# Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Sasankasekhar Mohanta'
_publ_contact_author_email       'SM CU CHEM@YAHOO.CO.IN'

_publ_section_title              
;
Syntheses and Crystal Structures of
CuIIBiIII, CuIIBaIICuII, [CuIIPbII]2 and Cocrystallized
(UVIO2)2.4CuII Complexes: Structural Diversity of the
Coordination Compounds Derived from N,N?-Ethylenebis(3-Ethoxysalicylaldiimine)
;
loop_
_publ_author_name
'Sasankasekhar Mohanta'
'Susanta Hazra'
'Judith Howard'
'Malabika Nayak'
'Sujit Sasmal'
'Hazel A. Sparkes'

# Attachment '1-4.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 735468'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 Bi Cu N5 O13'
_chemical_formula_weight         812.95

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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   8.5795(10)
_cell_length_b                   13.7534(12)
_cell_length_c                   20.8299(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2457.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6910
_cell_measurement_theta_min      2.798
_cell_measurement_theta_max      29.987

_exptl_crystal_description       block
_exptl_crystal_colour            dark_red
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1572
_exptl_absorpt_coefficient_mu    8.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_T_max  0.379
_exptl_absorpt_process_details   'SADABS, (G. Sheldrick, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bede Microsource'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Proteum M'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23632
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         28.28
_reflns_number_total             6057
_reflns_number_gt                5706
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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.
A combination of TWIN and BASF was tested due to the FLACK parameter value
of -0.015 however, the BASF value refined to zero.
;

_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_number_reflns         6057
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0151
_refine_ls_wR_factor_ref         0.0358
_refine_ls_wR_factor_gt          0.0353
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_restrained_S_all      0.818
_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
Bi1 Bi 1.760846(9) 0.002233(6) 0.597349(4) 0.01288(3) Uani 1 1 d . . .
Cu1 Cu 1.43450(4) 0.06042(2) 0.681438(15) 0.01602(7) Uani 1 1 d . . .
O1 O 1.6628(2) -0.17363(12) 0.57311(8) 0.0159(4) Uani 1 1 d . . .
N1 N 1.3009(2) -0.01010(16) 0.73808(9) 0.0160(4) Uani 1 1 d . . .
C1 C 1.8552(3) -0.3057(2) 0.55833(14) 0.0240(6) Uani 1 1 d . . .
H1A H 1.9356 -0.2666 0.5796 0.036 Uiso 1 1 calc R . .
H1B H 1.9036 -0.3469 0.5256 0.036 Uiso 1 1 calc R . .
H1C H 1.8025 -0.3466 0.5902 0.036 Uiso 1 1 calc R . .
O2 O 1.5462(2) -0.05236(12) 0.65497(8) 0.0152(4) Uani 1 1 d . . .
N2 N 1.3243(3) 0.17391(15) 0.70780(10) 0.0168(5) Uani 1 1 d . . .
C2 C 1.7375(3) -0.23892(17) 0.52691(11) 0.0178(5) Uani 1 1 d . . .
H2A H 1.7904 -0.1997 0.4936 0.021 Uiso 1 1 calc R . .
H2B H 1.6565 -0.2787 0.5055 0.021 Uiso 1 1 calc R . .
O3 O 1.5934(2) 0.12865(12) 0.63636(9) 0.0176(4) Uani 1 1 d . . .
N3 N 1.8686(3) -0.05304(17) 0.72544(11) 0.0216(5) Uani 1 1 d . . .
C3 C 1.5459(3) -0.21050(17) 0.61203(11) 0.0136(5) Uani 1 1 d . . .
O4 O 1.8241(2) 0.18969(13) 0.56862(9) 0.0178(4) Uani 1 1 d . . .
N4 N 2.1134(3) -0.02290(16) 0.58062(10) 0.0227(5) Uani 1 1 d . . .
C4 C 1.4861(3) -0.30370(18) 0.60900(12) 0.0173(5) Uani 1 1 d . . .
H4 H 1.5272 -0.3488 0.5789 0.021 Uiso 1 1 calc R . .
O5 O 1.8667(2) -0.11364(12) 0.67949(9) 0.0214(4) Uani 1 1 d . . .
N5 N 1.6372(2) 0.00409(18) 0.46404(10) 0.0204(4) Uani 1 1 d . . .
C5 C 1.3660(3) -0.33167(19) 0.64979(12) 0.0205(6) Uani 1 1 d . . .
H5 H 1.3253 -0.3958 0.6477 0.025 Uiso 1 1 calc R . .
O6 O 1.9116(3) -0.07662(16) 0.77938(9) 0.0347(5) Uani 1 1 d . . .
C6 C 1.3058(3) -0.26592(18) 0.69348(13) 0.0187(6) Uani 1 1 d . . .
H6 H 1.2269 -0.2862 0.7225 0.022 Uiso 1 1 calc R . .
O7 O 1.8210(2) 0.03305(13) 0.71355(9) 0.0235(5) Uani 1 1 d . . .
C7 C 1.3602(3) -0.16893(18) 0.69556(12) 0.0151(6) Uani 1 1 d . . .
O8 O 2.0496(2) 0.04038(12) 0.61617(9) 0.0221(4) Uani 1 1 d . . .
C8 C 1.4843(3) -0.14228(18) 0.65521(11) 0.0137(5) Uani 1 1 d . . .
O9 O 2.2557(2) -0.02705(18) 0.57683(11) 0.0418(6) Uani 1 1 d . . .
C9 C 1.2813(3) -0.10238(18) 0.73888(12) 0.0181(5) Uani 1 1 d . . .
H9 H 1.2112 -0.1288 0.7696 0.022 Uiso 1 1 calc R . .
O10 O 2.0246(2) -0.08148(15) 0.55050(10) 0.0308(5) Uani 1 1 d . . .
C10 C 1.2229(3) 0.05717(19) 0.78364(11) 0.0190(5) Uani 1 1 d . . .
H10A H 1.2922 0.0707 0.8206 0.023 Uiso 1 1 calc R . .
H10B H 1.1255 0.0276 0.8000 0.023 Uiso 1 1 calc R . .
O11 O 1.7818(2) -0.01153(15) 0.47363(8) 0.0245(4) Uani 1 1 d . . .
C11 C 1.1866(3) 0.15100(19) 0.74790(12) 0.0191(6) Uani 1 1 d . . .
H11A H 1.0931 0.1425 0.7206 0.023 Uiso 1 1 calc R . .
H11B H 1.1664 0.2044 0.7787 0.023 Uiso 1 1 calc R . .
O12 O 1.5786(2) -0.00449(15) 0.41106(8) 0.0319(4) Uani 1 1 d . . .
C12 C 1.3560(3) 0.26146(18) 0.69046(12) 0.0167(6) Uani 1 1 d . . .
H12 H 1.2895 0.3116 0.7057 0.020 Uiso 1 1 calc R . .
O13 O 1.5564(2) 0.02974(13) 0.51273(9) 0.0244(4) Uani 1 1 d . . .
C13 C 1.4853(3) 0.28989(19) 0.64942(12) 0.0163(5) Uani 1 1 d . . .
C14 C 1.4963(3) 0.38856(18) 0.63243(12) 0.0198(6) Uani 1 1 d . . .
H14 H 1.4189 0.4328 0.6469 0.024 Uiso 1 1 calc R . .
C15 C 1.6167(3) 0.42216(18) 0.59530(13) 0.0216(6) Uani 1 1 d . . .
H15 H 1.6210 0.4890 0.5839 0.026 Uiso 1 1 calc R . .
C16 C 1.7327(3) 0.35909(18) 0.57418(12) 0.0191(5) Uani 1 1 d . . .
H16 H 1.8179 0.3830 0.5497 0.023 Uiso 1 1 calc R . .
C17 C 1.7227(3) 0.26075(17) 0.58927(11) 0.0140(5) Uani 1 1 d . . .
C18 C 1.5973(3) 0.22413(17) 0.62614(12) 0.0144(5) Uani 1 1 d . . .
C19 C 1.9601(3) 0.22035(19) 0.53213(12) 0.0196(6) Uani 1 1 d . . .
H19A H 1.9285 0.2702 0.5004 0.023 Uiso 1 1 calc R . .
H19B H 2.0026 0.1640 0.5083 0.023 Uiso 1 1 calc R . .
C20 C 2.0847(3) 0.2615(2) 0.57499(13) 0.0238(6) Uani 1 1 d . . .
H20A H 2.0430 0.3174 0.5986 0.036 Uiso 1 1 calc R . .
H20B H 2.1735 0.2824 0.5488 0.036 Uiso 1 1 calc R . .
H20C H 2.1189 0.2116 0.6055 0.036 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi1 O2 2.3231(17) . ?
Bi1 O3 2.3974(17) . ?
Bi1 O5 2.5082(18) . ?
Bi1 O7 2.5110(19) . ?
Bi1 O13 2.5153(19) . ?
Bi1 O8 2.5626(19) . ?
Bi1 O11 2.5902(17) . ?
Bi1 O1 2.6101(17) . ?
Bi1 O4 2.7018(18) . ?
Bi1 O10 2.720(2) . ?
Cu1 O3 1.9026(18) . ?
Cu1 O2 1.9048(18) . ?
Cu1 N2 1.906(2) . ?
Cu1 N1 1.910(2) . ?
O1 C3 1.386(3) . ?
O1 C2 1.464(3) . ?
N1 C9 1.280(3) . ?
N1 C10 1.484(3) . ?
C1 C2 1.513(4) . ?
O2 C8 1.346(3) . ?
N2 C12 1.286(3) . ?
N2 C11 1.481(3) . ?
O3 C18 1.331(3) . ?
N3 O6 1.226(3) . ?
N3 O5 1.269(3) . ?
N3 O7 1.277(3) . ?
C3 C4 1.382(3) . ?
C3 C8 1.403(3) . ?
O4 C17 1.377(3) . ?
O4 C19 1.455(3) . ?
N4 O9 1.225(3) . ?
N4 O8 1.267(3) . ?
N4 O10 1.274(3) . ?
C4 C5 1.390(4) . ?
N5 O12 1.218(2) . ?
N5 O11 1.276(3) . ?
N5 O13 1.278(3) . ?
C5 C6 1.383(4) . ?
C6 C7 1.414(3) . ?
C7 C8 1.405(3) . ?
C7 C9 1.453(3) . ?
C10 C11 1.522(4) . ?
C12 C13 1.454(4) . ?
C13 C14 1.406(4) . ?
C13 C18 1.406(4) . ?
C14 C15 1.371(4) . ?
C15 C16 1.391(4) . ?
C16 C17 1.391(3) . ?
C17 C18 1.415(3) . ?
C19 C20 1.504(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Bi1 O3 65.43(6) . . ?
O2 Bi1 O5 74.29(6) . . ?
O3 Bi1 O5 116.52(6) . . ?
O2 Bi1 O7 73.71(6) . . ?
O3 Bi1 O7 70.97(6) . . ?
O5 Bi1 O7 51.34(6) . . ?
O2 Bi1 O13 81.82(6) . . ?
O3 Bi1 O13 73.17(6) . . ?
O5 Bi1 O13 145.69(6) . . ?
O7 Bi1 O13 142.51(6) . . ?
O2 Bi1 O8 138.91(6) . . ?
O3 Bi1 O8 112.28(6) . . ?
O5 Bi1 O8 71.09(6) . . ?
O7 Bi1 O8 67.62(6) . . ?
O13 Bi1 O8 138.64(6) . . ?
O2 Bi1 O11 123.06(6) . . ?
O3 Bi1 O11 115.59(6) . . ?
O5 Bi1 O11 127.37(6) . . ?
O7 Bi1 O11 163.16(7) . . ?
O13 Bi1 O11 50.38(6) . . ?
O8 Bi1 O11 95.73(6) . . ?
O2 Bi1 O1 62.93(6) . . ?
O3 Bi1 O1 122.99(6) . . ?
O5 Bi1 O1 70.11(6) . . ?
O7 Bi1 O1 114.15(6) . . ?
O13 Bi1 O1 77.24(6) . . ?
O8 Bi1 O1 122.06(6) . . ?
O11 Bi1 O1 76.24(6) . . ?
O2 Bi1 O4 125.60(6) . . ?
O3 Bi1 O4 60.23(6) . . ?
O5 Bi1 O4 133.21(6) . . ?
O7 Bi1 O4 90.64(6) . . ?
O13 Bi1 O4 80.87(6) . . ?
O8 Bi1 O4 69.17(5) . . ?
O11 Bi1 O4 80.53(6) . . ?
O1 Bi1 O4 154.98(6) . . ?
O2 Bi1 O10 135.08(7) . . ?
O3 Bi1 O10 158.00(6) . . ?
O5 Bi1 O10 71.02(6) . . ?
O7 Bi1 O10 104.26(6) . . ?
O13 Bi1 O10 113.11(6) . . ?
O8 Bi1 O10 48.49(6) . . ?
O11 Bi1 O10 63.53(6) . . ?
O1 Bi1 O10 78.84(6) . . ?
O4 Bi1 O10 99.05(6) . . ?
O3 Cu1 O2 84.17(7) . . ?
O3 Cu1 N2 95.38(9) . . ?
O2 Cu1 N2 179.53(9) . . ?
O3 Cu1 N1 170.21(9) . . ?
O2 Cu1 N1 93.85(8) . . ?
N2 Cu1 N1 86.56(9) . . ?
C3 O1 C2 118.48(18) . . ?
C3 O1 Bi1 117.33(14) . . ?
C2 O1 Bi1 123.68(14) . . ?
C9 N1 C10 123.4(2) . . ?
C9 N1 Cu1 126.17(19) . . ?
C10 N1 Cu1 110.42(16) . . ?
C8 O2 Cu1 123.29(16) . . ?
C8 O2 Bi1 127.71(15) . . ?
Cu1 O2 Bi1 106.57(7) . . ?
C12 N2 C11 121.8(2) . . ?
C12 N2 Cu1 125.50(19) . . ?
C11 N2 Cu1 112.59(16) . . ?
O1 C2 C1 112.3(2) . . ?
C18 O3 Cu1 125.70(17) . . ?
C18 O3 Bi1 130.27(16) . . ?
Cu1 O3 Bi1 103.83(7) . . ?
O6 N3 O5 121.4(2) . . ?
O6 N3 O7 121.3(2) . . ?
O5 N3 O7 117.3(2) . . ?
C4 C3 O1 125.5(2) . . ?
C4 C3 C8 120.7(2) . . ?
O1 C3 C8 113.8(2) . . ?
C17 O4 C19 117.64(19) . . ?
C17 O4 Bi1 118.76(14) . . ?
C19 O4 Bi1 123.60(14) . . ?
O9 N4 O8 120.0(2) . . ?
O9 N4 O10 122.3(2) . . ?
O8 N4 O10 117.6(2) . . ?
C3 C4 C5 120.3(2) . . ?
N3 O5 Bi1 95.86(14) . . ?
O12 N5 O11 121.8(2) . . ?
O12 N5 O13 121.5(2) . . ?
O11 N5 O13 116.73(19) . . ?
C6 C5 C4 119.9(2) . . ?
C5 C6 C7 120.9(2) . . ?
N3 O7 Bi1 95.52(14) . . ?
C8 C7 C6 118.5(2) . . ?
C8 C7 C9 124.1(2) . . ?
C6 C7 C9 117.4(2) . . ?
N4 O8 Bi1 100.81(15) . . ?
O2 C8 C3 117.6(2) . . ?
O2 C8 C7 122.7(2) . . ?
C3 C8 C7 119.6(2) . . ?
N1 C9 C7 123.7(2) . . ?
N4 O10 Bi1 93.05(14) . . ?
N1 C10 C11 107.93(19) . . ?
N5 O11 Bi1 94.35(13) . . ?
N2 C11 C10 107.0(2) . . ?
N2 C12 C13 125.3(2) . . ?
N5 O13 Bi1 97.84(14) . . ?
C14 C13 C18 119.2(2) . . ?
C14 C13 C12 117.3(2) . . ?
C18 C13 C12 123.5(2) . . ?
C15 C14 C13 121.2(2) . . ?
C14 C15 C16 120.5(2) . . ?
C17 C16 C15 119.4(2) . . ?
O4 C17 C16 125.5(2) . . ?
O4 C17 C18 113.4(2) . . ?
C16 C17 C18 121.0(2) . . ?
O3 C18 C13 124.2(2) . . ?
O3 C18 C17 117.2(2) . . ?
C13 C18 C17 118.6(2) . . ?
O4 C19 C20 111.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.074

