Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Vitaly Pavlishchuk'
_publ_contact_author_email       SHCHUK@INPHYSCHEM-NAS.KIEV.UA
loop_
_publ_author_name
V.Pavlishchuk
A.Addison
V.Golub
S.V.Kolotilov
D.Schollmeyer
;
L.K.Thompson
;

# Attachment 'Cu2-revised.cif'

data_publication_text
_database_code_depnum_ccdc_archive 'CCDC 662399'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H14 Cu2 N9 O10.25'
_chemical_formula_weight         611.86

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           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   26.551(5)
_cell_length_b                   26.551(5)
_cell_length_c                   19.976(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_volume                     12196(4)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5530
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       \q/2\w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47903
_diffrn_reflns_av_R_equivalents  0.1518
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         28.34
_reflns_number_total             6759
_reflns_number_gt                3519
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Enraf Nonius Software V5'
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dr\"ager, 1971)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6759
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1628
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.2488
_refine_ls_wR_factor_gt          0.2023
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.003

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
C1 C 0.2271(4) -0.1179(3) 0.5725(4) 0.0566(19) Uani 1 1 d . . .
C2 C 0.2798(3) -0.1183(4) 0.5752(3) 0.061(2) Uani 1 1 d . . .
C3 C 0.2832(3) -0.1702(4) 0.5656(4) 0.056(2) Uani 1 1 d . . .
C4 C 0.3419(4) -0.2150(4) 0.5641(5) 0.075(3) Uani 1 1 d . . .
H32A H 0.3490 -0.2182 0.5171 0.090 Uiso 1 1 calc R . .
H32B H 0.3063 -0.2499 0.5770 0.090 Uiso 1 1 calc R . .
C5 C 0.3903(4) -0.2097(4) 0.6039(5) 0.077(3) Uani 1 1 d . . .
H29A H 0.3883 -0.2472 0.6041 0.093 Uiso 1 1 calc R . .
H29B H 0.3848 -0.2012 0.6497 0.093 Uiso 1 1 calc R . .
C6 C 0.4519(3) -0.1635(3) 0.5819(4) 0.059(2) Uani 1 1 d . . .
H26A H 0.4804 -0.1658 0.6102 0.071 Uiso 1 1 calc R . .
H26B H 0.4585 -0.1711 0.5361 0.071 Uiso 1 1 calc R . .
C7 C 0.5131(3) -0.0612(3) 0.5830(3) 0.0373(14) Uani 1 1 d . . .
C8 C 0.5182(3) -0.0029(3) 0.5872(3) 0.0357(14) Uani 1 1 d . . .
C9 C 0.5746(3) 0.0483(3) 0.5848(4) 0.0532(18) Uani 1 1 d . . .
C10 C 0.3671(4) 0.1171(3) 0.5442(3) 0.0524(19) Uani 1 1 d . . .
H17A H 0.3342 0.0833 0.5244 0.063 Uiso 1 1 calc R . .
H17B H 0.3758 0.1509 0.5172 0.063 Uiso 1 1 calc R . .
C11 C 0.3527(3) 0.1257(3) 0.6150(3) 0.0512(18) Uani 1 1 d . . .
H15A H 0.3834 0.1622 0.6328 0.061 Uiso 1 1 calc R . .
H15B H 0.3166 0.1264 0.6158 0.061 Uiso 1 1 calc R . .
C12 C 0.3511(3) 0.0852(3) 0.7295(3) 0.0481(17) Uani 1 1 d . . .
H19A H 0.3824 0.1238 0.7408 0.058 Uiso 1 1 calc R . .
H19B H 0.3150 0.0807 0.7470 0.058 Uiso 1 1 calc R . .
C13 C 0.3627(3) 0.0400(3) 0.7585(3) 0.0494(17) Uani 1 1 d . . .
H27A H 0.3291 0.0017 0.7519 0.059 Uiso 1 1 calc R . .
H27B H 0.3698 0.0464 0.8062 0.059 Uiso 1 1 calc R . .
N1 N 0.3316(3) -0.0711(3) 0.5865(3) 0.0619(18) Uani 1 1 d . . .
N2 N 0.3353(2) -0.1649(3) 0.5743(3) 0.0654(19) Uani 1 1 d . . .
N3 N 0.4595(2) -0.1047(2) 0.5862(3) 0.0457(13) Uani 1 1 d . . .
N4 N 0.4706(2) -0.0011(2) 0.5935(3) 0.0425(13) Uani 1 1 d . . .
N5 N 0.1837(4) -0.1188(3) 0.5686(4) 0.076(2) Uani 1 1 d . . .
N6 N 0.6191(4) 0.0876(3) 0.5831(5) 0.090(3) Uani 1 1 d . . .
N7 N 0.4187(2) 0.1087(2) 0.5467(3) 0.0424(13) Uani 1 1 d . . .
N8 N 0.3472(2) 0.0767(2) 0.6555(3) 0.0413(12) Uani 1 1 d . . .
N9 N 0.4146(3) 0.0436(3) 0.7247(3) 0.0480(14) Uani 1 1 d . . .
O1 O 0.3309(3) -0.0250(2) 0.5936(2) 0.0662(16) Uani 1 1 d . . .
O2 O 0.2372(2) -0.2157(3) 0.5493(3) 0.0677(16) Uani 1 1 d . . .
O3 O 0.55953(17) -0.06301(18) 0.5769(2) 0.0392(10) Uani 1 1 d . . .
O4 O 0.4750(2) 0.0504(2) 0.5974(3) 0.0568(13) Uani 1 1 d . . .
O5 O 0.39652(18) -0.07461(19) 0.7099(2) 0.0409(10) Uani 1 1 d . . .
O6 O 0.2212(8) 0.0163(7) 0.5881(10) 0.125(6) Uani 0.50 1 d P . .
O7 O 0.2081(8) 0.0587(8) 0.6910(13) 0.157(9) Uani 0.50 1 d P . .
O8 O 0.2357(3) -0.2780(4) 0.4409(4) 0.137(4) Uani 1 1 d . . .
O9 O 0.1802(11) -0.3908(12) 0.3632(19) 0.211(13) Uani 0.50 1 d P . .
O10 O 0.308(3) -0.344(6) 0.4370(19) 0.36(3) Uiso 0.50 1 d P . .
O11 O 0.208(3) 0.069(3) 0.520(3) 0.42(3) Uiso 0.50 1 d P . .
O12 O 0.207(3) -0.488(4) 0.344(4) 0.52(5) Uiso 0.50 1 d P . .
O13 O 0.184(2) -0.365(2) 0.306(3) 0.32(2) Uiso 0.50 1 d P . .
O14 O 0.1790(15) 0.0231(15) 0.4523(19) 0.245(13) Uiso 0.50 1 d P . .
O15 O 0.195(4) -0.407(4) 0.298(5) 0.30(4) Uiso 0.25 1 d P . .
Cu1 Cu 0.39875(3) -0.08442(4) 0.59433(4) 0.0440(3) Uani 1 1 d . . .
Cu2 Cu 0.40980(3) 0.05959(3) 0.62698(4) 0.0388(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.057(5) 0.051(5) 0.048(4) -0.010(3) -0.010(4) 0.016(4)
C2 0.024(3) 0.079(6) 0.033(4) 0.006(3) -0.007(3) -0.009(4)
C3 0.048(5) 0.069(5) 0.037(4) -0.002(3) 0.008(3) 0.018(4)
C4 0.048(5) 0.069(6) 0.098(7) -0.021(5) -0.001(5) 0.022(4)
C5 0.062(6) 0.063(6) 0.094(7) -0.004(5) -0.006(5) 0.022(5)
C6 0.037(4) 0.040(4) 0.093(6) -0.015(4) -0.001(4) 0.014(3)
C7 0.041(4) 0.050(4) 0.031(3) -0.002(3) 0.000(3) 0.030(3)
C8 0.043(4) 0.046(4) 0.029(3) 0.009(3) 0.009(2) 0.030(3)
C9 0.058(5) 0.040(4) 0.066(5) 0.009(3) 0.022(4) 0.027(4)
C10 0.087(6) 0.057(4) 0.036(4) 0.003(3) 0.004(3) 0.054(4)
C11 0.075(5) 0.064(5) 0.044(4) 0.002(3) 0.004(3) 0.057(4)
C12 0.067(5) 0.051(4) 0.037(4) 0.000(3) 0.010(3) 0.037(4)
C13 0.070(5) 0.055(4) 0.038(4) 0.007(3) 0.013(3) 0.042(4)
N1 0.081(5) 0.084(5) 0.042(4) 0.008(3) 0.015(3) 0.057(4)
N2 0.029(3) 0.096(5) 0.053(4) 0.007(3) 0.004(3) 0.017(3)
N3 0.030(3) 0.047(3) 0.060(4) -0.001(3) 0.002(2) 0.019(3)
N4 0.054(3) 0.051(3) 0.035(3) 0.011(2) 0.013(2) 0.036(3)
N5 0.078(5) 0.065(5) 0.086(6) -0.006(4) -0.003(4) 0.037(4)
N6 0.072(5) 0.059(5) 0.136(8) 0.015(5) 0.042(5) 0.030(4)
N7 0.063(4) 0.043(3) 0.037(3) 0.008(2) 0.010(3) 0.037(3)
N8 0.054(3) 0.043(3) 0.036(3) -0.002(2) 0.005(2) 0.031(3)
N9 0.061(4) 0.058(4) 0.035(3) 0.012(3) 0.005(3) 0.037(3)
O1 0.118(5) 0.060(3) 0.041(3) -0.003(2) 0.005(3) 0.060(4)
O2 0.031(3) 0.093(4) 0.061(3) -0.023(3) 0.004(2) 0.017(3)
O3 0.035(2) 0.045(3) 0.045(3) 0.0019(19) 0.0045(19) 0.025(2)
O4 0.062(3) 0.058(3) 0.070(3) 0.027(3) 0.029(3) 0.046(3)
O5 0.043(2) 0.046(3) 0.036(2) 0.0078(19) 0.0067(19) 0.025(2)
O6 0.116(13) 0.096(12) 0.177(17) -0.007(11) 0.009(12) 0.065(11)
O7 0.087(12) 0.086(12) 0.28(3) -0.022(14) -0.050(14) 0.032(10)
O8 0.090(6) 0.135(7) 0.126(7) -0.062(6) 0.012(5) 0.011(5)
O9 0.128(19) 0.14(2) 0.29(4) 0.04(2) 0.02(2) 0.013(15)
Cu1 0.0349(4) 0.0631(6) 0.0400(5) 0.0062(4) 0.0038(3) 0.0289(4)
Cu2 0.0508(5) 0.0408(5) 0.0371(4) 0.0079(3) 0.0105(3) 0.0322(4)

