) 0.2595(4) 0.0318(10) Uani 1 1 d . . .
O17 O 0.6074(4) 0.31922(15) 0.2372(5) 0.0541(14) Uani 1 1 d . . .
O18 O 0.6748(3) 0.33306(12) 0.4588(5) 0.0377(11) Uani 1 1 d . . .
O19 O 0.5609(8) 0.6713(4) 0.6196(15) 0.195(4) Uani 1 1 d D . .
H19 H 0.5268 0.6674 0.6716 0.234 Uiso 1 1 d R . .
O20 O 0.2477(8) 0.6639(3) -0.0442(13) 0.192(4) Uani 1 1 d D . .
H20 H 0.2803 0.6566 -0.0953 0.288 Uiso 1 1 d RD . .
C1 C 0.4985(4) 0.64355(18) 0.1788(7) 0.0341(15) Uani 1 1 d . . .
C2 C 0.5271(5) 0.59985(19) 0.1961(7) 0.0404(17) Uani 1 1 d . . .
C3 C 0.4815(6) 0.5721(2) 0.2567(9) 0.060(2) Uani 1 1 d . . .
H3A H 0.4308 0.5806 0.2826 0.072 Uiso 1 1 calc R . .
C4 C 0.5103(6) 0.5328(2) 0.2783(10) 0.071(2) Uani 1 1 d . . .
H4A H 0.4792 0.5151 0.3209 0.085 Uiso 1 1 calc R . .
C5 C 0.5832(6) 0.5180(2) 0.2401(9) 0.063(2) Uani 1 1 d U . .
C6 C 0.6267(7) 0.5459(3) 0.1764(12) 0.0905(13) Uani 1 1 d U B .
C7 C 0.5995(5) 0.5856(2) 0.1539(8) 0.054(2) Uani 1 1 d . . .
H7A H 0.6299 0.6033 0.1099 0.064 Uiso 1 1 calc R . .
C8 C 0.6099(6) 0.4737(2) 0.2655(9) 0.057(2) Uani 1 1 d . . .
C9 C 0.6521(8) 0.4576(3) 0.3913(12) 0.0884(14) Uani 1 1 d U C .
C10 C 0.6654(6) 0.4158(2) 0.4145(9) 0.064(3) Uani 1 1 d . . .
H10A H 0.6969 0.4063 0.5030 0.076 Uiso 1 1 calc R . .
C11 C 0.6326(5) 0.38851(19) 0.3084(8) 0.0441(18) Uani 1 1 d . . .
C12 C 0.5856(7) 0.4041(2) 0.1814(9) 0.066(3) Uani 1 1 d . . .
H12A H 0.5602 0.3863 0.1078 0.079 Uiso 1 1 calc R . .
C13 C 0.5751(7) 0.4458(2) 0.1605(10) 0.074(3) Uani 1 1 d . . .
H13A H 0.5435 0.4554 0.0723 0.088 Uiso 1 1 calc R . .
C14 C 0.6394(5) 0.34370(19) 0.3343(7) 0.0377(16) Uani 1 1 d . . .
C15 C 0.2191(4) 0.74732(18) 0.1966(6) 0.0269(14) Uani 1 1 d . . .
C16 C 0.1279(4) 0.7484(2) 0.2231(6) 0.0327(15) Uani 1 1 d . . .
C17 C 0.0711(4) 0.7810(2) 0.1712(7) 0.0406(17) Uani 1 1 d . . .
H17A H 0.0902 0.8018 0.1233 0.049 Uiso 1 1 calc R . .
C18 C -0.0147(4) 0.7825(2) 0.1905(9) 0.053(2) Uani 1 1 d . A .
C19 C -0.0428(4) 0.7528(2) 0.2724(7) 0.0434(18) Uani 1 1 d . . .
C20 C 0.0188(4) 0.7197(2) 0.3212(7) 0.0405(17) Uani 1 1 d . . .
H20A H 0.0029 0.6989 0.3730 0.049 Uiso 1 1 calc R . .
C21 C 0.0999(4) 0.7180(2) 0.2936(7) 0.0349(16) Uani 1 1 d . . .
H21A H 0.1376 0.6954 0.3236 0.042 Uiso 1 1 calc R . .
C22 C -0.1335(4) 0.7538(2) 0.3023(7) 0.0405(17) Uani 1 1 d . . .
C23 C -0.1931(4) 0.72271(19) 0.2530(7) 0.0343(13) Uani 1 1 d U . .
H23A H -0.1743 0.7002 0.2116 0.041 Uiso 1 1 calc R . .
C24 C -0.2822(4) 0.7237(2) 0.2629(7) 0.0403(17) Uani 1 1 d . . .
H24A H -0.3238 0.7034 0.2206 0.048 Uiso 1 1 calc R . .
C25 C -0.3086(4) 0.7549(2) 0.3353(6) 0.0315(15) Uani 1 1 d . . .
C26 C -0.2439(4) 0.7845(2) 0.3985(7) 0.0363(16) Uani 1 1 d . . .
H26A H -0.2580 0.8044 0.4553 0.044 Uiso 1 1 calc R . .
C27 C -0.1589(5) 0.7844(2) 0.3766(6) 0.0447(19) Uani 1 1 d . . .
C28 C -0.4029(4) 0.75761(18) 0.3487(6) 0.0251(13) Uani 1 1 d . . .
C29 C 0.6310(13) 0.6183(6) 0.7589(17) 0.195(4) Uani 1 1 d DU . .
H29A H 0.5818 0.6004 0.7623 0.293 Uiso 1 1 calc R . .
H29B H 0.6336 0.6412 0.8201 0.293 Uiso 1 1 calc R . .
H29C H 0.6879 0.6036 0.7879 0.293 Uiso 1 1 calc R . .
C30 C 0.6150(11) 0.6336(5) 0.6127(17) 0.195(4) Uani 1 1 d DU . .
H30A H 0.5653 0.6152 0.5634 0.234 Uiso 1 1 calc R . .
C31 C 0.6839(11) 0.6241(6) 0.536(2) 0.195(4) Uani 1 1 d D . .
H31A H 0.6695 0.6396 0.4512 0.293 Uiso 1 1 calc R . .
H31B H 0.6821 0.5953 0.5150 0.293 Uiso 1 1 calc R . .
H31C H 0.7442 0.6313 0.5935 0.293 Uiso 1 1 calc R . .
C32 C 0.1596(13) 0.6057(5) -0.1378(17) 0.192(4) Uani 1 1 d D . .
H32A H 0.1814 0.6158 -0.2120 0.288 Uiso 1 1 calc R . .
H32B H 0.0963 0.6129 -0.1556 0.288 Uiso 1 1 calc R . .
H32C H 0.1659 0.5764 -0.1323 0.288 Uiso 1 1 calc R . .
C33 C 0.2092(13) 0.6239(5) 0.1441(15) 0.192(4) Uani 1 1 d D . .
H33A H 0.2545 0.6420 0.2010 0.288 Uiso 1 1 calc R . .
H33B H 0.2201 0.5965 0.1804 0.288 Uiso 1 1 calc R . .
H33C H 0.1494 0.6326 0.1445 0.288 Uiso 1 1 calc R . .
C34 C 0.2151(13) 0.6246(4) -0.0016(14) 0.192(4) Uani 1 1 d D . .
H34A H 0.2714 0.6085 0.0129 0.231 Uiso 1 1 calc RD . .
N1 N 0.7103(6) 0.5346(2) 0.1314(9) 0.0948(14) Uani 1 1 d DU . .
N2 N -0.0748(4) 0.8161(2) 0.1271(7) 0.070(2) Uani 1 1 d DU . .
N3 N -0.0952(3) 0.8153(2) 0.4551(7) 0.0584(19) Uani 1 1 d D . .
N4 N 0.6921(6) 0.4840(2) 0.5186(8) 0.0907(15) Uani 1 1 d DU . .


_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
Cu3 O6 1.922(4) . ?
Cu3 O1 1.928(4) . ?
Cu3 O4 1.989(4) . ?
Cu3 O2 2.075(4) . ?
Cu3 O16 2.093(4) 1_655 ?
Cu3 Cu1 2.9980(10) . ?
Cu2 O15 1.909(4) 4_675 ?
Cu2 O3 1.943(4) . ?
Cu2 O1 1.946(4) . ?
Cu2 O6 1.995(4) 4_575 ?
Cu2 Cu1 2.9898(10) . ?
Cu1 O18 1.910(4) 2_655 ?
Cu1 O1 1.940(4) . ?
Cu1 O5 1.942(4) . ?
Cu1 O6 1.988(4) 4_575 ?
Cu1 O4 2.416(4) 4_575 ?
O1 H1 0.8500 . ?
O2 C1 1.261(8) . ?
O3 C1 1.268(8) . ?
O4 C15 1.270(7) . ?
O4 Cu1 2.416(4) 4_576 ?
O5 C15 1.254(7) . ?
O6 Cu1 1.988(4) 4_576 ?
O6 Cu2 1.995(4) 4_576 ?
O6 H6 0.8500 . ?
O7A N2 1.221(8) . ?
O7B N2 1.219(8) . ?
O8A N2 1.227(8) . ?
O8B N2 1.219(8) . ?
O9 N3 1.207(6) . ?
O10 N3 1.209(9) . ?
O11A N1 1.229(9) . ?
O11B N1 1.210(8) . ?
O11B O12B 1.82(2) . ?
O12A N1 1.222(9) . ?
O12B N1 1.226(9) . ?
O13A N4 1.238(9) . ?
O13B N4 1.209(8) . ?
O14A N4 1.218(9) . ?
O14B N4 1.225(9) . ?
O15 C28 1.255(7) . ?
O15 Cu2 1.909(4) 4_476 ?
O16 C28 1.258(7) . ?
O16 Cu3 2.093(4) 1_455 ?
O17 C14 1.244(8) . ?
O18 C14 1.257(8) . ?
O18 Cu1 1.910(4) 2_645 ?
O19 C30 1.497(14) . ?
O19 H19 0.8500 . ?
O20 C34 1.486(12) . ?
O20 H20 0.8498 . ?
C1 C2 1.486(8) . ?
C2 C7 1.378(10) . ?
C2 C3 1.388(10) . ?
C3 C4 1.351(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.391(14) . ?
C5 C8 1.502(10) . ?
C6 C7 1.359(12) . ?
C6 N1 1.521(13) . ?
C7 H7A 0.9300 . ?
C8 C9 1.345(13) . ?
C8 C13 1.376(12) . ?
C9 C10 1.389(11) . ?
C9 N4 1.513(13) . ?
C10 C11 1.365(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.365(11) . ?
C11 C14 1.483(9) . ?
C12 C13 1.378(11) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.494(8) . ?
C16 C21 1.360(9) . ?
C16 C17 1.373(9) . ?
C17 C18 1.382(9) . ?
C17 H17A 0.9300 . ?
C18 C19 1.420(10) . ?
C18 N2 1.451(9) . ?
C19 C20 1.419(10) . ?
C19 C22 1.503(8) . ?
C20 C21 1.349(9) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.356(9) . ?
C22 C27 1.369(10) . ?
C23 C24 1.395(9) . ?
C23 H23A 0.9300 . ?
C24 C25 1.377(9) . ?
C24 H24A 0.9300 . ?
C25 C26 1.395(9) . ?
C25 C28 1.490(8) . ?
C26 C27 1.381(10) . ?
C26 H26A 0.9300 . ?
C27 N3 1.461(9) . ?
C29 C30 1.502(16) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.509(16) . ?
C30 H30A 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C34 1.512(15) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.494(15) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Cu3 O1 170.46(15) . . ?
O6 Cu3 O4 84.17(16) . . ?
O1 Cu3 O4 93.73(16) . . ?
O6 Cu3 O2 100.20(16) . . ?
O1 Cu3 O2 88.79(16) . . ?
O4 Cu3 O2 122.39(18) . . ?
O6 Cu3 O16 90.77(16) . 1_655 ?
O1 Cu3 O16 86.14(16) . 1_655 ?
O4 Cu3 O16 148.35(17) . 1_655 ?
O2 Cu3 O16 89.26(17) . 1_655 ?
O6 Cu3 Cu1 131.29(11) . . ?
O1 Cu3 Cu1 39.35(10) . . ?
O4 Cu3 Cu1 77.51(12) . . ?
O2 Cu3 Cu1 127.75(12) . . ?
O16 Cu3 Cu1 82.70(12) 1_655 . ?
O15 Cu2 O3 90.52(17) 4_675 . ?
O15 Cu2 O1 174.72(16) 4_675 . ?
O3 Cu2 O1 94.77(16) . . ?
O15 Cu2 O6 93.89(16) 4_675 4_575 ?
O3 Cu2 O6 171.98(17) . 4_575 ?
O1 Cu2 O6 80.88(15) . 4_575 ?
O15 Cu2 Cu1 135.15(13) 4_675 . ?
O3 Cu2 Cu1 133.84(13) . . ?
O1 Cu2 Cu1 39.64(10) . . ?
O6 Cu2 Cu1 41.27(11) 4_575 . ?
O18 Cu1 O1 164.65(18) 2_655 . ?
O18 Cu1 O5 92.46(18) 2_655 . ?
O1 Cu1 O5 92.44(16) . . ?
O18 Cu1 O6 94.44(17) 2_655 4_575 ?
O1 Cu1 O6 81.19(15) . 4_575 ?
O5 Cu1 O6 173.00(16) . 4_575 ?
O18 Cu1 O4 94.07(17) 2_655 4_575 ?
O1 Cu1 O4 98.55(15) . 4_575 ?
O5 Cu1 O4 105.99(15) . 4_575 ?
O6 Cu1 O4 72.35(14) 4_575 4_575 ?
O18 Cu1 Cu2 133.70(13) 2_655 . ?
O1 Cu1 Cu2 39.76(11) . . ?
O5 Cu1 Cu2 132.19(13) . . ?
O6 Cu1 Cu2 41.45(10) 4_575 . ?
O4 Cu1 Cu2 85.50(10) 4_575 . ?
O18 Cu1 Cu3 128.04(14) 2_655 . ?
O1 Cu1 Cu3 39.05(11) . . ?
O5 Cu1 Cu3 80.23(12) . . ?
O6 Cu1 Cu3 96.39(11) 4_575 . ?
O4 Cu1 Cu3 137.56(10) 4_575 . ?
Cu2 Cu1 Cu3 62.64(2) . . ?
Cu3 O1 Cu1 101.60(17) . . ?
Cu3 O1 Cu2 106.95(17) . . ?
Cu1 O1 Cu2 100.60(16) . . ?
Cu3 O1 H1 115.3 . . ?
Cu1 O1 H1 115.2 . . ?
Cu2 O1 H1 115.3 . . ?
C1 O2 Cu3 127.6(4) . . ?
C1 O3 Cu2 128.3(4) . . ?
C15 O4 Cu3 128.2(4) . . ?
C15 O4 Cu1 131.9(4) . 4_576 ?
Cu3 O4 Cu1 92.33(15) . 4_576 ?
C15 O5 Cu1 127.4(4) . . ?
Cu3 O6 Cu1 109.36(17) . 4_576 ?
Cu3 O6 Cu2 109.74(18) . 4_576 ?
Cu1 O6 Cu2 97.28(16) 4_576 4_576 ?
Cu3 O6 H6 113.1 . . ?
Cu1 O6 H6 113.1 4_576 . ?
Cu2 O6 H6 113.1 4_576 . ?
N1 O11B O12B 42.1(8) . . ?
N1 O12B O11B 41.4(8) . . ?
C28 O15 Cu2 127.9(4) . 4_476 ?
C28 O16 Cu3 130.9(4) . 1_455 ?
C14 O18 Cu1 107.5(4) . 2_645 ?
C30 O19 H19 110.6 . . ?
C34 O20 H20 103.6 . . ?
O2 C1 O3 127.8(5) . . ?
O2 C1 C2 116.7(6) . . ?
O3 C1 C2 115.4(6) . . ?
C7 C2 C3 117.9(6) . . ?
C7 C2 C1 121.5(6) . . ?
C3 C2 C1 120.6(6) . . ?
C4 C3 C2 120.5(8) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C3 C4 C5 122.9(8) . . ?
C3 C4 H4A 118.6 . . ?
C5 C4 H4A 118.6 . . ?
C4 C5 C6 115.9(7) . . ?
C4 C5 C8 119.6(8) . . ?
C6 C5 C8 124.5(8) . . ?
C7 C6 C5 122.5(9) . . ?
C7 C6 N1 115.1(9) . . ?
C5 C6 N1 122.4(8) . . ?
C6 C7 C2 120.2(8) . . ?
C6 C7 H7A 119.9 . . ?
C2 C7 H7A 119.9 . . ?
C9 C8 C13 115.6(7) . . ?
C9 C8 C5 124.5(8) . . ?
C13 C8 C5 118.8(7) . . ?
C8 C9 C10 123.2(9) . . ?
C8 C9 N4 122.3(8) . . ?
C10 C9 N4 114.5(8) . . ?
C11 C10 C9 120.5(8) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C10 C11 C12 117.3(6) . . ?
C10 C11 C14 120.9(6) . . ?
C12 C11 C14 121.5(7) . . ?
C11 C12 C13 121.1(8) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C8 C13 C12 122.4(8) . . ?
C8 C13 H13A 118.8 . . ?
C12 C13 H13A 118.8 . . ?
O17 C14 O18 123.9(6) . . ?
O17 C14 C11 120.3(6) . . ?
O18 C14 C11 115.8(6) . . ?
O5 C15 O4 125.8(5) . . ?
O5 C15 C16 116.3(5) . . ?
O4 C15 C16 117.9(5) . . ?
C21 C16 C17 120.0(5) . . ?
C21 C16 C15 122.0(6) . . ?
C17 C16 C15 118.0(6) . . ?
C16 C17 C18 119.8(6) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 121.2(6) . . ?
C17 C18 N2 118.1(6) . . ?
C19 C18 N2 120.7(6) . . ?
C20 C19 C18 115.9(6) . . ?
C20 C19 C22 120.3(6) . . ?
C18 C19 C22 123.8(6) . . ?
C21 C20 C19 121.1(6) . . ?
C21 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C20 C21 C16 121.8(6) . . ?
C20 C21 H21A 119.1 . . ?
C16 C21 H21A 119.1 . . ?
C23 C22 C27 118.4(6) . . ?
C23 C22 C19 118.1(6) . . ?
C27 C22 C19 123.5(7) . . ?
C22 C23 C24 121.4(6) . . ?
C22 C23 H23A 119.3 . . ?
C24 C23 H23A 119.3 . . ?
C25 C24 C23 120.0(6) . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
C24 C25 C26 118.3(6) . . ?
C24 C25 C28 122.3(5) . . ?
C26 C25 C28 119.4(6) . . ?
C27 C26 C25 119.8(6) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C22 C27 C26 121.5(7) . . ?
C22 C27 N3 123.2(7) . . ?
C26 C27 N3 114.7(6) . . ?
O15 C28 O16 126.0(5) . . ?
O15 C28 C25 116.5(5) . . ?
O16 C28 C25 117.5(5) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C29 C30 C31 119.7(14) . . ?
C29 C30 O19 99.2(13) . . ?
C31 C30 O19 132.2(15) . . ?
C29 C30 H30A 99.8 . . ?
C31 C30 H30A 99.8 . . ?
O19 C30 H30A 99.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C32 H32A 109.5 . . ?
C34 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C34 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O20 C34 C33 114.7(13) . . ?
O20 C34 C32 103.7(11) . . ?
C33 C34 C32 134.5(15) . . ?
O20 C34 H34A 98.7 . . ?
C33 C34 H34A 98.7 . . ?
C32 C34 H34A 98.7 . . ?
O11B N1 O12A 117.5(13) . . ?
O11B N1 O12B 96.5(15) . . ?
O12A N1 O12B 55.2(12) . . ?
O11B N1 O11A 43.6(10) . . ?
O12A N1 O11A 116.6(12) . . ?
O12B N1 O11A 134.6(15) . . ?
O11B N1 C6 121.7(12) . . ?
O12A N1 C6 119.6(10) . . ?
O12B N1 C6 106.2(13) . . ?
O11A N1 C6 113.4(11) . . ?
O7B N2 O8B 110.7(10) . . ?
O7B N2 O7A 37.6(8) . . ?
O8B N2 O7A 93.7(11) . . ?
O7B N2 O8A 111.6(10) . . ?
O8B N2 O8A 56.5(8) . . ?
O7A N2 O8A 130.3(10) . . ?
O7B N2 C18 119.6(8) . . ?
O8B N2 C18 126.1(9) . . ?
O7A N2 C18 114.2(8) . . ?
O8A N2 C18 115.4(8) . . ?
O9 N3 O10 119.9(7) . . ?
O9 N3 C27 119.5(7) . . ?
O10 N3 C27 120.1(6) . . ?
O13B N4 O14A 118.9(14) . . ?
O13B N4 O14B 115.6(15) . . ?
O14A N4 O14B 36.2(10) . . ?
O13B N4 O13A 33.8(12) . . ?
O14A N4 O13A 120.2(13) . . ?
O14B N4 O13A 139.4(13) . . ?
O13B N4 C9 118.4(11) . . ?
O14A N4 C9 122.6(10) . . ?
O14B N4 C9 112.3(10) . . ?
O13A N4 C9 107.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.028
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.126
_database_code_depnum_ccdc_archive 'CCDC 977431'
#######################################################################
#
#                 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_508

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C4 H10 O)'
_chemical_formula_sum            'C36 H34 Cu3 N4 O20'
_chemical_formula_weight         1033.29

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'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.348(2)
_cell_length_b                   32.866(4)
_cell_length_c                   10.1122(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.642(2)
_cell_angle_gamma                90.00
_cell_volume                     4887.2(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9646
_cell_measurement_theta_min      1.14
_cell_measurement_theta_max      26.60