##===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 735469'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H44 Ba Cu2 N6 O14.20'
_chemical_formula_sum            'C40 H44 Ba Cu2 N6 O14.20'
_chemical_formula_weight         1100.43

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'
Ba Ba -0.3244 2.2819 '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                   11.7008(2)
_cell_length_b                   31.3666(6)
_cell_length_c                   12.3487(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.2340(10)
_cell_angle_gamma                90.00
_cell_volume                     4164.60(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9756
_cell_measurement_theta_min      2.412
_cell_measurement_theta_max      26.323

_exptl_crystal_description       plate
_exptl_crystal_colour            dark_red
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2214
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_process_details   'SADABS, (G. Sheldrick, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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 Proteum M'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34506
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         25.03
_reflns_number_total             7338
_reflns_number_gt                6092
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0313P)²+4.5768P] 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         7338
_refine_ls_number_parameters     633
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.031
_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
Ba1 Ba 0.734878(17) 0.124905(6) 0.664068(17) 0.02595(6) Uani 1 1 d . A .
Cu1 Cu 0.43575(4) 0.174816(14) 0.64893(4) 0.03039(11) Uani 1 1 d . . .
Cu2 Cu 0.46011(4) 0.055682(14) 0.56330(4) 0.03344(11) Uani 1 1 d . . .
O1 O 0.7972(2) 0.21200(8) 0.6328(2) 0.0375(6) Uani 1 1 d . A .
O2 O 0.5800(2) 0.19523(7) 0.6318(2) 0.0313(5) Uani 1 1 d . A .
O3 O 0.5315(2) 0.12727(7) 0.73332(19) 0.0300(5) Uani 1 1 d . A .
O4 O 0.7193(2) 0.08817(7) 0.88848(19) 0.0309(5) Uani 1 1 d . A .
O5 O 0.6116(2) 0.15932(8) 0.4111(2) 0.0370(6) Uani 1 1 d . A .
O6 O 0.5062(2) 0.10259(8) 0.4919(2) 0.0351(6) Uani 1 1 d . A .
O7 O 0.6327(2) 0.04352(7) 0.6462(2) 0.0318(5) Uani 1 1 d . A .
O8 O 0.8726(2) 0.04399(7) 0.7527(2) 0.0322(5) Uani 1 1 d . A .
O9A O 0.8159(11) 0.0898(12) 0.4837(11) 0.0487(14) Uani 0.57 1 d P A 1
O9B O 0.7891(16) 0.0895(16) 0.4798(14) 0.0487(14) Uani 0.43 1 d P A 2
O10A O 0.949(3) 0.1288(2) 0.6108(10) 0.0487(14) Uani 0.57 1 d P A 1
O10B O 0.959(4) 0.1179(3) 0.6141(13) 0.0487(14) Uani 0.43 1 d P A 2
O11A O 0.9719(6) 0.1106(2) 0.4499(6) 0.0705(15) Uani 0.57 1 d PU A 1
O11B O 0.9702(9) 0.0864(3) 0.4639(8) 0.0705(15) Uani 0.43 1 d PU A 2
O12A O 0.9343(3) 0.14614(14) 0.8652(4) 0.0477(6) Uani 0.80 1 d P A 1
O12B O 0.8228(12) 0.1768(5) 0.8687(12) 0.0477(6) Uani 0.20 1 d P A 2
O13A O 1.0069(7) 0.1947(3) 0.9955(9) 0.0477(6) Uani 0.80 1 d P A 1
O13B O 0.9744(15) 0.1400(6) 0.8590(16) 0.0477(6) Uani 0.20 1 d P A 2
O14A O 1.1208(3) 0.16918(11) 0.9080(3) 0.0477(6) Uani 0.80 1 d P A 1
O14B O 1.023(3) 0.1971(14) 0.995(4) 0.0477(6) Uani 0.20 1 d P A 2
N1 N 0.3303(3) 0.21967(10) 0.5563(3) 0.0394(7) Uani 1 1 d . A .
N2A N 0.2930(10) 0.1614(2) 0.6837(8) 0.0311(17) Uani 0.71 1 d P A 1
N2B N 0.287(2) 0.1478(6) 0.658(2) 0.029(4) Uani 0.29 1 d P A 2
N3A N 0.2866(6) 0.07203(15) 0.4932(5) 0.0365(13) Uani 0.67 1 d PDU A 1
N3B N 0.2813(12) 0.0601(3) 0.4754(11) 0.0365(13) Uani 0.33 1 d PDU A 2
N4A N 0.4034(5) 0.00494(17) 0.6106(4) 0.0329(12) Uani 0.67 1 d PDU A 1
N4B N 0.4171(9) 0.0090(3) 0.6469(10) 0.0329(12) Uani 0.33 1 d PDU A 2
N5A N 0.908(3) 0.1096(6) 0.509(2) 0.046(3) Uani 0.57 1 d P A 1
N5B N 0.913(4) 0.0978(9) 0.525(3) 0.046(3) Uani 0.43 1 d P A 2
N6A N 1.0223(3) 0.17045(12) 0.9236(3) 0.0328(8) Uani 0.80 1 d P A 1
N6B N 0.9265(14) 0.1682(5) 0.9069(13) 0.0328(8) Uani 0.20 1 d P A 2
C1 C 0.9620(4) 0.26156(14) 0.7485(4) 0.0547(11) Uani 1 1 d . A .
H1A H 0.9143 0.2872 0.7122 0.082 Uiso 1 1 calc R . .
H1B H 1.0509 0.2673 0.7722 0.082 Uiso 1 1 calc R . .
H1C H 0.9457 0.2538 0.8179 0.082 Uiso 1 1 calc R . .
C2 C 0.9237(3) 0.22559(13) 0.6614(4) 0.0444(10) Uani 1 1 d . . .
H2A H 0.9324 0.2347 0.5883 0.053 Uiso 1 1 calc R A .
H2B H 0.9803 0.2011 0.6943 0.053 Uiso 1 1 calc R . .
C3 C 0.7043(3) 0.24031(11) 0.5722(3) 0.0343(8) Uani 1 1 d . . .
C4 C 0.7193(4) 0.27464(11) 0.5100(3) 0.0396(9) Uani 1 1 d . A .
H4 H 0.7982 0.2802 0.5079 0.047 Uiso 1 1 calc R . .
C5 C 0.6187(4) 0.30156(12) 0.4496(3) 0.0446(10) Uani 1 1 d . . .
H5 H 0.6294 0.3254 0.4070 0.054 Uiso 1 1 calc R A .
C6 C 0.5062(4) 0.29352(12) 0.4521(3) 0.0440(9) Uani 1 1 d . A .
H6 H 0.4388 0.3122 0.4120 0.053 Uiso 1 1 calc R . .
C7 C 0.4865(3) 0.25784(11) 0.5131(3) 0.0348(8) Uani 1 1 d . . .
C8 C 0.5867(3) 0.23018(11) 0.5742(3) 0.0322(8) Uani 1 1 d . A .
C9 C 0.3634(4) 0.25078(12) 0.5073(3) 0.0417(9) Uani 1 1 d . A .
H9 H 0.3010 0.2707 0.4637 0.050 Uiso 1 1 calc R . .
C10A C 0.1980(6) 0.2129(2) 0.5276(6) 0.0378(16) Uani 0.71 1 d P A 1
H10A H 0.1613 0.1941 0.4579 0.045 Uiso 0.71 1 calc PR A 1
H10B H 0.1526 0.2403 0.5106 0.045 Uiso 0.71 1 calc PR A 1
C10B C 0.2101(17) 0.2176(7) 0.5867(17) 0.043(4) Uani 0.29 1 d P A 2
H10C H 0.2294 0.2284 0.6674 0.052 Uiso 0.29 1 calc PR A 2
H10D H 0.1420 0.2350 0.5303 0.052 Uiso 0.29 1 calc PR A 2
C11A C 0.1910(5) 0.1919(2) 0.6358(6) 0.0407(13) Uani 0.71 1 d P A 1
H11A H 0.1976 0.2138 0.6957 0.049 Uiso 0.71 1 calc PR A 1
H11B H 0.1103 0.1771 0.6140 0.049 Uiso 0.71 1 calc PR A 1
C11B C 0.1736(12) 0.1716(5) 0.5775(14) 0.044(3) Uani 0.29 1 d P A 2
H11C H 0.1476 0.1615 0.4953 0.053 Uiso 0.29 1 calc PR A 2
H11D H 0.1038 0.1674 0.6026 0.053 Uiso 0.29 1 calc PR A 2
C12 C 0.2860(3) 0.12895(14) 0.7471(4) 0.0445(10) Uani 1 1 d . . .
H12 H 0.2065 0.1223 0.7465 0.053 Uiso 1 1 calc R A 1
C13 C 0.3885(3) 0.10241(11) 0.8175(3) 0.0316(8) Uani 1 1 d . A .
C14 C 0.3723(3) 0.07645(12) 0.9038(3) 0.0392(9) Uani 1 1 d . . .
H14 H 0.2930 0.0750 0.9077 0.047 Uiso 1 1 calc R A .
C15 C 0.4685(4) 0.05353(13) 0.9813(4) 0.0453(10) Uani 1 1 d . A .
H15 H 0.4551 0.0355 1.0370 0.054 Uiso 1 1 calc R . .
C16 C 0.5874(4) 0.05634(12) 0.9793(3) 0.0421(9) Uani 1 1 d . . .
H16 H 0.6548 0.0408 1.0348 0.051 Uiso 1 1 calc R A .
C17 C 0.6059(3) 0.08180(11) 0.8963(3) 0.0313(7) Uani 1 1 d . A .
C18 C 0.5065(3) 0.10455(10) 0.8115(3) 0.0289(7) Uani 1 1 d . . .
C19 C 0.8299(3) 0.07549(11) 0.9875(3) 0.0337(8) Uani 1 1 d . . .
H19A H 0.9012 0.0754 0.9635 0.040 Uiso 1 1 calc R A .
H19B H 0.8189 0.0460 1.0106 0.040 Uiso 1 1 calc R . .
C20 C 0.8592(4) 0.10455(13) 1.0926(3) 0.0429(9) Uani 1 1 d . A .
H20A H 0.8700 0.1338 1.0702 0.064 Uiso 1 1 calc R . .
H20B H 0.9359 0.0950 1.1565 0.064 Uiso 1 1 calc R . .
H20C H 0.7906 0.1037 1.1191 0.064 Uiso 1 1 calc R . .
C21 C 0.6621(5) 0.15208(15) 0.2383(4) 0.0586(12) Uani 1 1 d . A .
H21A H 0.6954 0.1235 0.2638 0.088 Uiso 1 1 calc R . .
H21B H 0.7081 0.1656 0.1962 0.088 Uiso 1 1 calc R . .
H21C H 0.5739 0.1500 0.1859 0.088 Uiso 1 1 calc R . .
C22 C 0.6757(4) 0.17849(12) 0.3445(3) 0.0432(9) Uani 1 1 d . . .
H22A H 0.7650 0.1815 0.3957 0.052 Uiso 1 1 calc R A .
H22B H 0.6416 0.2073 0.3185 0.052 Uiso 1 1 calc R . .
C23 C 0.4845(3) 0.15934(12) 0.3626(3) 0.0367(8) Uani 1 1 d . . .
C24 C 0.4115(4) 0.18649(13) 0.2739(3) 0.0458(10) Uani 1 1 d . A .
H24 H 0.4497 0.2069 0.2421 0.055 Uiso 1 1 calc R . .
C25 C 0.2821(4) 0.18399(14) 0.2311(4) 0.0527(11) Uani 1 1 d . . .
H25 H 0.2323 0.2021 0.1687 0.063 Uiso 1 1 calc R A .
C26 C 0.2272(4) 0.15566(15) 0.2785(3) 0.0489(11) Uani 1 1 d . A .
H26 H 0.1391 0.1548 0.2502 0.059 Uiso 1 1 calc R . .
C27 C 0.2992(3) 0.12723(13) 0.3697(3) 0.0419(9) Uani 1 1 d D . .
C28 C 0.4305(3) 0.12844(12) 0.4114(3) 0.0357(8) Uani 1 1 d . A .
C29 C 0.2341(3) 0.09693(15) 0.4118(3) 0.0536(12) Uani 1 1 d D A .
H29 H 0.1459 0.0961 0.3748 0.064 Uiso 1 1 calc R B 1
C30A C 0.2080(5) 0.04596(19) 0.5335(5) 0.0355(13) Uani 0.67 1 d PD A 1
H30A H 0.1217 0.0452 0.4734 0.043 Uiso 0.67 1 calc PR A 1
H30B H 0.2069 0.0575 0.6077 0.043 Uiso 0.67 1 calc PR A 1
C30B C 0.2200(11) 0.0224(5) 0.5061(10) 0.035(3) Uani 0.33 1 d PD A 2
H30D H 0.2135 -0.0010 0.4502 0.042 Uiso 0.33 1 calc PR A 2
H30C H 0.1344 0.0306 0.4951 0.042 Uiso 0.33 1 calc PR A 2
C31A C 0.2650(5) 0.00146(19) 0.5534(7) 0.0343(13) Uani 0.67 1 d PD A 1
H31A H 0.2340 -0.0152 0.6043 0.041 Uiso 0.67 1 calc PR A 1
H31B H 0.2404 -0.0136 0.4770 0.041 Uiso 0.67 1 calc PR A 1
C31B C 0.2871(9) 0.0059(4) 0.6303(11) 0.039(3) Uani 0.33 1 d PD A 2
H31C H 0.2696 0.0238 0.6880 0.047 Uiso 0.33 1 calc PR A 2
H31D H 0.2635 -0.0239 0.6375 0.047 Uiso 0.33 1 calc PR A 2
C32 C 0.4769(4) -0.02325(12) 0.6860(4) 0.0532(12) Uani 1 1 d D . .
H32 H 0.4373 -0.0460 0.7084 0.064 Uiso 1 1 calc R A 1
C33 C 0.6117(3) -0.02275(11) 0.7376(3) 0.0383(9) Uani 1 1 d D A .
C34 C 0.6737(4) -0.05643(12) 0.8129(4) 0.0454(10) Uani 1 1 d . . .
H34 H 0.6267 -0.0792 0.8255 0.055 Uiso 1 1 calc R A .
C35 C 0.8004(4) -0.05703(12) 0.8683(4) 0.0458(10) Uani 1 1 d . A .
H35 H 0.8408 -0.0798 0.9201 0.055 Uiso 1 1 calc R . .
C36 C 0.8709(4) -0.02412(11) 0.8488(3) 0.0401(9) Uani 1 1 d . . .
H36 H 0.9591 -0.0248 0.8862 0.048 Uiso 1 1 calc R A .
C37 C 0.8123(3) 0.00944(11) 0.7750(3) 0.0329(8) Uani 1 1 d . A .
C38 C 0.6813(3) 0.01102(11) 0.7163(3) 0.0325(8) Uani 1 1 d . . .
C39 C 1.0065(3) 0.04396(12) 0.7995(3) 0.0384(8) Uani 1 1 d . . .
H39A H 1.0391 0.0344 0.8826 0.046 Uiso 1 1 calc R A .
H39B H 1.0365 0.0734 0.7980 0.046 Uiso 1 1 calc R . .
C40 C 1.0560(4) 0.01512(13) 0.7301(4) 0.0487(10) Uani 1 1 d . A .
H40A H 1.0250 -0.0139 0.7299 0.073 Uiso 1 1 calc R . .
H40B H 1.1471 0.0150 0.7665 0.073 Uiso 1 1 calc R . .
H40C H 1.0282 0.0255 0.6489 0.073 Uiso 1 1 calc R . .
O15B O 1.2318(19) 0.1537(7) 0.9527(18) 0.087(6) Uiso 0.20 1 d P C 2