_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
C1 N5 1.144(10) . ?
C1 C2 1.405(12) . ?
C2 N1 1.337(9) . ?
C2 C3 1.438(12) . ?
C3 O2 1.257(9) . ?
C3 N2 1.330(10) . ?
C4 N2 1.439(11) . ?
C4 C5 1.459(12) . ?
C5 C6 1.539(11) . ?
C6 N3 1.474(9) . ?
C7 O3 1.263(7) . ?
C7 N3 1.311(8) . ?
C7 C8 1.488(8) . ?
C8 N4 1.295(8) . ?
C8 C9 1.434(10) . ?
C9 N6 1.119(10) . ?
C10 N7 1.495(9) . ?
C10 C11 1.511(9) . ?
C11 N8 1.475(8) . ?
C12 C13 1.494(9) . ?
C12 N8 1.492(8) . ?
C13 N9 1.494(9) . ?
N1 O1 1.239(8) . ?
N1 Cu1 1.991(6) . ?
N2 Cu1 1.990(7) . ?
N3 Cu1 1.946(5) . ?
N4 O4 1.316(7) . ?
N4 Cu1 2.076(6) . ?
N7 Cu2 2.006(5) . ?
N8 Cu2 2.012(5) . ?
N9 Cu2 2.016(5) . ?
O1 Cu2 2.274(6) . ?
O4 Cu2 1.956(4) . ?
O5 Cu1 2.327(4) . ?
O10 O10 1.02(11) 3_655 ?
O10 O10 1.02(11) 2_545 ?
O10 O12 3.87(13) . ?

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
N5 C1 C2 177.8(9) . . ?
N1 C2 C1 124.1(9) . . ?
N1 C2 C3 113.2(7) . . ?
C1 C2 C3 122.7(7) . . ?
O2 C3 N2 126.5(8) . . ?
O2 C3 C2 117.3(7) . . ?
N2 C3 C2 116.2(7) . . ?
N2 C4 C5 110.0(7) . . ?
C4 C5 C6 117.1(8) . . ?
N3 C6 C5 110.8(6) . . ?
O3 C7 N3 128.4(6) . . ?
O3 C7 C8 117.5(6) . . ?
N3 C7 C8 114.0(5) . . ?
N4 C8 C9 123.0(6) . . ?
N4 C8 C7 117.4(6) . . ?
C9 C8 C7 119.6(5) . . ?
N6 C9 C8 178.5(8) . . ?
N7 C10 C11 108.1(5) . . ?
N8 C11 C10 107.6(5) . . ?
C13 C12 N8 106.8(5) . . ?
C12 C13 N9 109.1(5) . . ?
O1 N1 C2 115.4(7) . . ?
O1 N1 Cu1 128.5(6) . . ?
C2 N1 Cu1 116.0(6) . . ?
C3 N2 C4 118.9(7) . . ?
C3 N2 Cu1 114.6(6) . . ?
C4 N2 Cu1 126.3(5) . . ?
C7 N3 C6 116.3(5) . . ?
C7 N3 Cu1 116.5(4) . . ?
C6 N3 Cu1 127.2(4) . . ?
C8 N4 O4 117.5(6) . . ?
C8 N4 Cu1 110.9(4) . . ?
O4 N4 Cu1 131.6(4) . . ?
C10 N7 Cu2 107.8(4) . . ?
C11 N8 C12 116.2(5) . . ?
C11 N8 Cu2 108.3(4) . . ?
C12 N8 Cu2 108.2(4) . . ?
C13 N9 Cu2 107.3(4) . . ?
N1 O1 Cu2 123.2(5) . . ?
N4 O4 Cu2 121.5(4) . . ?
O10 O10 O10 60.00(4) 3_655 2_545 ?
O10 O10 O12 145(8) 3_655 . ?
O10 O10 O12 97(10) 2_545 . ?
N3 Cu1 N2 93.5(3) . . ?
N3 Cu1 N1 169.5(3) . . ?
N2 Cu1 N1 79.8(3) . . ?
N3 Cu1 N4 81.2(2) . . ?
N2 Cu1 N4 167.2(2) . . ?
N1 Cu1 N4 103.7(3) . . ?
N3 Cu1 O5 100.6(2) . . ?
N2 Cu1 O5 105.3(2) . . ?
N1 Cu1 O5 89.0(2) . . ?
N4 Cu1 O5 87.14(18) . . ?
O4 Cu2 N7 90.9(2) . . ?
O4 Cu2 N8 174.8(2) . . ?
N7 Cu2 N8 85.5(2) . . ?
O4 Cu2 N9 96.5(2) . . ?
N7 Cu2 N9 155.9(2) . . ?
N8 Cu2 N9 85.4(2) . . ?
O4 Cu2 O1 102.9(2) . . ?
N7 Cu2 O1 99.1(2) . . ?
N8 Cu2 O1 81.3(2) . . ?
N9 Cu2 O1 101.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.191

# Attachment 'Cu3Ba.cif'

data_cu3ba
_database_code_depnum_ccdc_archive 'CCDC 662400'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H26 Ba Cu3 N12 O16'
_chemical_formula_weight         994.47

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'
Ba Ba -0.3244 2.2819 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   ' C 2/c '