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8212
_exptl_absorpt_correction_T_max  0.8868
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32939
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8446
_reflns_number_gt                6568
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0790P)²+24.9545P] 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     SHELXL
_refine_ls_extinction_coef       0.00051(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8446
_refine_ls_number_parameters     581
_refine_ls_number_restraints     191
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.1914
_refine_ls_wR_factor_gt          0.1827
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.105
_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 0.15488(5) 0.27467(2) 0.46082(8) 0.0220(2) Uani 1 1 d . . .
Cu2 Cu 0.00823(5) 0.21721(2) 0.48399(8) 0.0253(2) Uani 1 1 d . . .
Cu3 Cu 0.08122(5) 0.21667(2) 0.22564(8) 0.0229(2) Uani 1 1 d . . .
O1 O 0.1187(3) 0.21828(11) 0.4254(4) 0.0219(9) Uani 1 1 d D . .
H1A H 0.1589 0.2009 0.4645 0.026 Uiso 1 1 d R . .
O2 O 0.0330(3) 0.15784(13) 0.2353(5) 0.0355(11) Uani 1 1 d . . .
O3 O -0.0269(3) 0.16248(12) 0.4150(5) 0.0302(10) Uani 1 1 d . . .
O4 O 0.2067(3) 0.22830(14) 0.2132(5) 0.0301(10) Uani 1 1 d . . .
O5 O 0.2636(3) 0.26713(13) 0.4012(5) 0.0304(10) Uani 1 1 d . . .
O6 O 0.0453(3) 0.22509(11) 0.0289(4) 0.0221(9) Uani 1 1 d D . .
H6A H 0.0052 0.2082 -0.0141 0.027 Uiso 1 1 d R . .
O7 O 0.5386(7) 0.3404(3) 0.4291(12) 0.132(3) Uani 1 1 d DU A .
O8A O 0.6457(6) 0.3078(4) 0.4014(13) 0.064(3) Uani 0.50 1 d PDU A 1
O8B O 0.5973(15) 0.3373(6) 0.295(2) 0.127(6) Uani 0.50 1 d PDU A 2
O9 O 0.5036(5) 0.3097(3) 0.0190(9) 0.098(3) Uani 1 1 d DU . .
O10 O 0.6118(5) 0.3408(3) -0.0230(9) 0.099(3) Uani 1 1 d DU . .
O11 O -0.2421(8) -0.0001(3) 0.3422(15) 0.158(4) Uani 1 1 d DU B .
O12A O -0.199(2) 0.0401(9) 0.4908(19) 0.172(9) Uani 0.50 1 d PDU B 1
O12B O -0.2609(11) 0.0583(5) 0.389(2) 0.110(5) Uani 0.50 1 d PDU B 2
O13 O -0.2201(7) 0.0154(3) 0.0184(11) 0.133(4) Uani 1 1 d DU . .
O14 O -0.1857(8) -0.0286(3) -0.1194(10) 0.135(4) Uani 1 1 d DU . .
O15 O 0.9023(3) 0.27869(13) 0.0488(5) 0.0328(11) Uani 1 1 d . . .
O16 O 0.9556(3) 0.23974(14) 0.2367(5) 0.0311(10) Uani 1 1 d . . .
O17 O -0.0995(4) -0.18052(15) 0.2683(6) 0.0512(14) Uani 1 1 d . . .
O18 O -0.1639(3) -0.16733(13) 0.0465(5) 0.0370(11) Uani 1 1 d . . .
O19 O -0.0777(10) 0.1717(5) -0.1248(17) 0.215(6) Uani 1 1 d DU . .
H19 H -0.0354 0.1693 -0.1631 0.323 Uiso 1 1 d R . .
O20 O 0.2394(9) 0.1626(4) 0.5496(14) 0.203(5) Uani 1 1 d DU . .
H20 H 0.2001 0.1602 0.5937 0.304 Uiso 1 1 d R . .
C1 C -0.0071(5) 0.14377(19) 0.3170(7) 0.0322(15) Uani 1 1 d . . .
C2 C -0.0339(5) 0.09978(19) 0.3000(7) 0.0354(15) Uani 1 1 d . . .
C3 C 0.0109(6) 0.0732(2) 0.2369(10) 0.059(2) Uani 1 1 d . . .
H3A H 0.0580 0.0828 0.2045 0.071 Uiso 1 1 calc R . .
C4 C -0.0127(7) 0.0327(2) 0.2207(11) 0.064(3) Uani 1 1 d . . .
H4A H 0.0204 0.0153 0.1810 0.077 Uiso 1 1 calc R . .
C5 C -0.0845(6) 0.0174(2) 0.2622(9) 0.053(2) Uani 1 1 d . . .
C6 C -0.1293(6) 0.0449(2) 0.3251(10) 0.058(2) Uani 1 1 d . B .
C7 C -0.1033(6) 0.0848(2) 0.3455(9) 0.050(2) Uani 1 1 d . . .
H7A H -0.1333 0.1019 0.3911 0.060 Uiso 1 1 calc R . .
C8 C -0.1071(6) -0.0270(2) 0.2398(9) 0.056(2) Uani 1 1 d . . .
C9 C -0.1493(7) -0.0436(2) 0.1104(10) 0.066(3) Uani 1 1 d . . .
C10 C -0.1580(6) -0.0849(2) 0.0882(9) 0.056(2) Uani 1 1 d . . .
H10A H -0.1870 -0.0948 0.0005 0.067 Uiso 1 1 calc R . .
C11 C -0.1239(5) -0.1114(2) 0.1947(8) 0.0428(18) Uani 1 1 d . . .
C12 C -0.0784(7) -0.0957(2) 0.3238(9) 0.062(2) Uani 1 1 d . . .
H12A H -0.0530 -0.1134 0.3966 0.075 Uiso 1 1 calc R . .
C13 C -0.0704(7) -0.0539(2) 0.3452(10) 0.068(3) Uani 1 1 d . . .
H13A H -0.0398 -0.0440 0.4323 0.081 Uiso 1 1 calc R . .
C14 C -0.1290(5) -0.1567(2) 0.1710(8) 0.0389(17) Uani 1 1 d . . .
C15 C 0.2695(4) 0.24767(18) 0.2967(6) 0.0257(13) Uani 1 1 d . . .
C16 C 0.3606(4) 0.2483(2) 0.2704(7) 0.0308(14) Uani 1 1 d . . .
C17 C 0.4182(5) 0.2805(2) 0.3229(8) 0.0436(19) Uani 1 1 d . . .
H17A H 0.4006 0.3008 0.3737 0.052 Uiso 1 1 calc R . .
C18 C 0.5023(5) 0.2820(3) 0.2988(9) 0.049(2) Uani 1 1 d . A .
C19 C 0.5317(4) 0.2522(3) 0.2218(8) 0.0429(18) Uani 1 1 d . . .
C20 C 0.4733(4) 0.2198(2) 0.1760(8) 0.0397(18) Uani 1 1 d . . .
H20A H 0.4913 0.1987 0.1286 0.048 Uiso 1 1 calc R . .
C21 C 0.3888(5) 0.2181(2) 0.1989(8) 0.0414(18) Uani 1 1 d . . .
H21A H 0.3506 0.1962 0.1652 0.050 Uiso 1 1 calc R . .
C22 C 0.6215(4) 0.2534(3) 0.1907(7) 0.0441(19) Uani 1 1 d . . .
C23 C 0.6852(5) 0.2235(3) 0.2470(9) 0.050(2) Uani 1 1 d . . .
H23A H 0.6684 0.2020 0.2942 0.060 Uiso 1 1 calc R . .
C24 C 0.7726(4) 0.2245(2) 0.2354(8) 0.0396(17) Uani 1 1 d . . .
H24A H 0.8140 0.2045 0.2776 0.047 Uiso 1 1 calc R . .
C25 C 0.7988(4) 0.2552(2) 0.1613(7) 0.0315(15) Uani 1 1 d . . .
C26 C 0.7340(4) 0.2844(2) 0.0971(8) 0.0353(16) Uani 1 1 d . . .
H26A H 0.7496 0.3046 0.0438 0.042 Uiso 1 1 calc R . .
C27 C 0.6482(5) 0.2834(2) 0.1116(7) 0.0349(15) Uani 1 1 d U . .
C28 C 0.8938(4) 0.25794(18) 0.1497(6) 0.0251(13) Uani 1 1 d . . .
C29 C -0.1892(18) 0.1332(8) -0.043(3) 0.277(9) Uani 1 1 d DU . .
H29A H -0.1740 0.1514 0.0345 0.416 Uiso 1 1 calc R . .
H29B H -0.1973 0.1062 -0.0125 0.416 Uiso 1 1 calc R . .
H29C H -0.2445 0.1422 -0.1085 0.416 Uiso 1 1 calc R . .
C30 C -0.1134(16) 0.1331(5) -0.111(2) 0.272(9) Uani 1 1 d DU . .
H30A H -0.0640 0.1161 -0.0552 0.326 Uiso 1 1 calc R . .
C31 C -0.148(2) 0.1143(7) -0.253(2) 0.274(8) Uani 1 1 d DU . .
H31A H -0.1020 0.1166 -0.3012 0.329 Uiso 1 1 calc R . .
H31B H -0.2017 0.1290 -0.3063 0.329 Uiso 1 1 calc R . .
C32 C -0.173(2) 0.0690(7) -0.243(3) 0.290(9) Uani 1 1 d DU . .
H32A H -0.1737 0.0553 -0.3271 0.435 Uiso 1 1 calc R . .
H32B H -0.2315 0.0670 -0.2277 0.435 Uiso 1 1 calc R . .
H32C H -0.1281 0.0565 -0.1673 0.435 Uiso 1 1 calc R . .
C33 C 0.2950(14) 0.1237(6) 0.3876(15) 0.203(5) Uani 1 1 d DU . .
H33A H 0.2438 0.1321 0.3131 0.304 Uiso 1 1 calc R . .
H33B H 0.3133 0.0968 0.3693 0.304 Uiso 1 1 calc R . .
H33C H 0.3445 0.1422 0.3957 0.304 Uiso 1 1 calc R . .
C34 C 0.2687(12) 0.1234(6) 0.5211(17) 0.249(7) Uani 1 1 d DU . .
H34A H 0.2193 0.1038 0.5132 0.299 Uiso 1 1 calc R . .
C35 C 0.3510(15) 0.1096(6) 0.6323(17) 0.253(7) Uani 1 1 d DU . .
H35A H 0.3368 0.1090 0.7198 0.304 Uiso 1 1 calc R . .
H35B H 0.3999 0.1290 0.6403 0.304 Uiso 1 1 calc R . .
C36 C 0.3830(18) 0.0678(6) 0.604(3) 0.281(8) Uani 1 1 d DU . .
H36A H 0.4357 0.0603 0.6769 0.421 Uiso 1 1 calc R . .
H36B H 0.3981 0.0684 0.5178 0.421 Uiso 1 1 calc R . .
H36C H 0.3354 0.0484 0.5977 0.421 Uiso 1 1 calc R . .
N1 N -0.2083(9) 0.0326(3) 0.3704(15) 0.117(4) Uani 1 1 d DU . .
N2 N 0.5637(5) 0.3153(3) 0.3628(9) 0.076(2) Uani 1 1 d DU . .
N3 N 0.5843(4) 0.3141(2) 0.0379(8) 0.0580(18) Uani 1 1 d DU . .
N4 N -0.1877(7) -0.0165(3) -0.0070(10) 0.089(3) Uani 1 1 d DU . .


_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 O18 1.914(4) 2 ?
Cu1 O1 1.939(4) . ?
Cu1 O5 1.946(4) . ?
Cu1 O6 1.991(4) 4_566 ?
Cu1 Cu2 2.9983(10) . ?
Cu1 Cu3 3.0046(10) . ?
Cu2 O15 1.923(4) 4_466 ?
Cu2 O3 1.949(4) . ?
Cu2 O1 1.949(4) . ?
Cu2 O6 1.995(4) 4_566 ?
Cu3 O6 1.926(4) . ?
Cu3 O1 1.936(4) . ?
Cu3 O4 2.002(4) . ?
Cu3 O2 2.082(4) . ?
Cu3 O16 2.104(4) 1_455 ?
O1 H1A 0.8498 . ?
O2 C1 1.252(7) . ?
O3 C1 1.275(8) . ?
O4 C15 1.258(7) . ?
O5 C15 1.260(7) . ?
O6 Cu1 1.991(4) 4_565 ?
O6 Cu2 1.995(4) 4_565 ?
O6 H6A 0.8496 . ?
O7 N2 1.196(8) . ?
O8A N2 1.232(9) . ?
O8B N2 1.214(10) . ?
O9 N3 1.208(8) . ?
O10 N3 1.212(9) . ?
O11 N1 1.192(9) . ?
O12A N1 1.210(10) . ?
O12B N1 1.218(10) . ?
O13 N4 1.221(8) . ?
O14 N4 1.212(8) . ?
O15 C28 1.264(7) . ?
O15 Cu2 1.923(4) 4_665 ?
O16 C28 1.246(7) . ?
O16 Cu3 2.104(4) 1_655 ?
O17 C14 1.237(9) . ?
O18 C14 1.268(9) . ?
O18 Cu1 1.914(4) 2_545 ?
O19 C30 1.405(10) . ?
O19 H19 0.8500 . ?
O20 C34 1.422(16) . ?
O20 H20 0.8500 . ?
C1 C2 1.499(9) . ?
C2 C7 1.368(9) . ?
C2 C3 1.376(10) . ?
C3 C4 1.377(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.380(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.394(11) . ?
C5 C8 1.503(10) . ?
C6 C7 1.370(10) . ?
C6 N1 1.469(13) . ?
C7 H7A 0.9300 . ?
C8 C13 1.376(12) . ?
C8 C9 1.394(12) . ?
C9 C10 1.375(11) . ?
C9 N4 1.466(13) . ?
C10 C11 1.368(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.392(12) . ?
C11 C14 1.506(9) . ?
C12 C13 1.390(11) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.497(8) . ?
C16 C21 1.369(9) . ?
C16 C17 1.383(10) . ?
C17 C18 1.381(10) . ?
C17 H17A 0.9300 . ?
C18 C19 1.404(11) . ?
C18 N2 1.466(11) . ?
C19 C20 1.383(10) . ?
C19 C22 1.500(8) . ?
C20 C21 1.382(9) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.388(11) . ?
C22 C27 1.402(10) . ?
C23 C24 1.379(9) . ?
C23 H23A 0.9300 . ?
C24 C25 1.383(9) . ?
C24 H24A 0.9300 . ?
C25 C26 1.400(9) . ?
C25 C28 1.498(8) . ?
C26 C27 1.367(9) . ?
C26 H26A 0.9300 . ?
C27 N3 1.456(10) . ?
C29 C30 1.507(10) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.520(11) . ?
C30 H30A 0.9800 . ?
C31 C32 1.547(10) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.516(10) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.501(10) . ?
C34 H34A 0.9800 . ?
C35 C36 1.512(10) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Cu1 O1 164.8(2) 2 . ?
O18 Cu1 O5 92.10(19) 2 . ?
O1 Cu1 O5 92.68(16) . . ?
O18 Cu1 O6 95.01(17) 2 4_566 ?
O1 Cu1 O6 80.90(15) . 4_566 ?
O5 Cu1 O6 172.65(17) . 4_566 ?
O18 Cu1 Cu2 134.00(14) 2 . ?
O1 Cu1 Cu2 39.68(11) . . ?
O5 Cu1 Cu2 132.34(13) . . ?
O6 Cu1 Cu2 41.26(11) 4_566 . ?
O18 Cu1 Cu3 128.02(15) 2 . ?
O1 Cu1 Cu3 39.13(12) . . ?
O5 Cu1 Cu3 80.53(13) . . ?
O6 Cu1 Cu3 96.48(12) 4_566 . ?
Cu2 Cu1 Cu3 62.71(2) . . ?
O15 Cu2 O3 90.72(17) 4_466 . ?
O15 Cu2 O1 174.49(17) 4_466 . ?
O3 Cu2 O1 94.78(16) . . ?
O15 Cu2 O6 94.00(17) 4_466 4_566 ?
O3 Cu2 O6 172.22(17) . 4_566 ?
O1 Cu2 O6 80.54(15) . 4_566 ?
O15 Cu2 Cu1 135.15(13) 4_466 . ?
O3 Cu2 Cu1 133.66(12) . . ?
O1 Cu2 Cu1 39.41(11) . . ?
O6 Cu2 Cu1 41.17(10) 4_566 . ?
O6 Cu3 O1 170.17(16) . . ?
O6 Cu3 O4 84.45(17) . . ?
O1 Cu3 O4 93.27(17) . . ?
O6 Cu3 O2 100.46(17) . . ?
O1 Cu3 O2 88.83(17) . . ?
O4 Cu3 O2 122.75(18) . . ?
O6 Cu3 O16 90.44(16) . 1_455 ?
O1 Cu3 O16 86.42(16) . 1_455 ?
O4 Cu3 O16 147.88(18) . 1_455 ?
O2 Cu3 O16 89.37(18) . 1_455 ?
O6 Cu3 Cu1 131.14(12) . . ?
O1 Cu3 Cu1 39.18(11) . . ?
O4 Cu3 Cu1 77.18(13) . . ?
O2 Cu3 Cu1 127.59(13) . . ?
O16 Cu3 Cu1 82.65(13) 1_455 . ?
Cu3 O1 Cu1 101.68(18) . . ?
Cu3 O1 Cu2 107.0(2) . . ?
Cu1 O1 Cu2 100.92(16) . . ?
Cu3 O1 H1A 115.2 . . ?
Cu1 O1 H1A 115.1 . . ?
Cu2 O1 H1A 115.2 . . ?
C1 O2 Cu3 128.5(4) . . ?
C1 O3 Cu2 128.3(4) . . ?
C15 O4 Cu3 128.3(4) . . ?
C15 O5 Cu1 126.8(4) . . ?
Cu3 O6 Cu1 109.75(19) . 4_565 ?
Cu3 O6 Cu2 110.51(19) . 4_565 ?
Cu1 O6 Cu2 97.57(16) 4_565 4_565 ?
Cu3 O6 H6A 112.7 . . ?
Cu1 O6 H6A 112.7 4_565 . ?
Cu2 O6 H6A 112.7 4_565 . ?
C28 O15 Cu2 127.3(4) . 4_665 ?
C28 O16 Cu3 131.2(4) . 1_655 ?
C14 O18 Cu1 107.4(4) . 2_545 ?
C30 O19 H19 109.4 . . ?
C34 O20 H20 109.5 . . ?
O2 C1 O3 127.3(6) . . ?
O2 C1 C2 116.8(6) . . ?
O3 C1 C2 115.8(5) . . ?
C7 C2 C3 117.9(6) . . ?
C7 C2 C1 121.6(6) . . ?
C3 C2 C1 120.5(6) . . ?
C2 C3 C4 121.3(7) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 C5 121.5(7) . . ?
C3 C4 H4A 119.3 . . ?
C5 C4 H4A 119.3 . . ?
C4 C5 C6 116.4(7) . . ?
C4 C5 C8 118.6(7) . . ?
C6 C5 C8 125.0(7) . . ?
C7 C6 C5 121.8(7) . . ?
C7 C6 N1 116.5(8) . . ?
C5 C6 N1 121.7(8) . . ?
C2 C7 C6 121.1(7) . . ?
C2 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C13 C8 C9 116.9(7) . . ?
C13 C8 C5 118.8(8) . . ?
C9 C8 C5 123.2(8) . . ?
C10 C9 C8 122.5(8) . . ?
C10 C9 N4 118.0(9) . . ?
C8 C9 N4 119.5(7) . . ?
C11 C10 C9 120.2(8) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 118.6(7) . . ?
C10 C11 C14 120.9(7) . . ?
C12 C11 C14 120.3(7) . . ?
C13 C12 C11 120.7(8) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C8 C13 C12 121.1(9) . . ?
C8 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
O17 C14 O18 124.7(6) . . ?
O17 C14 C11 120.6(7) . . ?
O18 C14 C11 114.7(7) . . ?
O4 C15 O5 126.5(5) . . ?
O4 C15 C16 117.6(5) . . ?
O5 C15 C16 115.9(5) . . ?
C21 C16 C17 119.5(6) . . ?
C21 C16 C15 122.4(6) . . ?
C17 C16 C15 118.1(6) . . ?
C18 C17 C16 119.2(7) . . ?
C18 C17 H17A 120.4 . . ?
C16 C17 H17A 120.4 . . ?
C17 C18 C19 122.4(7) . . ?
C17 C18 N2 117.7(7) . . ?
C19 C18 N2 119.8(6) . . ?
C20 C19 C18 116.3(6) . . ?
C20 C19 C22 119.8(7) . . ?
C18 C19 C22 123.9(7) . . ?
C21 C20 C19 121.6(7) . . ?
C21 C20 H20A 119.2 . . ?
C19 C20 H20A 119.2 . . ?
C16 C21 C20 120.9(7) . . ?
C16 C21 H21A 119.6 . . ?
C20 C21 H21A 119.6 . . ?
C23 C22 C27 116.4(6) . . ?
C23 C22 C19 118.5(7) . . ?
C27 C22 C19 125.1(7) . . ?
C24 C23 C22 122.4(7) . . ?
C24 C23 H23A 118.8 . . ?
C22 C23 H23A 118.8 . . ?
C23 C24 C25 120.3(7) . . ?
C23 C24 H24A 119.8 . . ?
C25 C24 H24A 119.8 . . ?
C24 C25 C26 118.1(6) . . ?
C24 C25 C28 121.8(6) . . ?
C26 C25 C28 120.0(6) . . ?
C27 C26 C25 120.9(6) . . ?
C27 C26 H26A 119.6 . . ?
C25 C26 H26A 119.6 . . ?
C26 C27 C22 121.7(6) . . ?
C26 C27 N3 117.2(6) . . ?
C22 C27 N3 121.1(6) . . ?
O16 C28 O15 126.5(5) . . ?
O16 C28 C25 118.5(5) . . ?
O15 C28 C25 115.1(5) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C29 114.8(15) . . ?
O19 C30 C31 108.2(14) . . ?
C29 C30 C31 108.8(14) . . ?
O19 C30 H30A 108.3 . . ?
C29 C30 H30A 108.3 . . ?
C31 C30 H30A 108.3 . . ?
C30 C31 C32 110.7(14) . . ?
C30 C31 H31A 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O20 C34 C35 111.7(11) . . ?
O20 C34 C33 110.8(10) . . ?
C35 C34 C33 106.7(7) . . ?
O20 C34 H34A 109.2 . . ?
C35 C34 H34A 109.2 . . ?
C33 C34 H34A 109.2 . . ?
C34 C35 C36 112.3(13) . . ?
C34 C35 H35A 109.1 . . ?
C36 C35 H35A 109.1 . . ?
C34 C35 H35B 109.1 . . ?
C36 C35 H35B 109.1 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O11 N1 O12A 109.9(19) . . ?
O11 N1 O12B 113.6(15) . . ?
O12A N1 O12B 66.5(17) . . ?
O11 N1 C6 120.8(12) . . ?
O12A N1 C6 112.8(17) . . ?
O12B N1 C6 120.0(12) . . ?
O7 N2 O8B 99.4(13) . . ?
O7 N2 O8A 115.2(11) . . ?
O8B N2 O8A 74.8(12) . . ?
O7 N2 C18 119.5(8) . . ?
O8B N2 C18 121.2(13) . . ?
O8A N2 C18 117.4(9) . . ?
O9 N3 O10 119.9(8) . . ?
O9 N3 C27 120.4(7) . . ?
O10 N3 C27 118.6(6) . . ?
O14 N4 O13 126.9(11) . . ?
O14 N4 C9 116.7(9) . . ?
O13 N4 C9 116.4(10) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.115
_database_code_depnum_ccdc_archive 'CCDC 977432'
#######################################################################
#
#                 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_521b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C3 H6 O)'
_chemical_formula_sum            'C34 H26 Cu3 N4 O20'
_chemical_formula_weight         1001.21

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   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.3086(19)
_cell_length_b                   32.447(4)
_cell_length_c                   10.0075(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.563(2)
_cell_angle_gamma                90.00
_cell_volume                     4739.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6477
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      27.03