_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
Ba1 O12A 2.736(4) . ?
Ba1 O6 2.771(2) . ?
Ba1 O2 2.782(2) . ?
Ba1 O7 2.790(2) . ?
Ba1 O9B 2.82(3) . ?
Ba1 O3 2.830(2) . ?
Ba1 O10A 2.84(3) . ?
Ba1 O12B 2.836(13) . ?
Ba1 O1 2.893(2) . ?
Ba1 O13B 2.924(17) . ?
Ba1 O10B 2.94(4) . ?
Ba1 O9A 2.956(19) . ?
Ba1 O8 2.974(2) . ?
Ba1 O4 3.072(2) . ?
Ba1 O5 3.074(2) . ?
Ba1 N6B 3.249(16) . ?
Cu1 O2 1.893(2) . ?
Cu1 O3 1.909(2) . ?
Cu1 N1 1.923(3) . ?
Cu1 N2A 1.928(10) . ?
Cu1 N2B 1.98(3) . ?
Cu2 O6 1.899(2) . ?
Cu2 N4A 1.903(6) . ?
Cu2 O7 1.908(2) . ?
Cu2 N3A 1.936(6) . ?
Cu2 N3B 1.945(13) . ?
Cu2 N4B 1.969(11) . ?
O1 C3 1.374(4) . ?
O1 C2 1.444(4) . ?
O2 C8 1.326(4) . ?
O3 C18 1.321(4) . ?
O4 C17 1.382(4) . ?
O4 C19 1.443(4) . ?
O5 C23 1.366(4) . ?
O5 C22 1.445(4) . ?
O6 C28 1.318(4) . ?
O7 C38 1.313(4) . ?
O8 C37 1.379(4) . ?
O8 C39 1.441(4) . ?
O9A N5A 1.18(3) . ?
O9B N5B 1.36(5) . ?
O10A N5A 1.31(3) . ?
O10B N5B 1.19(5) . ?
O11A N5A 1.23(3) . ?
O11B N5B 1.24(4) . ?
O12A N6A 1.255(5) . ?
O12B N6B 1.147(19) . ?
O13A N6A 1.235(11) . ?
O13B N6B 1.31(2) . ?
O14A N6A 1.242(5) . ?
O14B N6B 1.52(4) . ?
N1 C9 1.285(5) . ?
N1 C10A 1.462(7) . ?
N1 C10B 1.594(18) . ?
N2A C12 1.306(11) . ?
N2A C11A 1.461(12) . ?
N2B C12 1.26(3) . ?
N2B C11B 1.50(3) . ?
N3A C29 1.229(6) . ?
N3A C30A 1.458(7) . ?
N3B C29 1.385(9) . ?
N3B C30B 1.505(9) . ?
N4A C32 1.325(6) . ?
N4A C31A 1.493(6) . ?
N4B C32 1.215(9) . ?
N4B C31B 1.455(9) . ?
C1 C2 1.500(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.373(5) . ?
C3 C8 1.422(5) . ?
C4 C5 1.401(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.353(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.418(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.414(5) . ?
C7 C9 1.431(5) . ?
C9 H9 0.9500 . ?
C10A C11A 1.520(9) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10B C11B 1.50(3) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12 C13 1.437(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.412(5) . ?
C13 C18 1.414(5) . ?
C14 C15 1.360(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.404(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.413(5) . ?
C19 C20 1.510(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.505(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.384(5) . ?
C23 C28 1.415(5) . ?
C24 C25 1.396(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.357(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.423(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.415(5) . ?
C27 C29 1.438(5) . ?
C29 H29 0.9500 . ?
C30A C31A 1.525(7) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C30B C31B 1.513(9) . ?
C30B H30D 0.9900 . ?
C30B H30C 0.9900 . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C32 C33 1.450(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.405(6) . ?
C33 C38 1.422(5) . ?
C34 C35 1.367(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.400(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.384(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.414(5) . ?
C39 C40 1.510(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
O12A Ba1 O6 167.83(9) . . ?
O12A Ba1 O2 102.20(10) . . ?
O6 Ba1 O2 73.32(7) . . ?
O12A Ba1 O7 118.68(11) . . ?
O6 Ba1 O7 56.94(7) . . ?
O2 Ba1 O7 118.65(7) . . ?
O12A Ba1 O9B 116.4(3) . . ?
O6 Ba1 O9B 74.8(3) . . ?
O2 Ba1 O9B 122.5(9) . . ?
O7 Ba1 O9B 78.6(8) . . ?
O12A Ba1 O3 103.73(9) . . ?
O6 Ba1 O3 64.27(7) . . ?
O2 Ba1 O3 56.25(6) . . ?
O7 Ba1 O3 70.29(6) . . ?
O9B Ba1 O3 137.6(2) . . ?
O12A Ba1 O10A 71.6(3) . . ?
O6 Ba1 O10A 120.5(3) . . ?
O2 Ba1 O10A 121.20(15) . . ?
O7 Ba1 O10A 114.34(15) . . ?
O9B Ba1 O10A 47.8(4) . . ?
O3 Ba1 O10A 174.5(2) . . ?
O6 Ba1 O12B 136.8(3) . . ?
O2 Ba1 O12B 70.1(3) . . ?
O7 Ba1 O12B 126.1(3) . . ?
O9B Ba1 O12B 145.8(4) . . ?
O3 Ba1 O12B 76.6(3) . . ?
O10A Ba1 O12B 98.0(4) . . ?
O12A Ba1 O1 73.83(11) . . ?
O6 Ba1 O1 110.74(7) . . ?
O2 Ba1 O1 54.29(7) . . ?
O7 Ba1 O1 167.48(7) . . ?
O9B Ba1 O1 96.6(9) . . ?
O3 Ba1 O1 107.58(7) . . ?
O10A Ba1 O1 68.61(14) . . ?
O12B Ba1 O1 63.6(3) . . ?
O12A Ba1 O13B 10.3(3) . . ?
O6 Ba1 O13B 173.8(4) . . ?
O2 Ba1 O13B 110.4(3) . . ?
O7 Ba1 O13B 117.1(4) . . ?
O9B Ba1 O13B 106.3(4) . . ?
O3 Ba1 O13B 113.2(3) . . ?
O10A Ba1 O13B 62.3(4) . . ?
O12B Ba1 O13B 44.0(4) . . ?
O1 Ba1 O13B 75.3(4) . . ?
O12A Ba1 O10B 72.3(4) . . ?
O6 Ba1 O10B 119.5(4) . . ?
O2 Ba1 O10B 128.0(2) . . ?
O7 Ba1 O10B 107.8(2) . . ?
O9B Ba1 O10B 45.2(5) . . ?
O3 Ba1 O10B 174.3(3) . . ?
O12B Ba1 O10B 101.0(5) . . ?
O1 Ba1 O10B 75.5(2) . . ?
O13B Ba1 O10B 62.5(5) . . ?
O12A Ba1 O9A 111.3(2) . . ?
O6 Ba1 O9A 80.05(18) . . ?
O2 Ba1 O9A 124.9(6) . . ?
O7 Ba1 O9A 81.6(6) . . ?
O9B Ba1 O9A 5.2(4) . . ?
O3 Ba1 O9A 142.7(2) . . ?
O10A Ba1 O9A 42.7(3) . . ?
O12B Ba1 O9A 140.7(4) . . ?
O1 Ba1 O9A 94.5(6) . . ?
O13B Ba1 O9A 101.1(4) . . ?
O12A Ba1 O8 74.30(10) . . ?
O6 Ba1 O8 106.60(7) . . ?
O2 Ba1 O8 163.17(6) . . ?
O7 Ba1 O8 53.22(6) . . ?
O9B Ba1 O8 72.5(9) . . ?
O3 Ba1 O8 108.02(6) . . ?
O10A Ba1 O8 73.88(17) . . ?
O12B Ba1 O8 102.0(3) . . ?
O1 Ba1 O8 136.61(6) . . ?
O13B Ba1 O8 68.4(4) . . ?
O10B Ba1 O8 67.2(2) . . ?
O9A Ba1 O8 70.8(7) . . ?
O12A Ba1 O4 66.77(10) . . ?
O6 Ba1 O4 102.37(6) . . ?
O2 Ba1 O4 99.18(6) . . ?
O7 Ba1 O4 63.39(6) . . ?
O9B Ba1 O4 133.8(10) . . ?
O3 Ba1 O4 51.75(6) . . ?
O10A Ba1 O4 126.8(3) . . ?
O12B Ba1 O4 62.7(3) . . ?
O1 Ba1 O4 125.62(7) . . ?
O13B Ba1 O4 72.4(4) . . ?
O10B Ba1 O4 122.6(3) . . ?
O9A Ba1 O4 133.7(7) . . ?
O8 Ba1 O4 64.17(6) . . ?
O12A Ba1 O5 136.66(10) . . ?
O6 Ba1 O5 52.06(7) . . ?
O2 Ba1 O5 63.75(7) . . ?
O7 Ba1 O5 103.08(7) . . ?
O9B Ba1 O5 58.9(9) . . ?
O3 Ba1 O5 100.62(6) . . ?
O10A Ba1 O5 81.5(3) . . ?
O12B Ba1 O5 124.3(3) . . ?
O1 Ba1 O5 64.83(7) . . ?
O13B Ba1 O5 133.8(4) . . ?
O10B Ba1 O5 85.0(3) . . ?
O9A Ba1 O5 61.8(6) . . ?
O8 Ba1 O5 129.99(6) . . ?
O4 Ba1 O5 151.31(6) . . ?
O6 Ba1 N6B 156.8(3) . . ?
O2 Ba1 N6B 88.5(3) . . ?
O7 Ba1 N6B 125.0(3) . . ?
O9B Ba1 N6B 128.0(4) . . ?
O3 Ba1 N6B 93.8(3) . . ?
O10A Ba1 N6B 81.1(4) . . ?
O12B Ba1 N6B 20.3(4) . . ?
O1 Ba1 N6B 67.1(3) . . ?
O13B Ba1 N6B 23.7(4) . . ?
O10B Ba1 N6B 82.9(5) . . ?
O9A Ba1 N6B 122.8(3) . . ?
O8 Ba1 N6B 86.6(3) . . ?
O4 Ba1 N6B 65.7(3) . . ?
O5 Ba1 N6B 131.9(3) . . ?
O2 Cu1 O3 88.19(9) . . ?
O2 Cu1 N1 94.40(12) . . ?
O3 Cu1 N1 175.66(12) . . ?
O2 Cu1 N2A 170.9(2) . . ?
O3 Cu1 N2A 94.7(3) . . ?
N1 Cu1 N2A 83.3(3) . . ?
O2 Cu1 N2B 173.7(4) . . ?
O3 Cu1 N2B 88.6(7) . . ?
N1 Cu1 N2B 88.5(7) . . ?
O2 Cu1 Ba1 45.18(7) . . ?
O3 Cu1 Ba1 46.79(6) . . ?
