# Electronic Supplementary MAterial for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Jian-Fang Ma'
_publ_contact_author_email       JIANFANGMA@YAHOO.COM.CN

_publ_section_title              
;
A Series of 2D and 3D Metal-Organic Frameworks Based
on Different Polycarboxylate Anions and Flexible
2,2'-bis(1H-imidazolyl)ether Ligand

;
loop_
_publ_author_name
'Jian-Fang Ma.'
'Zhi-Fang Jia.'
'Guo-Hua Wei.'
'Yun-Peng Xie.'
'Jin Yang.'
;
Lai-Ping Zhang
;

# Attachment 'zhang.cif'

data_Compound-1
_database_code_depnum_ccdc_archive 'CCDC 682065'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 N4 Ni O5'
_chemical_formula_sum            'C18 H18 N4 Ni O5'
_chemical_formula_weight         429.07

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'
Ni Ni 0.3393 1.1124 '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'
_symmetry_space_group_name_hall  '-C 2yc '

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                   6.961(4)
_cell_length_b                   19.331(8)
_cell_length_c                   13.812(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.43(2)
_cell_angle_gamma                90.00
_cell_volume                     1850.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2113
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.105
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8974
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         27.47
_reflns_number_total             2113
_reflns_number_gt                1807
_reflns_threshold_expression     >2sigma(I)

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

_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+1.5046P] 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         2113
_refine_ls_number_parameters     128
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
C9 C -0.6934(3) -0.00125(9) 0.51667(12) 0.0261(4) Uani 1 1 d . . .
H1 H -0.8231 -0.0021 0.5278 0.031 Uiso 1 1 calc R . .
C8 C -0.5609(3) 0.03285(9) 0.58148(13) 0.0260(4) Uani 1 1 d . . .
H2 H -0.6018 0.0547 0.6359 0.031 Uiso 1 1 calc R . .
C7 C -0.3671(3) 0.03427(8) 0.56501(12) 0.0236(4) Uani 1 1 d . . .
C6 C -0.2227(3) 0.07161(8) 0.63446(12) 0.0246(4) Uani 1 1 d . . .
C2 C 0.0578(4) 0.25931(13) 0.8833(2) 0.0579(7) Uani 1 1 d . . .
H5 H 0.1917 0.2569 0.8860 0.069 Uiso 1 1 calc R . .
C3 C -0.0432(4) 0.31195(13) 0.9178(2) 0.0579(7) Uani 1 1 d . . .
H6 H 0.0072 0.3520 0.9476 0.069 Uiso 1 1 calc R . .
C1 C -0.2396(3) 0.23358(10) 0.85514(13) 0.0335(4) Uani 1 1 d . . .
H7 H -0.3533 0.2105 0.8343 0.040 Uiso 1 1 calc R . .
C4 C -0.3971(4) 0.33889(12) 0.91695(16) 0.0485(6) Uani 1 1 d . . .
H8A H -0.3672 0.3657 0.9758 0.058 Uiso 1 1 calc R . .
H8B H -0.5079 0.3100 0.9261 0.058 Uiso 1 1 calc R . .
C5 C -0.4460(4) 0.38682(12) 0.83317(19) 0.0570(7) Uani 1 1 d . . .
H9A H -0.5515 0.4170 0.8467 0.068 Uiso 1 1 calc R . .
H9B H -0.3352 0.4152 0.8223 0.068 Uiso 1 1 calc R . .
N1 N -0.0667(3) 0.21000(8) 0.84374(12) 0.0353(4) Uani 1 1 d . . .
N2 N -0.2329(3) 0.29515(9) 0.90054(12) 0.0388(4) Uani 1 1 d . . .
O1 O -0.04655(18) 0.05789(7) 0.63585(9) 0.0329(3) Uani 1 1 d . . .
O2 O -0.28244(19) 0.11672(7) 0.69096(10) 0.0337(3) Uani 1 1 d . . .
O3 O -0.5000 0.34599(10) 0.7500 0.0453(5) Uani 1 2 d S . .
Ni1 Ni 0.0000 0.134449(16) 0.7500 0.02476(11) Uani 1 2 d S . .


_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
C9 C8 1.389(2) . ?
C9 C7 1.396(2) 5_456 ?
C9 H1 0.9300 . ?
C8 C7 1.389(3) . ?
C8 H2 0.9300 . ?
C7 C9 1.396(2) 5_456 ?
C7 C6 1.506(2) . ?
C6 O1 1.253(2) . ?
C6 O2 1.266(2) . ?
C6 Ni1 2.4407(19) . ?
C2 C3 1.349(4) . ?
C2 N1 1.367(3) . ?
C2 H5 0.9300 . ?
C3 N2 1.358(3) . ?
C3 H6 0.9300 . ?
C1 N1 1.310(3) . ?
C1 N2 1.344(2) . ?
C1 H7 0.9300 . ?
C4 N2 1.457(3) . ?
C4 C5 1.496(3) . ?
C4 H8A 0.9700 . ?
C4 H8B 0.9700 . ?
C5 O3 1.415(3) . ?
C5 H9A 0.9700 . ?
C5 H9B 0.9700 . ?
N1 Ni1 2.0344(18) . ?
O1 Ni1 2.1644(14) . ?
O2 Ni1 2.0843(18) . ?
O3 C5 1.415(3) 2_456 ?
Ni1 N1 2.0344(18) 2_556 ?
Ni1 O2 2.0843(18) 2_556 ?
Ni1 O1 2.1644(14) 2_556 ?
Ni1 C6 2.4407(19) 2_556 ?

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
C8 C9 C7 120.33(17) . 5_456 ?
C8 C9 H1 119.8 . . ?
C7 C9 H1 119.8 5_456 . ?
C7 C8 C9 119.97(16) . . ?
C7 C8 H2 120.0 . . ?
C9 C8 H2 120.0 . . ?
C8 C7 C9 119.70(16) . 5_456 ?
C8 C7 C6 120.33(16) . . ?
C9 C7 C6 119.97(16) 5_456 . ?
O1 C6 O2 120.95(16) . . ?
O1 C6 C7 120.09(16) . . ?
O2 C6 C7 118.96(16) . . ?
O1 C6 Ni1 62.31(9) . . ?
O2 C6 Ni1 58.64(9) . . ?
C7 C6 Ni1 177.59(14) . . ?
C3 C2 N1 109.6(2) . . ?
C3 C2 H5 125.2 . . ?
N1 C2 H5 125.2 . . ?
C2 C3 N2 106.8(2) . . ?
C2 C3 H6 126.6 . . ?
N2 C3 H6 126.6 . . ?
N1 C1 N2 111.86(18) . . ?
N1 C1 H7 124.1 . . ?
N2 C1 H7 124.1 . . ?
N2 C4 C5 111.3(2) . . ?
N2 C4 H8A 109.4 . . ?
C5 C4 H8A 109.4 . . ?
N2 C4 H8B 109.4 . . ?
C5 C4 H8B 109.4 . . ?
H8A C4 H8B 108.0 . . ?
O3 C5 C4 107.82(18) . . ?
O3 C5 H9A 110.1 . . ?
C4 C5 H9A 110.1 . . ?
O3 C5 H9B 110.1 . . ?
C4 C5 H9B 110.1 . . ?
H9A C5 H9B 108.5 . . ?
C1 N1 C2 105.33(18) . . ?
C1 N1 Ni1 126.43(13) . . ?
C2 N1 Ni1 125.48(17) . . ?
C1 N2 C3 106.49(19) . . ?
C1 N2 C4 126.40(19) . . ?
C3 N2 C4 126.71(19) . . ?
C6 O1 Ni1 86.86(10) . . ?
C6 O2 Ni1 90.10(11) . . ?
C5 O3 C5 112.2(2) . 2_456 ?
N1 Ni1 N1 88.24(10) . 2_556 ?
N1 Ni1 O2 95.93(7) . . ?
N1 Ni1 O2 97.63(7) 2_556 . ?
N1 Ni1 O2 97.63(7) . 2_556 ?
N1 Ni1 O2 95.93(7) 2_556 2_556 ?
O2 Ni1 O2 161.07(8) . 2_556 ?
N1 Ni1 O1 157.98(6) . . ?
N1 Ni1 O1 93.14(7) 2_556 . ?
O2 Ni1 O1 62.09(5) . . ?
O2 Ni1 O1 104.07(6) 2_556 . ?
N1 Ni1 O1 93.14(7) . 2_556 ?
N1 Ni1 O1 157.98(6) 2_556 2_556 ?
O2 Ni1 O1 104.07(6) . 2_556 ?
O2 Ni1 O1 62.09(5) 2_556 2_556 ?
O1 Ni1 O1 93.72(8) . 2_556 ?
N1 Ni1 C6 127.17(7) . . ?
N1 Ni1 C6 96.34(7) 2_556 . ?
O2 Ni1 C6 31.25(6) . . ?
O2 Ni1 C6 133.73(6) 2_556 . ?
O1 Ni1 C6 30.84(6) . . ?
O1 Ni1 C6 100.25(6) 2_556 . ?
N1 Ni1 C6 96.34(7) . 2_556 ?
N1 Ni1 C6 127.17(7) 2_556 2_556 ?
O2 Ni1 C6 133.73(6) . 2_556 ?
O2 Ni1 C6 31.25(6) 2_556 2_556 ?
O1 Ni1 C6 100.25(6) . 2_556 ?
O1 Ni1 C6 30.84(6) 2_556 2_556 ?
C6 Ni1 C6 120.31(8) . 2_556 ?