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

_cell_length_a                   18.2664(10)
_cell_length_b                   19.1141(11)
_cell_length_c                   11.0179(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.647(3)
_cell_angle_gamma                90.00
_cell_volume                     3343.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    3.131
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_T_max  0.7659
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12202
_diffrn_reflns_av_R_equivalents  0.1724
_diffrn_reflns_av_sigmaI/netI    0.1923
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         28.36
_reflns_number_total             4163
_reflns_number_gt                2118
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4163
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0876
_refine_ls_wR_factor_ref         0.2459
_refine_ls_wR_factor_gt          0.2043
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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
Cu2 Cu 0.5000 -0.07866(9) 0.2500 0.0260(5) Uani 1 2 d S . .
Cu1 Cu 0.39878(8) 0.06521(7) -0.00732(12) 0.0261(4) Uani 1 1 d . . .
O1 O 0.3972(4) -0.0881(4) 0.0733(7) 0.0291(17) Uani 1 1 d . . .
N2 N 0.3570(5) -0.0314(4) 0.0061(8) 0.0267(19) Uani 1 1 d . . .
C3 C 0.2769(7) -0.0358(6) -0.0789(10) 0.027(2) Uani 1 1 d . . .
C4 C 0.2335(7) -0.1008(7) -0.0898(11) 0.036(3) Uani 1 1 d . . .
N5 N 0.2017(7) -0.1531(6) -0.0981(12) 0.062(3) Uani 1 1 d . . .
C6 C 0.2314(7) 0.0276(6) -0.1606(10) 0.028(2) Uani 1 1 d . . .
O7 O 0.1509(5) 0.0238(4) -0.2388(7) 0.0366(19) Uani 1 1 d . . .
N8 N 0.2795(6) 0.0810(5) -0.1397(9) 0.031(2) Uani 1 1 d . . .
C9 C 0.2420(7) 0.1467(6) -0.2059(13) 0.044(3) Uani 1 1 d . . .
H9A H 0.2152 0.1685 -0.1562 0.053 Uiso 1 1 calc R . .
H9B H 0.1974 0.1377 -0.3033 0.053 Uiso 1 1 calc R . .
C10 C 0.3050(9) 0.1967(7) -0.2067(15) 0.058(4) Uani 1 1 d . . .
H10A H 0.2740 0.2383 -0.2618 0.069 Uiso 1 1 calc R . .
H10B H 0.3312 0.1740 -0.2567 0.069 Uiso 1 1 calc R . .
C11 C 0.3766(8) 0.2224(7) -0.0634(14) 0.052(4) Uani 1 1 d . . .
H11A H 0.4099 0.2591 -0.0772 0.063 Uiso 1 1 calc R . .
H11B H 0.3524 0.2424 -0.0080 0.063 Uiso 1 1 calc R . .
N12 N 0.4314(6) 0.1617(5) 0.0115(10) 0.038(2) Uani 1 1 d . . .
C13 C 0.5124(8) 0.1764(6) 0.1031(12) 0.034(3) Uani 1 1 d . . .
O14 O 0.5501(5) 0.2322(4) 0.1393(8) 0.043(2) Uani 1 1 d . . .
C15 C 0.5614(7) 0.1100(6) 0.1666(11) 0.029(2) Uani 1 1 d . . .
C16 C 0.6509(8) 0.1130(6) 0.2652(11) 0.036(3) Uani 1 1 d . . .
N17 N 0.7210(6) 0.1179(6) 0.3447(10) 0.047(3) Uani 1 1 d . . .
N18 N 0.5184(6) 0.0512(5) 0.1316(8) 0.028(2) Uani 1 1 d . . .
O19 O 0.5621(4) -0.0080(4) 0.1839(7) 0.0285(16) Uani 1 1 d . . .
O20 O 0.5000 -0.1810(6) 0.2500 0.060(4) Uani 1 2 d S . .
Ba1 Ba 0.0000 0.02165(5) -0.2500 0.0409(4) Uani 1 2 d S . .
O1W O 0.1157(8) 0.0526(6) 0.0223(10) 0.093(4) Uani 1 1 d . . .
H1W1 H 0.1262 0.0296 0.0952 0.139 Uiso 1 1 d R . .
H1W2 H 0.1321 0.0363 -0.0289 0.139 Uiso 1 1 d R . .
O2W O 0.0000 0.1599(6) -0.2500 0.055(4) Uani 1 2 d S . .
H2W H 0.0155 0.1929 -0.2841 0.083 Uiso 1 1 d R . .
O3W O -0.0079(7) -0.0921(6) -0.4122(17) 0.131(6) Uani 1 1 d . . .
H3W1 H -0.0354 -0.0541 -0.4372 0.196 Uiso 1 1 d R . .
H3W2 H 0.0372 -0.0977 -0.4102 0.196 Uiso 1 1 d R . .
O4W O -0.0823(6) -0.2233(5) -0.4419(8) 0.054(2) Uani 1 1 d . . .
H4W1 H -0.0736 -0.1811 -0.4312 0.081 Uiso 1 1 d R . .
H5W2 H -0.0723 -0.2377 -0.5053 0.081 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu2 0.0221(9) 0.0188(10) 0.0243(9) 0.000 0.0017(7) 0.000
Cu1 0.0271(7) 0.0195(7) 0.0275(6) 0.0001(5) 0.0103(6) -0.0042(5)
O1 0.030(4) 0.013(4) 0.029(4) 0.001(3) 0.003(3) -0.004(3)
N2 0.027(5) 0.015(5) 0.030(4) -0.004(4) 0.009(4) 0.000(4)
C3 0.029(6) 0.025(6) 0.024(5) -0.008(4) 0.010(4) -0.008(5)
C4 0.031(6) 0.038(7) 0.038(6) -0.002(5) 0.016(5) -0.009(6)
N5 0.053(8) 0.045(7) 0.075(8) -0.007(6) 0.023(6) -0.023(6)
C6 0.029(6) 0.038(7) 0.017(4) 0.001(4) 0.010(4) 0.010(5)
O7 0.029(4) 0.041(5) 0.039(4) 0.002(4) 0.016(3) 0.001(4)
N8 0.036(5) 0.016(5) 0.036(5) 0.008(4) 0.014(4) 0.000(4)
C9 0.033(7) 0.035(7) 0.054(7) 0.011(6) 0.013(6) 0.018(6)
C10 0.064(10) 0.030(8) 0.078(10) 0.018(7) 0.033(8) 0.011(7)
C11 0.047(8) 0.043(8) 0.063(9) 0.014(7) 0.025(7) 0.004(7)
N12 0.053(6) 0.018(5) 0.048(6) -0.004(4) 0.029(5) -0.012(5)
C13 0.048(7) 0.024(6) 0.043(6) -0.020(5) 0.033(6) -0.014(6)
O14 0.056(6) 0.027(5) 0.062(6) -0.023(4) 0.041(5) -0.026(4)
C15 0.035(6) 0.027(6) 0.033(5) -0.008(5) 0.023(5) -0.006(5)
C16 0.047(8) 0.030(7) 0.029(6) -0.010(5) 0.017(5) -0.015(6)
N17 0.039(6) 0.058(8) 0.039(5) 0.000(5) 0.015(5) -0.020(5)
N18 0.029(5) 0.026(5) 0.032(5) -0.002(4) 0.018(4) -0.004(4)
O19 0.024(4) 0.029(4) 0.035(4) 0.001(3) 0.016(3) -0.002(3)
O20 0.080(10) 0.018(6) 0.033(6) 0.000 -0.010(6) 0.000
Ba1 0.0115(4) 0.0242(6) 0.0677(7) 0.000 0.0049(4) 0.000
O1W 0.127(11) 0.102(10) 0.038(5) -0.017(6) 0.033(6) -0.047(8)
O2W 0.095(11) 0.026(7) 0.064(8) 0.000 0.054(8) 0.000
O3W 0.073(9) 0.045(8) 0.237(16) -0.073(9) 0.048(10) -0.007(7)
O4W 0.070(6) 0.041(6) 0.044(5) 0.006(4) 0.023(5) 0.028(5)