N1 Cu1 Ba1 134.29(10) . . ?
N2A Cu1 Ba1 140.1(3) . . ?
N2B Cu1 Ba1 129.8(6) . . ?
O6 Cu2 N4A 170.99(15) . . ?
O6 Cu2 O7 88.26(10) . . ?
N4A Cu2 O7 95.26(16) . . ?
O6 Cu2 N3A 91.54(17) . . ?
N4A Cu2 N3A 85.8(2) . . ?
O7 Cu2 N3A 173.83(18) . . ?
O6 Cu2 N3B 97.3(3) . . ?
O7 Cu2 N3B 172.5(3) . . ?
O6 Cu2 N4B 176.4(4) . . ?
O7 Cu2 N4B 90.3(3) . . ?
N3B Cu2 N4B 84.5(4) . . ?
O6 Cu2 Ba1 47.72(7) . . ?
N4A Cu2 Ba1 139.16(14) . . ?
O7 Cu2 Ba1 48.36(7) . . ?
N3A Cu2 Ba1 128.27(14) . . ?
N3B Cu2 Ba1 138.9(3) . . ?
N4B Cu2 Ba1 129.4(3) . . ?
C3 O1 C2 117.2(3) . . ?
C3 O1 Ba1 119.7(2) . . ?
C2 O1 Ba1 122.3(2) . . ?
C8 O2 Cu1 125.7(2) . . ?
C8 O2 Ba1 124.0(2) . . ?
Cu1 O2 Ba1 105.96(9) . . ?
C18 O3 Cu1 124.7(2) . . ?
C18 O3 Ba1 131.4(2) . . ?
Cu1 O3 Ba1 103.76(9) . . ?
C17 O4 C19 117.8(3) . . ?
C17 O4 Ba1 121.14(19) . . ?
C19 O4 Ba1 121.02(18) . . ?
C23 O5 C22 118.0(3) . . ?
C23 O5 Ba1 116.02(19) . . ?
C22 O5 Ba1 125.7(2) . . ?
C28 O6 Cu2 126.7(2) . . ?
C28 O6 Ba1 125.6(2) . . ?
Cu2 O6 Ba1 101.81(9) . . ?
C38 O7 Cu2 126.9(2) . . ?
C38 O7 Ba1 126.7(2) . . ?
Cu2 O7 Ba1 100.91(9) . . ?
C37 O8 C39 118.7(3) . . ?
C37 O8 Ba1 119.90(19) . . ?
C39 O8 Ba1 119.59(19) . . ?
N5A O9A Ba1 98.1(19) . . ?
N5B O9B Ba1 98(2) . . ?
N5A O10A Ba1 101(2) . . ?
N5B O10B Ba1 96(3) . . ?
N6A O12A Ba1 151.9(3) . . ?
N6B O12B Ba1 100.6(11) . . ?
N6B O13B Ba1 92.2(11) . . ?
C9 N1 C10A 118.9(4) . . ?
C9 N1 C10B 126.8(8) . . ?
C9 N1 Cu1 126.4(3) . . ?
C10A N1 Cu1 114.0(3) . . ?
C10B N1 Cu1 104.4(7) . . ?
C12 N2A C11A 121.3(8) . . ?
C12 N2A Cu1 124.6(7) . . ?
C11A N2A Cu1 114.1(6) . . ?
C12 N2B C11B 120.0(19) . . ?
C12 N2B Cu1 124.2(16) . . ?
C11B N2B Cu1 108.6(16) . . ?
C29 N3A C30A 117.2(5) . . ?
C29 N3A Cu2 129.2(5) . . ?
C30A N3A Cu2 113.0(4) . . ?
C29 N3B C30B 132.4(12) . . ?
C29 N3B Cu2 118.4(7) . . ?
C30B N3B Cu2 108.6(7) . . ?
C32 N4A C31A 124.5(5) . . ?
C32 N4A Cu2 124.4(4) . . ?
C31A N4A Cu2 111.1(4) . . ?
C32 N4B C31B 114.0(10) . . ?
C32 N4B Cu2 126.9(8) . . ?
C31B N4B Cu2 116.4(7) . . ?
O9A N5A O11A 125(3) . . ?
O9A N5A O10A 116(2) . . ?
O11A N5A O10A 119(3) . . ?
O9A N5A Ba1 61.4(16) . . ?
O11A N5A Ba1 170.1(12) . . ?
O10A N5A Ba1 56.8(17) . . ?
O10B N5B O11B 124(4) . . ?
O10B N5B O9B 120(3) . . ?
O11B N5B O9B 116(4) . . ?
O10B N5B Ba1 62(3) . . ?
O11B N5B Ba1 174(3) . . ?
O9B N5B Ba1 58.1(18) . . ?
O13A N6A O14A 122.6(4) . . ?
O13A N6A O12A 117.9(4) . . ?
O14A N6A O12A 119.5(4) . . ?
O12B N6B O13B 123.1(17) . . ?
O12B N6B O14B 121(2) . . ?
O13B N6B O14B 114(2) . . ?
O12B N6B Ba1 59.1(10) . . ?
O13B N6B Ba1 64.1(10) . . ?
O14B N6B Ba1 163.3(18) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 112.6(3) . . ?
O1 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
O1 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 O1 124.3(3) . . ?
C4 C3 C8 121.5(3) . . ?
O1 C3 C8 114.1(3) . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 121.5(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 C9 122.6(3) . . ?
C6 C7 C9 117.8(3) . . ?
O2 C8 C7 125.5(3) . . ?
O2 C8 C3 117.2(3) . . ?
C7 C8 C3 117.3(3) . . ?
N1 C9 C7 125.3(3) . . ?
N1 C9 H9 117.4 . . ?
C7 C9 H9 117.4 . . ?
N1 C10A C11A 105.6(5) . . ?
N1 C10A H10A 110.6 . . ?
C11A C10A H10A 110.6 . . ?
N1 C10A H10B 110.6 . . ?
C11A C10A H10B 110.6 . . ?
H10A C10A H10B 108.7 . . ?
C11B C10B N1 105.8(12) . . ?
C11B C10B H10C 110.6 . . ?
N1 C10B H10C 110.6 . . ?
C11B C10B H10D 110.6 . . ?
N1 C10B H10D 110.6 . . ?
H10C C10B H10D 108.7 . . ?
N2A C11A C10A 108.7(6) . . ?
N2A C11A H11A 109.9 . . ?
C10A C11A H11A 109.9 . . ?
N2A C11A H11B 109.9 . . ?
C10A C11A H11B 109.9 . . ?
H11A C11A H11B 108.3 . . ?
C10B C11B N2B 106.1(14) . . ?
C10B C11B H11C 110.5 . . ?
N2B C11B H11C 110.5 . . ?
C10B C11B H11D 110.5 . . ?
N2B C11B H11D 110.5 . . ?
H11C C11B H11D 108.7 . . ?
N2B C12 C13 120.6(11) . . ?
N2A C12 C13 125.4(6) . . ?
N2B C12 H12 116.4 . . ?
N2A C12 H12 117.3 . . ?
C13 C12 H12 117.3 . . ?
C14 C13 C18 119.4(3) . . ?
C14 C13 C12 117.5(3) . . ?
C18 C13 C12 122.7(3) . . ?
C15 C14 C13 121.1(3) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 119.7(4) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
O4 C17 C16 124.8(3) . . ?
O4 C17 C18 114.0(3) . . ?
C16 C17 C18 121.2(3) . . ?
O3 C18 C17 117.3(3) . . ?
O3 C18 C13 124.5(3) . . ?
C17 C18 C13 118.2(3) . . ?
O4 C19 C20 112.7(3) . . ?
O4 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
O4 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C21 111.5(3) . . ?
O5 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
O5 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
O5 C23 C24 124.9(4) . . ?
O5 C23 C28 113.9(3) . . ?
C24 C23 C28 121.2(4) . . ?
C23 C24 C25 120.2(4) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 120.0(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 121.3(4) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 119.3(4) . . ?
C28 C27 C29 122.7(4) . . ?
C26 C27 C29 117.9(4) . . ?
O6 C28 C23 117.5(3) . . ?
O6 C28 C27 124.6(3) . . ?
C23 C28 C27 117.8(3) . . ?
N3A C29 C27 123.4(4) . . ?
N3B C29 C27 127.4(7) . . ?
N3A C29 H29 118.3 . . ?
N3B C29 H29 111.4 . . ?
C27 C29 H29 118.3 . . ?
N3A C30A C31A 105.9(5) . . ?
N3A C30A H30A 110.6 . . ?
C31A C30A H30A 110.6 . . ?
N3A C30A H30B 110.6 . . ?
C31A C30A H30B 110.6 . . ?
H30A C30A H30B 108.7 . . ?
N3B C30B C31B 114.5(9) . . ?
N3B C30B H30D 108.6 . . ?
C31B C30B H30D 108.6 . . ?
N3B C30B H30C 108.6 . . ?
C31B C30B H30C 108.6 . . ?
H30D C30B H30C 107.6 . . ?
N4A C31A C30A 109.4(4) . . ?
N4A C31A H31A 109.8 . . ?
C30A C31A H31A 109.8 . . ?
N4A C31A H31B 109.8 . . ?
C30A C31A H31B 109.8 . . ?
H31A C31A H31B 108.2 . . ?
N4B C31B C30B 102.4(9) . . ?
N4B C31B H31C 111.3 . . ?
C30B C31B H31C 111.3 . . ?
N4B C31B H31D 111.3 . . ?
C30B C31B H31D 111.3 . . ?
H31C C31B H31D 109.2 . . ?
N4B C32 C33 121.5(6) . . ?
N4A C32 C33 126.4(4) . . ?
N4B C32 H32 118.1 . . ?
N4A C32 H32 116.8 . . ?
C33 C32 H32 116.8 . . ?
C34 C33 C38 119.9(4) . . ?
C34 C33 C32 118.1(3) . . ?
C38 C33 C32 122.0(3) . . ?
C35 C34 C33 121.1(3) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 120.0(4) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.1(4) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
O8 C37 C36 124.7(3) . . ?
O8 C37 C38 114.0(3) . . ?
C36 C37 C38 121.3(3) . . ?
O7 C38 C37 117.7(3) . . ?
O7 C38 C33 124.7(3) . . ?
C37 C38 C33 117.6(3) . . ?
O8 C39 C40 111.9(3) . . ?
O8 C39 H39A 109.2 . . ?
C40 C39 H39A 109.2 . . ?
O8 C39 H39B 109.2 . . ?
C40 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.072