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
C7 C9 C8 C7 0.1(3) 5_456 . . . ?
C9 C8 C7 C9 -0.1(3) . . . 5_456 ?
C9 C8 C7 C6 179.50(15) . . . . ?
C8 C7 C6 O1 160.53(16) . . . . ?
C9 C7 C6 O1 -19.9(2) 5_456 . . . ?
C8 C7 C6 O2 -19.4(2) . . . . ?
C9 C7 C6 O2 160.18(16) 5_456 . . . ?
N1 C2 C3 N2 0.6(3) . . . . ?
N2 C4 C5 O3 62.5(3) . . . . ?
N2 C1 N1 C2 -0.5(3) . . . . ?
N2 C1 N1 Ni1 -162.35(13) . . . . ?
C3 C2 N1 C1 -0.1(3) . . . . ?
C3 C2 N1 Ni1 162.02(18) . . . . ?
N1 C1 N2 C3 0.8(3) . . . . ?
N1 C1 N2 C4 173.97(19) . . . . ?
C2 C3 N2 C1 -0.8(3) . . . . ?
C2 C3 N2 C4 -173.9(2) . . . . ?
C5 C4 N2 C1 -88.2(3) . . . . ?
C5 C4 N2 C3 83.6(3) . . . . ?
O2 C6 O1 Ni1 0.23(17) . . . . ?
C7 C6 O1 Ni1 -179.73(14) . . . . ?
O1 C6 O2 Ni1 -0.23(17) . . . . ?
C7 C6 O2 Ni1 179.72(13) . . . . ?
C4 C5 O3 C5 178.5(3) . . . 2_456 ?
C1 N1 Ni1 N1 98.05(18) . . . 2_556 ?
C2 N1 Ni1 N1 -60.34(19) . . . 2_556 ?
C1 N1 Ni1 O2 0.56(18) . . . . ?
C2 N1 Ni1 O2 -157.83(19) . . . . ?
C1 N1 Ni1 O2 -166.20(17) . . . 2_556 ?
C2 N1 Ni1 O2 35.4(2) . . . 2_556 ?
C1 N1 Ni1 O1 4.0(3) . . . . ?
C2 N1 Ni1 O1 -154.36(19) . . . . ?
C1 N1 Ni1 O1 -103.95(18) . . . 2_556 ?
C2 N1 Ni1 O1 97.7(2) . . . 2_556 ?
C1 N1 Ni1 C6 1.4(2) . . . . ?
C2 N1 Ni1 C6 -156.96(18) . . . . ?
C1 N1 Ni1 C6 -134.74(18) . . . 2_556 ?
C2 N1 Ni1 C6 66.9(2) . . . 2_556 ?
C6 O2 Ni1 N1 178.66(11) . . . . ?
C6 O2 Ni1 N1 89.65(12) . . . 2_556 ?
C6 O2 Ni1 O2 -45.75(10) . . . 2_556 ?
C6 O2 Ni1 O1 0.13(10) . . . . ?
C6 O2 Ni1 O1 -86.59(11) . . . 2_556 ?
C6 O2 Ni1 C6 -76.70(16) . . . 2_556 ?
C6 O1 Ni1 N1 -4.0(2) . . . . ?
C6 O1 Ni1 N1 -97.11(11) . . . 2_556 ?
C6 O1 Ni1 O2 -0.13(10) . . . . ?
C6 O1 Ni1 O2 165.98(10) . . . 2_556 ?
C6 O1 Ni1 O1 103.83(11) . . . 2_556 ?
C6 O1 Ni1 C6 134.22(10) . . . 2_556 ?
O1 C6 Ni1 N1 178.10(10) . . . . ?
O2 C6 Ni1 N1 -1.68(13) . . . . ?
O1 C6 Ni1 N1 85.50(11) . . . 2_556 ?
O2 C6 Ni1 N1 -94.28(11) . . . 2_556 ?
O1 C6 Ni1 O2 179.77(17) . . . . ?
O1 C6 Ni1 O2 -18.98(14) . . . 2_556 ?
O2 C6 Ni1 O2 161.25(8) . . . 2_556 ?
O2 C6 Ni1 O1 -179.77(17) . . . . ?
O1 C6 Ni1 O1 -79.96(13) . . . 2_556 ?
O2 C6 Ni1 O1 100.27(11) . . . 2_556 ?
O1 C6 Ni1 C6 -54.77(9) . . . 2_556 ?
O2 C6 Ni1 C6 125.45(11) . . . 2_556 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.056

#=========================END

data_Compound-2
_database_code_depnum_ccdc_archive 'CCDC 682066'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Cu N4 O5'
_chemical_formula_sum            'C18 H18 Cu N4 O5'
_chemical_formula_weight         433.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   8.244(5)
_cell_length_b                   9.858(6)
_cell_length_c                   12.130(6)
_cell_angle_alpha                103.88(2)
_cell_angle_beta                 96.27(2)
_cell_angle_gamma                105.88(2)
_cell_volume                     904.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4077
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             446
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8853
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4064
_reflns_number_gt                3176
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.1168P)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_number_reflns         4064
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1684
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
C17 C 0.5304(4) 0.5454(4) 0.9023(3) 0.0279(7) Uani 1 1 d . . .
H1 H 0.5512 0.5751 0.8367 0.033 Uiso 1 1 calc R . .
C16 C 0.6124(4) 0.6402(4) 1.0123(3) 0.0247(6) Uani 1 1 d . . .
C18 C 0.4184(4) 0.4076(4) 0.8915(3) 0.0290(7) Uani 1 1 d . . .
H3 H 0.3630 0.3463 0.8184 0.035 Uiso 1 1 calc R . .
C15 C 0.7348(4) 0.7909(4) 1.0260(3) 0.0262(7) Uani 1 1 d . . .
C1 C 1.1154(4) 0.8877(4) 1.1870(3) 0.0324(8) Uani 1 1 d . . .
H5 H 1.0173 0.8899 1.2177 0.039 Uiso 1 1 calc R . .
C2 C 1.3025(4) 0.9056(4) 1.0777(3) 0.0388(9) Uani 1 1 d . . .
H6 H 1.3583 0.9233 1.0176 0.047 Uiso 1 1 calc R . .
C3 C 1.3637(5) 0.8588(5) 1.1649(4) 0.0389(9) Uani 1 1 d . . .
H7 H 1.4666 0.8377 1.1757 0.047 Uiso 1 1 calc R . .
C4 C 1.2454(5) 0.7955(5) 1.3362(3) 0.0399(9) Uani 1 1 d . . .
H8A H 1.1699 0.8310 1.3836 0.048 Uiso 1 1 calc R . .
H8B H 1.3608 0.8334 1.3817 0.048 Uiso 1 1 calc R . .
C5 C 1.1886(5) 0.6306(5) 1.3025(4) 0.0433(10) Uani 1 1 d . . .
H9A H 1.2631 0.5937 1.2550 0.052 Uiso 1 1 calc R . .
H9B H 1.1930 0.5961 1.3709 0.052 Uiso 1 1 calc R . .
C6 C 0.9672(5) 0.4344(5) 1.1658(3) 0.0408(9) Uani 1 1 d . . .
H10A H 1.0548 0.4241 1.1200 0.049 Uiso 1 1 calc R . .
H10B H 0.8610 0.4156 1.1130 0.049 Uiso 1 1 calc R . .
C7 C 0.9421(5) 0.3220(4) 1.2329(4) 0.0381(9) Uani 1 1 d . . .
H11A H 0.9293 0.2263 1.1813 0.046 Uiso 1 1 calc R . .
H11B H 1.0431 0.3478 1.2922 0.046 Uiso 1 1 calc R . .
C8 C 0.7605(4) 0.4215(4) 1.3664(3) 0.0331(8) Uani 1 1 d . . .
H12 H 0.8391 0.5147 1.3991 0.040 Uiso 1 1 calc R . .
C10 C 0.6457(5) 0.1947(4) 1.2610(4) 0.0425(10) Uani 1 1 d . . .
H13 H 0.6285 0.1030 1.2096 0.051 Uiso 1 1 calc R . .
C9 C 0.5336(5) 0.2358(4) 1.3237(4) 0.0437(10) Uani 1 1 d . . .
H14 H 0.4234 0.1765 1.3215 0.052 Uiso 1 1 calc R . .
C11 C 0.7072(4) 0.7415(4) 1.4713(3) 0.0260(7) Uani 1 1 d . . .
C12 C 0.8597(4) 0.8747(4) 1.4863(3) 0.0242(6) Uani 1 1 d . . .
C13 C 1.0012(4) 0.9142(4) 1.5751(3) 0.0292(7) Uani 1 1 d . . .
H17 H 1.0023 0.8574 1.6261 0.035 Uiso 1 1 calc R . .
C14 C 0.8589(4) 0.9619(4) 1.4120(3) 0.0299(7) Uani 1 1 d . . .
H18 H 0.7647 0.9375 1.3532 0.036 Uiso 1 1 calc R . .
N1 N 1.1456(3) 0.9228(3) 1.0913(2) 0.0292(6) Uani 1 1 d . . .
N2 N 1.2425(4) 0.8490(3) 1.2343(3) 0.0304(6) Uani 1 1 d . . .
N4 N 0.6060(4) 0.3786(3) 1.3914(2) 0.0297(6) Uani 1 1 d . . .
N3 N 0.7899(4) 0.3136(3) 1.2875(3) 0.0321(7) Uani 1 1 d . . .
O1 O 0.8236(3) 0.8033(3) 0.9471(2) 0.0315(6) Uani 1 1 d . . .
O2 O 0.7481(3) 0.8934(3) 1.1130(2) 0.0349(6) Uani 1 1 d . . .
O3 O 1.0164(3) 0.5805(3) 1.2392(2) 0.0389(6) Uani 1 1 d . . .
O4 O 0.5815(3) 0.7119(3) 1.3948(2) 0.0377(6) Uani 1 1 d . . .
O5 O 0.7181(3) 0.6644(3) 1.5415(2) 0.0279(5) Uani 1 1 d . . .
Cu1 Cu 1.0000 1.0000 1.0000 0.02387(18) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.5000 1.5000 0.02284(18) Uani 1 2 d S . .