_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
Cu2 O1 1.932(6) . ?
Cu2 O1 1.932(6) 2_655 ?
Cu2 O20 1.956(11) . ?
Cu2 O19 2.112(7) . ?
Cu2 O19 2.112(7) 2_655 ?
Cu1 N12 1.917(9) . ?
Cu1 N8 1.954(9) . ?
Cu1 N18 1.969(9) . ?
Cu1 N2 2.031(9) . ?
O1 N2 1.314(10) . ?
N2 C3 1.292(13) . ?
C3 C4 1.446(15) . ?
C3 C6 1.492(15) . ?
C4 N5 1.136(14) . ?
C6 O7 1.288(12) . ?
C6 N8 1.291(13) . ?
O7 Ba1 2.697(7) . ?
N8 C9 1.445(13) . ?
C9 C10 1.498(18) . ?
C10 C11 1.549(18) . ?
C11 N12 1.488(16) . ?
N12 C13 1.345(14) . ?
C13 O14 1.225(12) . ?
C13 C15 1.511(16) . ?
C15 N18 1.315(13) . ?
C15 C16 1.449(15) . ?
C16 N17 1.143(14) . ?
N18 O19 1.339(11) . ?
Ba1 O2W 2.643(12) . ?
Ba1 O7 2.697(7) 2_554 ?
Ba1 O1W 2.747(9) . ?
Ba1 O1W 2.747(9) 2_554 ?
Ba1 O3W 2.772(11) . ?
Ba1 O3W 2.772(11) 2_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu2 O1 169.3(4) . 2_655 ?
O1 Cu2 O20 84.6(2) . . ?
O1 Cu2 O20 84.6(2) 2_655 . ?
O1 Cu2 O19 97.6(3) . . ?
O1 Cu2 O19 89.3(3) 2_655 . ?
O20 Cu2 O19 129.8(2) . . ?
O1 Cu2 O19 89.3(3) . 2_655 ?
O1 Cu2 O19 97.6(3) 2_655 2_655 ?
O20 Cu2 O19 129.8(2) . 2_655 ?
O19 Cu2 O19 100.5(4) . 2_655 ?
N12 Cu1 N8 96.0(4) . . ?
N12 Cu1 N18 83.2(4) . . ?
N8 Cu1 N18 177.8(4) . . ?
N12 Cu1 N2 167.0(4) . . ?
N8 Cu1 N2 82.8(3) . . ?
N18 Cu1 N2 97.6(4) . . ?
N2 O1 Cu2 119.0(6) . . ?
C3 N2 O1 118.2(9) . . ?
C3 N2 Cu1 109.8(7) . . ?
O1 N2 Cu1 131.7(6) . . ?
N2 C3 C4 119.6(10) . . ?
N2 C3 C6 118.5(9) . . ?
C4 C3 C6 121.9(10) . . ?
N5 C4 C3 177.6(14) . . ?
O7 C6 N8 128.0(10) . . ?
O7 C6 C3 117.9(10) . . ?
N8 C6 C3 114.0(9) . . ?
C6 O7 Ba1 146.6(6) . . ?
C6 N8 C9 119.1(9) . . ?
C6 N8 Cu1 114.9(7) . . ?
C9 N8 Cu1 125.9(7) . . ?
N8 C9 C10 112.5(10) . . ?
C9 C10 C11 117.4(11) . . ?
N12 C11 C10 108.4(11) . . ?
C13 N12 C11 116.2(10) . . ?
C13 N12 Cu1 116.7(8) . . ?
C11 N12 Cu1 127.0(8) . . ?
O14 C13 N12 131.3(12) . . ?
O14 C13 C15 118.1(11) . . ?
N12 C13 C15 110.6(9) . . ?
N18 C15 C16 122.9(11) . . ?
N18 C15 C13 116.8(10) . . ?
C16 C15 C13 120.3(10) . . ?
N17 C16 C15 177.3(14) . . ?
C15 N18 O19 116.9(9) . . ?
C15 N18 Cu1 112.6(8) . . ?
O19 N18 Cu1 130.2(7) . . ?
N18 O19 Cu2 112.3(5) . . ?
O2W Ba1 O7 89.13(17) . 2_554 ?
O2W Ba1 O7 89.13(17) . . ?
O7 Ba1 O7 178.3(3) 2_554 . ?
O2W Ba1 O1W 77.6(3) . . ?
O7 Ba1 O1W 105.3(3) 2_554 . ?
O7 Ba1 O1W 74.3(3) . . ?
O2W Ba1 O1W 77.6(3) . 2_554 ?
O7 Ba1 O1W 74.3(3) 2_554 2_554 ?
O7 Ba1 O1W 105.3(3) . 2_554 ?
O1W Ba1 O1W 155.2(5) . 2_554 ?
O2W Ba1 O3W 141.6(4) . . ?
O7 Ba1 O3W 104.9(3) 2_554 . ?
O7 Ba1 O3W 76.5(3) . . ?
O1W Ba1 O3W 129.7(4) . . ?
O1W Ba1 O3W 72.4(4) 2_554 . ?
O2W Ba1 O3W 141.6(4) . 2_554 ?
O7 Ba1 O3W 76.5(3) 2_554 2_554 ?
O7 Ba1 O3W 104.9(3) . 2_554 ?
O1W Ba1 O3W 72.4(4) . 2_554 ?
O1W Ba1 O3W 129.7(4) 2_554 2_554 ?
O3W Ba1 O3W 76.7(7) . 2_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu2 O1 N2 179.1(7) 2_655 . . . ?
O20 Cu2 O1 N2 179.1(7) . . . . ?
O19 Cu2 O1 N2 -51.4(7) . . . . ?
O19 Cu2 O1 N2 49.0(7) 2_655 . . . ?
Cu2 O1 N2 C3 -154.4(7) . . . . ?
Cu2 O1 N2 Cu1 33.0(10) . . . . ?
N12 Cu1 N2 C3 87.7(19) . . . . ?
N8 Cu1 N2 C3 2.4(7) . . . . ?
N18 Cu1 N2 C3 -179.8(7) . . . . ?
N12 Cu1 N2 O1 -99.2(19) . . . . ?
N8 Cu1 N2 O1 175.5(8) . . . . ?
N18 Cu1 N2 O1 -6.7(9) . . . . ?
O1 N2 C3 C4 4.4(14) . . . . ?
Cu1 N2 C3 C4 178.5(8) . . . . ?
O1 N2 C3 C6 -177.2(8) . . . . ?
Cu1 N2 C3 C6 -3.1(11) . . . . ?
N2 C3 C4 N5 -40(32) . . . . ?
C6 C3 C4 N5 141(31) . . . . ?
N2 C3 C6 O7 -176.0(9) . . . . ?
C4 C3 C6 O7 2.4(14) . . . . ?
N2 C3 C6 N8 2.2(14) . . . . ?
C4 C3 C6 N8 -179.4(9) . . . . ?
N8 C6 O7 Ba1 -102.8(14) . . . . ?
C3 C6 O7 Ba1 75.1(16) . . . . ?
O7 C6 N8 C9 2.0(16) . . . . ?
C3 C6 N8 C9 -176.0(9) . . . . ?
O7 C6 N8 Cu1 178.0(8) . . . . ?
C3 C6 N8 Cu1 0.0(11) . . . . ?
N12 Cu1 N8 C6 -168.2(8) . . . . ?
N18 Cu1 N8 C6 -100(10) . . . . ?
N2 Cu1 N8 C6 -1.3(7) . . . . ?
N12 Cu1 N8 C9 7.5(10) . . . . ?
N18 Cu1 N8 C9 75(10) . . . . ?
N2 Cu1 N8 C9 174.4(9) . . . . ?
C6 N8 C9 C10 -163.3(11) . . . . ?
Cu1 N8 C9 C10 21.1(15) . . . . ?
N8 C9 C10 C11 -63.5(16) . . . . ?
C9 C10 C11 N12 66.4(15) . . . . ?
C10 C11 N12 C13 152.0(10) . . . . ?
C10 C11 N12 Cu1 -28.5(14) . . . . ?
N8 Cu1 N12 C13 176.9(8) . . . . ?
N18 Cu1 N12 C13 -1.0(8) . . . . ?
N2 Cu1 N12 C13 93.1(19) . . . . ?
N8 Cu1 N12 C11 -2.6(10) . . . . ?
N18 Cu1 N12 C11 179.5(10) . . . . ?
N2 Cu1 N12 C11 -86(2) . . . . ?
C11 N12 C13 O14 1.8(17) . . . . ?
Cu1 N12 C13 O14 -177.8(9) . . . . ?
C11 N12 C13 C15 -177.5(9) . . . . ?
Cu1 N12 C13 C15 2.9(11) . . . . ?
O14 C13 C15 N18 176.4(9) . . . . ?
N12 C13 C15 N18 -4.2(13) . . . . ?
O14 C13 C15 C16 -1.4(14) . . . . ?
N12 C13 C15 C16 178.0(9) . . . . ?
N18 C15 C16 N17 -145(27) . . . . ?
C13 C15 C16 N17 33(28) . . . . ?
C16 C15 N18 O19 -4.6(13) . . . . ?
C13 C15 N18 O19 177.7(8) . . . . ?
C16 C15 N18 Cu1 -178.8(8) . . . . ?
C13 C15 N18 Cu1 3.5(11) . . . . ?
N12 Cu1 N18 C15 -1.4(7) . . . . ?
N8 Cu1 N18 C15 -70(10) . . . . ?
N2 Cu1 N18 C15 -168.3(7) . . . . ?
N12 Cu1 N18 O19 -174.7(8) . . . . ?
N8 Cu1 N18 O19 117(10) . . . . ?
N2 Cu1 N18 O19 18.4(8) . . . . ?
C15 N18 O19 Cu2 138.6(7) . . . . ?
Cu1 N18 O19 Cu2 -48.4(9) . . . . ?
O1 Cu2 O19 N18 58.4(6) . . . . ?
O1 Cu2 O19 N18 -129.9(6) 2_655 . . . ?
O20 Cu2 O19 N18 147.7(5) . . . . ?
O19 Cu2 O19 N18 -32.3(5) 2_655 . . . ?
C6 O7 Ba1 O2W 85.5(14) . . . . ?
C6 O7 Ba1 O7 85.5(13) . . . 2_554 ?
C6 O7 Ba1 O1W 8.1(13) . . . . ?
C6 O7 Ba1 O1W 162.3(13) . . . 2_554 ?
C6 O7 Ba1 O3W -130.5(14) . . . . ?
C6 O7 Ba1 O3W -58.4(14) . . . 2_554 ?

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
O1W H1W1 O7 0.85 1.94 2.793(12) 179.3 6_556
O1W H1W2 O7 0.82 2.51 3.289(12) 158.9 .
O2W H2W O14 0.85 1.92 2.772(12) 179.6 8_455
O3W H3W1 O1W 0.85 2.41 3.260(16) 176.6 2_554
O3W H3W2 O1W 0.82 2.10 2.792(19) 142.1 6
O4W H4W1 O3W 0.82 2.03 2.794(15) 154.3 .
O4W H5W2 O14 0.85 1.81 2.658(11) 179.3 4_544

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.347

# Attachment 'Cu3Mn-revised2.cif'

data_sk1911
_database_code_depnum_ccdc_archive 'CCDC 662401'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H13 Cu1.50 Mn0.50 N6 O9.50'
_chemical_formula_weight         480.03

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'
Mn Mn 0.3368 0.7283 '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   ' c 2/c '