##===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 735470'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H44 Cu2 N8 O20 Pb2'
_chemical_formula_sum            'C40 H44 Cu2 N8 O20 Pb2'
_chemical_formula_weight         1498.29

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'
Pb Pb -3.3944 10.1111 '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                   14.368(2)
_cell_length_b                   13.590(2)
_cell_length_c                   12.525(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.438(7)
_cell_angle_gamma                90.00
_cell_volume                     2345.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5102
_cell_measurement_theta_min      2.426
_cell_measurement_theta_max      29.940

_exptl_crystal_description       block
_exptl_crystal_colour            dark_red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1444
_exptl_absorpt_coefficient_mu    8.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_process_details   'SADABS, (G. Sheldrick, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bede Microsource'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Proteum M'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17279
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4114
_reflns_number_gt                3860
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0268P)²+4.6821P] 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         4114
_refine_ls_number_parameters     337
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0558
_refine_ls_wR_factor_gt          0.0548
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.071
_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
Pb1 Pb 0.306155(10) 0.514014(10) 0.886752(12) 0.01741(6) Uani 1 1 d . . .
Cu1 Cu 0.15858(3) 0.65057(3) 1.00356(4) 0.01721(11) Uani 1 1 d . . .
O1A O 0.2781(7) 0.3442(7) 0.9906(5) 0.0222(15) Uani 0.66 1 d P A 1
O1B O 0.3007(15) 0.3534(16) 1.0264(12) 0.0222(15) Uani 0.34 1 d P A 2
O2 O 0.2054(2) 0.51830(19) 1.0128(2) 0.0205(6) Uani 1 1 d . A .
O3 O 0.21968(19) 0.67119(19) 0.8886(2) 0.0193(6) Uani 1 1 d . A .
O4 O 0.3341(2) 0.6694(2) 0.7568(2) 0.0225(6) Uani 1 1 d . A .
O5 O 0.4164(2) 0.6434(2) 1.0175(2) 0.0282(7) Uani 1 1 d . A .
O6 O 0.4558(3) 0.4992(2) 1.0881(3) 0.0344(8) Uani 1 1 d . A .
O7 O 0.5506(2) 0.6241(2) 1.1482(3) 0.0302(7) Uani 1 1 d . A .
O8 O 0.1299(2) 0.4658(3) 0.7844(3) 0.0384(8) Uani 1 1 d U A .
O9 O 0.2045(3) 0.4656(2) 0.6582(3) 0.0352(8) Uani 1 1 d . A .
O10 O 0.0493(3) 0.4412(3) 0.6139(3) 0.0508(10) Uani 1 1 d . A .
N1 N 0.0759(3) 0.6276(3) 1.0964(3) 0.0238(8) Uani 1 1 d . A .
N2 N 0.1309(2) 0.7875(2) 1.0184(3) 0.0202(7) Uani 1 1 d . A .
N3 N 0.4748(2) 0.5889(3) 1.0850(3) 0.0242(8) Uani 1 1 d . . .
N4 N 0.1269(3) 0.4576(3) 0.6835(3) 0.0275(8) Uani 1 1 d . . .
C1A C 0.4076(6) 0.2231(7) 1.0645(8) 0.0484(19) Uani 0.66 1 d P A 1
H1A H 0.4579 0.2722 1.0661 0.073 Uiso 0.66 1 calc PR A 1
H1B H 0.4304 0.1580 1.0493 0.073 Uiso 0.66 1 calc PR A 1
H1C H 0.3937 0.2221 1.1367 0.073 Uiso 0.66 1 calc PR A 1
C1B C 0.3447(12) 0.1898(13) 0.9803(15) 0.0484(19) Uani 0.34 1 d P A 2
H1D H 0.3171 0.2120 0.9033 0.073 Uiso 0.34 1 calc PR A 2
H1E H 0.2955 0.1531 1.0043 0.073 Uiso 0.34 1 calc PR A 2
H1F H 0.4006 0.1472 0.9846 0.073 Uiso 0.34 1 calc PR A 2
C2A C 0.3163(5) 0.2493(5) 0.9741(6) 0.0280(13) Uani 0.66 1 d P A 1
H2A H 0.3306 0.2487 0.9013 0.034 Uiso 0.66 1 calc PR A 1
H2B H 0.2663 0.1985 0.9719 0.034 Uiso 0.66 1 calc PR A 1
C2B C 0.3759(10) 0.2758(10) 1.0532(12) 0.0280(13) Uani 0.34 1 d P A 2
H2C H 0.4373 0.3020 1.0435 0.034 Uiso 0.34 1 calc PR A 2
H2D H 0.3880 0.2556 1.1319 0.034 Uiso 0.34 1 calc PR A 2
C3 C 0.2248(3) 0.3526(3) 1.0696(4) 0.0272(10) Uani 1 1 d . . .
C4 C 0.2083(4) 0.2756(3) 1.1337(4) 0.0364(12) Uani 1 1 d . A .
H4 H 0.2412 0.2149 1.1348 0.044 Uiso 1 1 calc R . .
C5 C 0.1438(4) 0.2869(3) 1.1963(4) 0.0404(12) Uani 1 1 d . . .
H5 H 0.1314 0.2335 1.2392 0.048 Uiso 1 1 calc R A .
C6 C 0.0979(4) 0.3748(3) 1.1967(4) 0.0363(11) Uani 1 1 d . A .
H6 H 0.0532 0.3817 1.2394 0.044 Uiso 1 1 calc R . .
C7 C 0.1158(3) 0.4558(3) 1.1346(4) 0.0252(9) Uani 1 1 d . . .
C8 C 0.1817(3) 0.4456(3) 1.0714(3) 0.0197(8) Uani 1 1 d . A .
C9 C 0.0659(3) 0.5465(3) 1.1439(4) 0.0266(9) Uani 1 1 d . A .
H9 H 0.0225 0.5458 1.1887 0.032 Uiso 1 1 calc R . .
C10 C 0.0184(3) 0.7146(3) 1.1073(4) 0.0306(10) Uani 1 1 d . . .
H10A H 0.0035 0.7131 1.1798 0.037 Uiso 1 1 calc R A .
H10B H -0.0436 0.7150 1.0473 0.037 Uiso 1 1 calc R . .
C11 C 0.0767(3) 0.8059(3) 1.0997(3) 0.0238(9) Uani 1 1 d . A .
H11A H 0.0328 0.8629 1.0758 0.029 Uiso 1 1 calc R . .
H11B H 0.1222 0.8211 1.1733 0.029 Uiso 1 1 calc R . .
C12 C 0.1613(3) 0.8593(3) 0.9704(3) 0.0205(8) Uani 1 1 d . . .
H12 H 0.1421 0.9239 0.9842 0.025 Uiso 1 1 calc R A .
C13 C 0.2220(3) 0.8493(3) 0.8974(3) 0.0208(9) Uani 1 1 d . A .
C14 C 0.2573(3) 0.9376(3) 0.8645(4) 0.0259(9) Uani 1 1 d . . .
H14 H 0.2376 0.9987 0.8879 0.031 Uiso 1 1 calc R A .
C15 C 0.3191(3) 0.9370(3) 0.7995(4) 0.0304(10) Uani 1 1 d . A .
H15 H 0.3438 0.9971 0.7800 0.037 Uiso 1 1 calc R . .
C16 C 0.3458(3) 0.8478(3) 0.7621(4) 0.0285(10) Uani 1 1 d . . .
H16 H 0.3881 0.8474 0.7159 0.034 Uiso 1 1 calc R A .
C17 C 0.3114(3) 0.7602(3) 0.7914(3) 0.0221(9) Uani 1 1 d . A .
C18 C 0.2497(3) 0.7585(3) 0.8611(3) 0.0184(8) Uani 1 1 d . . .
C19 C 0.3933(3) 0.6696(3) 0.6804(4) 0.0268(10) Uani 1 1 d . . .
H19A H 0.4568 0.7006 0.7162 0.032 Uiso 1 1 calc R A .
H19B H 0.3608 0.7080 0.6131 0.032 Uiso 1 1 calc R . .
C20 C 0.4082(3) 0.5654(3) 0.6487(4) 0.0299(10) Uani 1 1 d . A .
H20A H 0.4428 0.5285 0.7153 0.045 Uiso 1 1 calc R . .
H20B H 0.4464 0.5652 0.5951 0.045 Uiso 1 1 calc R . .
H20C H 0.3451 0.5346 0.6149 0.045 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.427(3) . ?
Pb1 O3 2.474(3) . ?
Pb1 O8 2.579(3) . ?
Pb1 O5 2.611(3) . ?
Pb1 O1A 2.735(10) . ?
Pb1 O4 2.764(3) . ?
Pb1 O1B 2.81(2) . ?
Pb1 O6 2.820(4) . ?
Pb1 O9 2.897(4) . ?