_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
C17 C18 1.384(5) . ?
C17 C16 1.403(5) . ?
C17 H1 0.9300 . ?
C16 C18 1.382(5) 2_667 ?
C16 C15 1.509(4) . ?
C18 C16 1.382(5) 2_667 ?
C18 H3 0.9300 . ?
C15 O2 1.245(4) . ?
C15 O1 1.275(4) . ?
C1 N1 1.319(4) . ?
C1 N2 1.329(5) . ?
C1 H5 0.9300 . ?
C2 C3 1.353(6) . ?
C2 N1 1.371(5) . ?
C2 H6 0.9300 . ?
C3 N2 1.373(5) . ?
C3 H7 0.9300 . ?
C4 N2 1.456(5) . ?
C4 C5 1.500(6) . ?
C4 H8A 0.9700 . ?
C4 H8B 0.9700 . ?
C5 O3 1.430(5) . ?
C5 H9A 0.9700 . ?
C5 H9B 0.9700 . ?
C6 O3 1.421(5) . ?
C6 C7 1.509(5) . ?
C6 H10A 0.9700 . ?
C6 H10B 0.9700 . ?
C7 N3 1.473(4) . ?
C7 H11A 0.9700 . ?
C7 H11B 0.9700 . ?
C8 N4 1.321(4) . ?
C8 N3 1.345(5) . ?
C8 H12 0.9300 . ?
C10 C9 1.345(6) . ?
C10 N3 1.365(5) . ?
C10 H13 0.9300 . ?
C9 N4 1.375(5) . ?
C9 H14 0.9300 . ?
C11 O4 1.231(4) . ?
C11 O5 1.282(4) . ?
C11 C12 1.506(4) . ?
C12 C14 1.387(5) . ?
C12 C13 1.396(5) . ?
C13 C14 1.394(5) 2_778 ?
C13 H17 0.9300 . ?
C14 C13 1.394(5) 2_778 ?
C14 H18 0.9300 . ?
N1 Cu1 1.965(3) . ?
N4 Cu2 2.000(3) . ?
O1 Cu1 1.986(3) . ?
O5 Cu2 1.982(2) . ?
Cu1 N1 1.965(3) 2_777 ?
Cu1 O1 1.986(3) 2_777 ?
Cu2 O5 1.982(2) 2_668 ?
Cu2 N4 2.000(3) 2_668 ?

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
C18 C17 C16 120.1(3) . . ?
C18 C17 H1 120.0 . . ?
C16 C17 H1 120.0 . . ?
C18 C16 C17 118.8(3) 2_667 . ?
C18 C16 C15 120.2(3) 2_667 . ?
C17 C16 C15 120.9(3) . . ?
C16 C18 C17 121.1(3) 2_667 . ?
C16 C18 H3 119.5 2_667 . ?
C17 C18 H3 119.5 . . ?
O2 C15 O1 123.8(3) . . ?
O2 C15 C16 119.6(3) . . ?
O1 C15 C16 116.5(3) . . ?
N1 C1 N2 111.7(3) . . ?
N1 C1 H5 124.2 . . ?
N2 C1 H5 124.2 . . ?
C3 C2 N1 109.8(3) . . ?
C3 C2 H6 125.1 . . ?
N1 C2 H6 125.1 . . ?
C2 C3 N2 105.7(3) . . ?
C2 C3 H7 127.1 . . ?
N2 C3 H7 127.1 . . ?
N2 C4 C5 110.9(3) . . ?
N2 C4 H8A 109.5 . . ?
C5 C4 H8A 109.5 . . ?
N2 C4 H8B 109.5 . . ?
C5 C4 H8B 109.5 . . ?
H8A C4 H8B 108.1 . . ?
O3 C5 C4 107.2(3) . . ?
O3 C5 H9A 110.3 . . ?
C4 C5 H9A 110.3 . . ?
O3 C5 H9B 110.3 . . ?
C4 C5 H9B 110.3 . . ?
H9A C5 H9B 108.5 . . ?
O3 C6 C7 112.2(3) . . ?
O3 C6 H10A 109.2 . . ?
C7 C6 H10A 109.2 . . ?
O3 C6 H10B 109.2 . . ?
C7 C6 H10B 109.2 . . ?
H10A C6 H10B 107.9 . . ?
N3 C7 C6 111.8(3) . . ?
N3 C7 H11A 109.3 . . ?
C6 C7 H11A 109.3 . . ?
N3 C7 H11B 109.3 . . ?
C6 C7 H11B 109.3 . . ?
H11A C7 H11B 107.9 . . ?
N4 C8 N3 111.6(3) . . ?
N4 C8 H12 124.2 . . ?
N3 C8 H12 124.2 . . ?
C9 C10 N3 106.7(3) . . ?
C9 C10 H13 126.7 . . ?
N3 C10 H13 126.7 . . ?
C10 C9 N4 109.9(3) . . ?
C10 C9 H14 125.1 . . ?
N4 C9 H14 125.1 . . ?
O4 C11 O5 123.6(3) . . ?
O4 C11 C12 120.1(3) . . ?
O5 C11 C12 116.3(3) . . ?
C14 C12 C13 119.0(3) . . ?
C14 C12 C11 119.7(3) . . ?
C13 C12 C11 121.4(3) . . ?
C14 C13 C12 120.7(3) 2_778 . ?
C14 C13 H17 119.7 2_778 . ?
C12 C13 H17 119.7 . . ?
C12 C14 C13 120.3(3) . 2_778 ?
C12 C14 H18 119.8 . . ?
C13 C14 H18 119.8 2_778 . ?
C1 N1 C2 105.4(3) . . ?
C1 N1 Cu1 125.2(3) . . ?
C2 N1 Cu1 129.3(3) . . ?
C1 N2 C3 107.5(3) . . ?
C1 N2 C4 125.8(3) . . ?
C3 N2 C4 126.6(3) . . ?
C8 N4 C9 105.1(3) . . ?
C8 N4 Cu2 126.8(2) . . ?
C9 N4 Cu2 128.1(2) . . ?
C8 N3 C10 106.8(3) . . ?
C8 N3 C7 127.6(3) . . ?
C10 N3 C7 125.5(3) . . ?
C15 O1 Cu1 107.9(2) . . ?
C6 O3 C5 113.6(3) . . ?
C11 O5 Cu2 106.4(2) . . ?
N1 Cu1 N1 180 . 2_777 ?
N1 Cu1 O1 89.83(12) . . ?
N1 Cu1 O1 90.17(12) 2_777 . ?
N1 Cu1 O1 90.17(12) . 2_777 ?
N1 Cu1 O1 89.83(12) 2_777 2_777 ?
O1 Cu1 O1 180 . 2_777 ?
O5 Cu2 O5 180 2_668 . ?
O5 Cu2 N4 90.54(11) 2_668 . ?
O5 Cu2 N4 89.46(11) . . ?
O5 Cu2 N4 89.46(11) 2_668 2_668 ?
O5 Cu2 N4 90.54(11) . 2_668 ?
N4 Cu2 N4 180 . 2_668 ?