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_T_max  0.8838
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32781
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8194
_reflns_number_gt                6209
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0846P)²+10.7170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8194
_refine_ls_number_parameters     604
_refine_ls_number_restraints     196
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1653
_refine_ls_wR_factor_gt          0.1530
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.65659(3) 0.726758(12) 0.00097(4) 0.02115(10) Uani 1 1 d . . .
Cu2 Cu 0.51068(3) 0.785676(13) 0.02646(4) 0.02289(10) Uani 1 1 d . . .
Cu3 Cu 0.58266(3) 0.783827(13) -0.23571(4) 0.02218(10) Uani 1 1 d . . .
O1 O 0.62112(15) 0.78450(7) -0.0321(2) 0.0202(5) Uani 1 1 d . . .
H1A H 0.6621 0.8021 0.0069 0.024 Uiso 1 1 d R . .
O2 O 0.53200(19) 0.84272(8) -0.2362(3) 0.0396(7) Uani 1 1 d . . .
O3 O 0.46823(17) 0.83957(7) -0.0605(3) 0.0302(6) Uani 1 1 d . . .
O4 O 0.70981(15) 0.77399(8) -0.2453(2) 0.0279(6) Uani 1 1 d . . .
O5 O 0.76668(16) 0.73468(8) -0.0541(3) 0.0304(6) Uani 1 1 d . . .
O6 O 0.54649(15) 0.72613(7) 0.0659(2) 0.0218(6) Uani 1 1 d . . .
H6A H 0.5055 0.7095 0.0198 0.026 Uiso 1 1 d R . .
O7A O 1.14449(13) 0.6880(2) -0.0493(8) 0.0730(19) Uani 0.50 1 d PDU A 1
O7B O 1.1020(2) 0.65911(13) -0.1555(5) 0.114(2) Uani 0.50 1 d PDU A 2
O8 O 1.03119(13) 0.65389(6) -0.0360(3) 0.1265(15) Uani 1 1 d DU A .
O9A O 1.00831(13) 0.68867(18) -0.4525(7) 0.0627(14) Uani 0.50 1 d PDU B 1
O9B O 1.0097(4) 0.6770(3) -0.4085(8) 0.0699(15) Uani 0.50 1 d PDU B 2
O10A O 1.1105(2) 0.65776(12) -0.4958(4) 0.0747(15) Uani 0.50 1 d PDU B 1
O10B O 1.1233(3) 0.64673(8) -0.4239(8) 0.0846(16) Uani 0.50 1 d PDU B 2
O11 O 0.2442(4) 1.00207(18) -0.1645(8) 0.155(2) Uani 1 1 d U C .
O12A O 0.25590(11) 0.94981(7) -0.0426(3) 0.139(4) Uani 0.50 1 d PDU C 1
O12B O 0.3146(9) 0.9677(2) 0.01979(14) 0.151(4) Uani 0.50 1 d PDU C 2
O13A O 0.3362(2) 1.0249(3) -0.6206(3) 0.127(2) Uani 0.50 1 d PDU D 1
O13B O 0.2865(9) 1.0299(3) -0.6434(5) 0.131(2) Uani 0.50 1 d PDU D 2
O14A O 0.2948(3) 0.98030(4) -0.5091(7) 0.0985(16) Uani 0.50 1 d PDU D 1
O14B O 0.26326(11) 0.98888(6) -0.4957(4) 0.1009(19) Uani 0.50 1 d PDU D 2
O15 O 1.40441(16) 0.71830(8) -0.4117(3) 0.0294(6) Uani 1 1 d . . .
O16 O 1.45852(15) 0.75920(8) -0.2233(2) 0.0280(6) Uani 1 1 d . . .
O17 O 0.3986(2) 1.18468(8) -0.2559(3) 0.0411(8) Uani 1 1 d . . .
O18 O 0.33674(18) 1.16844(7) -0.4808(3) 0.0334(7) Uani 1 1 d . . .
O19 O 0.7550(3) 0.83994(13) 0.0844(6) 0.1175(11) Uani 1 1 d DU . .
O20 O 0.4321(3) 0.66656(16) -0.0902(7) 0.1404(13) Uani 1 1 d DU . .
C1 C 0.4892(3) 0.85727(11) -0.1589(4) 0.0304(10) Uani 1 1 d . . .
C2 C 0.4591(3) 0.90112(12) -0.1862(4) 0.0350(10) Uani 1 1 d . . .
C3 C 0.4999(4) 0.92620(14) -0.2612(6) 0.0603(13) Uani 1 1 d . . .
H3A H 0.5446 0.9156 -0.2970 0.072 Uiso 1 1 calc R . .
C4 C 0.4745(4) 0.96697(15) -0.2834(6) 0.0724(16) Uani 1 1 d . . .
H4A H 0.5063 0.9838 -0.3278 0.087 Uiso 1 1 calc R . .
C5 C 0.4039(3) 0.98393(13) -0.2424(5) 0.0505(13) Uani 1 1 d . . .
C6 C 0.3662(4) 0.95834(14) -0.1655(6) 0.0617(11) Uani 1 1 d U C .
C7 C 0.3916(3) 0.91781(13) -0.1365(5) 0.0506(12) Uani 1 1 d . . .
H7A H 0.3637 0.9018 -0.0840 0.061 Uiso 1 1 calc R . .
C8 C 0.3830(4) 1.02849(13) -0.2691(5) 0.0520(14) Uani 1 1 d . . .
C9 C 0.3426(4) 1.04471(15) -0.4017(6) 0.0700(17) Uani 1 1 d U D .
C10 C 0.3360(4) 1.08632(14) -0.4279(5) 0.0588(16) Uani 1 1 d . . .
H10A H 0.3082 1.0958 -0.5185 0.071 Uiso 1 1 calc R . .
C11 C 0.3701(3) 1.11392(12) -0.3220(4) 0.0372(11) Uani 1 1 d . . .
C12 C 0.4092(4) 1.09864(15) -0.1900(5) 0.0710(19) Uani 1 1 d . . .
H12A H 0.4319 1.1168 -0.1157 0.085 Uiso 1 1 calc R . .
C13 C 0.4154(5) 1.05667(15) -0.1654(6) 0.076(2) Uani 1 1 d . . .
H13A H 0.4427 1.0474 -0.0745 0.092 Uiso 1 1 calc R . .
C14 C 0.3690(3) 1.15924(12) -0.3513(4) 0.0319(10) Uani 1 1 d . . .
C15 C 0.7735(2) 0.75367(11) -0.1607(4) 0.0253(9) Uani 1 1 d . . .
C16 C 0.8635(2) 0.75126(13) -0.1869(4) 0.0311(10) Uani 1 1 d . . .
C17 C 0.9195(3) 0.71809(14) -0.1348(4) 0.0401(11) Uani 1 1 d . . .
H17A H 0.9005 0.6977 -0.0844 0.048 Uiso 1 1 calc R . .
C18 C 1.0041(3) 0.71521(16) -0.1575(5) 0.0474(12) Uani 1 1 d . A .
C19 C 1.0355(3) 0.74446(16) -0.2340(4) 0.0435(12) Uani 1 1 d . . .
C20 C 0.9780(3) 0.77843(15) -0.2813(4) 0.0411(11) Uani 1 1 d . . .
H20A H 0.9973 0.7994 -0.3290 0.049 Uiso 1 1 calc R . .
C21 C 0.8936(2) 0.78167(14) -0.2592(4) 0.0372(11) Uani 1 1 d . . .
H21A H 0.8567 0.8045 -0.2930 0.045 Uiso 1 1 calc R . .
C22 C 1.1248(3) 0.74261(16) -0.2637(4) 0.0426(12) Uani 1 1 d . . .
C23 C 1.1875(3) 0.77354(16) -0.2115(5) 0.0495(13) Uani 1 1 d . . .
H23A H 1.1704 0.7956 -0.1656 0.059 Uiso 1 1 calc R . .
C24 C 1.2761(3) 0.77318(14) -0.2247(4) 0.0392(11) Uani 1 1 d . . .
H24A H 1.3174 0.7941 -0.1858 0.047 Uiso 1 1 calc R . .
C25 C 1.3010(2) 0.74120(13) -0.2963(4) 0.0300(9) Uani 1 1 d . . .
C26 C 1.2378(3) 0.71079(14) -0.3565(4) 0.0378(11) Uani 1 1 d . . .
H26A H 1.2538 0.6898 -0.4079 0.045 Uiso 1 1 calc R . .
C27 C 1.1521(3) 0.71150(15) -0.3408(4) 0.0428(12) Uani 1 1 d . B .
C28 C 1.3960(2) 0.73949(11) -0.3107(4) 0.0240(8) Uani 1 1 d . . .
C29 C 0.7729(7) 0.8798(3) -0.1042(7) 0.1430(19) Uani 1 1 d DU . .
H29A H 0.7295 0.8603 -0.1590 0.215 Uiso 1 1 calc R . .
H29B H 0.8293 0.8776 -0.1272 0.215 Uiso 1 1 calc R . .
H29C H 0.7488 0.9071 -0.1242 0.215 Uiso 1 1 calc R . .
C30 C 0.7907(5) 0.87056(19) 0.0507(6) 0.1301(13) Uani 1 1 d DU . .
C31 C 0.8545(6) 0.8950(3) 0.1699(9) 0.1393(19) Uani 1 1 d DU . .
H31A H 0.8556 0.8828 0.2578 0.209 Uiso 1 1 calc R . .
H31B H 0.8331 0.9229 0.1665 0.209 Uiso 1 1 calc R . .
H31C H 0.9152 0.8948 0.1609 0.209 Uiso 1 1 calc R . .
C32 C 0.3709(8) 0.6114(3) -0.2197(10) 0.163(2) Uani 1 1 d DU . .
H32A H 0.4166 0.6196 -0.2624 0.245 Uiso 1 1 calc R . .
H32B H 0.3115 0.6124 -0.2882 0.245 Uiso 1 1 calc R . .
H32C H 0.3833 0.5838 -0.1844 0.245 Uiso 1 1 calc R . .
C33 C 0.3732(3) 0.6407(2) -0.0989(7) 0.1499(13) Uani 1 1 d DU . .
C34 C 0.3058(4) 0.6320(4) -0.0183(8) 0.161(2) Uani 1 1 d DU . .
H34A H 0.3124 0.6526 0.0531 0.242 Uiso 1 1 calc R . .
H34B H 0.3179 0.6053 0.0243 0.242 Uiso 1 1 calc R . .
H34C H 0.2445 0.6328 -0.0813 0.242 Uiso 1 1 calc R . .
N1 N 0.2915(2) 0.97287(11) -0.10581(16) 0.1099(16) Uani 1 1 d DU . .
N2 N 1.06230(13) 0.68118(8) -0.0938(3) 0.0775(12) Uani 1 1 d DU . .
N3 N 1.08790(14) 0.67917(9) -0.4138(4) 0.0602(12) Uani 1 1 d DU . .
N4 N 0.30807(19) 1.01687(5) -0.5238(3) 0.0932(16) Uani 1 1 d DU . .


_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 O18 1.909(2) 2_644 ?
Cu1 O5 1.941(3) . ?
Cu1 O1 1.951(2) . ?
Cu1 O6 1.981(2) . ?
Cu1 O4 2.422(2) 4_576 ?
Cu1 Cu3 2.9499(6) . ?
Cu1 Cu2 3.0088(6) . ?
Cu2 O15 1.911(3) 4_476 ?
Cu2 O1 1.949(2) . ?
Cu2 O3 1.974(2) . ?
Cu2 O6 2.015(2) . ?
Cu3 O6 1.921(2) 4_575 ?
Cu3 O1 1.943(2) . ?
Cu3 O4 2.003(2) . ?
Cu3 O2 2.062(3) . ?
Cu3 O16 2.100(2) 1_455 ?
O1 H1A 0.8501 . ?
O2 C1 1.248(5) . ?
O3 C1 1.262(5) . ?
O4 C15 1.267(4) . ?
O4 Cu1 2.422(2) 4_575 ?
O5 C15 1.264(4) . ?
O6 Cu3 1.921(2) 4_576 ?
O6 H6A 0.8500 . ?
O7A N2 1.2217(19) . ?
O7B N2 1.220(2) . ?
O8 N2 1.2295(11) . ?
O9A N3 1.2019(19) . ?
O9B N3 1.216(7) . ?
O10A N3 1.202(2) . ?
O10B N3 1.202(2) . ?
O11 N1 1.229(6) . ?
O12A N1 1.2103(11) . ?
O12B N1 1.2104(10) . ?
O13A N4 1.202(2) . ?
O13B N4 1.217(4) . ?
O14A N4 1.2199(10) . ?
O14B N4 1.2207(11) . ?
O15 C28 1.260(4) . ?
O15 Cu2 1.911(3) 4_675 ?
O16 C28 1.259(4) . ?
O16 Cu3 2.100(2) 1_655 ?
O17 C14 1.240(5) . ?
O18 C14 1.275(4) . ?
O18 Cu1 1.909(2) 2_654 ?
O19 C30 1.229(5) . ?
O20 C33 1.216(5) . ?
C1 C2 1.495(5) . ?
C2 C3 1.377(6) . ?
C2 C7 1.385(6) . ?
C3 C4 1.378(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.373(7) . ?
C5 C8 1.487(6) . ?
C6 C7 1.377(6) . ?
C6 N1 1.517(7) . ?
C7 H7A 0.9300 . ?
C8 C13 1.359(7) . ?
C8 C9 1.388(7) . ?
C9 C10 1.373(7) . ?
C9 N4 1.483(6) . ?
C10 C11 1.365(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.368(6) . ?
C11 C14 1.498(5) . ?
C12 C13 1.382(7) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.480(5) . ?
C16 C17 1.377(6) . ?
C16 C21 1.382(6) . ?
C17 C18 1.384(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.393(7) . ?
C18 N2 1.441(5) . ?
C19 C20 1.401(6) . ?
C19 C22 1.485(6) . ?
C20 C21 1.379(6) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.379(6) . ?
C22 C27 1.409(7) . ?
C23 C24 1.402(6) . ?
C23 H23A 0.9300 . ?
C24 C25 1.379(6) . ?
C24 H24A 0.9300 . ?
C25 C26 1.386(5) . ?
C25 C28 1.505(5) . ?
C26 C27 1.368(6) . ?
C26 H26A 0.9300 . ?
C27 N3 1.472(5) . ?
C29 C30 1.521(7) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.518(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.531(11) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.515(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Cu1 O5 91.28(12) 2_644 . ?
O18 Cu1 O1 162.75(10) 2_644 . ?
O5 Cu1 O1 92.63(10) . . ?
O18 Cu1 O6 95.89(11) 2_644 . ?
O5 Cu1 O6 172.59(10) . . ?
O1 Cu1 O6 81.06(10) . . ?
O18 Cu1 O4 95.12(10) 2_644 4_576 ?
O5 Cu1 O4 104.63(9) . 4_576 ?
O1 Cu1 O4 100.12(9) . 4_576 ?
O6 Cu1 O4 72.92(8) . 4_576 ?
O18 Cu1 Cu3 123.85(8) 2_644 . ?
O5 Cu1 Cu3 81.07(7) . . ?
O1 Cu1 Cu3 40.66(7) . . ?
O6 Cu1 Cu3 96.40(6) . . ?
O4 Cu1 Cu3 140.75(6) 4_576 . ?
O18 Cu1 Cu2 134.71(8) 2_644 . ?
O5 Cu1 Cu2 132.08(8) . . ?
O1 Cu1 Cu2 39.50(7) . . ?
O6 Cu1 Cu2 41.57(7) . . ?
O4 Cu1 Cu2 86.61(6) 4_576 . ?
Cu3 Cu1 Cu2 63.543(15) . . ?
O15 Cu2 O1 174.82(10) 4_476 . ?
O15 Cu2 O3 90.19(11) 4_476 . ?
O1 Cu2 O3 94.88(10) . . ?
O15 Cu2 O6 94.57(10) 4_476 . ?
O1 Cu2 O6 80.25(9) . . ?
O3 Cu2 O6 165.91(10) . . ?
O15 Cu2 Cu1 135.29(8) 4_476 . ?
O1 Cu2 Cu1 39.53(6) . . ?
O3 Cu2 Cu1 132.81(8) . . ?
O6 Cu2 Cu1 40.73(7) . . ?
O6 Cu3 O1 170.94(10) 4_575 . ?
O6 Cu3 O4 84.54(10) 4_575 . ?
O1 Cu3 O4 93.48(9) . . ?
O6 Cu3 O2 99.35(10) 4_575 . ?
O1 Cu3 O2 89.25(10) . . ?
O4 Cu3 O2 121.18(11) . . ?
O6 Cu3 O16 90.77(9) 4_575 1_455 ?
O1 Cu3 O16 86.29(9) . 1_455 ?
O4 Cu3 O16 148.45(10) . 1_455 ?
O2 Cu3 O16 90.37(11) . 1_455 ?
O6 Cu3 Cu1 130.20(7) 4_575 . ?
O1 Cu3 Cu1 40.85(7) . . ?
O4 Cu3 Cu1 78.20(7) . . ?
O2 Cu3 Cu1 129.55(8) . . ?
O16 Cu3 Cu1 81.28(7) 1_455 . ?
Cu3 O1 Cu2 107.43(10) . . ?
Cu3 O1 Cu1 98.49(10) . . ?
Cu2 O1 Cu1 100.97(10) . . ?
Cu3 O1 H1A 115.9 . . ?
Cu2 O1 H1A 115.9 . . ?
Cu1 O1 H1A 115.9 . . ?
C1 O2 Cu3 128.1(2) . . ?
C1 O3 Cu2 128.3(2) . . ?
C15 O4 Cu3 127.9(2) . . ?
C15 O4 Cu1 130.0(2) . 4_575 ?
Cu3 O4 Cu1 91.58(8) . 4_575 ?
C15 O5 Cu1 127.2(2) . . ?
Cu3 O6 Cu1 109.41(10) 4_576 . ?
Cu3 O6 Cu2 109.90(11) 4_576 . ?
Cu1 O6 Cu2 97.70(10) . . ?
Cu3 O6 H6A 112.9 4_576 . ?
Cu1 O6 H6A 112.9 . . ?
Cu2 O6 H6A 113.0 . . ?
C28 O15 Cu2 126.8(2) . 4_675 ?
C28 O16 Cu3 131.6(2) . 1_655 ?
C14 O18 Cu1 108.9(2) . 2_654 ?
O2 C1 O3 128.1(3) . . ?
O2 C1 C2 115.9(3) . . ?
O3 C1 C2 116.0(3) . . ?
C3 C2 C7 118.3(4) . . ?
C3 C2 C1 119.7(4) . . ?
C7 C2 C1 121.9(4) . . ?
C2 C3 C4 120.2(5) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 C5 122.9(5) . . ?
C3 C4 H4A 118.6 . . ?
C5 C4 H4A 118.6 . . ?
C6 C5 C4 115.1(4) . . ?
C6 C5 C8 125.8(5) . . ?
C4 C5 C8 118.6(5) . . ?
C5 C6 C7 123.8(5) . . ?
C5 C6 N1 121.8(4) . . ?
C7 C6 N1 114.4(5) . . ?
C6 C7 C2 119.5(5) . . ?
C6 C7 H7A 120.3 . . ?
C2 C7 H7A 120.3 . . ?
C13 C8 C9 115.4(4) . . ?
C13 C8 C5 120.5(4) . . ?
C9 C8 C5 123.3(4) . . ?
C10 C9 C8 122.8(5) . . ?
C10 C9 N4 117.0(4) . . ?
C8 C9 N4 120.2(4) . . ?
C11 C10 C9 120.5(5) . . ?
C11 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
C10 C11 C12 117.7(4) . . ?
C10 C11 C14 120.9(4) . . ?
C12 C11 C14 121.4(4) . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C8 C13 C12 122.5(5) . . ?
C8 C13 H13A 118.8 . . ?
C12 C13 H13A 118.8 . . ?
O17 C14 O18 124.5(3) . . ?
O17 C14 C11 121.5(3) . . ?
O18 C14 C11 114.0(3) . . ?
O5 C15 O4 125.1(3) . . ?
O5 C15 C16 116.3(3) . . ?
O4 C15 C16 118.6(3) . . ?
C17 C16 C21 119.2(4) . . ?
C17 C16 C15 118.7(4) . . ?
C21 C16 C15 122.0(3) . . ?
C16 C17 C18 119.8(4) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 122.7(4) . . ?
C17 C18 N2 117.6(4) . . ?
C19 C18 N2 119.7(4) . . ?
C18 C19 C20 115.8(4) . . ?
C18 C19 C22 125.0(4) . . ?
C20 C19 C22 119.1(4) . . ?
C21 C20 C19 121.9(4) . . ?
C21 C20 H20A 119.0 . . ?
C19 C20 H20A 119.0 . . ?
C20 C21 C16 120.4(4) . . ?
C20 C21 H21A 119.8 . . ?
C16 C21 H21A 119.8 . . ?
C23 C22 C27 116.2(4) . . ?
C23 C22 C19 118.2(4) . . ?
C27 C22 C19 125.6(4) . . ?
C22 C23 C24 122.8(4) . . ?
C22 C23 H23A 118.6 . . ?
C24 C23 H23A 118.6 . . ?
C25 C24 C23 118.8(4) . . ?
C25 C24 H24A 120.6 . . ?
C23 C24 H24A 120.6 . . ?
C24 C25 C26 119.7(4) . . ?
C24 C25 C28 120.3(3) . . ?
C26 C25 C28 120.0(3) . . ?
C27 C26 C25 120.4(4) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C22 121.9(4) . . ?
C26 C27 N3 116.8(4) . . ?
C22 C27 N3 121.2(3) . . ?
O16 C28 O15 126.5(3) . . ?
O16 C28 C25 117.9(3) . . ?
O15 C28 C25 115.6(3) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C31 116.2(6) . . ?
O19 C30 C29 118.7(6) . . ?
C31 C30 C29 124.9(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O20 C33 C34 134.3(8) . . ?
O20 C33 C32 109.0(7) . . ?
C34 C33 C32 116.7(7) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O12A N1 O12B 53.7(5) . . ?
O12A N1 O11 115.7(5) . . ?
O12B N1 O11 123.4(7) . . ?
O12A N1 C6 121.7(4) . . ?
O12B N1 C6 110.3(7) . . ?
O11 N1 C6 117.2(4) . . ?
O7B N2 O7A 71.1(4) . . ?
O7B N2 O8 98.0(3) . . ?
O7A N2 O8 117.5(4) . . ?
O7B N2 C18 124.2(3) . . ?
O7A N2 C18 117.0(4) . . ?
O8 N2 C18 118.9(3) . . ?
O10B N3 O9A 129.5(4) . . ?
O10B N3 O10A 37.5(4) . . ?
O9A N3 O10A 113.6(5) . . ?
O10B N3 O9B 115.3(5) . . ?
O9A N3 O9B 27.6(5) . . ?
O10A N3 O9B 119.1(5) . . ?
O10B N3 C27 114.6(3) . . ?
O9A N3 C27 115.9(4) . . ?
O10A N3 C27 117.7(3) . . ?
O9B N3 C27 122.5(5) . . ?
O13A N4 O14A 114.9(6) . . ?
O13A N4 O14B 135.2(5) . . ?
O14A N4 O14B 28.8(3) . . ?
O13A N4 O13B 35.8(7) . . ?
O14A N4 O13B 116.7(6) . . ?
O14B N4 O13B 118.7(6) . . ?
O13A N4 C9 114.0(4) . . ?
O14A N4 C9 121.6(4) . . ?
O14B N4 C9 110.4(3) . . ?
O13B N4 C9 121.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.103
_database_code_depnum_ccdc_archive 'CCDC 977433'
#######################################################################
#
#                 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_522

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C3 H6 O)'
_chemical_formula_sum            'C34 H26 Cu3 N4 O20'
_chemical_formula_weight         1001.21

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   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.317(4)
_cell_length_b                   32.467(9)
_cell_length_c                   10.015(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.510(3)
_cell_angle_gamma                90.00
_cell_volume                     4750(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5532
_cell_measurement_theta_min      1.26
_cell_measurement_theta_max      26.98