Pb1 O7 2.909(3) 3_667 ?
Cu1 O3 1.908(3) . ?
Cu1 N1 1.908(3) . ?
Cu1 O2 1.911(3) . ?
Cu1 N2 1.923(3) . ?
O1A C3 1.417(11) . ?
O1A C2A 1.439(12) . ?
O1B C3 1.35(2) . ?
O1B C2B 1.48(3) . ?
O2 C8 1.330(5) . ?
O3 C18 1.340(5) . ?
O4 C17 1.378(5) . ?
O4 C19 1.449(5) . ?
O5 N3 1.251(4) . ?
O6 N3 1.252(5) . ?
O7 N3 1.246(5) . ?
O8 N4 1.258(5) . ?
O9 N4 1.247(5) . ?
O10 N4 1.226(5) . ?
N1 C9 1.280(6) . ?
N1 C10 1.471(5) . ?
N2 C12 1.286(5) . ?
N2 C11 1.468(5) . ?
C1A C2A 1.513(11) . ?
C1A H1A 0.9800 . ?
C1A H1B 0.9800 . ?
C1A H1C 0.9800 . ?
C1B C2B 1.47(2) . ?
C1B H1D 0.9800 . ?
C1B H1E 0.9800 . ?
C1B H1F 0.9800 . ?
C2A H2A 0.9900 . ?
C2A H2B 0.9900 . ?
C2B H2C 0.9900 . ?
C2B H2D 0.9900 . ?
C3 C4 1.379(6) . ?
C3 C8 1.411(6) . ?
C4 C5 1.382(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.412(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.402(6) . ?
C7 C9 1.448(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.515(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.438(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.409(6) . ?
C13 C18 1.410(6) . ?
C14 C15 1.363(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.410(6) . ?
C19 C20 1.502(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O3 65.14(9) . . ?
O2 Pb1 O8 69.29(10) . . ?
O3 Pb1 O8 78.38(10) . . ?
O2 Pb1 O5 86.74(10) . . ?
O3 Pb1 O5 68.27(9) . . ?
O8 Pb1 O5 144.98(10) . . ?
O2 Pb1 O1A 61.0(2) . . ?
O3 Pb1 O1A 125.6(2) . . ?
O8 Pb1 O1A 76.46(17) . . ?
O5 Pb1 O1A 114.52(12) . . ?
O2 Pb1 O4 125.30(8) . . ?
O3 Pb1 O4 60.21(8) . . ?
O8 Pb1 O4 100.80(10) . . ?
O5 Pb1 O4 72.03(9) . . ?
O1A Pb1 O4 172.06(15) . . ?
O2 Pb1 O1B 59.1(5) . . ?
O3 Pb1 O1B 124.2(5) . . ?
O8 Pb1 O1B 85.2(4) . . ?
O5 Pb1 O1B 104.5(3) . . ?
O1A Pb1 O1B 10.0(3) . . ?
O4 Pb1 O1B 173.5(4) . . ?
O2 Pb1 O6 82.18(10) . . ?
O3 Pb1 O6 108.11(9) . . ?
O8 Pb1 O6 145.01(11) . . ?
O5 Pb1 O6 46.64(9) . . ?
O1A Pb1 O6 72.07(14) . . ?
O4 Pb1 O6 112.34(9) . . ?
O1B Pb1 O6 62.4(3) . . ?
O2 Pb1 O9 114.93(10) . . ?
O3 Pb1 O9 95.22(9) . . ?
O8 Pb1 O9 45.70(10) . . ?
O5 Pb1 O9 145.05(9) . . ?
O1A Pb1 O9 100.21(12) . . ?
O4 Pb1 O9 73.04(9) . . ?
O1B Pb1 O9 110.1(3) . . ?
O6 Pb1 O9 155.65(10) . . ?
O2 Pb1 O7 133.76(9) . 3_667 ?
O3 Pb1 O7 159.53(9) . 3_667 ?
O8 Pb1 O7 113.51(10) . 3_667 ?
O5 Pb1 O7 101.51(9) . 3_667 ?
O1A Pb1 O7 74.5(2) . 3_667 ?
O4 Pb1 O7 100.19(9) . 3_667 ?
O1B Pb1 O7 74.9(5) . 3_667 ?
O6 Pb1 O7 72.30(9) . 3_667 ?
O9 Pb1 O7 83.40(9) . 3_667 ?
O3 Cu1 N1 169.36(14) . . ?
O3 Cu1 O2 87.42(12) . . ?
N1 Cu1 O2 94.46(14) . . ?
O3 Cu1 N2 94.74(13) . . ?
N1 Cu1 N2 85.31(14) . . ?
O2 Cu1 N2 169.48(14) . . ?
C3 O1A C2A 118.4(7) . . ?
C3 O1A Pb1 116.5(5) . . ?
C2A O1A Pb1 125.1(6) . . ?
C3 O1B C2B 121.7(16) . . ?
C3 O1B Pb1 115.1(12) . . ?
C2B O1B Pb1 123.2(13) . . ?
C8 O2 Cu1 126.3(3) . . ?
C8 O2 Pb1 129.3(2) . . ?
Cu1 O2 Pb1 104.32(11) . . ?
C18 O3 Cu1 125.0(2) . . ?
C18 O3 Pb1 124.3(2) . . ?
Cu1 O3 Pb1 102.70(11) . . ?
C17 O4 C19 116.2(3) . . ?
C17 O4 Pb1 114.3(2) . . ?
C19 O4 Pb1 126.9(2) . . ?
N3 O5 Pb1 101.4(2) . . ?
N3 O6 Pb1 91.2(2) . . ?
N4 O8 Pb1 105.7(3) . . ?
N4 O9 Pb1 90.3(2) . . ?
C9 N1 C10 120.6(4) . . ?
C9 N1 Cu1 126.6(3) . . ?
C10 N1 Cu1 112.8(3) . . ?
C12 N2 C11 120.8(3) . . ?
C12 N2 Cu1 125.7(3) . . ?
C11 N2 Cu1 113.4(3) . . ?
O7 N3 O5 120.1(4) . . ?
O7 N3 O6 120.8(4) . . ?
O5 N3 O6 119.1(4) . . ?
O10 N4 O9 122.3(4) . . ?
O10 N4 O8 119.7(4) . . ?
O9 N4 O8 118.0(4) . . ?
C2B C1B H1D 109.5 . . ?
C2B C1B H1E 109.5 . . ?
H1D C1B H1E 109.5 . . ?
C2B C1B H1F 109.5 . . ?
H1D C1B H1F 109.5 . . ?
H1E C1B H1F 109.5 . . ?
O1A C2A C1A 112.9(6) . . ?
O1A C2A H2A 109.0 . . ?
C1A C2A H2A 109.0 . . ?
O1A C2A H2B 109.0 . . ?
C1A C2A H2B 109.0 . . ?
H2A C2A H2B 107.8 . . ?
C1B C2B O1B 110.5(13) . . ?
C1B C2B H2C 109.6 . . ?
O1B C2B H2C 109.6 . . ?
C1B C2B H2D 109.6 . . ?
O1B C2B H2D 109.6 . . ?
H2C C2B H2D 108.1 . . ?
O1B C3 C4 122.2(10) . . ?
O1B C3 C8 114.0(10) . . ?
C4 C3 C8 121.4(4) . . ?
C4 C3 O1A 124.2(5) . . ?
C8 C3 O1A 114.2(5) . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.1(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 C9 123.9(4) . . ?
C6 C7 C9 116.6(4) . . ?
O2 C8 C7 123.8(4) . . ?
O2 C8 C3 118.3(4) . . ?
C7 C8 C3 117.8(4) . . ?
N1 C9 C7 124.9(4) . . ?
N1 C9 H9 117.5 . . ?
C7 C9 H9 117.5 . . ?
N1 C10 C11 108.5(3) . . ?
N1 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
N1 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C10 108.4(3) . . ?
N2 C11 H11A 110.0 . . ?
C10 C11 H11A 110.0 . . ?
N2 C11 H11B 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
N2 C12 C13 124.9(4) . . ?
N2 C12 H12 117.5 . . ?
C13 C12 H12 117.5 . . ?
C14 C13 C18 119.5(4) . . ?
C14 C13 C12 116.0(4) . . ?
C18 C13 C12 124.4(4) . . ?
C15 C14 C13 121.3(4) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 119.6(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
O4 C17 C16 123.7(4) . . ?
O4 C17 C18 115.2(3) . . ?
C16 C17 C18 121.0(4) . . ?
O3 C18 C17 118.6(3) . . ?
O3 C18 C13 123.5(4) . . ?
C17 C18 C13 118.0(4) . . ?
O4 C19 C20 109.1(3) . . ?
O4 C19 H19A 109.9 . . ?
C20 C19 H19A 109.9 . . ?
O4 C19 H19B 109.9 . . ?
C20 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.854
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.113

##===END

data_4
_database_code_depnum_ccdc_archive 'CCDC 735471'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C20 H22 Cu N2 O4), 0.5(N4 O18 U2), 2(H2 O)'
_chemical_formula_sum            'C40 H48 Cu2 N6 O19 U'
_chemical_formula_weight         1281.95

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.6881(4)
_cell_length_b                   13.5598(5)
_cell_length_c                   15.4935(7)
_cell_angle_alpha                115.9350(10)
_cell_angle_beta                 96.1930(10)
_cell_angle_gamma                100.8460(10)
_cell_volume                     2299.13(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7188
_cell_measurement_theta_min      2.272
_cell_measurement_theta_max      30.000