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
C18 C17 C16 C18 1.1(6) . . . 2_667 ?
C18 C17 C16 C15 -180.0(3) . . . . ?
C16 C17 C18 C16 -1.2(6) . . . 2_667 ?
C18 C16 C15 O2 -32.4(5) 2_667 . . . ?
C17 C16 C15 O2 148.7(3) . . . . ?
C18 C16 C15 O1 145.5(3) 2_667 . . . ?
C17 C16 C15 O1 -33.4(5) . . . . ?
N1 C2 C3 N2 -0.8(4) . . . . ?
N2 C4 C5 O3 -61.0(4) . . . . ?
O3 C6 C7 N3 69.2(4) . . . . ?
N3 C10 C9 N4 -1.2(5) . . . . ?
O4 C11 C12 C14 -1.3(5) . . . . ?
O5 C11 C12 C14 178.6(3) . . . . ?
O4 C11 C12 C13 177.5(3) . . . . ?
O5 C11 C12 C13 -2.6(5) . . . . ?
C14 C12 C13 C14 -0.9(6) . . . 2_778 ?
C11 C12 C13 C14 -179.7(3) . . . 2_778 ?
C13 C12 C14 C13 0.9(6) . . . 2_778 ?
C11 C12 C14 C13 179.8(3) . . . 2_778 ?
N2 C1 N1 C2 -0.3(4) . . . . ?
N2 C1 N1 Cu1 -175.3(2) . . . . ?
C3 C2 N1 C1 0.6(4) . . . . ?
C3 C2 N1 Cu1 175.4(3) . . . . ?
N1 C1 N2 C3 -0.2(4) . . . . ?
N1 C1 N2 C4 -176.0(3) . . . . ?
C2 C3 N2 C1 0.6(4) . . . . ?
C2 C3 N2 C4 176.4(3) . . . . ?
C5 C4 N2 C1 96.1(4) . . . . ?
C5 C4 N2 C3 -79.0(5) . . . . ?
N3 C8 N4 C9 -0.5(5) . . . . ?
N3 C8 N4 Cu2 -178.3(3) . . . . ?
C10 C9 N4 C8 1.0(5) . . . . ?
C10 C9 N4 Cu2 178.8(3) . . . . ?
N4 C8 N3 C10 -0.2(5) . . . . ?
N4 C8 N3 C7 176.0(4) . . . . ?
C9 C10 N3 C8 0.8(5) . . . . ?
C9 C10 N3 C7 -175.5(4) . . . . ?
C6 C7 N3 C8 -60.7(5) . . . . ?
C6 C7 N3 C10 114.8(4) . . . . ?
O2 C15 O1 Cu1 7.6(4) . . . . ?
C16 C15 O1 Cu1 -170.2(2) . . . . ?
C7 C6 O3 C5 71.9(4) . . . . ?
C4 C5 O3 C6 157.6(3) . . . . ?
O4 C11 O5 Cu2 -0.2(4) . . . . ?
C12 C11 O5 Cu2 179.9(2) . . . . ?
C1 N1 Cu1 O1 -71.8(3) . . . . ?
C2 N1 Cu1 O1 114.4(3) . . . . ?
C1 N1 Cu1 O1 108.2(3) . . . 2_777 ?
C2 N1 Cu1 O1 -65.6(3) . . . 2_777 ?
C15 O1 Cu1 N1 82.1(2) . . . . ?
C15 O1 Cu1 N1 -97.9(2) . . . 2_777 ?
C11 O5 Cu2 N4 90.5(2) . . . . ?
C11 O5 Cu2 N4 -89.5(2) . . . 2_668 ?
C8 N4 Cu2 O5 176.0(3) . . . 2_668 ?
C9 N4 Cu2 O5 -1.3(3) . . . 2_668 ?
C8 N4 Cu2 O5 -4.0(3) . . . . ?
C9 N4 Cu2 O5 178.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.469
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.134

#=================END

data_Compound-3
_database_code_depnum_ccdc_archive 'CCDC 682067'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Cu N4 O5'
_chemical_formula_sum            'C18 H18 Cu N4 O5'
_chemical_formula_weight         433.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_hall  '-P 2yn '

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

_cell_length_a                   10.352(5)
_cell_length_b                   12.761(5)
_cell_length_c                   14.229(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.241(18)
_cell_angle_gamma                90.00
_cell_volume                     1864.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4273
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17781
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4273
_reflns_number_gt                3041
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0527P)²+3.1273P] 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         4273
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1332
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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
C1 C -0.1983(3) 0.3781(2) 0.0330(2) 0.0315(7) Uani 1 1 d . . .
C2 C -0.3149(3) 0.3068(2) 0.0112(2) 0.0306(7) Uani 1 1 d . . .
C3 C -0.4371(4) 0.3537(3) 0.0067(3) 0.0440(9) Uani 1 1 d . . .
H3 H -0.4429 0.4238 0.0235 0.053 Uiso 1 1 calc R . .
C4 C -0.5498(4) 0.2983(4) -0.0221(3) 0.0551(11) Uani 1 1 d . . .
H4 H -0.6303 0.3311 -0.0244 0.066 Uiso 1 1 calc R . .
C5 C -0.5428(4) 0.1945(4) -0.0475(3) 0.0534(11) Uani 1 1 d . . .
H5 H -0.6183 0.1574 -0.0685 0.064 Uiso 1 1 calc R . .
C6 C -0.4223(3) 0.1457(3) -0.0415(3) 0.0422(8) Uani 1 1 d . . .
H6 H -0.4178 0.0753 -0.0577 0.051 Uiso 1 1 calc R . .
C7 C -0.3085(3) 0.1999(2) -0.0117(2) 0.0299(7) Uani 1 1 d . . .
C8 C -0.1833(3) 0.1397(2) 0.0050(2) 0.0318(7) Uani 1 1 d . . .
C9 C -0.1395(4) -0.0478(3) 0.1704(3) 0.0401(8) Uani 1 1 d . . .
H9 H -0.1531 0.0226 0.1826 0.048 Uiso 1 1 calc R . .
C10 C -0.1752(4) -0.1278(3) 0.2222(3) 0.0432(9) Uani 1 1 d . . .
H10 H -0.2168 -0.1233 0.2763 0.052 Uiso 1 1 calc R . .
C11 C -0.0805(3) -0.1888(3) 0.1049(2) 0.0359(7) Uani 1 1 d . . .
H11 H -0.0453 -0.2351 0.0644 0.043 Uiso 1 1 calc R . .
C12 C -0.1573(4) -0.3258(3) 0.2118(3) 0.0511(10) Uani 1 1 d . . .
H12A H -0.2177 -0.3250 0.2586 0.061 Uiso 1 1 calc R . .
H12B H -0.1964 -0.3671 0.1583 0.061 Uiso 1 1 calc R . .
C13 C -0.0383(6) -0.3758(4) 0.2521(5) 0.111(3) Uani 1 1 d . . .
H13A H -0.0639 -0.4271 0.2966 0.133 Uiso 1 1 calc R . .
H13B H -0.0085 -0.4156 0.2008 0.133 Uiso 1 1 calc R . .
C14 C 0.1775(4) -0.3728(3) 0.3169(3) 0.0564(11) Uani 1 1 d . . .
H14A H 0.1819 -0.4452 0.2968 0.068 Uiso 1 1 calc R . .
H14B H 0.1973 -0.3707 0.3853 0.068 Uiso 1 1 calc R . .
C15 C 0.2758(4) -0.3093(3) 0.2733(3) 0.0525(10) Uani 1 1 d . . .
H15A H 0.3593 -0.3449 0.2827 0.063 Uiso 1 1 calc R . .
H15B H 0.2493 -0.3036 0.2056 0.063 Uiso 1 1 calc R . .
C16 C 0.1993(4) -0.1249(3) 0.3083(3) 0.0461(9) Uani 1 1 d . . .
H16 H 0.1184 -0.1249 0.2715 0.055 Uiso 1 1 calc R . .
C17 C 0.2505(4) -0.0476(3) 0.3657(3) 0.0405(8) Uani 1 1 d . . .
H17 H 0.2098 0.0158 0.3750 0.049 Uiso 1 1 calc R . .
C18 C 0.3921(4) -0.1716(3) 0.3755(3) 0.0384(8) Uani 1 1 d . . .
H18 H 0.4671 -0.2110 0.3923 0.046 Uiso 1 1 calc R . .
N1 N -0.0796(3) -0.0857(2) 0.0960(2) 0.0335(6) Uani 1 1 d . . .
N2 N -0.1386(3) -0.2180(2) 0.1798(2) 0.0367(6) Uani 1 1 d . . .
N3 N 0.2902(3) -0.2035(2) 0.3148(2) 0.0406(7) Uani 1 1 d . . .
N4 N 0.3721(3) -0.0765(2) 0.4086(2) 0.0338(6) Uani 1 1 d . . .
O1 O -0.1101(2) 0.37232(16) -0.02276(16) 0.0306(5) Uani 1 1 d . . .
O2 O -0.1970(3) 0.4447(2) 0.09592(19) 0.0483(7) Uani 1 1 d . . .
O3 O -0.0987(2) 0.16441(18) 0.07196(19) 0.0403(6) Uani 1 1 d . . .
O4 O -0.1716(2) 0.06071(18) -0.04771(17) 0.0375(5) Uani 1 1 d . . .
O5 O 0.0547(4) -0.3350(3) 0.2910(5) 0.158(3) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.5000 0.0000 0.02791(15) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.0000 0.0000 0.02858(15) Uani 1 2 d S . .