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

_cell_length_a                   20.315(11)
_cell_length_b                   16.8866(14)
_cell_length_c                   11.475(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.88(3)
_cell_angle_gamma                90.00
_cell_volume                     3599(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4084
_exptl_absorpt_correction_T_max  0.6948
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5368
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         29.95
_reflns_number_total             5239
_reflns_number_gt                2785
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Enraf Nonius Software V5'
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dr\"ager, 1971)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0631P)^2^+26.4528P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5239
_refine_ls_number_parameters     244
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1880
_refine_ls_wR_factor_gt          0.1540
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.41503(4) 0.07827(4) 0.01248(8) 0.0443(2) Uani 1 1 d . . .
Cu2 Cu 0.5000 -0.08035(5) 0.2500 0.0401(3) Uani 1 2 d S . .
O1 O 0.41171(19) -0.0910(2) 0.0990(4) 0.0427(10) Uani 1 1 d . . .
N2 N 0.3780(2) -0.0277(2) 0.0365(4) 0.0317(9) Uani 1 1 d . . .
C3 C 0.3099(3) -0.0328(3) -0.0301(5) 0.0358(12) Uani 1 1 d . . .
C4 C 0.2725(3) 0.0374(3) -0.1057(6) 0.0461(15) Uani 1 1 d . . .
O5 O 0.5000 -0.1960(3) 0.2500 0.0560(17) Uani 1 2 d S . .
N6 N 0.3151(3) 0.0964(3) -0.0954(5) 0.0455(12) Uani 1 1 d . . .
C7 C 0.2851(5) 0.1711(4) -0.1606(8) 0.071(2) Uani 1 1 d . . .
H7A H 0.2461 0.1593 -0.2419 0.085 Uiso 1 1 calc R . .
H7B H 0.2651 0.2005 -0.1099 0.085 Uiso 1 1 calc R . .
C8 C 0.3374(6) 0.2205(5) -0.1826(12) 0.099(4) Uani 1 1 d . . .
H8A H 0.3125 0.2657 -0.2336 0.119 Uiso 1 1 calc R . .
H8B H 0.3579 0.1905 -0.2318 0.119 Uiso 1 1 calc R . .
C9 C 0.3986(6) 0.2508(5) -0.0620(13) 0.110(4) Uani 1 1 d . . .
H9A H 0.4270 0.2889 -0.0853 0.133 Uiso 1 1 calc R . .
H9B H 0.3786 0.2778 -0.0092 0.133 Uiso 1 1 calc R . .
N10 N 0.4455(4) 0.1866(3) 0.0112(7) 0.072(2) Uani 1 1 d . . .
C11 C 0.5120(5) 0.2008(4) 0.0803(9) 0.073(3) Uani 1 1 d . . .
C12 C 0.5540(4) 0.1291(5) 0.1474(6) 0.063(2) Uani 1 1 d . . .
N13 N 0.5183(3) 0.0631(4) 0.1262(4) 0.0499(14) Uani 1 1 d . . .
O14 O 0.5519(2) -0.0034(4) 0.1767(5) 0.0784(19) Uani 1 1 d . . .
C15 C 0.2697(3) -0.1029(4) -0.0313(6) 0.0478(16) Uani 1 1 d . . .
N16 N 0.2373(3) -0.1577(4) -0.0329(8) 0.081(2) Uani 1 1 d . . .
O17 O 0.2057(3) 0.0329(3) -0.1701(6) 0.086(2) Uani 1 1 d . . .
O18 O 0.5460(4) 0.2661(3) 0.0965(7) 0.101(3) Uani 1 1 d . . .
C19 C 0.6294(5) 0.1325(6) 0.2297(7) 0.089(3) Uani 1 1 d . . .
N20 N 0.6885(5) 0.1338(7) 0.2955(8) 0.126(4) Uani 1 1 d . . .
O1W O 0.5913(2) 0.3011(3) -0.0890(5) 0.0595(13) Uani 1 1 d . . .
H1W H 0.5727 0.3009 -0.0144 0.089 Uiso 1 1 d R . .
H2W H 0.6405 0.3091 -0.0627 0.089 Uiso 1 1 d R . .
O2W O 0.3240(7) 0.4604(7) -0.0891(7) 0.180(5) Uani 1 1 d D . .
H3W H 0.326(11) 0.465(14) -0.158(10) 0.270 Uiso 1 1 d D . .
Mn2 Mn 0.5000 0.45982(8) 0.2500 0.0594(5) Uani 1 2 d S . .
O1I O 0.5871(3) 0.3769(3) 0.2744(5) 0.0763(16) Uani 1 1 d . . .
H1IA H 0.5769 0.3263 0.2211 0.115 Uiso 1 1 d R . .
H1IB H 0.6104 0.4213 0.2755 0.115 Uiso 1 1 d R . .
O2I O 0.4220(3) 0.5537(3) 0.2179(7) 0.113(3) Uani 1 1 d . . .
H2I H 0.3801 0.5378 0.2177 0.135 Uiso 1 1 d R . .
O3I O 0.4669(4) 0.4442(5) 0.0460(5) 0.130(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0415(4) 0.0283(4) 0.0710(5) -0.0108(3) 0.0309(4) -0.0126(3)
Cu2 0.0210(4) 0.0211(4) 0.0616(7) 0.000 -0.0004(4) 0.000
O1 0.0274(18) 0.0269(19) 0.057(2) -0.0074(17) -0.0001(17) -0.0004(15)
N2 0.029(2) 0.026(2) 0.035(2) -0.0025(18) 0.0080(18) -0.0046(17)
C3 0.029(3) 0.032(3) 0.036(3) 0.004(2) 0.002(2) -0.006(2)
C4 0.048(3) 0.033(3) 0.036(3) 0.004(2) -0.004(3) -0.006(3)
O5 0.065(4) 0.023(3) 0.064(4) 0.000 0.008(3) 0.000
N6 0.055(3) 0.030(2) 0.048(3) 0.005(2) 0.018(2) -0.006(2)
C7 0.097(6) 0.035(3) 0.083(6) 0.020(4) 0.039(5) 0.011(4)
C8 0.128(9) 0.044(5) 0.168(11) 0.037(6) 0.102(9) 0.016(5)
C9 0.121(9) 0.030(4) 0.226(14) -0.015(6) 0.117(9) -0.011(5)
N10 0.073(4) 0.033(3) 0.133(6) -0.027(3) 0.067(4) -0.026(3)
C11 0.109(6) 0.048(4) 0.104(6) -0.049(4) 0.088(6) -0.046(4)
C12 0.066(5) 0.089(6) 0.050(4) -0.041(4) 0.039(4) -0.056(4)
N13 0.047(3) 0.071(4) 0.027(2) -0.005(2) 0.009(2) -0.036(3)
O14 0.036(2) 0.111(5) 0.063(3) 0.050(3) -0.006(2) -0.030(3)
C15 0.024(3) 0.036(3) 0.061(4) 0.012(3) -0.006(2) -0.005(2)
N16 0.047(4) 0.047(3) 0.122(6) 0.019(4) 0.006(4) -0.015(3)
O17 0.054(3) 0.049(3) 0.093(4) 0.021(3) -0.035(3) -0.010(2)
O18 0.144(6) 0.070(4) 0.144(6) -0.073(4) 0.115(5) -0.078(4)
C19 0.079(6) 0.146(9) 0.052(4) -0.041(5) 0.037(4) -0.087(6)
N20 0.084(6) 0.209(11) 0.077(5) -0.029(6) 0.024(4) -0.093(7)
O1W 0.042(2) 0.044(3) 0.085(3) -0.001(2) 0.018(2) -0.012(2)
O2W 0.219(11) 0.153(8) 0.076(5) 0.010(6) -0.036(6) 0.040(8)
Mn2 0.0787(11) 0.0350(7) 0.0383(7) 0.000 -0.0034(7) 0.000
O1I 0.102(4) 0.045(3) 0.071(3) -0.024(3) 0.024(3) -0.012(3)
O2I 0.047(3) 0.046(3) 0.173(7) 0.029(4) -0.029(4) 0.000(2)
O3I 0.155(7) 0.149(6) 0.039(3) 0.021(3) -0.009(3) -0.108(6)

_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 N6 1.926(5) . ?
Cu1 N10 1.934(5) . ?
Cu1 N13 1.988(6) . ?
Cu1 N2 2.002(4) . ?
Cu2 O1 1.933(4) . ?
Cu2 O1 1.933(4) 2_655 ?
Cu2 O5 1.953(6) . ?
Cu2 O14 2.056(5) 2_655 ?
Cu2 O14 2.056(5) . ?
O1 N2 1.315(5) . ?
N2 C3 1.285(6) . ?
C3 C15 1.435(8) . ?
C3 C4 1.484(8) . ?
C4 O17 1.258(7) . ?
C4 N6 1.293(7) . ?
N6 C7 1.468(8) . ?
C7 C8 1.450(12) . ?
C8 C9 1.526(15) . ?
C9 N10 1.462(12) . ?
N10 C11 1.283(11) . ?
C11 O18 1.273(8) . ?
C11 C12 1.501(13) . ?
C12 N13 1.299(8) . ?
C12 C19 1.439(11) . ?
N13 O14 1.320(8) . ?
C15 N16 1.132(8) . ?
C19 N20 1.131(11) . ?
Mn2 O2I 2.165(6) 2_655 ?
Mn2 O2I 2.165(6) . ?
Mn2 O3I 2.175(6) 2_655 ?
Mn2 O3I 2.175(6) . ?
Mn2 O1I 2.184(6) 2_655 ?
Mn2 O1I 2.184(6) . ?