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8065
_exptl_absorpt_correction_T_max  0.8723
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32942
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8217
_reflns_number_gt                5979
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0830P)²+5.2111P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8217
_refine_ls_number_parameters     604
_refine_ls_number_restraints     224
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1648
_refine_ls_wR_factor_gt          0.1521
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.65443(4) 0.726722(18) 0.00032(6) 0.02060(18) Uani 1 1 d . . .
Cu2 Cu 0.50863(4) 0.785652(18) 0.02590(6) 0.02219(18) Uani 1 1 d . . .
Cu3 Cu 0.58059(4) 0.783819(18) -0.23623(6) 0.02140(18) Uani 1 1 d . . .
O1 O 0.6186(2) 0.78446(9) -0.0335(3) 0.0189(7) Uani 1 1 d . . .
H1A H 0.6596 0.8020 0.0053 0.023 Uiso 1 1 d R . .
O2 O 0.5295(3) 0.84270(11) -0.2368(4) 0.0374(10) Uani 1 1 d . . .
O3 O 0.4658(3) 0.83957(10) -0.0608(4) 0.0290(8) Uani 1 1 d . . .
O4 O 0.7082(2) 0.77411(11) -0.2460(4) 0.0274(8) Uani 1 1 d . . .
O5 O 0.7646(2) 0.73478(11) -0.0548(4) 0.0294(8) Uani 1 1 d . . .
O6 O 0.5448(2) 0.72619(10) 0.0658(3) 0.0201(7) Uani 1 1 d . . .
H6A H 0.5039 0.7096 0.0198 0.024 Uiso 1 1 d R . .
O7A O 1.0958(8) 0.6579(4) -0.1570(12) 0.090(3) Uani 0.50 1 d PDU A 1
O7B O 1.1425(5) 0.6879(4) -0.0495(12) 0.077(3) Uani 0.50 1 d PDU A 2
O8 O 1.0277(5) 0.6544(2) -0.0393(10) 0.133(3) Uani 1 1 d DU . .
O9A O 1.1094(9) 0.6566(4) -0.4946(13) 0.065(3) Uani 0.50 1 d PDU A 1
O9B O 1.1198(11) 0.6459(4) -0.425(2) 0.100(5) Uani 0.50 1 d PDU A 2
O10 O 1.0045(4) 0.6844(2) -0.4363(7) 0.0909(19) Uani 1 1 d DU A .
O11A O 0.3134(14) 0.9681(7) 0.0111(15) 0.149(5) Uani 0.50 1 d PDU B 1
O11B O 0.2508(14) 0.9495(5) -0.055(2) 0.147(5) Uani 0.50 1 d PDU B 2
O12A O 0.2338(10) 0.9970(4) -0.1931(15) 0.099(4) Uani 0.50 1 d PDU B 1
O12B O 0.2584(11) 1.0083(3) -0.1233(17) 0.100(4) Uani 0.50 1 d PDU B 2
O13A O 0.3309(11) 1.0271(4) -0.6278(12) 0.092(4) Uani 0.50 1 d PDU C 1
O13B O 0.2632(12) 1.0322(5) -0.6347(15) 0.127(5) Uani 0.50 1 d PDU C 2
O14A O 0.2902(11) 0.9810(3) -0.5129(19) 0.093(4) Uani 0.50 1 d PDU C 1
O14B O 0.2620(11) 0.9905(4) -0.495(2) 0.104(5) Uani 0.50 1 d PDU C 2
O15 O 1.4022(2) 0.71842(11) -0.4124(4) 0.0283(8) Uani 1 1 d . . .
O16 O 1.4561(2) 0.75955(11) -0.2244(4) 0.0278(8) Uani 1 1 d . . .
O17 O 0.4002(3) 1.18477(11) -0.2558(4) 0.0387(10) Uani 1 1 d . . .
O18 O 0.3380(3) 1.16861(10) -0.4801(4) 0.0328(9) Uani 1 1 d . . .
O19 O 0.7539(5) 0.8398(2) 0.0839(8) 0.112(2) Uani 1 1 d U . .
O20 O 0.4298(6) 0.6672(3) -0.0896(10) 0.137(3) Uani 1 1 d DU . .
C1 C 0.4867(4) 0.85720(16) -0.1595(6) 0.0300(12) Uani 1 1 d . . .
C2 C 0.4574(4) 0.90124(16) -0.1862(6) 0.0329(13) Uani 1 1 d . . .
C3 C 0.4981(6) 0.9263(2) -0.2616(8) 0.061(2) Uani 1 1 d . . .
H3A H 0.5424 0.9155 -0.2980 0.074 Uiso 1 1 calc R . .
C4 C 0.4735(6) 0.9669(2) -0.2829(9) 0.067(2) Uani 1 1 d . . .
H4A H 0.5052 0.9836 -0.3277 0.081 Uiso 1 1 calc R . .
C5 C 0.4041(5) 0.98384(19) -0.2408(7) 0.0492(17) Uani 1 1 d . . .
C6 C 0.3647(6) 0.9589(2) -0.1639(8) 0.0592(19) Uani 1 1 d U B .
C7 C 0.3901(5) 0.91796(19) -0.1361(7) 0.0495(18) Uani 1 1 d . . .
H7A H 0.3621 0.9018 -0.0841 0.059 Uiso 1 1 calc R . .
C8 C 0.3830(5) 1.02898(19) -0.2675(7) 0.0494(17) Uani 1 1 d . . .
C9 C 0.3443(6) 1.04497(19) -0.4005(8) 0.064(2) Uani 1 1 d . C .
C10 C 0.3364(5) 1.08666(19) -0.4271(8) 0.062(2) Uani 1 1 d . . .
H10A H 0.3077 1.0962 -0.5171 0.074 Uiso 1 1 calc R . .
C11 C 0.3713(4) 1.11384(17) -0.3197(6) 0.0364(14) Uani 1 1 d . . .
C12 C 0.4095(6) 1.0986(2) -0.1910(7) 0.063(2) Uani 1 1 d . . .
H12A H 0.4329 1.1167 -0.1168 0.076 Uiso 1 1 calc R . .
C13 C 0.4149(6) 1.0565(2) -0.1654(8) 0.067(2) Uani 1 1 d . . .
H13A H 0.4415 1.0472 -0.0744 0.080 Uiso 1 1 calc R . .
C14 C 0.3703(4) 1.15934(16) -0.3502(6) 0.0303(12) Uani 1 1 d . . .
C15 C 0.7713(3) 0.75340(16) -0.1613(5) 0.0245(11) Uani 1 1 d . . .
C16 C 0.8601(4) 0.75134(17) -0.1877(5) 0.0294(12) Uani 1 1 d . . .
C17 C 0.9173(4) 0.7177(2) -0.1349(6) 0.0399(15) Uani 1 1 d . A .
H17A H 0.8983 0.6972 -0.0852 0.048 Uiso 1 1 calc R . .
C18 C 1.0016(4) 0.7151(2) -0.1568(7) 0.0478(17) Uani 1 1 d . . .
C19 C 1.0330(4) 0.7444(2) -0.2347(6) 0.0424(16) Uani 1 1 d . A .
C20 C 0.9763(4) 0.7779(2) -0.2820(6) 0.0398(15) Uani 1 1 d . . .
H20A H 0.9958 0.7985 -0.3306 0.048 Uiso 1 1 calc R A .
C21 C 0.8919(4) 0.78187(19) -0.2601(6) 0.0372(14) Uani 1 1 d . A .
H21A H 0.8561 0.8050 -0.2935 0.045 Uiso 1 1 calc R . .
C22 C 1.1232(4) 0.7427(2) -0.2647(6) 0.0422(15) Uani 1 1 d . . .
C23 C 1.1860(4) 0.7735(2) -0.2115(7) 0.0472(17) Uani 1 1 d . A .
H23A H 1.1688 0.7955 -0.1655 0.057 Uiso 1 1 calc R . .
C24 C 1.2735(4) 0.7729(2) -0.2238(6) 0.0386(14) Uani 1 1 d . . .
H24A H 1.3150 0.7936 -0.1837 0.046 Uiso 1 1 calc R A .
C25 C 1.2985(4) 0.74106(17) -0.2965(5) 0.0294(12) Uani 1 1 d . A .
C26 C 1.2358(4) 0.71104(19) -0.3571(6) 0.0347(13) Uani 1 1 d . . .
H26A H 1.2522 0.6901 -0.4084 0.042 Uiso 1 1 calc R A .
C27 C 1.1502(4) 0.7115(2) -0.3431(6) 0.0385(14) Uani 1 1 d . A .
C28 C 1.3936(3) 0.73946(15) -0.3112(5) 0.0231(11) Uani 1 1 d . . .
C29 C 0.7687(9) 0.8811(4) -0.1083(12) 0.137(3) Uani 1 1 d DU . .
H29A H 0.7267 0.8616 -0.1653 0.206 Uiso 1 1 calc R . .
H29B H 0.8250 0.8806 -0.1319 0.206 Uiso 1 1 calc R . .
H29C H 0.7426 0.9082 -0.1245 0.206 Uiso 1 1 calc R . .
C30 C 0.7878(8) 0.8698(4) 0.0466(11) 0.124(2) Uani 1 1 d DU . .
C31 C 0.8508(8) 0.8960(4) 0.1641(13) 0.133(3) Uani 1 1 d DU . .
H31A H 0.8528 0.8845 0.2532 0.200 Uiso 1 1 calc R . .
H31B H 0.8277 0.9236 0.1578 0.200 Uiso 1 1 calc R . .
H31C H 0.9114 0.8963 0.1547 0.200 Uiso 1 1 calc R . .
C32 C 0.3710(10) 0.6129(4) -0.2290(14) 0.159(3) Uani 1 1 d DU . .
H32A H 0.4142 0.6231 -0.2733 0.239 Uiso 1 1 calc R . .
H32B H 0.3107 0.6131 -0.2950 0.239 Uiso 1 1 calc R . .
H32C H 0.3872 0.5852 -0.1972 0.239 Uiso 1 1 calc R . .
C33 C 0.3724(8) 0.6404(4) -0.1035(14) 0.145(3) Uani 1 1 d DU . .
C34 C 0.3060(9) 0.6277(4) -0.0249(15) 0.157(3) Uani 1 1 d DU . .
H34A H 0.3110 0.6465 0.0512 0.236 Uiso 1 1 calc R . .
H34B H 0.3203 0.6004 0.0113 0.236 Uiso 1 1 calc R . .
H34C H 0.2446 0.6284 -0.0874 0.236 Uiso 1 1 calc R . .
N1 N 0.2874(7) 0.9735(3) -0.1166(11) 0.113(3) Uani 1 1 d DU . .
N2 N 1.0602(4) 0.6815(2) -0.0937(7) 0.0700(18) Uani 1 1 d DU A .
N3 N 1.0859(4) 0.6795(2) -0.4143(7) 0.0607(16) Uani 1 1 d DU . .
N4 N 0.3087(6) 1.0170(2) -0.5250(9) 0.093(2) Uani 1 1 d DU . .


_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 O18 1.905(3) 2_644 ?
Cu1 O5 1.944(3) . ?
Cu1 O1 1.954(3) . ?
Cu1 O6 1.978(3) . ?
Cu1 O4 2.423(4) 4_576 ?
Cu1 Cu3 2.9523(10) . ?
Cu1 Cu2 3.0096(10) . ?
Cu2 O15 1.914(3) 4_476 ?
Cu2 O1 1.949(3) . ?
Cu2 O3 1.976(3) . ?
Cu2 O6 2.015(3) . ?
Cu3 O6 1.920(3) 4_575 ?
Cu3 O1 1.937(3) . ?
Cu3 O4 2.012(3) . ?
Cu3 O2 2.065(4) . ?
Cu3 O16 2.099(3) 1_455 ?
O1 H1A 0.8499 . ?
O2 C1 1.248(7) . ?
O3 C1 1.263(6) . ?
O4 C15 1.270(6) . ?
O4 Cu1 2.423(4) 4_575 ?
O5 C15 1.257(6) . ?
O6 Cu3 1.920(3) 4_576 ?
O6 H6A 0.8500 . ?
O7A N2 1.221(2) . ?
O7A O8 1.797(13) . ?
O7B N2 1.222(2) . ?
O8 N2 1.218(2) . ?
O9A N3 1.227(11) . ?
O9B N3 1.227(14) . ?
O10 N3 1.209(7) . ?
O11A N1 1.233(10) . ?
O11B N1 1.226(10) . ?
O12A N1 1.2105(11) . ?
O12B N1 1.2099(11) . ?
O13A N4 1.2206(11) . ?
O13B N4 1.215(9) . ?
O14A N4 1.2200(11) . ?
O14B N4 1.213(2) . ?
O15 C28 1.262(6) . ?
O15 Cu2 1.914(3) 4_675 ?
O16 C28 1.264(6) . ?
O16 Cu3 2.099(3) 1_655 ?
O17 C14 1.234(6) . ?
O18 C14 1.281(7) . ?
O18 Cu1 1.905(3) 2_654 ?
O19 C30 1.215(12) . ?
O20 C33 1.213(5) . ?
C1 C2 1.499(7) . ?
C2 C3 1.379(8) . ?
C2 C7 1.385(8) . ?
C3 C4 1.371(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.372(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.375(10) . ?
C5 C8 1.507(8) . ?
C6 C7 1.391(9) . ?
C6 N1 1.479(11) . ?
C7 H7A 0.9300 . ?
C8 C13 1.335(9) . ?
C8 C9 1.385(10) . ?
C9 C10 1.378(9) . ?
C9 N4 1.505(10) . ?
C10 C11 1.369(9) . ?
C10 H10A 0.9300 . ?
C11 C12 1.340(9) . ?
C11 C14 1.508(8) . ?
C12 C13 1.388(9) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.464(7) . ?
C16 C21 1.399(8) . ?
C16 C17 1.400(8) . ?
C17 C18 1.376(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.405(9) . ?
C18 N2 1.433(9) . ?
C19 C20 1.382(9) . ?
C19 C22 1.501(8) . ?
C20 C21 1.381(8) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.380(9) . ?
C22 C27 1.418(9) . ?
C23 C24 1.383(8) . ?
C23 H23A 0.9300 . ?
C24 C25 1.382(8) . ?
C24 H24A 0.9300 . ?
C25 C26 1.375(8) . ?
C25 C28 1.507(7) . ?
C26 C27 1.360(8) . ?
C26 H26A 0.9300 . ?
C27 N3 1.460(8) . ?
C29 C30 1.534(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.536(4) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.538(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.5197(11) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Cu1 O5 90.99(16) 2_644 . ?
O18 Cu1 O1 162.71(15) 2_644 . ?
O5 Cu1 O1 92.51(14) . . ?
O18 Cu1 O6 96.40(15) 2_644 . ?
O5 Cu1 O6 172.33(15) . . ?
O1 Cu1 O6 81.03(13) . . ?
O18 Cu1 O4 95.05(14) 2_644 4_576 ?
O5 Cu1 O4 104.39(14) . 4_576 ?
O1 Cu1 O4 100.46(13) . 4_576 ?
O6 Cu1 O4 72.99(12) . 4_576 ?
O18 Cu1 Cu3 123.88(12) 2_644 . ?
O5 Cu1 Cu3 80.99(11) . . ?
O1 Cu1 Cu3 40.42(9) . . ?
O6 Cu1 Cu3 96.49(10) . . ?
O4 Cu1 Cu3 140.85(9) 4_576 . ?
O18 Cu1 Cu2 135.17(12) 2_644 . ?
O5 Cu1 Cu2 131.93(11) . . ?
O1 Cu1 Cu2 39.48(9) . . ?
O6 Cu1 Cu2 41.55(9) . . ?
O4 Cu1 Cu2 86.84(8) 4_576 . ?
Cu3 Cu1 Cu2 63.53(2) . . ?
O15 Cu2 O1 174.80(14) 4_476 . ?
O15 Cu2 O3 90.05(15) 4_476 . ?
O1 Cu2 O3 94.95(14) . . ?
O15 Cu2 O6 94.59(14) 4_476 . ?
O1 Cu2 O6 80.22(13) . . ?
O3 Cu2 O6 166.11(14) . . ?
O15 Cu2 Cu1 135.20(11) 4_476 . ?
O1 Cu2 Cu1 39.60(9) . . ?
O3 Cu2 Cu1 133.01(10) . . ?
O6 Cu2 Cu1 40.62(9) . . ?
O6 Cu3 O1 170.85(13) 4_575 . ?
O6 Cu3 O4 84.42(14) 4_575 . ?
O1 Cu3 O4 93.59(14) . . ?
O6 Cu3 O2 99.42(15) 4_575 . ?
O1 Cu3 O2 89.27(14) . . ?
O4 Cu3 O2 121.19(16) . . ?
O6 Cu3 O16 90.73(13) 4_575 1_455 ?
O1 Cu3 O16 86.38(13) . 1_455 ?
O4 Cu3 O16 148.93(15) . 1_455 ?
O2 Cu3 O16 89.88(15) . 1_455 ?
O6 Cu3 Cu1 130.10(10) 4_575 . ?
O1 Cu3 Cu1 40.86(9) . . ?
O4 Cu3 Cu1 78.32(10) . . ?
O2 Cu3 Cu1 129.56(11) . . ?
O16 Cu3 Cu1 81.61(10) 1_455 . ?
Cu3 O1 Cu2 107.76(15) . . ?
Cu3 O1 Cu1 98.72(14) . . ?
Cu2 O1 Cu1 100.91(14) . . ?
Cu3 O1 H1A 115.7 . . ?
Cu2 O1 H1A 115.7 . . ?
Cu1 O1 H1A 115.7 . . ?
C1 O2 Cu3 128.1(3) . . ?
C1 O3 Cu2 128.1(3) . . ?
C15 O4 Cu3 127.2(3) . . ?
C15 O4 Cu1 130.2(3) . 4_575 ?
Cu3 O4 Cu1 91.37(13) . 4_575 ?
C15 O5 Cu1 127.2(3) . . ?
Cu3 O6 Cu1 109.68(16) 4_576 . ?
Cu3 O6 Cu2 110.05(15) 4_576 . ?
Cu1 O6 Cu2 97.82(14) . . ?
Cu3 O6 H6A 112.8 4_576 . ?
Cu1 O6 H6A 112.8 . . ?
Cu2 O6 H6A 112.8 . . ?
N2 O7A O8 42.5(5) . . ?
N2 O8 O7A 42.6(5) . . ?
C28 O15 Cu2 127.0(3) . 4_675 ?
C28 O16 Cu3 131.9(3) . 1_655 ?
C14 O18 Cu1 108.9(3) . 2_654 ?
O2 C1 O3 128.2(5) . . ?
O2 C1 C2 115.7(5) . . ?
O3 C1 C2 116.1(5) . . ?
C3 C2 C7 118.4(5) . . ?
C3 C2 C1 119.9(5) . . ?
C7 C2 C1 121.7(5) . . ?
C4 C3 C2 120.2(6) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 122.7(6) . . ?
C3 C4 H4A 118.6 . . ?
C5 C4 H4A 118.6 . . ?
C4 C5 C6 116.6(6) . . ?
C4 C5 C8 118.7(6) . . ?
C6 C5 C8 124.3(6) . . ?
C5 C6 C7 122.0(7) . . ?
C5 C6 N1 121.3(6) . . ?
C7 C6 N1 116.5(7) . . ?
C2 C7 C6 119.8(6) . . ?
C2 C7 H7A 120.1 . . ?
C6 C7 H7A 120.1 . . ?
C13 C8 C9 116.0(6) . . ?
C13 C8 C5 120.3(6) . . ?
C9 C8 C5 122.8(6) . . ?
C10 C9 C8 122.8(6) . . ?
C10 C9 N4 116.3(6) . . ?
C8 C9 N4 121.0(6) . . ?
C11 C10 C9 119.4(6) . . ?
C11 C10 H10A 120.3 . . ?
C9 C10 H10A 120.3 . . ?
C12 C11 C10 118.1(6) . . ?
C12 C11 C14 122.1(5) . . ?
C10 C11 C14 119.7(5) . . ?
C11 C12 C13 121.7(6) . . ?
C11 C12 H12A 119.1 . . ?
C13 C12 H12A 119.1 . . ?
C8 C13 C12 122.0(7) . . ?
C8 C13 H13A 119.0 . . ?
C12 C13 H13A 119.0 . . ?
O17 C14 O18 124.2(5) . . ?
O17 C14 C11 121.4(5) . . ?
O18 C14 C11 114.4(5) . . ?
O5 C15 O4 125.6(5) . . ?
O5 C15 C16 116.7(4) . . ?
O4 C15 C16 117.7(5) . . ?
C21 C16 C17 118.2(5) . . ?
C21 C16 C15 123.3(5) . . ?
C17 C16 C15 118.5(5) . . ?
C18 C17 C16 119.9(6) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 122.7(6) . . ?
C17 C18 N2 118.1(6) . . ?
C19 C18 N2 119.2(5) . . ?
C20 C19 C18 116.0(5) . . ?
C20 C19 C22 118.8(6) . . ?
C18 C19 C22 125.1(6) . . ?
C19 C20 C21 122.8(6) . . ?
C19 C20 H20A 118.6 . . ?
C21 C20 H20A 118.6 . . ?
C20 C21 C16 120.2(6) . . ?
C20 C21 H21A 119.9 . . ?
C16 C21 H21A 119.9 . . ?
C23 C22 C27 116.5(5) . . ?
C23 C22 C19 118.2(6) . . ?
C27 C22 C19 125.3(6) . . ?
C22 C23 C24 122.4(6) . . ?
C22 C23 H23A 118.8 . . ?
C24 C23 H23A 118.8 . . ?
C25 C24 C23 119.3(6) . . ?
C25 C24 H24A 120.4 . . ?
C23 C24 H24A 120.4 . . ?
C26 C25 C24 119.6(5) . . ?
C26 C25 C28 119.9(5) . . ?
C24 C25 C28 120.5(5) . . ?
C27 C26 C25 120.9(5) . . ?
C27 C26 H26A 119.5 . . ?
C25 C26 H26A 119.5 . . ?
C26 C27 C22 121.1(5) . . ?
C26 C27 N3 118.1(6) . . ?
C22 C27 N3 120.8(5) . . ?
O15 C28 O16 126.2(5) . . ?
O15 C28 C25 115.8(4) . . ?
O16 C28 C25 118.0(4) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C29 122.3(10) . . ?
O19 C30 C31 116.0(10) . . ?
C29 C30 C31 121.8(11) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O20 C33 C34 135.2(12) . . ?
O20 C33 C32 110.0(11) . . ?
C34 C33 C32 114.8(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O12B N1 O12A 37.6(10) . . ?
O12B N1 O11B 114.0(15) . . ?
O12A N1 O11B 113.1(16) . . ?
O12B N1 O11A 101.0(15) . . ?
O12A N1 O11A 133.9(15) . . ?
O11B N1 O11A 56.2(12) . . ?
O12B N1 C6 126.7(12) . . ?
O12A N1 C6 117.1(12) . . ?
O11B N1 C6 119.2(11) . . ?
O11A N1 C6 104.3(12) . . ?
O8 N2 O7A 94.9(9) . . ?
O8 N2 O7B 118.6(9) . . ?
O7A N2 O7B 74.0(9) . . ?
O8 N2 C18 117.5(6) . . ?
O7A N2 C18 124.5(8) . . ?
O7B N2 C18 118.0(8) . . ?
O10 N3 O9B 122.7(10) . . ?
O10 N3 O9A 116.7(9) . . ?
O9B N3 O9A 35.6(9) . . ?
O10 N3 C27 120.2(6) . . ?
O9B N3 C27 115.7(9) . . ?
O9A N3 C27 117.6(8) . . ?
O14B N4 O13B 106.8(15) . . ?
O14B N4 O14A 28.5(12) . . ?
O13B N4 O14A 113.1(14) . . ?
O14B N4 O13A 136.9(13) . . ?
O13B N4 O13A 50.1(10) . . ?
O14A N4 O13A 118.2(13) . . ?
O14B N4 C9 108.6(11) . . ?
O13B N4 C9 118.1(11) . . ?
O14A N4 C9 122.2(11) . . ?
O13A N4 C9 114.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 977434'
#######################################################################
#
#                 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_522c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C3 H8 O)'
_chemical_formula_sum            'C34 H30 Cu3 N4 O20'
_chemical_formula_weight         1005.24

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'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.3248(19)
_cell_length_b                   32.715(4)
_cell_length_c                   10.0565(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.143(2)
_cell_angle_gamma                90.00
_cell_volume                     4817.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4714
_cell_measurement_theta_min      1.46
_cell_measurement_theta_max      26.35