_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 O2 1.234(4) . ?
C1 O1 1.285(4) . ?
C1 C2 1.512(5) . ?
C2 C3 1.393(5) . ?
C2 C7 1.406(5) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.386(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.500(4) . ?
C8 O3 1.250(4) . ?
C8 O4 1.271(4) . ?
C9 C10 1.338(5) . ?
C9 N1 1.380(4) . ?
C9 H9 0.9300 . ?
C10 N2 1.374(5) . ?
C10 H10 0.9300 . ?
C11 N1 1.322(4) . ?
C11 N2 1.342(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.441(7) . ?
C12 N2 1.469(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 O5 1.170(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O5 1.366(5) . ?
C14 C15 1.495(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N3 1.474(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.345(5) . ?
C16 N3 1.371(5) . ?
C16 H16 0.9300 . ?
C17 N4 1.378(4) . ?
C17 H17 0.9300 . ?
C18 N4 1.328(4) . ?
C18 N3 1.340(4) . ?
C18 H18 0.9300 . ?
N1 Cu2 2.005(3) . ?
N4 Cu1 1.991(3) 2_545 ?
O1 Cu1 1.991(2) . ?
O4 Cu2 1.978(2) . ?
Cu1 O1 1.991(2) 3_565 ?
Cu1 N4 1.991(3) 2 ?
Cu1 N4 1.991(3) 4_565 ?
Cu2 O4 1.978(2) 3 ?
Cu2 N1 2.005(3) 3 ?

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 C1 O1 123.0(3) . . ?
O2 C1 C2 119.9(3) . . ?
O1 C1 C2 116.7(3) . . ?
C3 C2 C7 118.4(3) . . ?
C3 C2 C1 116.6(3) . . ?
C7 C2 C1 124.8(3) . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C7 C6 C5 121.2(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C2 119.5(3) . . ?
C6 C7 C8 118.5(3) . . ?
C2 C7 C8 121.8(3) . . ?
O3 C8 O4 122.7(3) . . ?
O3 C8 C7 119.9(3) . . ?
O4 C8 C7 117.2(3) . . ?
C10 C9 N1 109.7(3) . . ?
C10 C9 H9 125.1 . . ?
N1 C9 H9 125.1 . . ?
C9 C10 N2 106.7(3) . . ?
C9 C10 H10 126.7 . . ?
N2 C10 H10 126.7 . . ?
N1 C11 N2 111.2(3) . . ?
N1 C11 H11 124.4 . . ?
N2 C11 H11 124.4 . . ?
C13 C12 N2 113.5(4) . . ?
C13 C12 H12A 108.9 . . ?
N2 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
N2 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
O5 C13 C12 127.0(5) . . ?
O5 C13 H13A 105.5 . . ?
C12 C13 H13A 105.5 . . ?
O5 C13 H13B 105.5 . . ?
C12 C13 H13B 105.5 . . ?
H13A C13 H13B 106.1 . . ?
O5 C14 C15 110.9(4) . . ?
O5 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N3 C15 C14 111.7(3) . . ?
N3 C15 H15A 109.3 . . ?
C14 C15 H15A 109.3 . . ?
N3 C15 H15B 109.3 . . ?
C14 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 N3 106.3(3) . . ?
C17 C16 H16 126.8 . . ?
N3 C16 H16 126.8 . . ?
C16 C17 N4 109.9(3) . . ?
C16 C17 H17 125.0 . . ?
N4 C17 H17 125.0 . . ?
N4 C18 N3 111.1(3) . . ?
N4 C18 H18 124.4 . . ?
N3 C18 H18 124.4 . . ?
C11 N1 C9 105.4(3) . . ?
C11 N1 Cu2 128.1(2) . . ?
C9 N1 Cu2 126.5(2) . . ?
C11 N2 C10 107.0(3) . . ?
C11 N2 C12 126.5(3) . . ?
C10 N2 C12 126.5(3) . . ?
C18 N3 C16 107.4(3) . . ?
C18 N3 C15 124.6(3) . . ?
C16 N3 C15 127.6(3) . . ?
C18 N4 C17 105.2(3) . . ?
C18 N4 Cu1 124.0(2) . 2_545 ?
C17 N4 Cu1 130.8(2) . 2_545 ?
C1 O1 Cu1 106.81(19) . . ?
C8 O4 Cu2 104.8(2) . . ?
C13 O5 C14 130.8(5) . . ?
O1 Cu1 O1 180 . 3_565 ?
O1 Cu1 N4 91.44(10) . 2 ?
O1 Cu1 N4 88.56(10) 3_565 2 ?
O1 Cu1 N4 88.56(10) . 4_565 ?
O1 Cu1 N4 91.44(10) 3_565 4_565 ?
N4 Cu1 N4 180 2 4_565 ?
O4 Cu2 O4 180 3 . ?
O4 Cu2 N1 88.91(11) 3 . ?
O4 Cu2 N1 91.09(11) . . ?
O4 Cu2 N1 91.09(11) 3 3 ?
O4 Cu2 N1 88.91(11) . 3 ?
N1 Cu2 N1 180 . 3 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 43.8(5) . . . . ?
O1 C1 C2 C3 -129.4(3) . . . . ?
O2 C1 C2 C7 -141.3(3) . . . . ?
O1 C1 C2 C7 45.5(4) . . . . ?
C7 C2 C3 C4 -2.0(6) . . . . ?
C1 C2 C3 C4 173.3(4) . . . . ?
C2 C3 C4 C5 -0.2(7) . . . . ?
C3 C4 C5 C6 1.6(7) . . . . ?
C4 C5 C6 C7 -0.9(6) . . . . ?
C5 C6 C7 C2 -1.2(5) . . . . ?
C5 C6 C7 C8 172.4(4) . . . . ?
C3 C2 C7 C6 2.6(5) . . . . ?
C1 C2 C7 C6 -172.2(3) . . . . ?
C3 C2 C7 C8 -170.8(3) . . . . ?
C1 C2 C7 C8 14.4(5) . . . . ?
C6 C7 C8 O3 -142.9(3) . . . . ?
C2 C7 C8 O3 30.6(5) . . . . ?
C6 C7 C8 O4 33.2(4) . . . . ?
C2 C7 C8 O4 -153.4(3) . . . . ?
N1 C9 C10 N2 -0.5(4) . . . . ?
N2 C12 C13 O5 28.5(11) . . . . ?
O5 C14 C15 N3 69.6(5) . . . . ?
N3 C16 C17 N4 -0.2(5) . . . . ?
N2 C11 N1 C9 0.6(4) . . . . ?
N2 C11 N1 Cu2 177.5(2) . . . . ?
C10 C9 N1 C11 -0.1(4) . . . . ?
C10 C9 N1 Cu2 -177.0(3) . . . . ?
N1 C11 N2 C10 -1.0(4) . . . . ?
N1 C11 N2 C12 -179.9(3) . . . . ?
C9 C10 N2 C11 0.9(4) . . . . ?
C9 C10 N2 C12 179.8(4) . . . . ?
C13 C12 N2 C11 70.6(6) . . . . ?
C13 C12 N2 C10 -108.0(6) . . . . ?
N4 C18 N3 C16 0.0(4) . . . . ?
N4 C18 N3 C15 -173.4(3) . . . . ?
C17 C16 N3 C18 0.1(5) . . . . ?
C17 C16 N3 C15 173.3(4) . . . . ?
C14 C15 N3 C18 105.9(4) . . . . ?
C14 C15 N3 C16 -66.1(5) . . . . ?
N3 C18 N4 C17 -0.1(4) . . . . ?
N3 C18 N4 Cu1 -179.6(2) . . . 2_545 ?
C16 C17 N4 C18 0.2(4) . . . . ?
C16 C17 N4 Cu1 179.7(3) . . . 2_545 ?
O2 C1 O1 Cu1 -9.1(4) . . . . ?
C2 C1 O1 Cu1 163.9(2) . . . . ?
O3 C8 O4 Cu2 -1.4(4) . . . . ?
C7 C8 O4 Cu2 -177.4(2) . . . . ?
C12 C13 O5 C14 -167.5(7) . . . . ?
C15 C14 O5 C13 122.0(9) . . . . ?
C1 O1 Cu1 N4 95.0(2) . . . 2 ?
C1 O1 Cu1 N4 -85.0(2) . . . 4_565 ?
C8 O4 Cu2 N1 86.9(2) . . . . ?
C8 O4 Cu2 N1 -93.1(2) . . . 3 ?
C11 N1 Cu2 O4 -60.0(3) . . . 3 ?
C9 N1 Cu2 O4 116.3(3) . . . 3 ?
C11 N1 Cu2 O4 120.0(3) . . . . ?
C9 N1 Cu2 O4 -63.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.079

#=============END

data_Compound-4
_database_code_depnum_ccdc_archive 'CCDC 682068'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 Co N4 O5'
_chemical_formula_sum            'C12 H14 Co N4 O5'
_chemical_formula_weight         353.20

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'