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
N6 Cu1 N10 95.8(3) . . ?
N6 Cu1 N13 178.1(2) . . ?
N10 Cu1 N13 82.6(3) . . ?
N6 Cu1 N2 82.74(18) . . ?
N10 Cu1 N2 170.3(2) . . ?
N13 Cu1 N2 98.6(2) . . ?
O1 Cu2 O1 169.3(2) . 2_655 ?
O1 Cu2 O5 84.65(11) . . ?
O1 Cu2 O5 84.65(11) 2_655 . ?
O1 Cu2 O14 88.99(18) . 2_655 ?
O1 Cu2 O14 97.79(18) 2_655 2_655 ?
O5 Cu2 O14 129.2(2) . 2_655 ?
O1 Cu2 O14 97.79(18) . . ?
O1 Cu2 O14 88.99(18) 2_655 . ?
O5 Cu2 O14 129.2(2) . . ?
O14 Cu2 O14 101.6(4) 2_655 . ?
N2 O1 Cu2 120.1(3) . . ?
C3 N2 O1 117.8(4) . . ?
C3 N2 Cu1 110.6(4) . . ?
O1 N2 Cu1 131.4(3) . . ?
N2 C3 C15 122.2(5) . . ?
N2 C3 C4 117.8(5) . . ?
C15 C3 C4 119.9(5) . . ?
O17 C4 N6 128.6(6) . . ?
O17 C4 C3 118.1(5) . . ?
N6 C4 C3 113.3(5) . . ?
C4 N6 C7 119.4(6) . . ?
C4 N6 Cu1 115.4(4) . . ?
C7 N6 Cu1 125.2(5) . . ?
C8 C7 N6 113.7(7) . . ?
C7 C8 C9 114.9(9) . . ?
N10 C9 C8 112.0(7) . . ?
C11 N10 C9 119.6(7) . . ?
C11 N10 Cu1 115.6(6) . . ?
C9 N10 Cu1 124.8(6) . . ?
O18 C11 N10 128.7(10) . . ?
O18 C11 C12 117.5(8) . . ?
N10 C11 C12 113.8(6) . . ?
N13 C12 C19 121.5(9) . . ?
N13 C12 C11 116.0(7) . . ?
C19 C12 C11 122.5(7) . . ?
C12 N13 O14 119.8(6) . . ?
C12 N13 Cu1 111.9(6) . . ?
O14 N13 Cu1 128.2(4) . . ?
N13 O14 Cu2 117.2(4) . . ?
N16 C15 C3 179.2(7) . . ?
N20 C19 C12 178.7(11) . . ?
O2I Mn2 O2I 85.8(3) 2_655 . ?
O2I Mn2 O3I 91.1(3) 2_655 2_655 ?
O2I Mn2 O3I 99.1(3) . 2_655 ?
O2I Mn2 O3I 99.1(3) 2_655 . ?
O2I Mn2 O3I 91.1(3) . . ?
O3I Mn2 O3I 166.0(4) 2_655 . ?
O2I Mn2 O1I 172.1(3) 2_655 2_655 ?
O2I Mn2 O1I 87.1(2) . 2_655 ?
O3I Mn2 O1I 86.7(3) 2_655 2_655 ?
O3I Mn2 O1I 84.4(2) . 2_655 ?
O2I Mn2 O1I 87.1(2) 2_655 . ?
O2I Mn2 O1I 172.1(3) . . ?
O3I Mn2 O1I 84.4(2) 2_655 . ?
O3I Mn2 O1I 86.7(3) . . ?
O1I Mn2 O1I 100.3(3) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu2 O1 N2 -177.6(4) 2_655 . . . ?
O5 Cu2 O1 N2 -177.6(4) . . . . ?
O14 Cu2 O1 N2 52.9(4) 2_655 . . . ?
O14 Cu2 O1 N2 -48.6(4) . . . . ?
Cu2 O1 N2 C3 -154.5(4) . . . . ?
Cu2 O1 N2 Cu1 31.2(6) . . . . ?
N6 Cu1 N2 C3 1.4(4) . . . . ?
N10 Cu1 N2 C3 83.7(16) . . . . ?
N13 Cu1 N2 C3 -179.9(4) . . . . ?
N6 Cu1 N2 O1 176.1(5) . . . . ?
N10 Cu1 N2 O1 -101.7(16) . . . . ?
N13 Cu1 N2 O1 -5.2(5) . . . . ?
O1 N2 C3 C15 4.0(9) . . . . ?
Cu1 N2 C3 C15 179.5(5) . . . . ?
O1 N2 C3 C4 -177.0(5) . . . . ?
Cu1 N2 C3 C4 -1.6(7) . . . . ?
N2 C3 C4 O17 -179.4(7) . . . . ?
C15 C3 C4 O17 -0.4(10) . . . . ?
N2 C3 C4 N6 0.7(9) . . . . ?
C15 C3 C4 N6 179.7(6) . . . . ?
O17 C4 N6 C7 2.8(12) . . . . ?
C3 C4 N6 C7 -177.3(6) . . . . ?
O17 C4 N6 Cu1 -179.3(7) . . . . ?
C3 C4 N6 Cu1 0.5(7) . . . . ?
N10 Cu1 N6 C4 -171.4(5) . . . . ?
N13 Cu1 N6 C4 -137(7) . . . . ?
N2 Cu1 N6 C4 -1.1(5) . . . . ?
N10 Cu1 N6 C7 6.3(6) . . . . ?
N13 Cu1 N6 C7 41(7) . . . . ?
N2 Cu1 N6 C7 176.7(6) . . . . ?
C4 N6 C7 C8 -158.1(8) . . . . ?
Cu1 N6 C7 C8 24.2(11) . . . . ?
N6 C7 C8 C9 -64.3(10) . . . . ?
C7 C8 C9 N10 66.7(11) . . . . ?
C8 C9 N10 C11 151.2(8) . . . . ?
C8 C9 N10 Cu1 -28.5(11) . . . . ?
N6 Cu1 N10 C11 177.2(6) . . . . ?
N13 Cu1 N10 C11 -1.7(5) . . . . ?
N2 Cu1 N10 C11 96.1(15) . . . . ?
N6 Cu1 N10 C9 -3.1(8) . . . . ?
N13 Cu1 N10 C9 177.9(8) . . . . ?
N2 Cu1 N10 C9 -84.3(18) . . . . ?
C9 N10 C11 O18 0.1(12) . . . . ?
Cu1 N10 C11 O18 179.8(6) . . . . ?
C9 N10 C11 C12 -178.5(7) . . . . ?
Cu1 N10 C11 C12 1.1(8) . . . . ?
O18 C11 C12 N13 -178.2(6) . . . . ?
N10 C11 C12 N13 0.6(9) . . . . ?
O18 C11 C12 C19 1.4(10) . . . . ?
N10 C11 C12 C19 -179.8(7) . . . . ?
C19 C12 N13 O14 -2.8(10) . . . . ?
C11 C12 N13 O14 176.8(6) . . . . ?
C19 C12 N13 Cu1 178.5(5) . . . . ?
C11 C12 N13 Cu1 -1.9(7) . . . . ?
N6 Cu1 N13 C12 -32(7) . . . . ?
N10 Cu1 N13 C12 2.0(5) . . . . ?
N2 Cu1 N13 C12 -168.3(4) . . . . ?
N6 Cu1 N13 O14 149(7) . . . . ?
N10 Cu1 N13 O14 -176.6(6) . . . . ?
N2 Cu1 N13 O14 13.1(6) . . . . ?
C12 N13 O14 Cu2 138.7(5) . . . . ?
Cu1 N13 O14 Cu2 -42.8(7) . . . . ?
O1 Cu2 O14 N13 55.1(5) . . . . ?
O1 Cu2 O14 N13 -133.2(5) 2_655 . . . ?
O5 Cu2 O14 N13 144.6(4) . . . . ?
O14 Cu2 O14 N13 -35.4(4) 2_655 . . . ?
N2 C3 C15 N16 166(100) . . . . ?
C4 C3 C15 N16 -13(63) . . . . ?
N13 C12 C19 N20 -23(54) . . . . ?
C11 C12 C19 N20 158(54) . . . . ?