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2036
_exptl_absorpt_coefficient_mu    1.385
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8088
_exptl_absorpt_correction_T_max  0.8855
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33567
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8360
_reflns_number_gt                5780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0862P)²+12.7397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8360
_refine_ls_number_parameters     604
_refine_ls_number_restraints     251
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.1905
_refine_ls_wR_factor_gt          0.1751
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.180
_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 0.83487(5) 0.77455(2) 0.53219(8) 0.0225(2) Uani 1 1 d . . .
Cu2 Cu 0.98277(5) 0.71722(2) 0.51079(8) 0.0254(2) Uani 1 1 d . . .
Cu3 Cu 0.90931(5) 0.71617(2) 0.76875(8) 0.0234(2) Uani 1 1 d . . .
O1 O 0.8725(3) 0.71822(12) 0.5680(4) 0.0219(9) Uani 1 1 d D . .
H1A H 0.8324 0.7007 0.5279 0.026 Uiso 1 1 d R . .
O2 O 0.9585(3) 0.65696(14) 0.7607(5) 0.0369(12) Uani 1 1 d . . .
O3 O 1.0192(3) 0.66232(13) 0.5814(5) 0.0309(10) Uani 1 1 d . . .
O4 O 0.7841(3) 0.72738(14) 0.7804(5) 0.0293(10) Uani 1 1 d . . .
O5 O 0.7265(3) 0.76667(14) 0.5913(5) 0.0311(10) Uani 1 1 d . . .
O6 O 0.9451(3) 0.72493(12) 0.9664(4) 0.0246(9) Uani 1 1 d D . .
H6A H 0.9852 0.7080 1.0106 0.029 Uiso 1 1 d R . .
O7A O 0.4668(12) 0.8470(4) 0.623(2) 0.095(5) Uani 0.50 1 d PDU A 1
O7B O 0.4484(12) 0.8383(5) 0.5456(16) 0.080(4) Uani 0.50 1 d PDU A 2
O8A O 0.3663(10) 0.8301(5) 0.6667(18) 0.103(4) Uani 0.50 1 d PDU A 1
O8B O 0.3438(6) 0.8073(4) 0.5899(13) 0.062(3) Uani 0.50 1 d PDU A 2
O9 O 0.4873(4) 0.8110(2) 0.9677(8) 0.086(2) Uani 1 1 d DU . .
O10 O 0.3790(5) 0.8423(2) 1.0130(9) 0.101(3) Uani 1 1 d DU . .
O11A O 1.2603(11) 0.5070(5) 0.7053(18) 0.095(5) Uani 0.50 1 d PDU B 1
O11B O 1.2283(15) 0.4970(4) 0.622(2) 0.123(7) Uani 0.50 1 d PDU B 2
O12A O 1.1915(19) 0.5408(9) 0.5076(17) 0.173(9) Uani 0.50 1 d PDU B 1
O12B O 1.2526(13) 0.5599(6) 0.590(2) 0.129(7) Uani 0.50 1 d PDU B 2
O13A O 1.2324(13) 0.5120(5) 0.984(2) 0.106(5) Uani 0.50 1 d PDU C 1
O13B O 1.1975(14) 0.5209(3) 1.004(2) 0.106(5) Uani 0.50 1 d PDU C 2
O14A O 1.1782(11) 0.4718(4) 1.1274(13) 0.078(4) Uani 0.50 1 d PDU C 1
O14B O 1.2384(15) 0.4686(6) 1.1246(17) 0.135(7) Uani 0.50 1 d PDU C 2
O15 O 0.0887(3) 0.77835(14) 0.9472(5) 0.0337(11) Uani 1 1 d . . .
O16 O 0.0352(3) 0.73946(14) 0.7589(5) 0.0304(11) Uani 1 1 d . . .
O17 O 1.1076(4) 0.31916(16) 0.7370(6) 0.0524(14) Uani 1 1 d . . .
O18 O 1.1743(3) 0.33264(13) 0.9587(5) 0.0387(12) Uani 1 1 d . . .
O19 O 0.7362(9) 0.6628(3) 0.4423(12) 0.186(4) Uani 1 1 d DU . .
H19 H 0.7762 0.6632 0.3992 0.279 Uiso 1 1 d R . .
O20 O 1.0697(9) 0.6702(4) 1.1127(14) 0.202(6) Uani 1 1 d DU . .
H20 H 1.0261 0.6711 1.1489 0.302 Uiso 1 1 d R . .
C1 C 0.9995(5) 0.64353(19) 0.6780(7) 0.0316(15) Uani 1 1 d . . .
C2 C 1.0294(5) 0.5998(2) 0.6980(8) 0.0362(17) Uani 1 1 d . . .
C3 C 0.9845(6) 0.5726(2) 0.7605(10) 0.057(2) Uani 1 1 d . . .
H3A H 0.9356 0.5815 0.7900 0.068 Uiso 1 1 calc R . .
C4 C 1.0123(7) 0.5324(3) 0.7792(11) 0.069(3) Uani 1 1 d . . .
H4A H 0.9802 0.5143 0.8186 0.083 Uiso 1 1 calc R . .
C5 C 1.0867(6) 0.5180(2) 0.7409(9) 0.053(2) Uani 1 1 d . . .
C6 C 1.1280(6) 0.5452(3) 0.6777(10) 0.059(2) Uani 1 1 d . B .
C7 C 1.1001(6) 0.5853(2) 0.6537(9) 0.051(2) Uani 1 1 d . . .
H7A H 1.1293 0.6027 0.6073 0.062 Uiso 1 1 calc R . .
C8 C 1.1096(6) 0.4735(2) 0.7650(9) 0.055(2) Uani 1 1 d . . .
C9 C 1.1525(7) 0.4567(3) 0.8935(10) 0.064(3) Uani 1 1 d . C .
C10 C 1.1643(6) 0.4152(2) 0.9167(10) 0.059(2) Uani 1 1 d . . .
H10A H 1.1945 0.4053 1.0050 0.070 Uiso 1 1 calc R . .
C11 C 1.1313(5) 0.3891(2) 0.8091(8) 0.0427(19) Uani 1 1 d . . .
C12 C 1.0855(7) 0.4042(2) 0.6820(9) 0.062(3) Uani 1 1 d . . .
H12A H 1.0600 0.3864 0.6088 0.075 Uiso 1 1 calc R . .
C13 C 1.0764(8) 0.4461(3) 0.6607(10) 0.071(3) Uani 1 1 d . . .
H13A H 1.0467 0.4558 0.5719 0.085 Uiso 1 1 calc R . .
C14 C 1.1375(5) 0.3436(2) 0.8321(8) 0.0377(17) Uani 1 1 d . . .
C15 C 0.7199(4) 0.74722(19) 0.6952(7) 0.0275(15) Uani 1 1 d . . .
C16 C 0.6294(4) 0.7478(2) 0.7222(7) 0.0301(15) Uani 1 1 d . . .
C17 C 0.5709(5) 0.7800(2) 0.6692(8) 0.0421(19) Uani 1 1 d . . .
H17A H 0.5888 0.8007 0.6192 0.051 Uiso 1 1 calc R . .
C18 C 0.4857(5) 0.7815(3) 0.6907(9) 0.051(2) Uani 1 1 d . A .
C19 C 0.4577(5) 0.7521(3) 0.7701(8) 0.0437(19) Uani 1 1 d . . .
C20 C 0.5179(5) 0.7193(2) 0.8191(8) 0.0406(19) Uani 1 1 d . . .
H20A H 0.5011 0.6986 0.8699 0.049 Uiso 1 1 calc R . .
C21 C 0.6008(4) 0.7172(2) 0.7937(8) 0.0354(16) Uani 1 1 d . . .
H21A H 0.6384 0.6947 0.8253 0.042 Uiso 1 1 calc R . .
C22 C 0.3680(5) 0.7532(3) 0.8026(8) 0.0417(18) Uani 1 1 d . . .
C23 C 0.3064(5) 0.7230(3) 0.7507(8) 0.050(2) Uani 1 1 d . . .
H23A H 0.3238 0.7009 0.7059 0.060 Uiso 1 1 calc R . .
C24 C 0.2179(5) 0.7239(2) 0.7624(8) 0.0430(19) Uani 1 1 d . . .
H24A H 0.1764 0.7035 0.7212 0.052 Uiso 1 1 calc R . .
C25 C 0.1923(4) 0.7549(2) 0.8346(7) 0.0307(15) Uani 1 1 d . . .
C26 C 0.2555(5) 0.7846(2) 0.8962(8) 0.0392(18) Uani 1 1 d . . .
H26A H 0.2397 0.8052 0.9485 0.047 Uiso 1 1 calc R . .
C27 C 0.3426(5) 0.7838(2) 0.8802(8) 0.0430(19) Uani 1 1 d . . .
C28 C 0.0978(4) 0.75778(19) 0.8472(6) 0.0235(14) Uani 1 1 d . . .
C29 C 0.7007(14) 0.6223(5) 0.6247(13) 0.207(6) Uani 1 1 d DU . .
H29A H 0.7480 0.6358 0.6954 0.311 Uiso 1 1 calc R . .
H29B H 0.6936 0.5949 0.6536 0.311 Uiso 1 1 calc R . .
H29C H 0.6443 0.6369 0.6105 0.311 Uiso 1 1 calc R . .
C30 C 0.7266(8) 0.6214(3) 0.4875(14) 0.200(5) Uani 1 1 d DU . .
H30A H 0.7841 0.6065 0.5015 0.240 Uiso 1 1 calc R . .
C31 C 0.6490(14) 0.5994(4) 0.3764(16) 0.212(6) Uani 1 1 d DU . .
H31A H 0.6637 0.5985 0.2900 0.319 Uiso 1 1 calc R . .
H31B H 0.5928 0.6141 0.3635 0.319 Uiso 1 1 calc R . .
H31C H 0.6424 0.5721 0.4068 0.319 Uiso 1 1 calc R . .
C32 C 1.1382(14) 0.6138(6) 1.2668(18) 0.237(12) Uani 1 1 d D . .
H32A H 1.0895 0.6146 1.3088 0.355 Uiso 1 1 calc R . .
H32B H 1.1869 0.6313 1.3177 0.355 Uiso 1 1 calc R . .
H32C H 1.1603 0.5863 1.2687 0.355 Uiso 1 1 calc R . .
C33 C 1.1025(10) 0.6286(4) 1.1147(15) 0.216(10) Uani 1 1 d DU . .
H33A H 1.0526 0.6109 1.0627 0.259 Uiso 1 1 calc R . .
C34 C 1.1809(15) 0.6274(6) 1.047(2) 0.249(12) Uani 1 1 d DU . .
H34A H 1.1586 0.6364 0.9524 0.373 Uiso 1 1 calc R . .
H34B H 1.2035 0.6000 1.0499 0.373 Uiso 1 1 calc R . .
H34C H 1.2293 0.6451 1.0977 0.373 Uiso 1 1 calc R . .
N1 N 1.2110(10) 0.5332(4) 0.6321(17) 0.142(5) Uani 1 1 d DU . .
N2 N 0.4259(5) 0.8151(3) 0.6248(9) 0.070(2) Uani 1 1 d DU . .
N3 N 0.4061(4) 0.8150(2) 0.9532(8) 0.0534(18) Uani 1 1 d DU . .
N4 N 1.1890(8) 0.4842(3) 1.0184(11) 0.100(3) Uani 1 1 d DU . .


_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 O18 1.910(4) 2_756 ?
Cu1 O1 1.933(4) . ?
Cu1 O5 1.940(4) . ?
Cu1 O6 1.988(4) 4_575 ?
Cu1 O4 2.420(4) 4_575 ?
Cu1 Cu2 2.9980(10) . ?
Cu1 Cu3 3.0013(11) . ?
Cu2 O15 1.918(4) 4_675 ?
Cu2 O1 1.939(4) . ?
Cu2 O3 1.952(4) . ?
Cu2 O6 1.991(4) 4_575 ?
Cu3 O6 1.921(4) . ?
Cu3 O1 1.931(4) . ?
Cu3 O4 1.991(4) . ?
Cu3 O2 2.089(4) . ?
Cu3 O16 2.103(4) 1_655 ?
O1 H1A 0.8499 . ?
O2 C1 1.261(8) . ?
O3 C1 1.259(8) . ?
O4 C15 1.276(8) . ?
O4 Cu1 2.420(4) 4_576 ?
O5 C15 1.252(8) . ?
O6 Cu1 1.988(4) 4_576 ?
O6 Cu2 1.991(4) 4_576 ?
O6 H6A 0.8500 . ?
O7A N2 1.220(5) . ?
O7A O8A 1.81(2) . ?
O7B N2 1.221(5) . ?
O8A N2 1.216(5) . ?
O8B N2 1.230(5) . ?
O9 N3 1.217(5) . ?
O10 N3 1.215(5) . ?
O11A N1 1.230(5) . ?
O11B N1 1.222(6) . ?
O12A N1 1.224(6) . ?
O12B N1 1.227(6) . ?
O13A N4 1.235(6) . ?
O13B N4 1.221(5) . ?
O14A N4 1.225(5) . ?
O14B N4 1.223(6) . ?
O15 C28 1.251(7) . ?
O15 Cu2 1.918(4) 4_476 ?
O16 C28 1.251(7) . ?
O16 Cu3 2.103(4) 1_455 ?
O17 C14 1.227(9) . ?
O18 C14 1.283(9) . ?
O18 Cu1 1.910(4) 2_746 ?
O19 C30 1.449(2) . ?
O19 H19 0.8500 . ?
O20 C33 1.448(2) . ?
O20 H20 0.8501 . ?
C1 C2 1.499(9) . ?
C2 C7 1.370(10) . ?
C2 C3 1.383(10) . ?
C3 C4 1.380(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.353(12) . ?
C5 C8 1.502(10) . ?
C6 C7 1.380(11) . ?
C6 N1 1.526(16) . ?
C7 H7A 0.9300 . ?
C8 C13 1.358(12) . ?
C8 C9 1.379(12) . ?
C9 C10 1.381(11) . ?
C9 N4 1.512(13) . ?
C10 C11 1.355(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(11) . ?
C11 C14 1.504(10) . ?
C12 C13 1.389(11) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.490(8) . ?
C16 C21 1.378(10) . ?
C16 C17 1.385(10) . ?
C17 C18 1.385(10) . ?
C17 H17A 0.9300 . ?
C18 C19 1.397(11) . ?
C18 N2 1.460(10) . ?
C19 C20 1.405(11) . ?
C19 C22 1.503(9) . ?
C20 C21 1.370(9) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.360(11) . ?
C22 C27 1.394(11) . ?
C23 C24 1.395(10) . ?
C23 H23A 0.9300 . ?
C24 C25 1.371(10) . ?
C24 H24A 0.9300 . ?
C25 C26 1.383(10) . ?
C25 C28 1.494(8) . ?
C26 C27 1.390(10) . ?
C26 H26A 0.9300 . ?
C27 N3 1.453(10) . ?
C29 C30 1.544(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.547(4) . ?
C30 H30A 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.543(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.544(4) . ?
C33 H33A 0.9800 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Cu1 O1 164.2(2) 2_756 . ?
O18 Cu1 O5 92.0(2) 2_756 . ?
O1 Cu1 O5 92.98(18) . . ?
O18 Cu1 O6 95.13(18) 2_756 4_575 ?
O1 Cu1 O6 80.44(16) . 4_575 ?
O5 Cu1 O6 172.74(18) . 4_575 ?
O18 Cu1 O4 94.04(19) 2_756 4_575 ?
O1 Cu1 O4 98.99(16) . 4_575 ?
O5 Cu1 O4 106.09(17) . 4_575 ?
O6 Cu1 O4 72.21(16) 4_575 4_575 ?
O18 Cu1 Cu2 133.95(15) 2_756 . ?
O1 Cu1 Cu2 39.32(11) . . ?
O5 Cu1 Cu2 132.29(14) . . ?
O6 Cu1 Cu2 41.14(12) 4_575 . ?
O4 Cu1 Cu2 85.72(10) 4_575 . ?
O18 Cu1 Cu3 127.69(16) 2_756 . ?
O1 Cu1 Cu3 39.00(12) . . ?
O5 Cu1 Cu3 80.34(13) . . ?
O6 Cu1 Cu3 96.19(12) 4_575 . ?
O4 Cu1 Cu3 137.94(11) 4_575 . ?
Cu2 Cu1 Cu3 62.62(2) . . ?
O15 Cu2 O1 174.28(18) 4_675 . ?
O15 Cu2 O3 90.64(18) 4_675 . ?
O1 Cu2 O3 95.08(17) . . ?
O15 Cu2 O6 94.10(17) 4_675 4_575 ?
O1 Cu2 O6 80.22(16) . 4_575 ?
O3 Cu2 O6 171.74(18) . 4_575 ?
O15 Cu2 Cu1 135.14(13) 4_675 . ?
O1 Cu2 Cu1 39.18(11) . . ?
O3 Cu2 Cu1 133.71(13) . . ?
O6 Cu2 Cu1 41.06(11) 4_575 . ?
O6 Cu3 O1 169.44(17) . . ?
O6 Cu3 O4 84.12(18) . . ?
O1 Cu3 O4 93.79(17) . . ?
O6 Cu3 O2 100.51(18) . . ?
O1 Cu3 O2 89.37(17) . . ?
O4 Cu3 O2 122.55(19) . . ?
O6 Cu3 O16 90.49(17) . 1_655 ?
O1 Cu3 O16 85.84(17) . 1_655 ?
O4 Cu3 O16 148.14(19) . 1_655 ?
O2 Cu3 O16 89.31(19) . 1_655 ?
O6 Cu3 Cu1 130.62(12) . . ?
O1 Cu3 Cu1 39.06(11) . . ?
O4 Cu3 Cu1 77.40(13) . . ?
O2 Cu3 Cu1 128.06(13) . . ?
O16 Cu3 Cu1 82.64(13) 1_655 . ?
Cu3 O1 Cu1 101.94(18) . . ?
Cu3 O1 Cu2 107.36(19) . . ?
Cu1 O1 Cu2 101.50(17) . . ?
Cu3 O1 H1A 114.8 . . ?
Cu1 O1 H1A 114.8 . . ?
Cu2 O1 H1A 114.8 . . ?
C1 O2 Cu3 127.2(4) . . ?
C1 O3 Cu2 128.5(4) . . ?
C15 O4 Cu3 128.3(4) . . ?
C15 O4 Cu1 131.5(4) . 4_576 ?
Cu3 O4 Cu1 92.23(17) . 4_576 ?
C15 O5 Cu1 127.6(4) . . ?
Cu3 O6 Cu1 109.5(2) . 4_576 ?
Cu3 O6 Cu2 110.5(2) . 4_576 ?
Cu1 O6 Cu2 97.80(17) 4_576 4_576 ?
Cu3 O6 H6A 112.7 . . ?
Cu1 O6 H6A 112.7 4_576 . ?
Cu2 O6 H6A 112.7 4_576 . ?
N2 O7A O8A 42.0(7) . . ?
N2 O8A O7A 42.2(8) . . ?
C28 O15 Cu2 127.9(4) . 4_476 ?
C28 O16 Cu3 131.5(4) . 1_455 ?
C14 O18 Cu1 108.0(4) . 2_746 ?
C30 O19 H19 109.4 . . ?
C33 O20 H20 109.9 . . ?
O3 C1 O2 128.2(6) . . ?
O3 C1 C2 115.9(6) . . ?
O2 C1 C2 115.9(6) . . ?
C7 C2 C3 118.2(7) . . ?
C7 C2 C1 121.7(6) . . ?
C3 C2 C1 120.1(7) . . ?
C4 C3 C2 119.9(8) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C3 C4 C5 122.1(8) . . ?
C3 C4 H4A 118.9 . . ?
C5 C4 H4A 118.9 . . ?
C6 C5 C4 116.3(7) . . ?
C6 C5 C8 126.5(8) . . ?
C4 C5 C8 117.1(8) . . ?
C5 C6 C7 122.9(8) . . ?
C5 C6 N1 121.2(8) . . ?
C7 C6 N1 115.9(9) . . ?
C2 C7 C6 120.3(8) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C13 C8 C9 115.4(8) . . ?
C13 C8 C5 119.9(8) . . ?
C9 C8 C5 124.1(8) . . ?
C8 C9 C10 123.4(8) . . ?
C8 C9 N4 120.0(8) . . ?
C10 C9 N4 116.5(9) . . ?
C11 C10 C9 119.1(8) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
C10 C11 C12 119.3(7) . . ?
C10 C11 C14 120.7(7) . . ?
C12 C11 C14 119.8(7) . . ?
C11 C12 C13 120.4(9) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C8 C13 C12 122.2(9) . . ?
C8 C13 H13A 118.9 . . ?
C12 C13 H13A 118.9 . . ?
O17 C14 O18 123.0(6) . . ?
O17 C14 C11 122.2(7) . . ?
O18 C14 C11 114.7(7) . . ?
O5 C15 O4 125.6(5) . . ?
O5 C15 C16 117.0(6) . . ?
O4 C15 C16 117.4(6) . . ?
C21 C16 C17 119.1(6) . . ?
C21 C16 C15 122.8(6) . . ?
C17 C16 C15 118.1(6) . . ?
C16 C17 C18 119.9(7) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 121.9(7) . . ?
C17 C18 N2 116.7(7) . . ?
C19 C18 N2 121.4(7) . . ?
C18 C19 C20 116.4(6) . . ?
C18 C19 C22 124.2(7) . . ?
C20 C19 C22 119.4(7) . . ?
C21 C20 C19 121.6(7) . . ?
C21 C20 H20A 119.2 . . ?
C19 C20 H20A 119.2 . . ?
C20 C21 C16 120.9(7) . . ?
C20 C21 H21A 119.5 . . ?
C16 C21 H21A 119.5 . . ?
C23 C22 C27 117.3(7) . . ?
C23 C22 C19 118.4(7) . . ?
C27 C22 C19 124.3(7) . . ?
C22 C23 C24 122.3(7) . . ?
C22 C23 H23A 118.9 . . ?
C24 C23 H23A 118.9 . . ?
C25 C24 C23 119.9(7) . . ?
C25 C24 H24A 120.1 . . ?
C23 C24 H24A 120.1 . . ?
C24 C25 C26 119.0(6) . . ?
C24 C25 C28 121.9(6) . . ?
C26 C25 C28 119.1(6) . . ?
C25 C26 C27 120.2(7) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C26 C27 C22 121.1(7) . . ?
C26 C27 N3 116.8(7) . . ?
C22 C27 N3 122.1(7) . . ?
O16 C28 O15 125.8(6) . . ?
O16 C28 C25 118.0(5) . . ?
O15 C28 C25 116.2(6) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C29 109.8(3) . . ?
O19 C30 C31 109.5(3) . . ?
C29 C30 C31 108.0(4) . . ?
O19 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
C31 C30 H30A 109.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O20 C33 C32 109.2(3) . . ?
O20 C33 C34 109.2(3) . . ?
C32 C33 C34 109.4(4) . . ?
O20 C33 H33A 109.6 . . ?
C32 C33 H33A 109.6 . . ?
C34 C33 H33A 109.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O11B N1 O12A 96(2) . . ?
O11B N1 O12B 121(2) . . ?
O12A N1 O12B 60.0(15) . . ?
O11B N1 O11A 43.0(12) . . ?
O12A N1 O11A 132(2) . . ?
O12B N1 O11A 114.2(19) . . ?
O11B N1 C6 119.7(16) . . ?
O12A N1 C6 106.3(17) . . ?
O12B N1 C6 118.8(15) . . ?
O11A N1 C6 114.8(14) . . ?
O8A N2 O7A 95.8(15) . . ?
O8A N2 O7B 111.2(13) . . ?
O7A N2 O7B 38.3(10) . . ?
O8A N2 O8B 51.1(10) . . ?
O7A N2 O8B 131.3(13) . . ?
O7B N2 O8B 113.9(13) . . ?
O8A N2 C18 125.5(11) . . ?
O7A N2 C18 113.2(11) . . ?
O7B N2 C18 120.3(10) . . ?
O8B N2 C18 115.2(9) . . ?
O10 N3 O9 120.5(8) . . ?
O10 N3 C27 119.4(7) . . ?
O9 N3 C27 119.6(7) . . ?
O13B N4 O14B 116.9(17) . . ?
O13B N4 O14A 118.5(16) . . ?
O14B N4 O14A 45.0(12) . . ?
O13B N4 O13A 32.6(13) . . ?
O14B N4 O13A 107.8(18) . . ?
O14A N4 O13A 136.1(16) . . ?
O13B N4 C9 120.9(13) . . ?
O14B N4 C9 117.4(14) . . ?
O14A N4 C9 115.6(11) . . ?
O13A N4 C9 107.7(13) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.112
_database_code_depnum_ccdc_archive 'CCDC 977435'
#######################################################################
#
#                 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_516

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C3 H8 O)'
_chemical_formula_sum            'C34 H30 Cu3 N4 O20'
_chemical_formula_weight         1005.24

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'
_symmetry_space_group_name_Hall  '-P 2ybc  '

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

_cell_length_a                   15.319(2)
_cell_length_b                   32.720(4)
_cell_length_c                   10.0665(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.137(2)
_cell_angle_gamma                90.00
_cell_volume                     4821.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7904
_cell_measurement_theta_min      1.58
_cell_measurement_theta_max      26.25