_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                   9.472(4)
_cell_length_b                   17.653(5)
_cell_length_c                   8.516(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.072(15)
_cell_angle_gamma                90.00
_cell_volume                     1413.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3226
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.123
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13685
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3215
_reflns_number_gt                2659
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0213P)²+1.2557P] 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         3215
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0617
_refine_ls_wR_factor_gt          0.0579
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_restrained_S_all      0.914
_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
C1 C 0.53074(18) -0.02496(10) 0.0710(2) 0.0214(4) Uani 1 1 d . . .
C2 C -0.02318(18) 0.04111(9) 0.0157(2) 0.0194(4) Uani 1 1 d . . .
C3 C 0.1237(2) -0.07246(12) 0.3791(3) 0.0330(5) Uani 1 1 d . . .
H3 H 0.0771 -0.0977 0.2918 0.040 Uiso 1 1 calc R . .
C4 C 0.2542(2) 0.00504(12) 0.5241(3) 0.0327(5) Uani 1 1 d . . .
H4 H 0.3162 0.0445 0.5559 0.039 Uiso 1 1 calc R . .
C5 C 0.1955(2) -0.04209(12) 0.6234(3) 0.0347(5) Uani 1 1 d . . .
H5 H 0.2092 -0.0411 0.7334 0.042 Uiso 1 1 calc R . .
C6 C 0.0286(2) -0.15504(12) 0.5808(3) 0.0369(5) Uani 1 1 d . . .
H6A H -0.0691 -0.1509 0.5317 0.044 Uiso 1 1 calc R . .
H6B H 0.0283 -0.1525 0.6946 0.044 Uiso 1 1 calc R . .
C7 C 0.0885(2) -0.23026(12) 0.5381(3) 0.0356(5) Uani 1 1 d . . .
H7A H 0.0250 -0.2707 0.5616 0.043 Uiso 1 1 calc R . .
H7B H 0.0967 -0.2316 0.4257 0.043 Uiso 1 1 calc R . .
C8 C 0.3115(2) -0.29311(12) 0.5533(3) 0.0381(5) Uani 1 1 d . . .
H8A H 0.2525 -0.3233 0.4759 0.046 Uiso 1 1 calc R . .
H8B H 0.3575 -0.3272 0.6332 0.046 Uiso 1 1 calc R . .
C9 C 0.4232(2) -0.25277(14) 0.4734(3) 0.0440(6) Uani 1 1 d . . .
H9A H 0.4665 -0.2884 0.4071 0.053 Uiso 1 1 calc R . .
H9B H 0.3782 -0.2133 0.4056 0.053 Uiso 1 1 calc R . .
N1 N 0.20896(17) -0.01399(9) 0.3692(2) 0.0281(4) Uani 1 1 d . . .
N2 N 0.11171(18) -0.09141(10) 0.5292(2) 0.0305(4) Uani 1 1 d . . .
O1 O 0.46044(13) -0.02842(8) 0.18664(16) 0.0283(3) Uani 1 1 d . . .
O2 O 0.64604(14) -0.05841(7) 0.05888(17) 0.0280(3) Uani 1 1 d . . .
O3 O 0.07007(13) 0.08470(7) 0.08252(16) 0.0260(3) Uani 1 1 d . . .
O4 O -0.14994(13) 0.05759(7) -0.02864(17) 0.0270(3) Uani 1 1 d . . .
O5 O 0.22412(16) -0.24095(9) 0.62562(19) 0.0400(4) Uani 1 1 d . . .
Co1 Co 0.26760(2) 0.031938(13) 0.15546(3) 0.02033(7) Uani 1 1 d . . .
C10 C 0.5433(2) -0.14615(11) 0.6331(2) 0.0283(4) Uani 1 1 d . . .
H10 H 0.4787 -0.1087 0.5956 0.034 Uiso 1 1 calc R . .
C11 C 0.7208(2) -0.20383(11) 0.7611(3) 0.0303(4) Uani 1 1 d . . .
H11 H 0.8032 -0.2132 0.8297 0.036 Uiso 1 1 calc R . .
C12 C 0.6473(2) -0.25636(12) 0.6684(3) 0.0361(5) Uani 1 1 d . . .
H12 H 0.6690 -0.3075 0.6615 0.043 Uiso 1 1 calc R . .
N3 N 0.53429(17) -0.21899(10) 0.5868(2) 0.0315(4) Uani 1 1 d . . .
N4 N 0.65532(16) -0.13451(9) 0.7386(2) 0.0260(3) Uani 1 1 d . . .


_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 O2 1.257(2) . ?
C1 O1 1.257(2) . ?
C1 C1 1.550(4) 3_655 ?
C2 O4 1.248(2) . ?
C2 O3 1.254(2) . ?
C2 C2 1.549(3) 3 ?
C3 N1 1.320(3) . ?
C3 N2 1.339(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.354(3) . ?
C4 N1 1.377(3) . ?
C4 H4 0.9300 . ?
C5 N2 1.369(3) . ?
C5 H5 0.9300 . ?
C6 N2 1.470(3) . ?
C6 C7 1.506(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O5 1.417(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O5 1.428(3) . ?
C8 C9 1.506(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.464(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N1 Co1 2.1281(18) . ?
O1 Co1 2.1030(14) . ?
O2 Co1 2.1417(16) 3_655 ?
O3 Co1 2.1137(14) . ?
O4 Co1 2.1471(14) 3 ?
Co1 N4 2.1126(16) 3_656 ?
Co1 O2 2.1417(16) 3_655 ?
Co1 O4 2.1471(14) 3 ?
C10 N4 1.320(2) . ?
C10 N3 1.345(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.354(3) . ?
C11 N4 1.375(2) . ?
C11 H11 0.9300 . ?
C12 N3 1.371(3) . ?
C12 H12 0.9300 . ?
N4 Co1 2.1126(16) 3_656 ?

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 C1 O1 126.22(17) . . ?
O2 C1 C1 116.8(2) . 3_655 ?
O1 C1 C1 117.02(19) . 3_655 ?
O4 C2 O3 126.29(16) . . ?
O4 C2 C2 116.68(18) . 3 ?
O3 C2 C2 117.03(18) . 3 ?
N1 C3 N2 112.37(18) . . ?
N1 C3 H3 123.8 . . ?
N2 C3 H3 123.8 . . ?
C5 C4 N1 110.17(19) . . ?
C5 C4 H4 124.9 . . ?
N1 C4 H4 124.9 . . ?
C4 C5 N2 106.13(19) . . ?
C4 C5 H5 126.9 . . ?
N2 C5 H5 126.9 . . ?
N2 C6 C7 111.72(18) . . ?
N2 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
O5 C7 C6 109.54(18) . . ?
O5 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
O5 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C9 111.53(18) . . ?
O5 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
O5 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N3 C9 C8 112.5(2) . . ?
N3 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
N3 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C3 N1 C4 104.50(17) . . ?
C3 N1 Co1 125.38(14) . . ?
C4 N1 Co1 130.01(14) . . ?
C3 N2 C5 106.83(17) . . ?
C3 N2 C6 125.99(18) . . ?
C5 N2 C6 127.14(19) . . ?
C1 O1 Co1 114.35(11) . . ?
C1 O2 Co1 113.21(12) . 3_655 ?
C2 O3 Co1 114.30(11) . . ?
C2 O4 Co1 113.64(11) . 3 ?
C7 O5 C8 113.31(17) . . ?
O1 Co1 N4 97.54(6) . 3_656 ?
O1 Co1 O3 169.73(5) . . ?
N4 Co1 O3 89.69(6) 3_656 . ?
O1 Co1 N1 90.75(6) . . ?
N4 Co1 N1 94.26(7) 3_656 . ?
O3 Co1 N1 96.00(6) . . ?
O1 Co1 O2 78.53(5) . 3_655 ?
N4 Co1 O2 91.64(6) 3_656 3_655 ?
O3 Co1 O2 94.04(6) . 3_655 ?
N1 Co1 O2 168.37(6) . 3_655 ?
O1 Co1 O4 94.56(6) . 3 ?
N4 Co1 O4 167.52(6) 3_656 3 ?
O3 Co1 O4 77.92(5) . 3 ?
N1 Co1 O4 88.62(6) . 3 ?
O2 Co1 O4 87.76(6) 3_655 3 ?
N4 C10 N3 111.42(18) . . ?
N4 C10 H10 124.3 . . ?
N3 C10 H10 124.3 . . ?
C12 C11 N4 109.73(18) . . ?
C12 C11 H11 125.1 . . ?
N4 C11 H11 125.1 . . ?
C11 C12 N3 106.23(18) . . ?
C11 C12 H12 126.9 . . ?
N3 C12 H12 126.9 . . ?
C10 N3 C12 107.10(16) . . ?
C10 N3 C9 126.67(19) . . ?
C12 N3 C9 126.21(18) . . ?
C10 N4 C11 105.52(16) . . ?
C10 N4 Co1 129.12(13) . 3_656 ?
C11 N4 Co1 125.26(13) . 3_656 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.055

#================END

data_Compound-5
_database_code_depnum_ccdc_archive 'CCDC 682069'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H15 Cu N4 O5'
_chemical_formula_sum            'C15 H15 Cu N4 O5'
_chemical_formula_weight         394.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_hall  '-C 2yc '