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
O1W H1W O18 1.07 1.68 2.704(8) 159.7 .
O1W H2W N16 0.93 1.94 2.854(8) 168.7 3
O1I H1IA O18 1.02 1.66 2.643(7) 160.7 .
O1I H1IB O17 0.88 1.94 2.699(8) 143.3 8_556
O1I H1IB O2I 0.88 2.34 2.995(7) 130.9 2_655
O2I H2I O17 0.89 2.00 2.831(8) 155.1 7

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.95
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.119

data_sk1811
_database_code_depnum_ccdc_archive 'CCDC 662402'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H15 Co0.50 Cu1.50 N6 O9.50'
_chemical_formula_weight         484.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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   'C 2/c'

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

_cell_length_a                   20.262(4)
_cell_length_b                   16.8033(9)
_cell_length_c                   11.446(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.3650(10)
_cell_angle_gamma                90.00
_cell_volume                     3549.9(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    2.324
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5726
_exptl_absorpt_correction_T_max  0.8359
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_method       \q/2\w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5310
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         29.99
_reflns_number_total             5181
_reflns_number_gt                2290
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Enraf Nonius Software V5'
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dr\"ager, 1971)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0424P)^2^+20.1566P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5181
_refine_ls_number_parameters     253
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.2045
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1620
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.009
_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
C3 C 0.6922(3) 0.0327(3) 0.5330(5) 0.0322(13) Uani 1 1 d . . .
C4 C 0.7293(4) -0.0382(4) 0.6077(6) 0.0445(17) Uani 1 1 d . . .
C7 C 0.7174(5) -0.1723(4) 0.6646(8) 0.067(2) Uani 1 1 d . . .
H7A H 0.7379 -0.2017 0.6146 0.081 Uiso 1 1 calc R . .
H7B H 0.7565 -0.1602 0.7470 0.081 Uiso 1 1 calc R . .
C8 C 0.6646(6) -0.2226(5) 0.6853(11) 0.094(4) Uani 1 1 d . . .
H8A H 0.6442 -0.1929 0.7351 0.113 Uiso 1 1 calc R . .
H8B H 0.6897 -0.2683 0.7360 0.113 Uiso 1 1 calc R . .
C9 C 0.6029(6) -0.2523(5) 0.5638(13) 0.106(4) Uani 1 1 d . . .
H9A H 0.6228 -0.2790 0.5103 0.128 Uiso 1 1 calc R . .
H9B H 0.5745 -0.2909 0.5865 0.128 Uiso 1 1 calc R . .
C11 C 0.4883(5) -0.2021(5) 0.4196(9) 0.075(3) Uani 1 1 d . . .
C12 C 0.4465(4) -0.1302(6) 0.3528(7) 0.060(2) Uani 1 1 d . . .
C15 C 0.7319(3) 0.1030(4) 0.5321(7) 0.0433(17) Uani 1 1 d . . .
C19 C 0.3699(5) -0.1326(7) 0.2696(8) 0.089(4) Uani 1 1 d . . .
N2 N 0.6232(2) 0.0278(3) 0.4655(4) 0.0302(11) Uani 1 1 d . . .
N6 N 0.6869(3) -0.0977(3) 0.5985(5) 0.0470(15) Uani 1 1 d . . .
N10 N 0.5554(4) -0.1875(4) 0.4906(7) 0.067(2) Uani 1 1 d . . .
N13 N 0.4816(3) -0.0628(4) 0.3737(5) 0.0503(17) Uani 1 1 d . . .
N16 N 0.7651(3) 0.1574(4) 0.5325(7) 0.073(2) Uani 1 1 d . . .
N20 N 0.3107(5) -0.1349(7) 0.2031(8) 0.130(4) Uani 1 1 d . . .
O1 O 0.5892(2) 0.0911(2) 0.4021(4) 0.0399(11) Uani 1 1 d . . .
O5 O 0.5000 0.1956(3) 0.2500 0.0534(19) Uani 1 2 d S . .
H5 H 0.4787 0.2275 0.2001 0.080 Uiso 1 1 d R . .
O14 O 0.4482(3) 0.0028(4) 0.3223(5) 0.079(2) Uani 1 1 d . . .
O17 O 0.7965(3) -0.0336(3) 0.6758(6) 0.082(2) Uani 1 1 d . . .
O18 O 0.4536(4) -0.2676(4) 0.4026(7) 0.098(3) Uani 1 1 d . . .
Cu1 Cu 0.58597(4) -0.07887(5) 0.48917(9) 0.0425(2) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.08034(6) 0.2500 0.0390(3) Uani 1 2 d S . .
O1I O 0.0825(3) 0.1234(3) 0.2772(6) 0.0697(18) Uani 1 1 d D . .
H1I H 0.1229(16) 0.105(4) 0.317(6) 0.105 Uiso 1 1 d D . .
H2I H 0.0795 0.1572 0.2355 0.105 Uiso 1 1 d R . .
O2I O 0.0757(3) -0.0506(3) 0.2730(7) 0.092(2) Uani 1 1 d D . .
H3I H 0.1174 -0.0454 0.2861 0.137 Uiso 1 1 d R . .
O3I O 0.0313(4) 0.0518(4) 0.4470(5) 0.105(3) Uani 1 1 d . . .
H5I H 0.0717 0.0580 0.4769 0.157 Uiso 1 1 d R . .
Co3 Co 0.0000 0.04015(7) 0.2500 0.0548(4) Uani 1 2 d S . .
H4I H 0.074(5) -0.080(5) 0.329(6) 0.082 Uiso 1 1 d D . .
O1W O 0.1765(8) 0.0366(7) 0.5810(8) 0.166(5) Uani 1 1 d D . .
H2W H 0.183(10) 0.080(5) 0.617(17) 0.249 Uiso 1 1 d D . .
O2W O 0.0898(2) -0.1954(3) 0.4109(5) 0.0590(14) Uani 1 1 d . . .
H3W H 0.0742 -0.1770 0.4592 0.088 Uiso 1 1 d R . .
H1W H 0.160(6) 0.012(7) 0.625(10) 0.088 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C3 0.026(3) 0.033(3) 0.026(3) 0.001(2) -0.001(2) -0.008(2)
C4 0.050(4) 0.036(3) 0.028(3) 0.003(3) -0.004(3) -0.014(3)
C7 0.090(6) 0.035(4) 0.076(6) 0.018(4) 0.035(5) 0.001(4)
C8 0.118(9) 0.045(5) 0.156(11) 0.030(6) 0.093(8) 0.008(5)
C9 0.123(9) 0.028(4) 0.214(14) -0.018(6) 0.115(10) -0.013(5)
C11 0.111(7) 0.059(5) 0.105(7) -0.058(5) 0.093(6) -0.054(5)
C12 0.060(5) 0.096(6) 0.038(4) -0.038(4) 0.034(4) -0.052(5)
C15 0.023(3) 0.032(3) 0.052(4) 0.011(3) -0.007(3) -0.001(2)
C19 0.080(6) 0.152(9) 0.046(5) -0.031(5) 0.038(5) -0.089(7)
N2 0.028(2) 0.028(2) 0.032(3) -0.009(2) 0.009(2) -0.006(2)
N6 0.062(4) 0.032(3) 0.044(3) 0.007(2) 0.018(3) -0.008(3)
N10 0.072(5) 0.036(3) 0.120(6) -0.026(4) 0.066(5) -0.028(3)
N13 0.047(3) 0.079(5) 0.021(3) -0.007(3) 0.010(2) -0.042(3)
N16 0.044(4) 0.040(3) 0.108(6) 0.019(4) 0.004(4) -0.017(3)
N20 0.080(6) 0.226(12) 0.072(6) -0.032(7) 0.020(5) -0.099(7)
O1 0.024(2) 0.025(2) 0.056(3) -0.0060(19) 0.0018(19) 0.0005(16)
O5 0.063(4) 0.024(3) 0.054(4) 0.000 0.004(3) 0.000
O14 0.033(3) 0.118(5) 0.059(3) 0.053(4) -0.009(2) -0.033(3)
O17 0.054(3) 0.045(3) 0.086(4) 0.020(3) -0.033(3) -0.009(3)
O18 0.130(5) 0.075(4) 0.143(6) -0.076(4) 0.111(5) -0.081(4)
Cu1 0.0409(5) 0.0308(4) 0.0637(6) -0.0131(4) 0.0295(4) -0.0159(4)
Cu2 0.0212(5) 0.0209(5) 0.0601(7) 0.000 0.0018(5) 0.000
O1I 0.101(5) 0.038(3) 0.056(3) 0.017(3) 0.018(3) 0.006(3)
O2I 0.048(3) 0.038(3) 0.124(6) 0.018(3) -0.029(3) 0.001(3)
O3I 0.122(5) 0.117(5) 0.034(3) 0.018(3) -0.010(3) -0.085(5)
Co3 0.0776(10) 0.0280(6) 0.0299(7) 0.000 -0.0070(7) 0.000
O1W 0.213(12) 0.143(10) 0.060(5) -0.004(5) -0.025(6) 0.060(9)
O2W 0.045(3) 0.041(3) 0.087(4) -0.008(3) 0.022(3) -0.011(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
C3 N2 1.292(6) . ?
C3 C15 1.431(8) . ?
C3 C4 1.479(8) . ?
C4 O17 1.262(7) . ?
C4 N6 1.293(8) . ?
C7 C8 1.458(11) . ?
C7 N6 1.464(8) . ?
C8 C9 1.521(14) . ?
C9 N10 1.466(12) . ?
C11 O18 1.276(8) . ?
C11 N10 1.287(11) . ?
C11 C12 1.493(13) . ?
C12 N13 1.305(9) . ?
C12 C19 1.450(11) . ?
C15 N16 1.134(8) . ?
C19 N20 1.124(11) . ?
N2 O1 1.311(6) . ?
N2 Cu1 2.005(5) . ?
N6 Cu1 1.934(6) . ?
N10 Cu1 1.930(6) . ?
N13 O14 1.300(8) . ?
N13 Cu1 1.996(6) . ?
O1 Cu2 1.932(4) . ?
O5 Cu2 1.938(6) . ?
O14 Cu2 2.049(5) . ?
Cu2 O1 1.932(4) 2_655 ?
Cu2 O14 2.049(5) 2_655 ?
O1I Co3 2.102(6) . ?
O2I Co3 2.100(6) . ?
O3I Co3 2.085(5) . ?
Co3 O3I 2.085(5) 2 ?
Co3 O2I 2.100(6) 2 ?
Co3 O1I 2.102(6) 2 ?