_exptl_crystal_description       block
_exptl_crystal_colour            dark_red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    4.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_T_max  0.406
_exptl_absorpt_process_details   'SADABS, (G. Sheldrick, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bede microsource'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Proteum M'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17268
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.62
_diffrn_reflns_theta_max         25.03
_reflns_number_total             8027
_reflns_number_gt                7602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0275P)²+0.9327P] 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         8027
_refine_ls_number_parameters     629
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0490
_refine_ls_wR_factor_gt          0.0484
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
U1 U 0.060698(7) 0.389051(7) 0.022877(7) 0.01978(4) Uani 1 1 d . . .
Cu1 Cu 0.46229(2) 1.06864(3) 0.11453(2) 0.02041(7) Uani 1 1 d . . .
Cu2 Cu 0.51449(2) 0.96664(2) 0.38095(2) 0.02044(7) Uani 1 1 d . . .
O1 O 0.61884(14) 0.83813(15) 0.18442(14) 0.0262(4) Uani 1 1 d . . .
O2 O 0.51162(14) 0.95816(14) 0.14014(13) 0.0222(4) Uani 1 1 d . . .
O3 O 0.60866(14) 1.16952(14) 0.17156(13) 0.0235(4) Uani 1 1 d . . .
O4 O 0.81603(15) 1.27264(16) 0.24575(15) 0.0312(4) Uani 1 1 d . . .
O5 O 0.71735(15) 1.07020(16) 0.24055(16) 0.0307(4) Uani 1 1 d D . .
H5A H 0.6639(16) 1.0162(17) 0.225(2) 0.037 Uiso 1 1 d D . .
H5B H 0.698(2) 1.1181(19) 0.227(2) 0.037 Uiso 1 1 d D . .
O6 O 0.85874(16) 1.09448(18) 0.55066(15) 0.0347(5) Uani 1 1 d . . .
O7 O 0.66221(15) 1.00178(15) 0.44726(13) 0.0262(4) Uani 1 1 d . . .
O8 O 0.54449(14) 1.11358(15) 0.38996(13) 0.0229(4) Uani 1 1 d . . .
O9 O 0.62107(15) 1.32249(15) 0.43109(14) 0.0286(4) Uani 1 1 d . . .
O10 O 0.77301(18) 1.18297(18) 0.42032(16) 0.0363(5) Uani 1 1 d D . .
H10C H 0.7088(13) 1.191(3) 0.417(3) 0.044 Uiso 1 1 d D . .
H10D H 0.775(2) 1.139(2) 0.444(2) 0.044 Uiso 1 1 d D . .
O11 O 0.21008(16) 0.52686(15) 0.17304(14) 0.0318(5) Uani 1 1 d . . .
O12 O 0.20581(17) 0.35141(16) 0.12428(17) 0.0427(6) Uani 1 1 d . . .
O13 O 0.33695(18) 0.48335(17) 0.24583(17) 0.0446(6) Uani 1 1 d . . .
O14 O 0.06118(16) 0.18482(16) -0.02398(16) 0.0355(5) Uani 1 1 d . . .
O15 O -0.06178(15) 0.20482(15) -0.11748(14) 0.0289(4) Uani 1 1 d . . .
O16 O -0.04364(17) 0.03547(16) -0.15302(17) 0.0431(5) Uani 1 1 d . . .
O17 O -0.03033(15) 0.38081(17) 0.09997(14) 0.0288(4) Uani 1 1 d . . .
O18 O 0.15436(16) 0.38837(16) -0.05404(15) 0.0334(5) Uani 1 1 d . . .
O19 O 0.07261(15) 0.58106(15) 0.07081(13) 0.0246(4) Uani 1 1 d . . .
N1 N 0.31532(17) 0.96841(19) 0.04721(16) 0.0256(5) Uani 1 1 d . . .
N2 N 0.40877(18) 1.1750(2) 0.08259(16) 0.0258(5) Uani 1 1 d . . .
N3 N 0.47560(19) 0.82157(18) 0.38113(16) 0.0261(5) Uani 1 1 d . . .
N4 N 0.36509(17) 0.92222(18) 0.30826(15) 0.0216(5) Uani 1 1 d . . .
N5 N 0.25439(19) 0.45566(19) 0.18383(18) 0.0321(6) Uani 1 1 d . . .
N6 N -0.01586(18) 0.13734(18) -0.10056(18) 0.0286(5) Uani 1 1 d . . .
C1 C 0.8055(2) 0.8509(3) 0.2383(2) 0.0371(7) Uani 1 1 d . . .
H1A H 0.8270 0.8884 0.1988 0.056 Uiso 1 1 calc R . .
H1B H 0.8580 0.8080 0.2428 0.056 Uiso 1 1 calc R . .
H1C H 0.8051 0.9084 0.3044 0.056 Uiso 1 1 calc R . .
C2 C 0.6930(2) 0.7716(2) 0.1906(2) 0.0314(6) Uani 1 1 d . . .
H2A H 0.6926 0.7124 0.1241 0.038 Uiso 1 1 calc R . .
H2B H 0.6701 0.7338 0.2301 0.038 Uiso 1 1 calc R . .
C3 C 0.5164(2) 0.7800(2) 0.12517(19) 0.0241(6) Uani 1 1 d . . .
C4 C 0.4703(2) 0.6650(2) 0.0884(2) 0.0290(6) Uani 1 1 d . . .
H4 H 0.5105 0.6198 0.1033 0.035 Uiso 1 1 calc R . .
C5 C 0.3639(2) 0.6149(2) 0.0289(2) 0.0313(6) Uani 1 1 d . . .
H5 H 0.3322 0.5356 0.0028 0.038 Uiso 1 1 calc R . .
C6 C 0.3061(2) 0.6802(2) 0.00865(19) 0.0279(6) Uani 1 1 d . . .
H6 H 0.2338 0.6457 -0.0309 0.033 Uiso 1 1 calc R . .
C7 C 0.3514(2) 0.7984(2) 0.04532(18) 0.0229(5) Uani 1 1 d . . .
C8 C 0.4594(2) 0.8501(2) 0.10425(18) 0.0213(5) Uani 1 1 d . . .
C9 C 0.2849(2) 0.8617(2) 0.02092(19) 0.0260(6) Uani 1 1 d . . .
H9 H 0.2128 0.8212 -0.0177 0.031 Uiso 1 1 calc R . .
C10 C 0.2384(2) 1.0262(3) 0.0238(2) 0.0338(7) Uani 1 1 d . . .
H10A H 0.1990 1.0561 0.0776 0.041 Uiso 1 1 calc R . .
H10B H 0.1835 0.9721 -0.0374 0.041 Uiso 1 1 calc R . .
C11 C 0.3028(2) 1.1227(3) 0.0110(2) 0.0328(7) Uani 1 1 d . . .
H11A H 0.3156 1.0937 -0.0566 0.039 Uiso 1 1 calc R . .
H11B H 0.2608 1.1801 0.0217 0.039 Uiso 1 1 calc R . .
C12 C 0.4565(2) 1.2811(2) 0.1165(2) 0.0271(6) Uani 1 1 d . . .
H12 H 0.4158 1.3257 0.1013 0.033 Uiso 1 1 calc R . .
C13 C 0.5665(2) 1.3382(2) 0.17550(19) 0.0252(6) Uani 1 1 d . . .
C14 C 0.6060(3) 1.4557(2) 0.2062(2) 0.0322(6) Uani 1 1 d . . .
H14 H 0.5570 1.4961 0.1953 0.039 Uiso 1 1 calc R . .
C15 C 0.7132(3) 1.5118(2) 0.2514(2) 0.0350(7) Uani 1 1 d . . .
H15 H 0.7380 1.5911 0.2731 0.042 Uiso 1 1 calc R . .
C16 C 0.7867(2) 1.4529(2) 0.2659(2) 0.0317(6) Uani 1 1 d . . .
H16 H 0.8618 1.4919 0.2956 0.038 Uiso 1 1 calc R . .
C17 C 0.7511(2) 1.3391(2) 0.23743(19) 0.0264(6) Uani 1 1 d . . .
C18 C 0.6385(2) 1.2785(2) 0.19394(19) 0.0235(5) Uani 1 1 d . . .
C19 C 0.9320(2) 1.3236(2) 0.2856(2) 0.0311(6) Uani 1 1 d . . .
H19A H 0.9452 1.3789 0.3561 0.037 Uiso 1 1 calc R . .
H19B H 0.9629 1.3641 0.2504 0.037 Uiso 1 1 calc R . .
C20 C 0.9851(3) 1.2302(3) 0.2732(3) 0.0502(9) Uani 1 1 d . . .
H20A H 0.9551 1.1919 0.3096 0.075 Uiso 1 1 calc R . .
H20B H 1.0646 1.2621 0.2985 0.075 Uiso 1 1 calc R . .
H20C H 0.9704 1.1753 0.2033 0.075 Uiso 1 1 calc R . .
C21 C 0.9730(3) 1.2805(3) 0.6526(3) 0.0464(8) Uani 1 1 d . . .
H21A H 0.9858 1.2903 0.5953 0.070 Uiso 1 1 calc R . .
H21B H 1.0369 1.3264 0.7071 0.070 Uiso 1 1 calc R . .
H21C H 0.9076 1.3051 0.6721 0.070 Uiso 1 1 calc R . .
C22 C 0.9558(2) 1.1585(3) 0.6274(2) 0.0383(7) Uani 1 1 d . . .
H22A H 1.0201 1.1319 0.6048 0.046 Uiso 1 1 calc R . .
H22B H 0.9468 1.1482 0.6859 0.046 Uiso 1 1 calc R . .
C23 C 0.8187(2) 0.9824(3) 0.5261(2) 0.0297(6) Uani 1 1 d . . .
C24 C 0.8756(3) 0.9175(3) 0.5507(2) 0.0373(7) Uani 1 1 d . . .
H24 H 0.9494 0.9502 0.5872 0.045 Uiso 1 1 calc R . .
C25 C 0.8244(3) 0.8032(3) 0.5216(2) 0.0408(8) Uani 1 1 d . . .
H25 H 0.8646 0.7579 0.5362 0.049 Uiso 1 1 calc R . .
C26 C 0.7175(3) 0.7572(3) 0.4726(2) 0.0359(7) Uani 1 1 d . . .
H26 H 0.6830 0.6806 0.4555 0.043 Uiso 1 1 calc R . .
C27 C 0.6565(2) 0.8212(2) 0.44655(19) 0.0292(6) Uani 1 1 d . . .
C28 C 0.7082(2) 0.9348(2) 0.47061(19) 0.0265(6) Uani 1 1 d . . .
C29 C 0.5404(2) 0.7727(2) 0.40628(19) 0.0288(6) Uani 1 1 d . . .
H29 H 0.5097 0.6986 0.3977 0.035 Uiso 1 1 calc R . .
C30 C 0.3556(2) 0.7720(2) 0.3534(2) 0.0285(6) Uani 1 1 d . . .
H30A H 0.3228 0.8030 0.4117 0.034 Uiso 1 1 calc R . .
H30B H 0.3385 0.6884 0.3262 0.034 Uiso 1 1 calc R . .
C31 C 0.3097(2) 0.8027(2) 0.27708(19) 0.0253(6) Uani 1 1 d . . .
H31A H 0.3231 0.7530 0.2122 0.030 Uiso 1 1 calc R . .
H31B H 0.2295 0.7926 0.2713 0.030 Uiso 1 1 calc R . .
C32 C 0.3150(2) 0.9858(2) 0.28797(18) 0.0228(5) Uani 1 1 d . . .
H32 H 0.2401 0.9536 0.2543 0.027 Uiso 1 1 calc R . .
C33 C 0.3634(2) 1.1023(2) 0.31227(18) 0.0221(5) Uani 1 1 d . . .
C34 C 0.2955(2) 1.1609(2) 0.28649(19) 0.0258(6) Uani 1 1 d . . .
H34 H 0.2207 1.1227 0.2546 0.031 Uiso 1 1 calc R . .
C35 C 0.3347(2) 1.2710(2) 0.3063(2) 0.0292(6) Uani 1 1 d . . .
H35 H 0.2881 1.3087 0.2876 0.035 Uiso 1 1 calc R . .
C36 C 0.4452(2) 1.3283(2) 0.3548(2) 0.0273(6) Uani 1 1 d . . .
H36 H 0.4732 1.4049 0.3686 0.033 Uiso 1 1 calc R . .
C37 C 0.5126(2) 1.2743(2) 0.38231(19) 0.0235(5) Uani 1 1 d . . .
C38 C 0.4746(2) 1.1586(2) 0.36153(18) 0.0207(5) Uani 1 1 d . . .
C39 C 0.6641(2) 1.4419(2) 0.4659(2) 0.0354(7) Uani 1 1 d . . .
H39A H 0.6184 1.4848 0.5081 0.042 Uiso 1 1 calc R . .
H39B H 0.6643 1.4587 0.4098 0.042 Uiso 1 1 calc R . .
C40 C 0.7791(3) 1.4751(3) 0.5236(3) 0.0482(9) Uani 1 1 d . . .
H40A H 0.7778 1.4585 0.5791 0.072 Uiso 1 1 calc R . .
H40B H 0.8113 1.5565 0.5482 0.072 Uiso 1 1 calc R . .
H40C H 0.8235 1.4318 0.4810 0.072 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O18 1.7699(19) . ?
U1 O17 1.7718(18) . ?
U1 O19 2.3184(18) 2_565 ?
U1 O19 2.3429(17) . ?
U1 O11 2.5318(18) . ?
U1 O15 2.5382(18) . ?
U1 O14 2.5387(19) . ?
U1 O12 2.559(2) . ?
U1 N6 2.982(2) . ?
U1 N5 2.991(2) . ?
U1 U1 3.9119(2) 2_565 ?
Cu1 O2 1.9007(18) . ?
Cu1 N2 1.925(2) . ?
Cu1 O3 1.9323(17) . ?
Cu1 N1 1.949(2) . ?
Cu2 O8 1.8957(17) . ?
Cu2 O7 1.9015(18) . ?
Cu2 N4 1.934(2) . ?