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                   17.302(8)
_cell_length_b                   13.499(7)
_cell_length_c                   13.768(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.085(16)
_cell_angle_gamma                90.00
_cell_volume                     3144(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3544
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14778
_diffrn_reflns_av_R_equivalents  0.1299
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3544
_reflns_number_gt                1676
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.1150P)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     SHELXL
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3544
_refine_ls_number_parameters     230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.2152
_refine_ls_wR_factor_gt          0.1695
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_restrained_S_all      0.936
_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
C1 C 0.3525(4) 0.9591(6) 0.3383(6) 0.049(2) Uani 1 1 d . . .
H1 H 0.3296 1.0212 0.3405 0.059 Uiso 1 1 calc R . .
C2 C 0.3187(4) 0.8823(6) 0.2832(6) 0.052(2) Uani 1 1 d . . .
H2 H 0.2691 0.8816 0.2411 0.063 Uiso 1 1 calc R . .
C3 C 0.4346(4) 0.8380(5) 0.3652(5) 0.0386(16) Uani 1 1 d . . .
H3 H 0.4793 0.7997 0.3889 0.046 Uiso 1 1 calc R . .
C4 C 0.3580(4) 0.7033(5) 0.2678(6) 0.0484(19) Uani 1 1 d . . .
H4A H 0.4087 0.6710 0.2724 0.058 Uiso 1 1 calc R . .
H4B H 0.3308 0.7025 0.1986 0.058 Uiso 1 1 calc R . .
C5 C 0.3099(4) 0.6460(5) 0.3287(6) 0.0464(18) Uani 1 1 d . . .
H5A H 0.3104 0.5759 0.3132 0.056 Uiso 1 1 calc R . .
H5B H 0.3318 0.6546 0.3990 0.056 Uiso 1 1 calc R . .
C6 C 0.1813(4) 0.6426(5) 0.3641(6) 0.0492(19) Uani 1 1 d . . .
H6A H 0.1988 0.6637 0.4325 0.059 Uiso 1 1 calc R . .
H6B H 0.1832 0.5708 0.3621 0.059 Uiso 1 1 calc R . .
C7 C 0.0987(4) 0.6777(5) 0.3244(6) 0.0474(19) Uani 1 1 d . . .
H7A H 0.0852 0.6654 0.2535 0.057 Uiso 1 1 calc R . .
H7B H 0.0627 0.6393 0.3549 0.057 Uiso 1 1 calc R . .
C8 C 0.1073(5) 0.8646(6) 0.2921(6) 0.055(2) Uani 1 1 d . . .
H8 H 0.1310 0.8632 0.2374 0.066 Uiso 1 1 calc R . .
C9 C 0.0870(4) 0.9446(6) 0.3363(6) 0.0464(18) Uani 1 1 d . . .
H9 H 0.0946 1.0095 0.3179 0.056 Uiso 1 1 calc R . .
C10 C 0.0536(4) 0.8206(5) 0.4141(5) 0.0335(15) Uani 1 1 d . . .
H10 H 0.0334 0.7818 0.4588 0.040 Uiso 1 1 calc R . .
C11 C 0.1050(3) 1.1390(4) 0.4926(5) 0.0289(14) Uani 1 1 d . . .
C12 C 0.1798(3) 1.1986(4) 0.5032(5) 0.0272(13) Uani 1 1 d . . .
C13 C 0.2502(3) 1.1475(4) 0.5044(4) 0.0261(12) Uani 1 1 d . . .
H13 H 0.2505 1.0787 0.5081 0.031 Uiso 1 1 calc R . .
C14 C 0.3203(3) 1.1976(4) 0.5001(5) 0.0270(14) Uani 1 1 d . . .
C15 C 0.3928(3) 1.1404(5) 0.4915(5) 0.0320(15) Uani 1 1 d . . .
N1 N 0.4267(3) 0.9314(4) 0.3915(4) 0.0383(14) Uani 1 1 d . . .
N2 N 0.3711(3) 0.8054(4) 0.3006(4) 0.0395(14) Uani 1 1 d . . .
N3 N 0.0868(3) 0.7838(4) 0.3424(5) 0.0384(14) Uani 1 1 d . . .
N4 N 0.0527(3) 0.9169(4) 0.4140(4) 0.0346(13) Uani 1 1 d . . .
O1 O 0.2313(3) 0.6834(3) 0.3043(4) 0.0454(13) Uani 1 1 d . . .
O2 O 0.1052(2) 1.0672(3) 0.5540(4) 0.0373(11) Uani 1 1 d . . .
O3 O 0.0488(2) 1.1584(3) 0.4242(3) 0.0368(11) Uani 1 1 d . . .
O4 O 0.4067(2) 1.0606(3) 0.5430(4) 0.0348(11) Uani 1 1 d . . .
O5 O 0.4327(2) 1.1664(3) 0.4314(3) 0.0358(11) Uani 1 1 d . . .
Cu1 Cu 0.5000 1.0000 0.5000 0.0295(3) Uani 1 2 d S . .
Cu2 Cu 0.0000 1.0000 0.5000 0.0299(3) Uani 1 2 d S . .


_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 C2 1.344(10) . ?
C1 N1 1.391(8) . ?
C1 H1 0.9300 . ?
C2 N2 1.365(9) . ?
C2 H2 0.9300 . ?
C3 N1 1.326(8) . ?
C3 N2 1.336(8) . ?
C3 H3 0.9300 . ?
C4 N2 1.453(8) . ?
C4 C5 1.513(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O1 1.424(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O1 1.424(8) . ?
C6 C7 1.496(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.475(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.323(10) . ?
C8 N3 1.378(9) . ?
C8 H8 0.9300 . ?
C9 N4 1.378(9) . ?
C9 H9 0.9300 . ?
C10 N4 1.300(8) . ?
C10 N3 1.338(8) . ?
C10 H10 0.9300 . ?
C11 O3 1.232(7) . ?
C11 O2 1.286(7) . ?
C11 C12 1.504(8) . ?
C12 C13 1.396(8) . ?
C12 C14 1.402(8) 7_576 ?
C13 C14 1.402(8) . ?
C13 H13 0.9300 . ?
C14 C12 1.402(8) 7_576 ?
C14 C15 1.498(8) . ?
C15 O5 1.234(8) . ?
C15 O4 1.284(8) . ?
N1 Cu1 1.976(5) . ?
N4 Cu2 1.986(5) . ?
O2 Cu2 2.030(4) . ?
O4 Cu1 2.006(4) . ?
Cu1 N1 1.976(5) 5_676 ?
Cu1 O4 2.006(4) 5_676 ?
Cu2 N4 1.986(5) 5_576 ?
Cu2 O2 2.030(4) 5_576 ?

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
C2 C1 N1 109.5(6) . . ?
C2 C1 H1 125.3 . . ?
N1 C1 H1 125.3 . . ?
C1 C2 N2 107.1(6) . . ?
C1 C2 H2 126.4 . . ?
N2 C2 H2 126.4 . . ?
N1 C3 N2 112.2(6) . . ?
N1 C3 H3 123.9 . . ?
N2 C3 H3 123.9 . . ?
N2 C4 C5 112.4(6) . . ?
N2 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
O1 C5 C4 107.3(6) . . ?
O1 C5 H5A 110.3 . . ?
C4 C5 H5A 110.3 . . ?
O1 C5 H5B 110.3 . . ?
C4 C5 H5B 110.3 . . ?
H5A C5 H5B 108.5 . . ?
O1 C6 C7 108.4(6) . . ?
O1 C6 H6A 110.0 . . ?
C7 C6 H6A 110.0 . . ?
O1 C6 H6B 110.0 . . ?
C7 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N3 C7 C6 113.7(6) . . ?
N3 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
N3 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 N3 107.0(7) . . ?
C9 C8 H8 126.5 . . ?
N3 C8 H8 126.5 . . ?
C8 C9 N4 109.6(7) . . ?
C8 C9 H9 125.2 . . ?
N4 C9 H9 125.2 . . ?
N4 C10 N3 112.2(6) . . ?
N4 C10 H10 123.9 . . ?
N3 C10 H10 123.9 . . ?
O3 C11 O2 123.7(5) . . ?
O3 C11 C12 119.1(6) . . ?
O2 C11 C12 117.1(5) . . ?
C13 C12 C14 119.3(5) . 7_576 ?
C13 C12 C11 117.9(5) . . ?
C14 C12 C11 122.4(5) 7_576 . ?
C12 C13 C14 121.4(5) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C12 119.2(5) . 7_576 ?
C13 C14 C15 120.0(5) . . ?
C12 C14 C15 120.6(5) 7_576 . ?
O5 C15 O4 122.8(5) . . ?
O5 C15 C14 120.0(6) . . ?
O4 C15 C14 116.9(6) . . ?
C3 N1 C1 104.4(6) . . ?
C3 N1 Cu1 124.5(5) . . ?
C1 N1 Cu1 130.3(5) . . ?
C3 N2 C2 106.8(6) . . ?
C3 N2 C4 124.9(6) . . ?
C2 N2 C4 127.8(6) . . ?
C10 N3 C8 105.8(6) . . ?
C10 N3 C7 125.5(6) . . ?
C8 N3 C7 128.7(6) . . ?
C10 N4 C9 105.4(6) . . ?
C10 N4 Cu2 124.8(5) . . ?
C9 N4 Cu2 129.4(5) . . ?
C6 O1 C5 113.1(6) . . ?
C11 O2 Cu2 102.6(4) . . ?
C15 O4 Cu1 104.4(4) . . ?
N1 Cu1 N1 180 . 5_676 ?
N1 Cu1 O4 90.8(2) . 5_676 ?
N1 Cu1 O4 89.2(2) 5_676 5_676 ?
N1 Cu1 O4 89.2(2) . . ?
N1 Cu1 O4 90.8(2) 5_676 . ?
O4 Cu1 O4 180 5_676 . ?
N4 Cu2 N4 180 5_576 . ?
N4 Cu2 O2 91.00(19) 5_576 . ?
N4 Cu2 O2 89.0(2) . . ?
N4 Cu2 O2 89.0(2) 5_576 5_576 ?
N4 Cu2 O2 91.00(19) . 5_576 ?
O2 Cu2 O2 180 . 5_576 ?