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2036
_exptl_absorpt_coefficient_mu    1.384
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_T_max  0.8740
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32842
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8324
_reflns_number_gt                6378
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0594P)²+26.1677P] 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     SHELXL
_refine_ls_extinction_coef       0.00049(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8324
_refine_ls_number_parameters     605
_refine_ls_number_restraints     230
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.1730
_refine_ls_wR_factor_gt          0.1642
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.058
_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 0.33453(4) 0.774658(19) 0.03314(7) 0.02214(19) Uani 1 1 d . . .
Cu2 Cu 0.48231(4) 0.71722(2) 0.01178(8) 0.0255(2) Uani 1 1 d . . .
Cu3 Cu 0.40889(4) 0.71625(2) 0.26955(7) 0.02324(19) Uani 1 1 d . . .
O1 O 0.3711(2) 0.71775(11) 0.0679(4) 0.0221(8) Uani 1 1 d . . .
H1A H 0.3309 0.7003 0.0279 0.027 Uiso 1 1 d R . .
O2 O 0.4577(3) 0.65707(12) 0.2619(5) 0.0375(10) Uani 1 1 d . . .
O3 O 0.5185(3) 0.66249(12) 0.0819(4) 0.0331(10) Uani 1 1 d . . .
O4 O 0.2834(2) 0.72735(12) 0.2814(4) 0.0293(9) Uani 1 1 d . . .
O5 O 0.2259(3) 0.76656(13) 0.0917(4) 0.0308(9) Uani 1 1 d . . .
O6 O 0.4448(2) 0.72465(11) 0.4670(4) 0.0231(8) Uani 1 1 d . . .
H6A H 0.4850 0.7077 0.5109 0.028 Uiso 1 1 d R . .
O7A O -0.0328(10) 0.8481(3) 0.124(2) 0.095(5) Uani 0.50 1 d PDU A 1
O7B O -0.0548(9) 0.8382(4) 0.0448(13) 0.074(4) Uani 0.50 1 d PDU A 2
O8A O -0.1210(10) 0.8353(5) 0.1892(16) 0.109(4) Uani 0.50 1 d PDU A 1
O8B O -0.1557(5) 0.8091(3) 0.0954(12) 0.063(3) Uani 0.50 1 d PDU A 2
O9 O -0.0131(3) 0.8110(2) 0.4690(8) 0.090(2) Uani 1 1 d DU . .
O10 O -0.1222(5) 0.8426(2) 0.5153(8) 0.100(2) Uani 1 1 d DU . .
O11A O 0.7574(10) 0.5066(5) 0.2021(17) 0.099(4) Uani 0.50 1 d PDU B 1
O11B O 0.7279(13) 0.4980(4) 0.115(2) 0.110(5) Uani 0.50 1 d PDU B 2
O12A O 0.7504(13) 0.5598(5) 0.091(2) 0.135(6) Uani 0.50 1 d PDU B 1
O12B O 0.6925(16) 0.5425(7) 0.0109(14) 0.146(6) Uani 0.50 1 d PDU B 2
O13A O 0.7298(11) 0.5126(4) 0.4839(19) 0.105(5) Uani 0.50 1 d PDU C 1
O13B O 0.6914(13) 0.5210(3) 0.505(2) 0.110(5) Uani 0.50 1 d PDU C 2
O14A O 0.7242(14) 0.4690(6) 0.6319(12) 0.119(5) Uani 0.50 1 d PDU C 1
O14B O 0.6729(12) 0.4720(5) 0.6222(14) 0.101(4) Uani 0.50 1 d PDU C 2
O15 O -0.4118(3) 0.77849(12) 0.4481(5) 0.0330(10) Uani 1 1 d . . .
O16 O -0.4656(2) 0.73946(13) 0.2601(4) 0.0301(9) Uani 1 1 d . . .
O17 O 0.6076(4) 0.31939(14) 0.2366(5) 0.0534(13) Uani 1 1 d . . .
O18 O 0.6740(3) 0.33276(12) 0.4583(5) 0.0381(10) Uani 1 1 d . . .
O19 O 0.2453(9) 0.6644(3) -0.0464(12) 0.191(4) Uani 1 1 d DU . .
H19 H 0.2733 0.6638 -0.1077 0.287 Uiso 1 1 d R . .
O20 O 0.5650(9) 0.6700(4) 0.6065(14) 0.199(5) Uani 1 1 d DU . .
H20 H 0.5308 0.6717 0.6592 0.299 Uiso 1 1 d R . .
C1 C 0.4985(4) 0.64337(17) 0.1796(6) 0.0308(13) Uani 1 1 d . . .
C2 C 0.5282(5) 0.59961(19) 0.1986(7) 0.0391(15) Uani 1 1 d . . .
C3 C 0.4834(6) 0.5725(2) 0.2606(9) 0.058(2) Uani 1 1 d . . .
H3A H 0.4348 0.5812 0.2909 0.070 Uiso 1 1 calc R . .
C4 C 0.5111(6) 0.5323(2) 0.2774(10) 0.068(3) Uani 1 1 d . . .
H4A H 0.4780 0.5142 0.3148 0.082 Uiso 1 1 calc R . .
C5 C 0.5854(6) 0.5176(2) 0.2417(9) 0.060(2) Uani 1 1 d . . .
C6 C 0.6277(6) 0.5452(2) 0.1776(10) 0.065(2) Uani 1 1 d . B .
C7 C 0.5995(5) 0.5855(2) 0.1543(9) 0.055(2) Uani 1 1 d . . .
H7A H 0.6289 0.6030 0.1085 0.066 Uiso 1 1 calc R . .
C8 C 0.6094(6) 0.4736(2) 0.2645(9) 0.058(2) Uani 1 1 d . . .
C9 C 0.6533(7) 0.4571(2) 0.3954(10) 0.069(2) Uani 1 1 d . C .
C10 C 0.6644(6) 0.4154(2) 0.4160(9) 0.063(2) Uani 1 1 d . . .
H10A H 0.6945 0.4055 0.5041 0.076 Uiso 1 1 calc R . .
C11 C 0.6319(5) 0.38883(19) 0.3089(7) 0.0435(16) Uani 1 1 d . . .
C12 C 0.5865(7) 0.4046(2) 0.1809(9) 0.066(2) Uani 1 1 d . . .
H12A H 0.5636 0.3869 0.1065 0.079 Uiso 1 1 calc R . .
C13 C 0.5740(7) 0.4460(2) 0.1597(9) 0.072(3) Uani 1 1 d . . .
H13A H 0.5408 0.4555 0.0724 0.087 Uiso 1 1 calc R . .
C14 C 0.6379(4) 0.34328(19) 0.3320(7) 0.0368(15) Uani 1 1 d . . .
C15 C 0.2192(4) 0.74749(18) 0.1961(6) 0.0281(13) Uani 1 1 d . . .
C16 C 0.1287(4) 0.7483(2) 0.2237(6) 0.0308(13) Uani 1 1 d . . .
C17 C 0.0701(4) 0.7806(2) 0.1710(7) 0.0399(16) Uani 1 1 d . . .
H17A H 0.0876 0.8013 0.1207 0.048 Uiso 1 1 calc R . .
C18 C -0.0140(4) 0.7819(2) 0.1937(8) 0.0484(19) Uani 1 1 d . A .
C19 C -0.0426(4) 0.7527(2) 0.2718(7) 0.0442(17) Uani 1 1 d . . .
C20 C 0.0180(4) 0.7196(2) 0.3211(7) 0.0417(17) Uani 1 1 d . . .
H20A H 0.0015 0.6990 0.3725 0.050 Uiso 1 1 calc R . .
C21 C 0.1014(4) 0.7175(2) 0.2943(7) 0.0361(15) Uani 1 1 d . . .
H21A H 0.1391 0.6950 0.3244 0.043 Uiso 1 1 calc R . .
C22 C -0.1328(4) 0.7534(2) 0.3017(7) 0.0433(17) Uani 1 1 d . . .
C23 C -0.1934(4) 0.7228(2) 0.2510(6) 0.0435(18) Uani 1 1 d . . .
H23A H -0.1754 0.7007 0.2075 0.052 Uiso 1 1 calc R . .
C24 C -0.2826(4) 0.7238(2) 0.2625(7) 0.0426(17) Uani 1 1 d . . .
H24A H -0.3241 0.7034 0.2213 0.051 Uiso 1 1 calc R . .
C25 C -0.3082(4) 0.75513(19) 0.3354(6) 0.0292(13) Uani 1 1 d . . .
C26 C -0.2454(4) 0.7846(2) 0.3984(7) 0.0403(16) Uani 1 1 d . . .
H26A H -0.2604 0.8046 0.4535 0.048 Uiso 1 1 calc R . .
C27 C -0.1585(5) 0.7841(2) 0.3785(7) 0.0435(17) Uani 1 1 d . . .
C28 C -0.4031(3) 0.75765(17) 0.3480(6) 0.0246(12) Uani 1 1 d . . .
C29 C 0.2028(14) 0.6236(5) 0.1292(13) 0.212(6) Uani 1 1 d DU . .
H29A H 0.2516 0.6356 0.2017 0.318 Uiso 1 1 calc R . .
H29B H 0.1922 0.5962 0.1547 0.318 Uiso 1 1 calc R . .
H29C H 0.1483 0.6395 0.1163 0.318 Uiso 1 1 calc R . .
C30 C 0.2295(8) 0.6229(3) -0.0087(13) 0.207(5) Uani 1 1 d DU . .
H30A H 0.2850 0.6065 0.0037 0.249 Uiso 1 1 calc R . .
C31 C 0.1494(13) 0.6041(5) -0.1263(15) 0.219(6) Uani 1 1 d DU . .
H31A H 0.1659 0.6032 -0.2112 0.329 Uiso 1 1 calc R . .
H31B H 0.0957 0.6206 -0.1395 0.329 Uiso 1 1 calc R . .
H31C H 0.1373 0.5769 -0.1007 0.329 Uiso 1 1 calc R . .
C32 C 0.6388(14) 0.6150(5) 0.7629(17) 0.221(10) Uani 1 1 d DU . .
H32A H 0.5910 0.6150 0.8066 0.331 Uiso 1 1 calc R . .
H32B H 0.6863 0.6334 0.8112 0.331 Uiso 1 1 calc R . .
H32C H 0.6634 0.5879 0.7660 0.331 Uiso 1 1 calc R . .
C33 C 0.5998(9) 0.6288(3) 0.6095(14) 0.223(10) Uani 1 1 d DU . .
H33A H 0.5505 0.6103 0.5602 0.267 Uiso 1 1 calc R . .
C34 C 0.6769(14) 0.6283(6) 0.539(2) 0.246(12) Uani 1 1 d DU . .
H34A H 0.6531 0.6375 0.4444 0.369 Uiso 1 1 calc R . .
H34B H 0.7001 0.6011 0.5397 0.369 Uiso 1 1 calc R . .
H34C H 0.7254 0.6462 0.5882 0.369 Uiso 1 1 calc R . .
N1 N 0.7091(9) 0.5333(3) 0.1333(14) 0.125(4) Uani 1 1 d DU . .
N2 N -0.0731(4) 0.8161(2) 0.1318(8) 0.072(2) Uani 1 1 d DU . .
N3 N -0.0952(3) 0.8152(2) 0.4537(7) 0.0570(17) Uani 1 1 d DU . .
N4 N 0.6895(7) 0.4839(3) 0.5172(10) 0.098(3) Uani 1 1 d DU . .


_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 O18 1.909(4) 2_655 ?
Cu1 O5 1.941(4) . ?
Cu1 O1 1.946(4) . ?
Cu1 O6 1.991(4) 4_575 ?
Cu1 O4 2.423(4) 4_575 ?
Cu1 Cu2 2.9984(9) . ?
Cu1 Cu3 3.0026(10) . ?
Cu2 O15 1.918(4) 4_675 ?
Cu2 O3 1.945(4) . ?
Cu2 O1 1.946(3) . ?
Cu2 O6 2.000(4) 4_575 ?
Cu3 O6 1.920(4) . ?
Cu3 O1 1.941(4) . ?
Cu3 O4 1.994(4) . ?
Cu3 O2 2.085(4) . ?
Cu3 O16 2.096(4) 1_655 ?
O1 H1A 0.8496 . ?
O2 C1 1.258(7) . ?
O3 C1 1.277(7) . ?
O4 C15 1.281(7) . ?
O4 Cu1 2.423(4) 4_576 ?
O5 C15 1.252(7) . ?
O6 Cu1 1.991(4) 4_576 ?
O6 Cu2 2.000(4) 4_576 ?
O6 H6A 0.8498 . ?
O7A N2 1.230(2) . ?
O7A O8A 1.721(19) . ?
O7B N2 1.230(2) . ?
O8A N2 1.230(2) . ?
O8B N2 1.231(2) . ?
O9 N3 1.228(2) . ?
O10 N3 1.229(2) . ?
O11A N1 1.221(2) . ?
O11B N1 1.220(2) . ?
O11B O12B 1.79(3) . ?
O12A N1 1.221(2) . ?
O12B N1 1.220(2) . ?
O13A N4 1.222(2) . ?
O13B N4 1.220(2) . ?
O14A N4 1.221(2) . ?
O14B N4 1.221(2) . ?
O15 C28 1.256(7) . ?
O15 Cu2 1.918(4) 4_476 ?
O16 C28 1.247(7) . ?
O16 Cu3 2.096(4) 1_455 ?
O17 C14 1.219(8) . ?
O18 C14 1.275(8) . ?
O18 Cu1 1.909(4) 2_645 ?
O19 C30 1.449(2) . ?
O19 H19 0.8499 . ?
O20 C33 1.449(2) . ?
O20 H20 0.8499 . ?
C1 C2 1.497(8) . ?
C2 C7 1.377(10) . ?
C2 C3 1.378(10) . ?
C3 C4 1.376(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.377(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.380(12) . ?
C5 C8 1.486(9) . ?
C6 C7 1.384(10) . ?
C6 N1 1.493(14) . ?
C7 H7A 0.9300 . ?
C8 C13 1.373(12) . ?
C8 C9 1.399(12) . ?
C9 C10 1.383(10) . ?
C9 N4 1.476(12) . ?
C10 C11 1.360(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.373(11) . ?
C11 C14 1.507(8) . ?
C12 C13 1.374(10) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.492(8) . ?
C16 C21 1.367(9) . ?
C16 C17 1.388(9) . ?
C17 C18 1.374(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.387(10) . ?
C18 N2 1.460(9) . ?
C19 C20 1.416(10) . ?
C19 C22 1.500(8) . ?
C20 C21 1.383(8) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.358(10) . ?
C22 C27 1.392(10) . ?
C23 C24 1.405(9) . ?
C23 H23A 0.9300 . ?
C24 C25 1.385(9) . ?
C24 H24A 0.9300 . ?
C25 C26 1.378(9) . ?
C25 C28 1.498(7) . ?
C26 C27 1.403(9) . ?
C26 H26A 0.9300 . ?
C27 N3 1.455(9) . ?
C29 C30 1.559(2) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.559(2) . ?
C30 H30A 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.549(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.549(2) . ?
C33 H33A 0.9800 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Cu1 O5 92.64(18) 2_655 . ?
O18 Cu1 O1 164.66(19) 2_655 . ?
O5 Cu1 O1 92.40(16) . . ?
O18 Cu1 O6 94.59(17) 2_655 4_575 ?
O5 Cu1 O6 172.63(16) . 4_575 ?
O1 Cu1 O6 80.98(14) . 4_575 ?
O18 Cu1 O4 93.96(17) 2_655 4_575 ?
O5 Cu1 O4 105.80(15) . 4_575 ?
O1 Cu1 O4 98.58(15) . 4_575 ?
O6 Cu1 O4 72.25(14) 4_575 4_575 ?
O18 Cu1 Cu2 133.67(14) 2_655 . ?
O5 Cu1 Cu2 132.02(12) . . ?
O1 Cu1 Cu2 39.62(10) . . ?
O6 Cu1 Cu2 41.40(10) 4_575 . ?
O4 Cu1 Cu2 85.77(9) 4_575 . ?
O18 Cu1 Cu3 127.79(15) 2_655 . ?
O5 Cu1 Cu3 80.28(12) . . ?
O1 Cu1 Cu3 39.35(11) . . ?
O6 Cu1 Cu3 96.38(11) 4_575 . ?
O4 Cu1 Cu3 137.90(10) 4_575 . ?
Cu2 Cu1 Cu3 62.60(2) . . ?
O15 Cu2 O3 90.55(17) 4_675 . ?
O15 Cu2 O1 174.63(16) 4_675 . ?
O3 Cu2 O1 94.79(16) . . ?
O15 Cu2 O6 94.02(16) 4_675 4_575 ?
O3 Cu2 O6 171.89(17) . 4_575 ?
O1 Cu2 O6 80.75(15) . 4_575 ?
O15 Cu2 Cu1 135.18(12) 4_675 . ?
O3 Cu2 Cu1 133.78(12) . . ?
O1 Cu2 Cu1 39.62(10) . . ?
O6 Cu2 Cu1 41.17(10) 4_575 . ?
O6 Cu3 O1 170.31(15) . . ?
O6 Cu3 O4 84.23(16) . . ?
O1 Cu3 O4 93.57(15) . . ?
O6 Cu3 O2 100.06(16) . . ?
O1 Cu3 O2 89.11(16) . . ?
O4 Cu3 O2 122.27(17) . . ?
O6 Cu3 O16 90.47(15) . 1_655 ?
O1 Cu3 O16 86.45(15) . 1_655 ?
O4 Cu3 O16 148.26(17) . 1_655 ?
O2 Cu3 O16 89.48(17) . 1_655 ?
O6 Cu3 Cu1 130.98(11) . . ?
O1 Cu3 Cu1 39.49(10) . . ?
O4 Cu3 Cu1 77.54(11) . . ?
O2 Cu3 Cu1 128.17(12) . . ?
O16 Cu3 Cu1 82.66(12) 1_655 . ?
Cu3 O1 Cu1 101.16(17) . . ?
Cu3 O1 Cu2 106.65(17) . . ?
Cu1 O1 Cu2 100.76(16) . . ?
Cu3 O1 H1A 115.5 . . ?
Cu1 O1 H1A 115.4 . . ?
Cu2 O1 H1A 115.4 . . ?
C1 O2 Cu3 127.5(4) . . ?
C1 O3 Cu2 128.5(4) . . ?
C15 O4 Cu3 128.1(4) . . ?
C15 O4 Cu1 131.5(4) . 4_576 ?
Cu3 O4 Cu1 92.14(14) . 4_576 ?
C15 O5 Cu1 127.8(4) . . ?
Cu3 O6 Cu1 109.58(18) . 4_576 ?
Cu3 O6 Cu2 110.20(18) . 4_576 ?
Cu1 O6 Cu2 97.43(15) 4_576 4_576 ?
Cu3 O6 H6A 112.8 . . ?
Cu1 O6 H6A 112.9 4_576 . ?
Cu2 O6 H6A 112.9 4_576 . ?
N2 O7A O8A 45.6(6) . . ?
N2 O8A O7A 45.6(6) . . ?
N1 O11B O12B 43.0(9) . . ?
N1 O12B O11B 43.0(9) . . ?
C28 O15 Cu2 127.4(4) . 4_476 ?
C28 O16 Cu3 131.6(4) . 1_455 ?
C14 O18 Cu1 107.4(4) . 2_645 ?
C30 O19 H19 109.1 . . ?
C33 O20 H20 109.8 . . ?
O2 C1 O3 127.7(5) . . ?
O2 C1 C2 116.6(5) . . ?
O3 C1 C2 115.7(5) . . ?
C7 C2 C3 118.6(6) . . ?
C7 C2 C1 121.3(6) . . ?
C3 C2 C1 120.1(6) . . ?
C4 C3 C2 119.6(7) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 123.4(7) . . ?
C3 C4 H4A 118.3 . . ?
C5 C4 H4A 118.3 . . ?
C4 C5 C6 115.5(7) . . ?
C4 C5 C8 119.0(8) . . ?
C6 C5 C8 125.3(8) . . ?
C5 C6 C7 122.5(8) . . ?
C5 C6 N1 121.1(8) . . ?
C7 C6 N1 116.3(8) . . ?
C2 C7 C6 120.2(7) . . ?
C2 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
C13 C8 C9 116.2(7) . . ?
C13 C8 C5 119.6(7) . . ?
C9 C8 C5 123.1(8) . . ?
C10 C9 C8 121.7(8) . . ?
C10 C9 N4 117.5(8) . . ?
C8 C9 N4 120.8(7) . . ?
C11 C10 C9 120.8(8) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C10 C11 C12 118.0(6) . . ?
C10 C11 C14 121.3(6) . . ?
C12 C11 C14 120.5(7) . . ?
C11 C12 C13 121.7(8) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C8 C13 C12 121.6(8) . . ?
C8 C13 H13A 119.2 . . ?
C12 C13 H13A 119.2 . . ?
O17 C14 O18 124.4(6) . . ?
O17 C14 C11 121.4(6) . . ?
O18 C14 C11 114.2(6) . . ?
O5 C15 O4 125.6(5) . . ?
O5 C15 C16 117.2(5) . . ?
O4 C15 C16 117.2(5) . . ?
C21 C16 C17 119.9(5) . . ?
C21 C16 C15 121.8(5) . . ?
C17 C16 C15 118.3(5) . . ?
C18 C17 C16 119.4(6) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 122.8(6) . . ?
C17 C18 N2 116.5(6) . . ?
C19 C18 N2 120.7(6) . . ?
C18 C19 C20 116.2(6) . . ?
C18 C19 C22 124.4(6) . . ?
C20 C19 C22 119.4(6) . . ?
C21 C20 C19 121.1(6) . . ?
C21 C20 H20A 119.4 . . ?
C19 C20 H20A 119.4 . . ?
C16 C21 C20 120.4(6) . . ?
C16 C21 H21A 119.8 . . ?
C20 C21 H21A 119.8 . . ?
C23 C22 C27 117.8(6) . . ?
C23 C22 C19 118.7(6) . . ?
C27 C22 C19 123.5(7) . . ?
C22 C23 C24 121.8(6) . . ?
C22 C23 H23A 119.1 . . ?
C24 C23 H23A 119.1 . . ?
C25 C24 C23 119.6(6) . . ?
C25 C24 H24A 120.2 . . ?
C23 C24 H24A 120.2 . . ?
C26 C25 C24 119.6(5) . . ?
C26 C25 C28 119.1(5) . . ?
C24 C25 C28 121.3(5) . . ?
C25 C26 C27 119.3(6) . . ?
C25 C26 H26A 120.4 . . ?
C27 C26 H26A 120.4 . . ?
C22 C27 C26 121.5(6) . . ?
C22 C27 N3 122.6(6) . . ?
C26 C27 N3 115.6(6) . . ?
O16 C28 O15 126.0(5) . . ?
O16 C28 C25 118.4(5) . . ?
O15 C28 C25 115.6(5) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C29 109.0(2) . . ?
O19 C30 C31 109.0(2) . . ?
C29 C30 C31 109.1(2) . . ?
O19 C30 H30A 109.9 . . ?
C29 C30 H30A 109.9 . . ?
C31 C30 H30A 109.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O20 C33 C34 108.9(2) . . ?
O20 C33 C32 108.9(2) . . ?
C34 C33 C32 109.5(2) . . ?
O20 C33 H33A 109.8 . . ?
C34 C33 H33A 109.8 . . ?
C32 C33 H33A 109.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O11B N1 O12B 94.0(18) . . ?
O11B N1 O12A 116.9(17) . . ?
O12B N1 O12A 56.6(13) . . ?
O11B N1 O11A 43.4(10) . . ?
O12B N1 O11A 131.3(18) . . ?
O12A N1 O11A 114.6(18) . . ?
O11B N1 C6 123.2(14) . . ?
O12B N1 C6 107.1(15) . . ?
O12A N1 C6 118.8(13) . . ?
O11A N1 C6 115.9(13) . . ?
O8A N2 O7A 88.8(13) . . ?
O8A N2 O7B 109.2(12) . . ?
O7A N2 O7B 39.5(9) . . ?
O8A N2 O8B 62.2(9) . . ?
O7A N2 O8B 129.2(11) . . ?
O7B N2 O8B 109.2(11) . . ?
O8A N2 C18 124.8(10) . . ?
O7A N2 C18 114.9(10) . . ?
O7B N2 C18 120.7(8) . . ?
O8B N2 C18 115.9(8) . . ?
O9 N3 O10 120.2(7) . . ?
O9 N3 C27 119.3(6) . . ?
O10 N3 C27 120.0(6) . . ?
O13B N4 O14A 118.5(15) . . ?
O13B N4 O14B 115.0(16) . . ?
O14A N4 O14B 36.7(11) . . ?
O13B N4 O13A 35.0(11) . . ?
O14A N4 O13A 116.9(16) . . ?
O14B N4 O13A 137.1(15) . . ?
O13B N4 C9 121.2(12) . . ?
O14A N4 C9 120.1(12) . . ?
O14B N4 C9 114.0(11) . . ?
O13A N4 C9 108.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 977436'
#######################################################################
#
#                 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_624a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C4 H10 O)'
_chemical_formula_sum            'C36 H34 Cu3 N4 O20'
_chemical_formula_weight         1033.29

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'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.3370(18)
_cell_length_b                   32.832(4)
_cell_length_c                   10.1057(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.549(2)
_cell_angle_gamma                90.00
_cell_volume                     4877.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6823
_cell_measurement_theta_min      1.08
_cell_measurement_theta_max      25.22