Cu2 N3 1.937(2) . ?
O1 C3 1.370(3) . ?
O1 C2 1.444(3) . ?
O2 C8 1.319(3) . ?
O3 C18 1.327(3) . ?
O4 C17 1.366(3) . ?
O4 C19 1.440(3) . ?
O5 H5A 0.83(3) . ?
O5 H5B 0.83(3) . ?
O6 C23 1.370(4) . ?
O6 C22 1.436(3) . ?
O7 C28 1.319(3) . ?
O8 C38 1.307(3) . ?
O9 C37 1.377(3) . ?
O9 C39 1.431(3) . ?
O10 H10C 0.83(3) . ?
O10 H10D 0.83(3) . ?
O11 N5 1.265(3) . ?
O12 N5 1.280(3) . ?
O13 N5 1.217(3) . ?
O14 N6 1.274(3) . ?
O15 N6 1.274(3) . ?
O16 N6 1.211(3) . ?
O19 U1 2.3184(18) 2_565 ?
N1 C9 1.284(4) . ?
N1 C10 1.470(4) . ?
N2 C12 1.286(4) . ?
N2 C11 1.474(3) . ?
N3 C29 1.277(4) . ?
N3 C30 1.475(3) . ?
N4 C32 1.283(3) . ?
N4 C31 1.472(3) . ?
C1 C2 1.497(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.381(4) . ?
C3 C8 1.416(4) . ?
C4 C5 1.405(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.362(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.417(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.418(3) . ?
C7 C9 1.443(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.509(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.444(4) . ?
C12 H12 0.9500 . ?
C13 C18 1.413(4) . ?
C13 C14 1.413(4) . ?
C14 C15 1.364(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.371(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.427(4) . ?
C19 C20 1.493(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.489(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.384(4) . ?
C23 C28 1.426(4) . ?
C24 C25 1.406(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.361(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.417(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.416(4) . ?
C27 C29 1.438(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.512(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.442(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.413(4) . ?
C33 C38 1.418(4) . ?
C34 C35 1.362(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.410(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.370(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.427(4) . ?
C39 C40 1.500(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
O18 U1 O17 175.72(9) . . ?
O18 U1 O19 92.84(8) . 2_565 ?
O17 U1 O19 90.26(8) . 2_565 ?
O18 U1 O19 90.37(8) . . ?
O17 U1 O19 93.59(8) . . ?
O19 U1 O19 65.89(7) 2_565 . ?
O18 U1 O11 90.30(8) . . ?
O17 U1 O11 89.87(8) . . ?
O19 U1 O11 131.38(6) 2_565 . ?
O19 U1 O11 65.59(6) . . ?
O18 U1 O15 88.83(8) . . ?
O17 U1 O15 89.63(8) . . ?
O19 U1 O15 67.46(6) 2_565 . ?
O19 U1 O15 133.24(6) . . ?
O11 U1 O15 161.15(6) . . ?
O18 U1 O14 87.90(8) . . ?
O17 U1 O14 88.05(8) . . ?
O19 U1 O14 117.54(6) 2_565 . ?
O19 U1 O14 176.22(6) . . ?
O11 U1 O14 111.05(6) . . ?
O15 U1 O14 50.10(6) . . ?
O18 U1 O12 87.30(9) . . ?
O17 U1 O12 89.54(8) . . ?
O19 U1 O12 178.75(6) 2_565 . ?
O19 U1 O12 115.35(6) . . ?
O11 U1 O12 49.85(6) . . ?
O15 U1 O12 111.30(6) . . ?
O14 U1 O12 61.22(6) . . ?
O18 U1 N6 87.27(8) . . ?
O17 U1 N6 89.64(8) . . ?
O19 U1 N6 92.53(6) 2_565 . ?
O19 U1 N6 158.16(6) . . ?
O11 U1 N6 136.09(6) . . ?
O15 U1 N6 25.07(6) . . ?
O14 U1 N6 25.07(6) . . ?
O12 U1 N6 86.24(6) . . ?
O18 U1 N5 87.62(8) . . ?
O17 U1 N5 90.74(8) . . ?
O19 U1 N5 156.09(6) 2_565 . ?
O19 U1 N5 90.21(6) . . ?
O11 U1 N5 24.74(6) . . ?
O15 U1 N5 136.43(6) . . ?
O14 U1 N5 86.37(6) . . ?
O12 U1 N5 25.15(6) . . ?
N6 U1 N5 111.36(6) . . ?
O18 U1 U1 91.91(7) . 2_565 ?
O17 U1 U1 92.30(6) . 2_565 ?
O19 U1 U1 33.14(4) 2_565 2_565 ?
O19 U1 U1 32.75(4) . 2_565 ?
O11 U1 U1 98.29(4) . 2_565 ?
O15 U1 U1 100.55(4) . 2_565 ?
O14 U1 U1 150.66(4) . 2_565 ?
O12 U1 U1 148.10(4) . 2_565 ?
N6 U1 U1 125.60(4) . 2_565 ?
N5 U1 U1 122.95(4) . 2_565 ?
O2 Cu1 N2 177.33(9) . . ?
O2 Cu1 O3 89.56(7) . . ?
N2 Cu1 O3 92.34(9) . . ?
O2 Cu1 N1 93.21(9) . . ?
N2 Cu1 N1 84.77(10) . . ?
O3 Cu1 N1 175.21(9) . . ?
O8 Cu2 O7 88.82(8) . . ?
O8 Cu2 N4 93.63(8) . . ?
O7 Cu2 N4 176.64(8) . . ?
O8 Cu2 N3 174.54(9) . . ?
O7 Cu2 N3 92.86(9) . . ?
N4 Cu2 N3 84.92(9) . . ?
C3 O1 C2 117.2(2) . . ?
C8 O2 Cu1 126.83(16) . . ?
C18 O3 Cu1 126.74(16) . . ?
C17 O4 C19 118.6(2) . . ?
H5A O5 H5B 110(2) . . ?
C23 O6 C22 117.6(2) . . ?
C28 O7 Cu2 126.64(17) . . ?
C38 O8 Cu2 126.81(16) . . ?
C37 O9 C39 117.7(2) . . ?
H10C O10 H10D 106(2) . . ?
N5 O11 U1 98.39(14) . . ?
N5 O12 U1 96.65(15) . . ?
N6 O14 U1 97.33(14) . . ?
N6 O15 U1 97.35(14) . . ?
U1 O19 U1 114.11(7) 2_565 . ?
C9 N1 C10 120.8(2) . . ?
C9 N1 Cu1 126.17(19) . . ?
C10 N1 Cu1 112.96(18) . . ?
C12 N2 C11 120.5(2) . . ?
C12 N2 Cu1 126.54(19) . . ?
C11 N2 Cu1 112.94(18) . . ?
C29 N3 C30 120.9(2) . . ?
C29 N3 Cu2 127.3(2) . . ?
C30 N3 Cu2 111.66(17) . . ?
C32 N4 C31 121.1(2) . . ?
C32 N4 Cu2 126.49(18) . . ?
C31 N4 Cu2 112.40(17) . . ?
O13 N5 O11 123.0(2) . . ?
O13 N5 O12 122.1(2) . . ?
O11 N5 O12 114.9(2) . . ?
O13 N5 U1 176.3(2) . . ?
O11 N5 U1 56.87(12) . . ?
O12 N5 U1 58.20(13) . . ?
O16 N6 O14 122.3(2) . . ?
O16 N6 O15 122.6(2) . . ?
O14 N6 O15 115.1(2) . . ?
O16 N6 U1 177.2(2) . . ?
O14 N6 U1 57.61(12) . . ?
O15 N6 U1 57.58(11) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 107.6(2) . . ?
O1 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O1 C3 C4 124.9(2) . . ?
O1 C3 C8 113.3(2) . . ?
C4 C3 C8 121.8(2) . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.5(2) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C8 119.4(2) . . ?
C6 C7 C9 118.2(2) . . ?
C8 C7 C9 122.4(2) . . ?
O2 C8 C3 117.3(2) . . ?
O2 C8 C7 125.1(2) . . ?
C3 C8 C7 117.6(2) . . ?
N1 C9 C7 125.3(2) . . ?
N1 C9 H9 117.4 . . ?
C7 C9 H9 117.4 . . ?
N1 C10 C11 108.6(2) . . ?
N1 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
N1 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C10 109.0(2) . . ?
N2 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N2 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N2 C12 C13 125.6(3) . . ?
N2 C12 H12 117.2 . . ?
C13 C12 H12 117.2 . . ?
C18 C13 C14 119.6(3) . . ?
C18 C13 C12 122.1(2) . . ?
C14 C13 C12 118.0(3) . . ?
C15 C14 C13 121.0(3) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 120.1(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
O4 C17 C16 125.3(2) . . ?
O4 C17 C18 113.5(2) . . ?
C16 C17 C18 121.1(3) . . ?
O3 C18 C13 124.3(2) . . ?
O3 C18 C17 118.1(2) . . ?
C13 C18 C17 117.6(2) . . ?
O4 C19 C20 107.5(2) . . ?
O4 C19 H19A 110.2 . . ?
C20 C19 H19A 110.2 . . ?
O4 C19 H19B 110.2 . . ?
C20 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O6 C22 C21 108.0(2) . . ?
O6 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
O6 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
O6 C23 C24 125.7(3) . . ?
O6 C23 C28 113.4(2) . . ?
C24 C23 C28 121.0(3) . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C27 121.3(3) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C28 C27 C26 119.4(3) . . ?
C28 C27 C29 121.8(2) . . ?
C26 C27 C29 118.4(3) . . ?
O7 C28 C27 125.4(3) . . ?
O7 C28 C23 116.6(2) . . ?
C27 C28 C23 118.0(2) . . ?
N3 C29 C27 124.9(3) . . ?
N3 C29 H29 117.5 . . ?
C27 C29 H29 117.5 . . ?
N3 C30 C31 107.5(2) . . ?
N3 C30 H30A 110.2 . . ?
C31 C30 H30A 110.2 . . ?
N3 C30 H30B 110.2 . . ?
C31 C30 H30B 110.2 . . ?
H30A C30 H30B 108.5 . . ?
N4 C31 C30 108.0(2) . . ?
N4 C31 H31A 110.1 . . ?
C30 C31 H31A 110.1 . . ?
N4 C31 H31B 110.1 . . ?
C30 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
N4 C32 C33 125.1(2) . . ?
N4 C32 H32 117.4 . . ?
C33 C32 H32 117.4 . . ?
C34 C33 C38 120.0(2) . . ?
C34 C33 C32 117.7(2) . . ?
C38 C33 C32 122.3(2) . . ?
C35 C34 C33 121.5(3) . . ?
C35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C34 C35 C36 119.3(2) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C37 C36 C35 120.5(2) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C36 C37 O9 125.3(2) . . ?
C36 C37 C38 121.6(2) . . ?
O9 C37 C38 113.0(2) . . ?
O8 C38 C33 125.4(2) . . ?
O8 C38 C37 117.6(2) . . ?
C33 C38 C37 117.0(2) . . ?
O9 C39 C40 107.3(3) . . ?
O9 C39 H39A 110.2 . . ?
C40 C39 H39A 110.2 . . ?
O9 C39 H39B 110.2 . . ?
C40 C39 H39B 110.2 . . ?
H39A C39 H39B 108.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10C O8 0.83(3) 2.06(2) 2.794(3) 146(3) .
O10 H10C O9 0.83(3) 2.22(2) 2.914(3) 140(3) .
O5 H5A O1 0.83(3) 2.150(18) 2.848(3) 142(3) .
O5 H5A O2 0.83(3) 2.02(2) 2.666(2) 135(3) .
O5 H5B O3 0.83(3) 1.769(16) 2.549(3) 156(3) .
O5 H5B O4 0.83(3) 2.22(2) 2.757(3) 123(2) .
O10 H10D O6 0.83(3) 2.225(18) 2.973(3) 150(3) .
O10 H10D O7 0.83(3) 2.14(2) 2.813(3) 138(3) .
O10 H10C O8 0.83(3) 2.06(2) 2.794(3) 146(3) .
O10 H10C O9 0.83(3) 2.22(2) 2.914(3) 140(3) .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.075