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
N2 C3 C15 121.5(5) . . ?
N2 C3 C4 117.4(5) . . ?
C15 C3 C4 121.1(5) . . ?
O17 C4 N6 127.5(6) . . ?
O17 C4 C3 118.0(5) . . ?
N6 C4 C3 114.5(5) . . ?
C8 C7 N6 113.5(7) . . ?
C7 C8 C9 115.1(9) . . ?
N10 C9 C8 112.1(7) . . ?
O18 C11 N10 129.2(11) . . ?
O18 C11 C12 117.4(9) . . ?
N10 C11 C12 113.3(7) . . ?
N13 C12 C19 120.0(9) . . ?
N13 C12 C11 117.2(7) . . ?
C19 C12 C11 122.8(8) . . ?
N16 C15 C3 178.0(7) . . ?
N20 C19 C12 178.6(11) . . ?
C3 N2 O1 118.1(5) . . ?
C3 N2 Cu1 110.6(4) . . ?
O1 N2 Cu1 131.2(3) . . ?
C4 N6 C7 119.7(6) . . ?
C4 N6 Cu1 114.6(4) . . ?
C7 N6 Cu1 125.7(5) . . ?
C11 N10 C9 119.5(7) . . ?
C11 N10 Cu1 115.8(6) . . ?
C9 N10 Cu1 124.8(6) . . ?
O14 N13 C12 120.7(6) . . ?
O14 N13 Cu1 128.7(4) . . ?
C12 N13 Cu1 110.6(6) . . ?
N2 O1 Cu2 120.4(3) . . ?
N13 O14 Cu2 117.7(4) . . ?
N10 Cu1 N6 95.6(3) . . ?
N10 Cu1 N13 82.9(3) . . ?
N6 Cu1 N13 178.2(3) . . ?
N10 Cu1 N2 170.5(2) . . ?
N6 Cu1 N2 82.9(2) . . ?
N13 Cu1 N2 98.3(2) . . ?
O1 Cu2 O1 169.3(2) . 2_655 ?
O1 Cu2 O5 84.65(12) . . ?
O1 Cu2 O5 84.65(12) 2_655 . ?
O1 Cu2 O14 98.02(19) . . ?
O1 Cu2 O14 88.79(18) 2_655 . ?
O5 Cu2 O14 129.5(2) . . ?
O1 Cu2 O14 88.79(18) . 2_655 ?
O1 Cu2 O14 98.02(19) 2_655 2_655 ?
O5 Cu2 O14 129.5(2) . 2_655 ?
O14 Cu2 O14 101.0(4) . 2_655 ?
O3I Co3 O3I 169.2(4) . 2 ?
O3I Co3 O2I 94.8(3) . 2 ?
O3I Co3 O2I 93.0(3) 2 2 ?
O3I Co3 O2I 93.0(3) . . ?
O3I Co3 O2I 94.8(3) 2 . ?
O2I Co3 O2I 86.9(3) 2 . ?
O3I Co3 O1I 84.8(2) . . ?
O3I Co3 O1I 88.0(3) 2 . ?
O2I Co3 O1I 175.1(2) 2 . ?
O2I Co3 O1I 88.3(2) . . ?
O3I Co3 O1I 88.0(3) . 2 ?
O3I Co3 O1I 84.8(2) 2 2 ?
O2I Co3 O1I 88.3(2) 2 2 ?
O2I Co3 O1I 175.1(2) . 2 ?
O1I Co3 O1I 96.5(3) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C3 C4 O17 -178.8(7) . . . . ?
C15 C3 C4 O17 3.4(10) . . . . ?
N2 C3 C4 N6 -1.3(9) . . . . ?
C15 C3 C4 N6 -179.2(6) . . . . ?
N6 C7 C8 C9 63.3(11) . . . . ?
C7 C8 C9 N10 -66.8(11) . . . . ?
O18 C11 C12 N13 177.8(6) . . . . ?
N10 C11 C12 N13 -0.2(10) . . . . ?
O18 C11 C12 C19 -1.0(11) . . . . ?
N10 C11 C12 C19 -179.0(7) . . . . ?
N2 C3 C15 N16 -155(24) . . . . ?
C4 C3 C15 N16 23(24) . . . . ?
N13 C12 C19 N20 97(53) . . . . ?
C11 C12 C19 N20 -84(53) . . . . ?
C15 C3 N2 O1 -4.4(9) . . . . ?
C4 C3 N2 O1 177.8(5) . . . . ?
C15 C3 N2 Cu1 179.7(5) . . . . ?
C4 C3 N2 Cu1 1.8(7) . . . . ?
O17 C4 N6 C7 -4.8(12) . . . . ?
C3 C4 N6 C7 178.0(6) . . . . ?
O17 C4 N6 Cu1 177.2(7) . . . . ?
C3 C4 N6 Cu1 0.1(8) . . . . ?
C8 C7 N6 C4 159.1(8) . . . . ?
C8 C7 N6 Cu1 -23.2(11) . . . . ?
O18 C11 N10 C9 1.3(13) . . . . ?
C12 C11 N10 C9 179.0(7) . . . . ?
O18 C11 N10 Cu1 -179.7(6) . . . . ?
C12 C11 N10 Cu1 -2.0(8) . . . . ?
C8 C9 N10 C11 -151.8(8) . . . . ?
C8 C9 N10 Cu1 29.3(11) . . . . ?
C19 C12 N13 O14 1.2(10) . . . . ?
C11 C12 N13 O14 -177.7(6) . . . . ?
C19 C12 N13 Cu1 -179.1(5) . . . . ?
C11 C12 N13 Cu1 2.1(8) . . . . ?
C3 N2 O1 Cu2 154.4(4) . . . . ?
Cu1 N2 O1 Cu2 -30.7(7) . . . . ?
C12 N13 O14 Cu2 -138.6(5) . . . . ?
Cu1 N13 O14 Cu2 41.7(8) . . . . ?
C11 N10 Cu1 N6 -176.4(6) . . . . ?
C9 N10 Cu1 N6 2.5(8) . . . . ?
C11 N10 Cu1 N13 2.5(6) . . . . ?
C9 N10 Cu1 N13 -178.6(8) . . . . ?
C11 N10 Cu1 N2 -95.7(16) . . . . ?
C9 N10 Cu1 N2 83.2(19) . . . . ?
C4 N6 Cu1 N10 171.2(5) . . . . ?
C7 N6 Cu1 N10 -6.5(7) . . . . ?
C4 N6 Cu1 N13 134(7) . . . . ?
C7 N6 Cu1 N13 -44(8) . . . . ?
C4 N6 Cu1 N2 0.7(5) . . . . ?
C7 N6 Cu1 N2 -177.1(6) . . . . ?
O14 N13 Cu1 N10 177.3(6) . . . . ?
C12 N13 Cu1 N10 -2.4(5) . . . . ?
O14 N13 Cu1 N6 -145(7) . . . . ?
C12 N13 Cu1 N6 35(8) . . . . ?
O14 N13 Cu1 N2 -12.2(6) . . . . ?
C12 N13 Cu1 N2 168.1(5) . . . . ?
C3 N2 Cu1 N10 -83.1(17) . . . . ?
O1 N2 Cu1 N10 101.6(17) . . . . ?
C3 N2 Cu1 N6 -1.4(4) . . . . ?
O1 N2 Cu1 N6 -176.6(5) . . . . ?
C3 N2 Cu1 N13 180.0(4) . . . . ?
O1 N2 Cu1 N13 4.7(5) . . . . ?
N2 O1 Cu2 O1 177.3(4) . . . 2_655 ?
N2 O1 Cu2 O5 177.3(4) . . . . ?
N2 O1 Cu2 O14 48.1(5) . . . . ?
N2 O1 Cu2 O14 -52.8(5) . . . 2_655 ?
N13 O14 Cu2 O1 -54.3(5) . . . . ?
N13 O14 Cu2 O1 134.0(5) . . . 2_655 ?
N13 O14 Cu2 O5 -143.9(4) . . . . ?
N13 O14 Cu2 O14 36.1(4) . . . 2_655 ?

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
O5 H5 O2W 0.77 1.94 2.700(6) 168.1 4
O1I H1I O17 0.82(5) 2.00(4) 2.736(9) 150(7) 5_656
O1I H2I O18 0.73 1.92 2.623(7) 163.9 4
O2I H3I O17 0.80 2.09 2.793(8) 146.6 5_656
O2I H4I O2W 0.82(7) 2.11(5) 2.849(7) 149(9) .
O3I H5I O1W 0.75 1.99 2.712(16) 159.6 .
O1W H1W O3I 0.82(11) 2.65(12) 2.712(16) 85(9) .
O1W H2W N20 0.82(12) 2.53(18) 2.990(19) 117(17) 6_556
O2W H3W O18 0.80 2.10 2.695(8) 130.6 7_546

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.697
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.119