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33795
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8512
_reflns_number_gt                6335
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0941P)²+34.4876P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8512
_refine_ls_number_parameters     596
_refine_ls_number_restraints     267
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0821
_refine_ls_wR_factor_ref         0.2202
_refine_ls_wR_factor_gt          0.2085
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.060
_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
Cu3 Cu 0.58029(4) 0.216635(19) 0.22464(7) 0.02227(15) Uani 1 1 d . . .
Cu2 Cu 0.50722(4) 0.217262(19) 0.48308(7) 0.02497(16) Uani 1 1 d . . .
Cu1 Cu 0.65408(4) 0.274672(18) 0.45990(7) 0.02106(15) Uani 1 1 d . . .
O1 O 0.6177(2) 0.21803(10) 0.4248(4) 0.0202(8) Uani 1 1 d . . .
H1 H 0.6577 0.2006 0.4639 0.024 Uiso 1 1 d R . .
O2 O 0.5324(3) 0.15784(12) 0.2347(4) 0.0345(10) Uani 1 1 d . . .
O3 O 0.4720(3) 0.16264(11) 0.4141(4) 0.0295(9) Uani 1 1 d . . .
O4 O 0.7051(2) 0.22832(13) 0.2109(4) 0.0304(10) Uani 1 1 d . . .
O5 O 0.7626(2) 0.26671(12) 0.4001(4) 0.0300(9) Uani 1 1 d . . .
O6 O 0.5443(2) 0.27519(10) 0.5272(4) 0.0213(8) Uani 1 1 d . . .
H6 H 0.5042 0.2921 0.4844 0.026 Uiso 1 1 d R . .
O7A O 1.0479(7) 0.3345(3) 0.4601(9) 0.088(2) Uani 0.50 1 d PDU A 1
O7B O 1.0255(6) 0.3457(2) 0.3957(13) 0.088(2) Uani 0.50 1 d PDU A 2
O8A O 1.0983(6) 0.3366(3) 0.2941(10) 0.088(2) Uani 0.50 1 d PDU A 1
O8B O 1.1428(4) 0.3069(4) 0.4012(14) 0.088(2) Uani 0.50 1 d PDU A 2
O9A O 1.0035(3) 0.3048(3) -0.0006(12) 0.0661(13) Uani 0.50 1 d PDU B 1
O9B O 1.0052(3) 0.3145(4) 0.0410(11) 0.0661(13) Uani 0.50 1 d PDU B 2
O10A O 1.1190(6) 0.3456(2) 0.0049(11) 0.0653(13) Uani 0.50 1 d PDU B 1
O10B O 1.1055(6) 0.3367(3) -0.0474(8) 0.0653(13) Uani 0.50 1 d PDU B 2
O11A O 0.2754(8) -0.0040(3) 0.3932(18) 0.115(4) Uani 0.50 1 d PDU C 1
O11B O 0.2425(8) 0.0024(2) 0.3021(15) 0.096(3) Uani 0.50 1 d PDU D 2
O12A O 0.2758(7) 0.0518(4) 0.4728(14) 0.138(3) Uani 0.50 1 d PDU C 1
O12B O 0.2247(6) 0.0595(4) 0.3631(18) 0.138(3) Uani 0.50 1 d PDU D 2
O13A O 0.2942(9) 0.01869(19) 0.0053(16) 0.101(2) Uani 0.50 1 d PDU E 1
O13B O 0.2651(6) 0.0097(3) 0.0221(14) 0.101(2) Uani 0.50 1 d PDU E 2
O14A O 0.2948(11) -0.0300(4) -0.1281(7) 0.101(2) Uani 0.50 1 d PDU E 1
O14B O 0.3385(6) -0.0264(4) -0.1087(8) 0.101(2) Uani 0.50 1 d PDU E 2
O15 O 1.4018(3) 0.27874(12) 0.0487(4) 0.0323(10) Uani 1 1 d . . .
O16 O 1.4543(2) 0.23979(12) 0.2354(4) 0.0302(9) Uani 1 1 d . . .
O17 O 0.4011(3) -0.18018(14) 0.2701(5) 0.0513(14) Uani 1 1 d . . .
O18 O 0.3360(3) -0.16751(12) 0.0463(4) 0.0377(11) Uani 1 1 d . . .
O19 O 0.73687(19) 0.16368(13) 0.5464(5) 0.213(2) Uani 1 1 d DU . .
H19 H 0.6978(4) 0.1588(9) 0.5895(10) 0.319 Uiso 1 1 d D . .
O20 O 0.4260(4) 0.32648(13) 0.3862(3) 0.240(2) Uani 1 1 d DU . .
H20 H 0.4095(12) 0.3179(2) 0.3035(5) 0.360 Uiso 1 1 d D . .
C1 C 0.4923(4) 0.14391(18) 0.3179(6) 0.0328(14) Uani 1 1 d . . .
C2 C 0.4655(4) 0.09983(17) 0.2993(6) 0.0330(14) Uani 1 1 d . . .
C3 C 0.5113(5) 0.0736(2) 0.2381(8) 0.057(2) Uani 1 1 d . . .
H3A H 0.5585 0.0833 0.2061 0.069 Uiso 1 1 calc R . .
C4 C 0.4882(6) 0.0325(2) 0.2227(10) 0.068(2) Uani 1 1 d . . .
H4A H 0.5226 0.0149 0.1859 0.081 Uiso 1 1 calc R . .
C5 C 0.4137(5) 0.01730(19) 0.2619(8) 0.0506(19) Uani 1 1 d . . .
C6 C 0.3698(5) 0.0447(2) 0.3252(8) 0.055(2) Uani 1 1 d D . .
C7 C 0.3951(5) 0.08483(19) 0.3467(8) 0.0484(18) Uani 1 1 d . . .
H7A H 0.3652 0.1019 0.3928 0.058 Uiso 1 1 calc R . .
C8 C 0.3932(5) -0.0269(2) 0.2400(8) 0.054(2) Uani 1 1 d . . .
C9 C 0.3515(6) -0.0434(2) 0.1132(9) 0.063(2) Uani 1 1 d . E .
C10 C 0.3421(5) -0.0851(2) 0.0883(8) 0.054(2) Uani 1 1 d . . .
H10A H 0.3127 -0.0950 0.0007 0.065 Uiso 1 1 calc R C .
C11 C 0.3774(5) -0.11131(18) 0.1963(7) 0.0406(16) Uani 1 1 d . . .
C12 C 0.4212(6) -0.0953(2) 0.3242(8) 0.059(2) Uani 1 1 d . . .
H12A H 0.4462 -0.1127 0.3976 0.071 Uiso 1 1 calc R C .
C13 C 0.4285(6) -0.0542(2) 0.3446(9) 0.065(3) Uani 1 1 d . . .
H13A H 0.4584 -0.0444 0.4321 0.078 Uiso 1 1 calc R . .
C14 C 0.3724(4) -0.15672(18) 0.1737(7) 0.0353(15) Uani 1 1 d . . .
C15 C 0.7694(4) 0.24775(17) 0.2966(6) 0.0261(13) Uani 1 1 d . . .
C16 C 0.8592(4) 0.24832(19) 0.2689(6) 0.0291(14) Uani 1 1 d . . .
C17 C 0.9173(5) 0.2805(2) 0.3223(7) 0.0480(18) Uani 1 1 d . . .
H17A H 0.8998 0.3007 0.3740 0.058 Uiso 1 1 calc R . .
C18 C 1.0011(4) 0.2823(2) 0.2979(7) 0.0482(19) Uani 1 1 d . A .
C19 C 1.0305(4) 0.2521(2) 0.2203(7) 0.0426(18) Uani 1 1 d U . .
C20 C 0.9728(4) 0.2194(2) 0.1754(7) 0.0399(17) Uani 1 1 d U . .
H20A H 0.9919 0.1980 0.1301 0.048 Uiso 1 1 calc R . .
C21 C 0.8873(4) 0.2177(2) 0.1960(7) 0.0418(17) Uani 1 1 d . . .
H21A H 0.8488 0.1960 0.1608 0.050 Uiso 1 1 calc R . .
C22 C 1.1210(4) 0.2534(2) 0.1903(7) 0.0410(13) Uani 1 1 d U . .
C23 C 1.1847(4) 0.2230(2) 0.2466(7) 0.0425(12) Uani 1 1 d U . .
H23A H 1.1676 0.2015 0.2936 0.051 Uiso 1 1 calc R . .
C24 C 1.2716(4) 0.2240(2) 0.2348(6) 0.0362(11) Uani 1 1 d U . .
H24A H 1.3129 0.2038 0.2764 0.043 Uiso 1 1 calc R . .
C25 C 1.2981(4) 0.2551(2) 0.1606(6) 0.0328(11) Uani 1 1 d U . .
C26 C 1.2341(4) 0.2843(2) 0.0979(6) 0.0339(12) Uani 1 1 d U . .
H26A H 1.2501 0.3050 0.0463 0.041 Uiso 1 1 calc R . .
C27 C 1.1473(4) 0.28298(19) 0.1112(6) 0.0340(11) Uani 1 1 d U B .
C28 C 1.3936(3) 0.25803(16) 0.1493(6) 0.0236(12) Uani 1 1 d . . .
C29 C 0.8429(5) 0.1082(2) 0.6394(5) 0.225(2) Uani 1 1 d DU . .
H29A H 0.8190 0.1081 0.7175 0.338 Uiso 1 1 calc R . .
H29B H 0.8959 0.1253 0.6588 0.338 Uiso 1 1 calc R . .
H29C H 0.8590 0.0810 0.6212 0.338 Uiso 1 1 calc R . .
C30 C 0.7698(4) 0.12489(18) 0.5114(5) 0.2230(13) Uani 1 1 d DU . .
H30A H 0.7192 0.1056 0.4834 0.268 Uiso 1 1 calc R . .
C31 C 0.8124(4) 0.1312(3) 0.3914(4) 0.2251(14) Uani 1 1 d DU . .
H31A H 0.8236 0.1599 0.3815 0.270 Uiso 1 1 calc R . .
H31B H 0.8701 0.1169 0.4113 0.270 Uiso 1 1 calc R . .
C32 C 0.7473(9) 0.1148(5) 0.2556(8) 0.230(2) Uani 1 1 d DU . .
H32A H 0.7761 0.1167 0.1830 0.346 Uiso 1 1 calc R . .
H32B H 0.6923 0.1306 0.2317 0.346 Uiso 1 1 calc R . .
H32C H 0.7329 0.0868 0.2678 0.346 Uiso 1 1 calc R . .
C33 C 0.3094(3) 0.3637(2) 0.4563(5) 0.244(2) Uani 1 1 d DU . .
H33A H 0.3321 0.3553 0.5509 0.366 Uiso 1 1 calc R . .
H33B H 0.2659 0.3441 0.4063 0.366 Uiso 1 1 calc R . .
H33C H 0.2807 0.3898 0.4520 0.366 Uiso 1 1 calc R . .
C34 C 0.3890(4) 0.36662(15) 0.3915(5) 0.2427(13) Uani 1 1 d DU . .
H34A H 0.4364 0.3846 0.4476 0.291 Uiso 1 1 calc R . .
C35 C 0.3538(6) 0.38389(14) 0.2437(5) 0.2434(14) Uani 1 1 d DU . .
H35A H 0.2927 0.3740 0.2011 0.292 Uiso 1 1 calc R . .
H35B H 0.3925 0.3745 0.1888 0.292 Uiso 1 1 calc R . .
C36 C 0.3536(15) 0.43104(16) 0.2470(15) 0.248(2) Uani 1 1 d DU . .
H36A H 0.3288 0.4413 0.1550 0.371 Uiso 1 1 calc R . .
H36B H 0.4147 0.4408 0.2840 0.371 Uiso 1 1 calc R . .
H36C H 0.3171 0.4403 0.3041 0.371 Uiso 1 1 calc R . .
N1A N 0.3125(8) 0.0291(3) 0.4097(14) 0.0827(19) Uani 0.50 1 d PDU C 1
N1B N 0.2789(7) 0.0347(3) 0.3434(16) 0.0827(19) Uani 0.50 1 d PD D 2
N2 N 1.0616(3) 0.3157(2) 0.3633(7) 0.075(2) Uani 1 1 d DU . .
N3 N 1.0838(3) 0.31499(16) 0.0362(6) 0.0529(14) Uani 1 1 d DU . .
N4 N 0.3111(6) -0.01697(18) -0.0103(7) 0.095(3) Uani 1 1 d DU . .


_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
Cu3 O6 1.931(4) 4_565 ?
Cu3 O1 1.939(4) . ?
Cu3 O4 1.996(4) . ?
Cu3 O2 2.078(4) . ?
Cu3 O16 2.107(4) 1_455 ?
Cu3 Cu1 3.0052(9) . ?
Cu2 O15 1.919(4) 4_466 ?
Cu2 O3 1.944(4) . ?
Cu2 O1 1.946(3) . ?
Cu2 O6 1.999(3) . ?
Cu2 Cu1 2.9969(9) . ?
Cu1 O18 1.907(4) 2_655 ?
Cu1 O5 1.944(4) . ?
Cu1 O1 1.945(3) . ?
Cu1 O6 1.988(3) . ?
Cu1 O4 2.434(4) 4_566 ?
O1 H1 0.8501 . ?
O2 C1 1.261(7) . ?
O3 C1 1.262(7) . ?
O4 C15 1.282(6) . ?
O4 Cu1 2.434(4) 4_565 ?
O5 C15 1.247(7) . ?
O6 Cu3 1.931(4) 4_566 ?
O6 H6 0.8497 . ?
O7A N2 1.223(5) . ?
O7B N2 1.220(5) . ?
O8A N2 1.225(5) . ?
O8B N2 1.228(5) . ?
O9A N3 1.226(4) . ?
O9B N3 1.220(4) . ?
O10A N3 1.226(5) . ?
O10B N3 1.223(5) . ?
O11A N1A 1.216(5) . ?
O11B N1B 1.218(5) . ?
O12A N1A 1.218(5) . ?
O12B N1B 1.219(5) . ?
O13A N4 1.219(5) . ?
O13B N4 1.226(5) . ?
O14A N4 1.222(5) . ?
O14B N4 1.225(5) . ?
O15 C28 1.259(7) . ?
O15 Cu2 1.919(4) 4_665 ?
O16 C28 1.233(6) . ?
O16 Cu3 2.107(4) 1_655 ?
O17 C14 1.221(8) . ?
O18 C14 1.298(8) . ?
O18 Cu1 1.907(4) 2_645 ?
O19 C30 1.450(4) . ?
O19 H19 0.850(2) . ?
O20 C34 1.441(4) . ?
O20 H20 0.850(2) . ?
C1 C2 1.502(8) . ?
C2 C3 1.365(9) . ?
C2 C7 1.390(9) . ?
C3 C4 1.392(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.403(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.385(10) . ?
C5 C8 1.489(9) . ?
C6 C7 1.372(9) . ?
C6 N1A 1.482(12) . ?
C6 N1B 1.494(11) . ?
C7 H7A 0.9300 . ?
C8 C9 1.371(11) . ?
C8 C13 1.373(11) . ?
C9 C10 1.391(10) . ?
C9 N4 1.502(10) . ?
C10 C11 1.374(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.380(10) . ?
C11 C14 1.507(8) . ?
C12 C13 1.363(10) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.481(8) . ?
C16 C21 1.386(9) . ?
C16 C17 1.388(9) . ?
C17 C18 1.378(9) . ?
C17 H17A 0.9300 . ?
C18 C19 1.415(10) . ?
C18 N2 1.468(9) . ?
C19 C20 1.381(9) . ?
C19 C22 1.503(8) . ?
C20 C21 1.386(9) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C27 1.390(9) . ?
C22 C23 1.398(9) . ?
C23 C24 1.372(9) . ?
C23 H23A 0.9300 . ?
C24 C25 1.395(9) . ?
C24 H24A 0.9300 . ?
C25 C26 1.390(8) . ?
C25 C28 1.504(7) . ?
C26 C27 1.375(8) . ?
C26 H26A 0.9300 . ?
C27 N3 1.486(8) . ?
C29 C30 1.551(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.546(5) . ?
C30 H30A 0.9800 . ?
C31 C32 1.546(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.545(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.544(4) . ?
C34 H34A 0.9800 . ?
C35 C36 1.549(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Cu3 O1 170.64(14) 4_565 . ?
O6 Cu3 O4 84.20(15) 4_565 . ?
O1 Cu3 O4 93.66(15) . . ?
O6 Cu3 O2 100.29(15) 4_565 . ?
O1 Cu3 O2 88.54(15) . . ?
O4 Cu3 O2 122.77(17) . . ?
O6 Cu3 O16 90.37(15) 4_565 1_455 ?
O1 Cu3 O16 86.60(15) . 1_455 ?
O4 Cu3 O16 147.76(16) . 1_455 ?
O2 Cu3 O16 89.46(16) . 1_455 ?
O6 Cu3 Cu1 131.42(11) 4_565 . ?
O1 Cu3 Cu1 39.38(10) . . ?
O4 Cu3 Cu1 77.34(12) . . ?
O2 Cu3 Cu1 127.51(12) . . ?
O16 Cu3 Cu1 82.80(11) 1_455 . ?
O15 Cu2 O3 90.65(16) 4_466 . ?
O15 Cu2 O1 174.70(15) 4_466 . ?
O3 Cu2 O1 94.62(15) . . ?
O15 Cu2 O6 94.13(15) 4_466 . ?
O3 Cu2 O6 171.96(16) . . ?
O1 Cu2 O6 80.70(14) . . ?
O15 Cu2 Cu1 135.24(12) 4_466 . ?
O3 Cu2 Cu1 133.68(12) . . ?
O1 Cu2 Cu1 39.61(10) . . ?
O6 Cu2 Cu1 41.12(10) . . ?
O18 Cu1 O5 92.32(18) 2_655 . ?
O18 Cu1 O1 165.28(17) 2_655 . ?
O5 Cu1 O1 92.39(16) . . ?
O18 Cu1 O6 94.92(16) 2_655 . ?
O5 Cu1 O6 172.58(16) . . ?
O1 Cu1 O6 80.99(14) . . ?
O18 Cu1 O4 93.99(16) 2_655 4_566 ?
O5 Cu1 O4 105.60(14) . 4_566 ?
O1 Cu1 O4 98.16(15) . 4_566 ?
O6 Cu1 O4 72.31(13) . 4_566 ?
O18 Cu1 Cu2 134.21(13) 2_655 . ?
O5 Cu1 Cu2 132.00(12) . . ?
O1 Cu1 Cu2 39.63(10) . . ?
O6 Cu1 Cu2 41.39(10) . . ?
O4 Cu1 Cu2 85.36(9) 4_566 . ?
O18 Cu1 Cu3 128.37(13) 2_655 . ?
O5 Cu1 Cu3 80.31(11) . . ?
O1 Cu1 Cu3 39.25(11) . . ?
O6 Cu1 Cu3 96.39(10) . . ?
O4 Cu1 Cu3 137.37(10) 4_566 . ?
Cu2 Cu1 Cu3 62.68(2) . . ?
Cu3 O1 Cu1 101.37(16) . . ?
Cu3 O1 Cu2 106.94(16) . . ?
Cu1 O1 Cu2 100.76(15) . . ?
Cu3 O1 H1 115.4 . . ?
Cu1 O1 H1 115.3 . . ?
Cu2 O1 H1 115.3 . . ?
C1 O2 Cu3 128.0(4) . . ?
C1 O3 Cu2 128.4(4) . . ?
C15 O4 Cu3 128.1(4) . . ?
C15 O4 Cu1 132.9(4) . 4_565 ?
Cu3 O4 Cu1 91.99(14) . 4_565 ?
C15 O5 Cu1 127.7(3) . . ?
Cu3 O6 Cu1 109.50(16) 4_566 . ?
Cu3 O6 Cu2 110.02(17) 4_566 . ?
Cu1 O6 Cu2 97.49(15) . . ?
Cu3 O6 H6 112.8 4_566 . ?
Cu1 O6 H6 113.0 . . ?
Cu2 O6 H6 113.0 . . ?
C28 O15 Cu2 127.1(3) . 4_665 ?
C28 O16 Cu3 131.2(4) . 1_655 ?
C14 O18 Cu1 106.8(4) . 2_645 ?
C30 O19 H19 108(2) . . ?
C34 O20 H20 109.3(5) . . ?
O2 C1 O3 127.7(5) . . ?
O2 C1 C2 115.7(5) . . ?
O3 C1 C2 116.6(5) . . ?
C3 C2 C7 118.9(6) . . ?
C3 C2 C1 120.5(6) . . ?
C7 C2 C1 120.6(6) . . ?
C2 C3 C4 120.9(7) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C3 C4 C5 121.1(7) . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 H4A 119.5 . . ?
C6 C5 C4 116.1(6) . . ?
C6 C5 C8 126.4(7) . . ?
C4 C5 C8 117.4(7) . . ?
C7 C6 C5 123.0(6) . . ?
C7 C6 N1A 115.4(7) . . ?
C5 C6 N1A 119.2(7) . . ?
C7 C6 N1B 115.0(7) . . ?
C5 C6 N1B 120.5(6) . . ?
N1A C6 N1B 28.9(7) . . ?
C6 C7 C2 119.8(6) . . ?
C6 C7 H7A 120.1 . . ?
C2 C7 H7A 120.1 . . ?
C9 C8 C13 116.0(6) . . ?
C9 C8 C5 123.1(7) . . ?
C13 C8 C5 120.1(7) . . ?
C8 C9 C10 123.7(7) . . ?
C8 C9 N4 121.4(6) . . ?
C10 C9 N4 114.9(7) . . ?
C11 C10 C9 118.4(7) . . ?
C11 C10 H10A 120.8 . . ?
C9 C10 H10A 120.8 . . ?
C10 C11 C12 118.8(6) . . ?
C10 C11 C14 120.5(6) . . ?
C12 C11 C14 120.6(6) . . ?
C13 C12 C11 121.1(7) . . ?
C13 C12 H12A 119.5 . . ?
C11 C12 H12A 119.5 . . ?
C12 C13 C8 122.1(7) . . ?
C12 C13 H13A 119.0 . . ?
C8 C13 H13A 119.0 . . ?
O17 C14 O18 125.0(5) . . ?
O17 C14 C11 120.8(6) . . ?
O18 C14 C11 114.2(5) . . ?
O5 C15 O4 125.7(5) . . ?
O5 C15 C16 117.1(5) . . ?
O4 C15 C16 117.2(5) . . ?
C21 C16 C17 119.7(6) . . ?
C21 C16 C15 122.5(5) . . ?
C17 C16 C15 117.7(5) . . ?
C18 C17 C16 119.4(7) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 122.1(6) . . ?
C17 C18 N2 116.9(6) . . ?
C19 C18 N2 120.9(6) . . ?
C20 C19 C18 116.7(6) . . ?
C20 C19 C22 119.9(6) . . ?
C18 C19 C22 123.4(6) . . ?
C19 C20 C21 121.8(6) . . ?
C19 C20 H20A 119.1 . . ?
C21 C20 H20A 119.1 . . ?
C20 C21 C16 120.1(6) . . ?
C20 C21 H21A 120.0 . . ?
C16 C21 H21A 120.0 . . ?
C27 C22 C23 116.7(6) . . ?
C27 C22 C19 124.9(6) . . ?
C23 C22 C19 118.4(6) . . ?
C24 C23 C22 122.1(6) . . ?
C24 C23 H23A 118.9 . . ?
C22 C23 H23A 118.9 . . ?
C23 C24 C25 120.2(6) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
C26 C25 C24 118.3(5) . . ?
C26 C25 C28 119.8(5) . . ?
C24 C25 C28 121.8(5) . . ?
C27 C26 C25 120.7(6) . . ?
C27 C26 H26A 119.6 . . ?
C25 C26 H26A 119.6 . . ?
C26 C27 C22 121.7(6) . . ?
C26 C27 N3 116.2(5) . . ?
C22 C27 N3 122.1(5) . . ?
O16 C28 O15 127.1(5) . . ?
O16 C28 C25 118.1(5) . . ?
O15 C28 C25 114.8(5) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C31 109.2(4) . . ?
O19 C30 C29 109.0(4) . . ?
C31 C30 C29 109.6(4) . . ?
O19 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
C29 C30 H30A 109.7 . . ?
C32 C31 C30 109.8(6) . . ?
C32 C31 H31A 109.7 . . ?
C30 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O20 C34 C35 109.4(3) . . ?
O20 C34 C33 109.0(4) . . ?
C35 C34 C33 109.4(3) . . ?
O20 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
C33 C34 H34A 109.7 . . ?
C34 C35 C36 110.4(6) . . ?
C34 C35 H35A 109.6 . . ?
C36 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
C36 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O11A N1A O12A 110.6(13) . . ?
O11A N1A C6 124.1(12) . . ?
O12A N1A C6 121.9(10) . . ?
O11B N1B O12B 111.7(11) . . ?
O11B N1B C6 120.2(10) . . ?
O12B N1B C6 125.3(9) . . ?
O7B N2 O7A 35.4(8) . . ?
O7B N2 O8A 91.0(9) . . ?
O7A N2 O8A 112.7(9) . . ?
O7B N2 O8B 127.2(9) . . ?
O7A N2 O8B 105.0(10) . . ?
O8A N2 O8B 73.7(8) . . ?
O7B N2 C18 116.6(6) . . ?
O7A N2 C18 120.4(7) . . ?
O8A N2 C18 119.7(7) . . ?
O8B N2 C18 114.8(8) . . ?
O9B N3 O10B 120.2(8) . . ?
O9B N3 O10A 122.4(8) . . ?
O10B N3 O10A 27.8(6) . . ?
O9B N3 O9A 24.6(8) . . ?
O10B N3 O9A 113.4(8) . . ?
O10A N3 O9A 128.6(8) . . ?
O9B N3 C27 118.8(7) . . ?
O10B N3 C27 119.7(6) . . ?
O10A N3 C27 116.0(5) . . ?
O9A N3 C27 114.7(7) . . ?
O13A N4 O14A 118.1(11) . . ?
O13A N4 O14B 118.9(12) . . ?
O14A N4 O14B 31.0(9) . . ?
O13A N4 O13B 28.3(9) . . ?
O14A N4 O13B 122.5(11) . . ?
O14B N4 O13B 139.0(11) . . ?
O13A N4 C9 120.0(9) . . ?
O14A N4 C9 121.9(8) . . ?
O14B N4 C9 111.8(8) . . ?
O13B N4 C9 108.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.149
_database_code_depnum_ccdc_archive 'CCDC 977437'
#######################################################################
#
#                 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_616a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H14 Cu3 N4 O18, 2(C4 H10 O)'
_chemical_formula_sum            'C36 H34 Cu3 N4 O20'
_chemical_formula_weight         1033.29

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'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.3332(15)
_cell_length_b                   32.852(3)
_cell_length_c                   10.1075(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.5650(10)
_cell_angle_gamma                90.00
_cell_volume                     4880.2(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7609
_cell_measurement_theta_min      1.18
_cell_measurement_theta_max      25.54

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Green'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    1.369
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33903
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8515
_reflns_number_gt                6481
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0962P)²+31.0992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8515
_refine_ls_number_parameters     596
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0800
_refine_ls_wR_factor_ref         0.2163
_refine_ls_wR_factor_gt          0.2051
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.057
_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
Cu3 Cu 0.57981(5) 0.21666(2) 0.22383(8) 0.0222(2) Uani 1 1 d . . .
Cu2 Cu 0.50667(5) 0.21733(2) 0.48218(9) 0.0253(2) Uani 1 1 d . . .
Cu1 Cu 0.65344(5) 0.27473(2) 0.45904(8) 0.0211(2) Uani 1 1 d . . .
O1 O 0.6172(3) 0.21805(12) 0.4237(4) 0.0211(9) Uani 1 1 d . . .
H1 H 0.6573 0.2006 0.4628 0.025 Uiso 1 1 d RD . .
O2 O 0.5319(3) 0.15800(13) 0.2335(5) 0.0338(11) Uani 1 1 d . . .
O3 O 0.4715(3) 0.16262(13) 0.4134(5) 0.0304(11) Uani 1 1 d . . .
O4 O 0.7049(3) 0.22826(15) 0.2105(5) 0.0292(10) Uani 1 1 d . . .
O5 O 0.7619(3) 0.26697(15) 0.3987(5) 0.0308(11) Uani 1 1 d . . .
O6 O 0.5437(3) 0.27520(12) 0.5267(4) 0.0209(9) Uani 1 1 d . . .
H6 H 0.5036 0.2921 0.4839 0.025 Uiso 1 1 d R . .
O7A O 1.0466(12) 0.3345(5) 0.4569(15) 0.087(2) Uani 0.50 1 d PDU A 1
O7B O 1.0254(12) 0.3459(4) 0.3929(19) 0.087(2) Uani 0.50 1 d PDU A 2
O8A O 1.0968(11) 0.3369(4) 0.2912(15) 0.087(2) Uani 0.50 1 d PDU A 1
O8B O 1.1423(7) 0.3071(5) 0.3995(17) 0.087(2) Uani 0.50 1 d PDU A 2
O9A O 1.0034(6) 0.3045(5) 0.0009(18) 0.069(3) Uani 0.50 1 d PDU B 1
O9B O 1.0044(6) 0.3143(5) 0.0377(18) 0.069(3) Uani 0.50 1 d PDU B 2
O10A O 1.1174(10) 0.3457(3) 0.0047(15) 0.066(3) Uani 0.50 1 d PDU B 1
O10B O 1.1058(10) 0.3364(4) -0.0475(13) 0.066(3) Uani 0.50 1 d PDU B 2
O11A O 0.2742(13) -0.0036(5) 0.387(2) 0.099(5) Uani 0.50 1 d PDU C 1
O11B O 0.2409(13) 0.0026(5) 0.296(2) 0.104(6) Uani 0.50 1 d PDU D 2
O12A O 0.2770(16) 0.0509(7) 0.475(2) 0.136(6) Uani 0.50 1 d PDU C 1
O12B O 0.2258(15) 0.0587(6) 0.366(3) 0.136(6) Uani 0.50 1 d PDU D 2
O13A O 0.2941(15) 0.0184(3) 0.008(2) 0.101(3) Uani 0.50 1 d PDU E 1
O13B O 0.2649(13) 0.0096(5) 0.021(2) 0.101(3) Uani 0.50 1 d PDU E 2
O14A O 0.2941(14) -0.0303(6) -0.1284(13) 0.101(3) Uani 0.50 1 d PDU E 1
O14B O 0.3387(13) -0.0266(7) -0.1091(16) 0.101(3) Uani 0.50 1 d PDU E 2
O15 O 1.4012(3) 0.27866(14) 0.0478(5) 0.0324(11) Uani 1 1 d . . .
O16 O 1.4540(3) 0.23979(14) 0.2346(5) 0.0295(10) Uani 1 1 d . . .
O17 O 0.4013(4) -0.18022(16) 0.2702(6) 0.0519(15) Uani 1 1 d . . .
O18 O 0.3370(3) -0.16749(14) 0.0473(5) 0.0365(12) Uani 1 1 d . . .
O19 O 0.7359(11) 0.1637(5) 0.5477(16) 0.209(5) Uani 1 1 d DU . .
H19 H 0.709(11) 0.158(3) 0.608(16) 0.313 Uiso 1 1 d D . .
O20 O 0.4255(13) 0.3262(5) 0.3829(19) 0.240(6) Uani 1 1 d DU . .
H20 H 0.41(2) 0.317(4) 0.301(5) 0.360 Uiso 1 1 d D . .
C1 C 0.4924(5) 0.1438(2) 0.3167(8) 0.0323(16) Uani 1 1 d . . .
C2 C 0.4652(5) 0.1000(2) 0.2989(8) 0.0334(16) Uani 1 1 d . . .
C3 C 0.5110(7) 0.0737(2) 0.2367(10) 0.056(2) Uani 1 1 d . . .
H3A H 0.5581 0.0835 0.2044 0.067 Uiso 1 1 calc R . .
C4 C 0.4879(7) 0.0326(3) 0.2214(11) 0.064(3) Uani 1 1 d . . .
H4A H 0.5220 0.0150 0.1836 0.077 Uiso 1 1 calc R . .
C5 C 0.4143(6) 0.0173(2) 0.2617(9) 0.052(2) Uani 1 1 d . . .
C6 C 0.3699(6) 0.0445(2) 0.3252(11) 0.057(2) Uani 1 1 d D . .
C7 C 0.3951(6) 0.0849(2) 0.3460(10) 0.050(2) Uani 1 1 d . . .
H7A H 0.3649 0.1020 0.3917 0.061 Uiso 1 1 calc R . .
C8 C 0.3933(6) -0.0268(2) 0.2402(10) 0.052(2) Uani 1 1 d . . .
C9 C 0.3514(7) -0.0436(2) 0.1128(10) 0.062(3) Uani 1 1 d . E .
C10 C 0.3427(7) -0.0850(2) 0.0888(10) 0.057(2) Uani 1 1 d . . .
H10A H 0.3136 -0.0950 0.0012 0.068 Uiso 1 1 calc R C .
C11 C 0.3779(5) -0.1113(2) 0.1971(9) 0.0403(18) Uani 1 1 d . . .
C12 C 0.4210(7) -0.0953(2) 0.3243(10) 0.059(3) Uani 1 1 d . . .
H12A H 0.4453 -0.1127 0.3980 0.071 Uiso 1 1 calc R C .
C13 C 0.4291(8) -0.0539(3) 0.3448(11) 0.065(3) Uani 1 1 d . . .
H13A H 0.4596 -0.0440 0.4319 0.079 Uiso 1 1 calc R . .
C14 C 0.3732(5) -0.1567(2) 0.1753(9) 0.0378(18) Uani 1 1 d . . .
C15 C 0.7683(4) 0.24786(19) 0.2959(7) 0.0253(14) Uani 1 1 d . . .
C16 C 0.8588(4) 0.2483(2) 0.2681(7) 0.0274(15) Uani 1 1 d . . .
C17 C 0.9169(6) 0.2806(3) 0.3217(9) 0.046(2) Uani 1 1 d . . .
H17A H 0.8996 0.3009 0.3732 0.055 Uiso 1 1 calc R . .
C18 C 1.0003(5) 0.2819(3) 0.2969(8) 0.045(2) Uani 1 1 d . A .
C19 C 1.0306(5) 0.2521(3) 0.2194(8) 0.0418(19) Uani 1 1 d . . .
C20 C 0.9727(4) 0.2193(3) 0.1750(8) 0.0394(19) Uani 1 1 d . . .
H20A H 0.9918 0.1977 0.1307 0.047 Uiso 1 1 calc R . .
C21 C 0.8864(5) 0.2180(2) 0.1951(8) 0.0405(18) Uani 1 1 d . . .
H21A H 0.8474 0.1965 0.1591 0.049 Uiso 1 1 calc R . .
C22 C 1.1207(5) 0.2535(3) 0.1907(8) 0.043(2) Uani 1 1 d . . .
C23 C 1.1845(5) 0.2230(3) 0.2453(9) 0.048(2) Uani 1 1 d . . .
H23A H 1.1672 0.2012 0.2911 0.058 Uiso 1 1 calc R . .
C24 C 1.2709(5) 0.2239(2) 0.2339(8) 0.0379(18) Uani 1 1 d . . .
H24A H 1.3121 0.2037 0.2753 0.045 Uiso 1 1 calc R . .
C25 C 1.2976(4) 0.2551(2) 0.1603(7) 0.0317(16) Uani 1 1 d . . .
C26 C 1.2334(4) 0.2844(2) 0.0959(8) 0.0346(17) Uani 1 1 d . . .
H26A H 1.2490 0.3047 0.0428 0.041 Uiso 1 1 calc R . .
C27 C 1.1468(5) 0.2831(2) 0.1112(8) 0.0351(17) Uani 1 1 d U B .
C28 C 1.3935(4) 0.25801(19) 0.1493(7) 0.0238(14) Uani 1 1 d . . .
C29 C 0.8445(14) 0.1090(6) 0.6394(18) 0.221(5) Uani 1 1 d DU . .
H29A H 0.8213 0.1088 0.7181 0.332 Uiso 1 1 calc R . .
H29B H 0.8970 0.1263 0.6578 0.332 Uiso 1 1 calc R . .
H29C H 0.8611 0.0819 0.6211 0.332 Uiso 1 1 calc R . .
C30 C 0.7702(10) 0.1253(4) 0.5121(14) 0.219(5) Uani 1 1 d DU . .
H30A H 0.7204 0.1056 0.4845 0.263 Uiso 1 1 calc R . .
C31 C 0.8118(12) 0.1323(6) 0.3913(16) 0.222(5) Uani 1 1 d DU . .
H31A H 0.8172 0.1612 0.3767 0.266 Uiso 1 1 calc R . .
H31B H 0.8721 0.1204 0.4135 0.266 Uiso 1 1 calc R . .
C32 C 0.7502(16) 0.1125(7) 0.2587(16) 0.227(5) Uani 1 1 d DU . .
H32A H 0.7791 0.1145 0.1862 0.341 Uiso 1 1 calc R . .
H32B H 0.6927 0.1264 0.2313 0.341 Uiso 1 1 calc R . .
H32C H 0.7405 0.0844 0.2761 0.341 Uiso 1 1 calc R . .
C33 C 0.3091(16) 0.3630(7) 0.455(2) 0.244(6) Uani 1 1 d DU . .
H33A H 0.3322 0.3547 0.5493 0.366 Uiso 1 1 calc R . .
H33B H 0.2659 0.3434 0.4049 0.366 Uiso 1 1 calc R . .
H33C H 0.2800 0.3891 0.4505 0.366 Uiso 1 1 calc R . .
C34 C 0.3886(12) 0.3663(5) 0.3896(15) 0.243(5) Uani 1 1 d DU . .
H34A H 0.4360 0.3841 0.4461 0.291 Uiso 1 1 calc R . .
C35 C 0.3530(17) 0.3839(5) 0.2424(15) 0.243(6) Uani 1 1 d DU . .
H35A H 0.2923 0.3736 0.1989 0.292 Uiso 1 1 calc R . .
H35B H 0.3923 0.3752 0.1876 0.292 Uiso 1 1 calc R . .
C36 C 0.3507(19) 0.4310(5) 0.247(2) 0.247(6) Uani 1 1 d DU . .
H36A H 0.3259 0.4414 0.1553 0.371 Uiso 1 1 calc R . .
H36B H 0.4113 0.4412 0.2851 0.371 Uiso 1 1 calc R . .
H36C H 0.3133 0.4395 0.3038 0.371 Uiso 1 1 calc R . .
N1A N 0.3142(12) 0.0287(5) 0.4111(19) 0.077(4) Uani 0.50 1 d PDU C 1
N1B N 0.2793(11) 0.0340(5) 0.344(2) 0.077(4) Uani 0.50 1 d PD D 2
N2 N 1.0610(5) 0.3157(3) 0.3609(9) 0.074(3) Uani 1 1 d DU . .
N3 N 1.0835(4) 0.3148(2) 0.0360(8) 0.0547(18) Uani 1 1 d DU . .
N4 N 0.3114(8) -0.0170(3) -0.0108(11) 0.094(3) Uani 1 1 d DU . .


_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
Cu3 O6 1.928(4) 4_565 ?
Cu3 O1 1.937(4) . ?
Cu3 O4 1.997(4) . ?
Cu3 O2 2.075(4) . ?
Cu3 O16 2.104(4) 1_455 ?
Cu3 Cu1 3.0060(11) . ?
Cu2 O15 1.919(4) 4_466 ?
Cu2 O3 1.947(4) . ?
Cu2 O1 1.948(4) . ?
Cu2 O6 1.998(4) . ?
Cu2 Cu1 2.9960(10) . ?
Cu1 O18 1.906(4) 2_655 ?
Cu1 O5 1.945(4) . ?
Cu1 O1 1.947(4) . ?
Cu1 O6 1.989(4) . ?
Cu1 O4 2.439(5) 4_566 ?
O1 H1 0.8500 . ?
O2 C1 1.257(8) . ?
O3 C1 1.273(8) . ?
O4 C15 1.276(8) . ?
O4 Cu1 2.439(5) 4_565 ?
O5 C15 1.242(8) . ?
O6 Cu3 1.928(4) 4_566 ?
O6 H6 0.8498 . ?
O7A N2 1.222(5) . ?
O7B N2 1.219(5) . ?
O8A N2 1.226(5) . ?
O8B N2 1.228(5) . ?
O9A N3 1.225(5) . ?
O9B N3 1.219(5) . ?
O10A N3 1.225(5) . ?
O10B N3 1.224(5) . ?
O11A N1A 1.216(5) . ?
O11B N1B 1.218(5) . ?
O12A N1A 1.218(5) . ?
O12B N1B 1.219(5) . ?
O13A N4 1.219(5) . ?
O13B N4 1.226(5) . ?
O14A N4 1.222(5) . ?
O14B N4 1.224(5) . ?
O15 C28 1.263(8) . ?
O15 Cu2 1.919(4) 4_665 ?
O16 C28 1.227(8) . ?
O16 Cu3 2.104(4) 1_655 ?
O17 C14 1.211(9) . ?
O18 C14 1.303(9) . ?
O18 Cu1 1.906(4) 2_645 ?
O19 C30 1.450(5) . ?
O19 H19 0.850(2) . ?
O20 C34 1.442(5) . ?
O20 H20 0.850(2) . ?
C1 C2 1.493(9) . ?
C2 C3 1.374(10) . ?
C2 C7 1.386(10) . ?
C3 C4 1.395(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.398(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.389(12) . ?
C5 C8 1.486(10) . ?
C6 C7 1.381(11) . ?
C6 N1A 1.475(15) . ?
C6 N1B 1.497(14) . ?
C7 H7A 0.9300 . ?
C8 C13 1.370(13) . ?
C8 C9 1.380(13) . ?
C9 C10 1.382(11) . ?
C9 N4 1.505(13) . ?
C10 C11 1.377(12) . ?
C10 H10A 0.9300 . ?
C11 C12 1.372(12) . ?
C11 C14 1.506(9) . ?
C12 C13 1.375(11) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.492(8) . ?
C16 C21 1.376(10) . ?
C16 C17 1.392(10) . ?
C17 C18 1.372(10) . ?
C17 H17A 0.9300 . ?
C18 C19 1.411(11) . ?
C18 N2 1.476(11) . ?
C19 C20 1.387(11) . ?
C19 C22 1.492(9) . ?
C20 C21 1.395(10) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C27 1.390(11) . ?
C22 C23 1.400(11) . ?
C23 C24 1.362(10) . ?
C23 H23A 0.9300 . ?
C24 C25 1.395(10) . ?
C24 H24A 0.9300 . ?
C25 C26 1.398(10) . ?
C25 C28 1.510(8) . ?
C26 C27 1.380(9) . ?
C26 H26A 0.9300 . ?
C27 N3 1.476(10) . ?
C29 C30 1.550(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.547(5) . ?
C30 H30A 0.9800 . ?
C31 C32 1.546(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.545(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.544(5) . ?
C34 H34A 0.9800 . ?
C35 C36 1.549(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Cu3 O1 170.67(17) 4_565 . ?
O6 Cu3 O4 84.39(18) 4_565 . ?
O1 Cu3 O4 93.53(18) . . ?
O6 Cu3 O2 100.16(18) 4_565 . ?
O1 Cu3 O2 88.63(17) . . ?
O4 Cu3 O2 122.7(2) . . ?
O6 Cu3 O16 90.33(17) 4_565 1_455 ?
O1 Cu3 O16 86.60(17) . 1_455 ?
O4 Cu3 O16 147.82(19) . 1_455 ?
O2 Cu3 O16 89.49(19) . 1_455 ?
O6 Cu3 Cu1 131.42(12) 4_565 . ?
O1 Cu3 Cu1 39.41(11) . . ?
O4 Cu3 Cu1 77.34(13) . . ?
O2 Cu3 Cu1 127.62(13) . . ?
O16 Cu3 Cu1 82.71(14) 1_455 . ?
O15 Cu2 O3 90.66(19) 4_466 . ?
O15 Cu2 O1 174.76(18) 4_466 . ?
O3 Cu2 O1 94.55(17) . . ?
O15 Cu2 O6 94.02(17) 4_466 . ?
O3 Cu2 O6 172.16(18) . . ?
O1 Cu2 O6 80.85(16) . . ?
O15 Cu2 Cu1 135.20(14) 4_466 . ?
O3 Cu2 Cu1 133.71(13) . . ?
O1 Cu2 Cu1 39.70(11) . . ?
O6 Cu2 Cu1 41.18(11) . . ?
O18 Cu1 O5 92.2(2) 2_655 . ?
O18 Cu1 O1 165.2(2) 2_655 . ?
O5 Cu1 O1 92.41(18) . . ?
O18 Cu1 O6 94.85(18) 2_655 . ?
O5 Cu1 O6 172.74(19) . . ?
O1 Cu1 O6 81.10(16) . . ?
O18 Cu1 O4 94.03(19) 2_655 4_566 ?
O5 Cu1 O4 105.67(17) . 4_566 ?
O1 Cu1 O4 98.23(17) . 4_566 ?
O6 Cu1 O4 72.29(16) . 4_566 ?
O18 Cu1 Cu2 134.11(15) 2_655 . ?
O5 Cu1 Cu2 132.13(14) . . ?
O1 Cu1 Cu2 39.72(11) . . ?
O6 Cu1 Cu2 41.41(11) . . ?
O4 Cu1 Cu2 85.42(11) 4_566 . ?
O18 Cu1 Cu3 128.34(16) 2_655 . ?
O5 Cu1 Cu3 80.26(13) . . ?
O1 Cu1 Cu3 39.17(13) . . ?
O6 Cu1 Cu3 96.50(12) . . ?
O4 Cu1 Cu3 137.35(12) 4_566 . ?
Cu2 Cu1 Cu3 62.69(2) . . ?
Cu3 O1 Cu1 101.43(19) . . ?
Cu3 O1 Cu2 107.0(2) . . ?
Cu1 O1 Cu2 100.57(17) . . ?
Cu3 O1 H1 115.4 . . ?
Cu1 O1 H1 115.3 . . ?
Cu2 O1 H1 115.3 . . ?
C1 O2 Cu3 128.4(4) . . ?
C1 O3 Cu2 128.2(4) . . ?
C15 O4 Cu3 127.8(4) . . ?
C15 O4 Cu1 133.1(4) . 4_565 ?
Cu3 O4 Cu1 91.79(17) . 4_565 ?
C15 O5 Cu1 127.4(4) . . ?
Cu3 O6 Cu1 109.5(2) 4_566 . ?
Cu3 O6 Cu2 110.1(2) 4_566 . ?
Cu1 O6 Cu2 97.40(17) . . ?
Cu3 O6 H6 112.9 4_566 . ?
Cu1 O6 H6 112.9 . . ?
Cu2 O6 H6 112.9 . . ?
C28 O15 Cu2 126.8(4) . 4_665 ?
C28 O16 Cu3 131.3(4) . 1_655 ?
C14 O18 Cu1 106.9(4) . 2_645 ?
C30 O19 H19 106(6) . . ?
C34 O20 H20 112(3) . . ?
O2 C1 O3 127.4(6) . . ?
O2 C1 C2 116.6(6) . . ?
O3 C1 C2 115.9(6) . . ?
C3 C2 C7 118.6(7) . . ?
C3 C2 C1 119.9(6) . . ?
C7 C2 C1 121.4(6) . . ?
C2 C3 C4 120.9(8) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C3 C4 C5 121.1(8) . . ?
C3 C4 H4A 119.4 . . ?
C5 C4 H4A 119.4 . . ?
C6 C5 C4 116.5(7) . . ?
C6 C5 C8 125.6(8) . . ?
C4 C5 C8 117.8(8) . . ?
C7 C6 C5 122.5(7) . . ?
C7 C6 N1A 115.6(10) . . ?
C5 C6 N1A 119.2(9) . . ?
C7 C6 N1B 115.6(10) . . ?
C5 C6 N1B 120.4(9) . . ?
N1A C6 N1B 29.3(10) . . ?
C6 C7 C2 120.2(8) . . ?
C6 C7 H7A 119.9 . . ?
C2 C7 H7A 119.9 . . ?
C13 C8 C9 116.0(7) . . ?
C13 C8 C5 119.8(8) . . ?
C9 C8 C5 123.3(8) . . ?
C8 C9 C10 123.6(9) . . ?
C8 C9 N4 121.0(8) . . ?
C10 C9 N4 115.5(8) . . ?
C11 C10 C9 118.8(9) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
C12 C11 C10 118.6(7) . . ?
C12 C11 C14 120.5(7) . . ?
C10 C11 C14 120.8(7) . . ?
C11 C12 C13 121.3(9) . . ?
C11 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
C8 C13 C12 121.7(9) . . ?
C8 C13 H13A 119.1 . . ?
C12 C13 H13A 119.1 . . ?
O17 C14 O18 124.5(6) . . ?
O17 C14 C11 121.7(7) . . ?
O18 C14 C11 113.8(7) . . ?
O5 C15 O4 126.5(6) . . ?
O5 C15 C16 116.9(6) . . ?
O4 C15 C16 116.6(6) . . ?
C21 C16 C17 120.0(6) . . ?
C21 C16 C15 122.6(6) . . ?
C17 C16 C15 117.4(6) . . ?
C18 C17 C16 118.6(7) . . ?
C18 C17 H17A 120.7 . . ?
C16 C17 H17A 120.7 . . ?
C17 C18 C19 123.5(7) . . ?
C17 C18 N2 116.6(7) . . ?
C19 C18 N2 119.9(7) . . ?
C20 C19 C18 115.8(6) . . ?
C20 C19 C22 120.3(7) . . ?
C18 C19 C22 123.8(7) . . ?
C19 C20 C21 121.6(7) . . ?
C19 C20 H20A 119.2 . . ?
C21 C20 H20A 119.2 . . ?
C16 C21 C20 120.3(7) . . ?
C16 C21 H21A 119.8 . . ?
C20 C21 H21A 119.8 . . ?
C27 C22 C23 116.5(6) . . ?
C27 C22 C19 124.7(7) . . ?
C23 C22 C19 118.8(7) . . ?
C24 C23 C22 122.5(7) . . ?
C24 C23 H23A 118.8 . . ?
C22 C23 H23A 118.8 . . ?
C23 C24 C25 120.1(7) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
C24 C25 C26 118.7(6) . . ?
C24 C25 C28 121.7(6) . . ?
C26 C25 C28 119.6(6) . . ?
C27 C26 C25 119.9(7) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C22 122.0(7) . . ?
C26 C27 N3 115.6(6) . . ?
C22 C27 N3 122.3(6) . . ?
O16 C28 O15 127.3(6) . . ?
O16 C28 C25 118.3(6) . . ?
O15 C28 C25 114.3(6) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O19 C30 C31 109.1(5) . . ?
O19 C30 C29 109.1(5) . . ?
C31 C30 C29 109.7(4) . . ?
O19 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
C29 C30 H30A 109.7 . . ?
C32 C31 C30 109.6(7) . . ?
C32 C31 H31A 109.8 . . ?
C30 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
C30 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O20 C34 C35 109.4(5) . . ?
O20 C34 C33 109.0(5) . . ?
C35 C34 C33 109.4(4) . . ?
O20 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
C33 C34 H34A 109.7 . . ?
C34 C35 C36 110.4(7) . . ?
C34 C35 H35A 109.6 . . ?
C36 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
C36 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O11A N1A O12A 110.0(19) . . ?
O11A N1A C6 122.3(16) . . ?
O12A N1A C6 122.7(17) . . ?
O11B N1B O12B 111.4(19) . . ?
O11B N1B C6 120.3(16) . . ?
O12B N1B C6 124.5(17) . . ?
O7B N2 O7A 35.2(11) . . ?
O7B N2 O8A 89.9(13) . . ?
O7A N2 O8A 112.4(14) . . ?
O7B N2 O8B 126.4(14) . . ?
O7A N2 O8B 105.1(14) . . ?
O8A N2 O8B 74.5(11) . . ?
O7B N2 C18 117.1(11) . . ?
O7A N2 C18 119.6(11) . . ?
O8A N2 C18 120.4(11) . . ?
O8B N2 C18 115.0(11) . . ?
O9B N3 O10B 119.5(13) . . ?
O9B N3 O10A 120.8(13) . . ?
O10B N3 O10A 28.0(10) . . ?
O9B N3 O9A 23.0(12) . . ?
O10B N3 O9A 114.4(13) . . ?
O10A N3 O9A 128.1(13) . . ?
O9B N3 C27 119.6(10) . . ?
O10B N3 C27 119.5(9) . . ?
O10A N3 C27 117.0(9) . . ?
O9A N3 C27 114.4(10) . . ?
O13A N4 O14A 119.5(18) . . ?
O13A N4 O14B 120.6(18) . . ?
O14A N4 O14B 31.6(13) . . ?
O13A N4 O13B 27.4(15) . . ?
O14A N4 O13B 121.8(18) . . ?
O14B N4 O13B 138.9(17) . . ?
O13A N4 C9 118.9(14) . . ?
O14A N4 C9 121.6(13) . . ?
O14B N4 C9 111.8(13) . . ?
O13B N4 C9 109.1(14) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.150

#==============================================================================

_database_code_depnum_ccdc_archive 'CCDC 977438'