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
N1 C1 C2 N2 -0.1(10) . . . . ?
N2 C4 C5 O1 70.2(7) . . . . ?
O1 C6 C7 N3 -70.9(8) . . . . ?
N3 C8 C9 N4 -0.6(9) . . . . ?
O3 C11 C12 C13 -124.1(6) . . . . ?
O2 C11 C12 C13 52.9(8) . . . . ?
O3 C11 C12 C14 48.1(9) . . . 7_576 ?
O2 C11 C12 C14 -134.9(6) . . . 7_576 ?
C14 C12 C13 C14 -1.4(10) 7_576 . . . ?
C11 C12 C13 C14 171.0(6) . . . . ?
C12 C13 C14 C12 1.4(10) . . . 7_576 ?
C12 C13 C14 C15 -174.1(6) . . . . ?
C13 C14 C15 O5 134.5(6) . . . . ?
C12 C14 C15 O5 -40.9(9) 7_576 . . . ?
C13 C14 C15 O4 -40.1(8) . . . . ?
C12 C14 C15 O4 144.5(6) 7_576 . . . ?
N2 C3 N1 C1 -0.5(8) . . . . ?
N2 C3 N1 Cu1 170.3(5) . . . . ?
C2 C1 N1 C3 0.3(9) . . . . ?
C2 C1 N1 Cu1 -169.6(6) . . . . ?
N1 C3 N2 C2 0.4(9) . . . . ?
N1 C3 N2 C4 -172.0(6) . . . . ?
C1 C2 N2 C3 -0.2(9) . . . . ?
C1 C2 N2 C4 171.9(7) . . . . ?
C5 C4 N2 C3 94.1(8) . . . . ?
C5 C4 N2 C2 -76.7(9) . . . . ?
N4 C10 N3 C8 -1.0(8) . . . . ?
N4 C10 N3 C7 178.3(6) . . . . ?
C9 C8 N3 C10 1.0(8) . . . . ?
C9 C8 N3 C7 -178.3(7) . . . . ?
C6 C7 N3 C10 -100.8(8) . . . . ?
C6 C7 N3 C8 78.4(10) . . . . ?
N3 C10 N4 C9 0.7(8) . . . . ?
N3 C10 N4 Cu2 174.1(4) . . . . ?
C8 C9 N4 C10 0.0(9) . . . . ?
C8 C9 N4 Cu2 -173.0(5) . . . . ?
C7 C6 O1 C5 -173.4(6) . . . . ?
C4 C5 O1 C6 -174.0(6) . . . . ?
O3 C11 O2 Cu2 4.0(7) . . . . ?
C12 C11 O2 Cu2 -172.9(4) . . . . ?
O5 C15 O4 Cu1 -0.4(7) . . . . ?
C14 C15 O4 Cu1 174.1(4) . . . . ?
C3 N1 Cu1 O4 42.2(6) . . . 5_676 ?
C1 N1 Cu1 O4 -149.7(7) . . . 5_676 ?
C3 N1 Cu1 O4 -137.8(6) . . . . ?
C1 N1 Cu1 O4 30.3(7) . . . . ?
C15 O4 Cu1 N1 -87.8(4) . . . . ?
C15 O4 Cu1 N1 92.2(4) . . . 5_676 ?
C10 N4 Cu2 O2 123.0(6) . . . . ?
C9 N4 Cu2 O2 -65.2(6) . . . . ?
C10 N4 Cu2 O2 -57.0(6) . . . 5_576 ?
C9 N4 Cu2 O2 114.8(6) . . . 5_576 ?
C11 O2 Cu2 N4 -91.4(4) . . . 5_576 ?
C11 O2 Cu2 N4 88.6(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         2.815
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.153

#==============END

data_Compound-6
_database_code_depnum_ccdc_archive 'CCDC 682070'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 Co2 N8 O10, H2 O '
_chemical_formula_sum            'C30 H32 Co2 N8 O11'
_chemical_formula_weight         798.50

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'

_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                   18.390(3)
_cell_length_b                   14.018(3)
_cell_length_c                   13.338(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.919(12)
_cell_angle_gamma                90.00
_cell_volume                     3364.3(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7608
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.180
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32024
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7608
_reflns_number_gt                5640
_reflns_threshold_expression     >2sigma(I)

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

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

The water H atoms could not be positioned reliably.
According to the results of elemental analyses and the reasonable
thermal parameters for O1W and O2W, the two water O atoms, O1W and O2W,
were assigned 0.6 and 0.4 occupancies, respectively.
;

_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)+(0.0532P)²+1.7444P] 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         7608
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1031
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4924(2) -0.0184(2) 0.2805(3) 0.0412(8) Uani 1 1 d . . .
H1 H 0.5244 0.0265 0.2618 0.049 Uiso 1 1 calc R . .
C2 C 0.49601(18) -0.0555(2) 0.3744(2) 0.0364(7) Uani 1 1 d . . .
H2 H 0.5314 -0.0400 0.4326 0.044 Uiso 1 1 calc R . .
C3 C 0.40227(19) -0.1201(2) 0.2757(2) 0.0345(7) Uani 1 1 d . . .
H3 H 0.3605 -0.1573 0.2513 0.041 Uiso 1 1 calc R . .
C4 C 0.4010(3) -0.0372(2) 0.1101(3) 0.0588(12) Uani 1 1 d . . .
H4A H 0.3778 -0.0937 0.0755 0.071 Uiso 1 1 calc R . .
H4B H 0.4404 -0.0173 0.0765 0.071 Uiso 1 1 calc R . .
C5 C 0.3446(3) 0.0408(2) 0.1028(3) 0.0551(11) Uani 1 1 d . . .
H5A H 0.3236 0.0550 0.0315 0.066 Uiso 1 1 calc R . .
H5B H 0.3046 0.0213 0.1358 0.066 Uiso 1 1 calc R . .
C6 C 0.3315(2) 0.2001(2) 0.1489(3) 0.0470(9) Uani 1 1 d . . .
H6A H 0.2976 0.1889 0.1945 0.056 Uiso 1 1 calc R . .
H6B H 0.3027 0.2091 0.0800 0.056 Uiso 1 1 calc R . .
C7 C 0.3783(2) 0.2864(2) 0.1826(3) 0.0485(9) Uani 1 1 d . . .
H7A H 0.4141 0.2936 0.1390 0.058 Uiso 1 1 calc R . .
H7B H 0.3466 0.3424 0.1733 0.058 Uiso 1 1 calc R . .
C8 C 0.3962(2) 0.3218(3) 0.3720(3) 0.0609(11) Uani 1 1 d . . .
H8 H 0.3524 0.3553 0.3714 0.073 Uiso 1 1 calc R . .
C9 C 0.4497(2) 0.3031(3) 0.4539(3) 0.0494(9) Uani 1 1 d . . .
H9 H 0.4495 0.3223 0.5206 0.059 Uiso 1 1 calc R . .
C10 C 0.48390(17) 0.24054(19) 0.3240(2) 0.0297(6) Uani 1 1 d . . .
H10 H 0.5110 0.2084 0.2829 0.036 Uiso 1 1 calc R . .
C11 C 0.64807(16) 0.34250(18) 0.6528(2) 0.0237(6) Uani 1 1 d . . .
C12 C 0.70352(15) 0.41185(16) 0.71302(19) 0.0203(5) Uani 1 1 d . . .
C13 C 0.74841(15) 0.46506(17) 0.66154(19) 0.0215(5) Uani 1 1 d . . .
H13 H 0.7493 0.4501 0.5939 0.026 Uiso 1 1 calc R . .
C14 C 0.79205(15) 0.54026(17) 0.70899(19) 0.0200(5) Uani 1 1 d . . .
C15 C 0.79083(15) 0.56287(16) 0.81062(19) 0.0205(5) Uani 1 1 d . . .
C16 C 0.74718(15) 0.50816(17) 0.86219(19) 0.0214(5) Uani 1 1 d . . .
H16 H 0.7462 0.5234 0.9298 0.026 Uiso 1 1 calc R . .
C17 C 0.70520(15) 0.43198(17) 0.81673(19) 0.0204(5) Uani 1 1 d . . .
C18 C 0.66699(15) 0.36893(18) 0.8807(2) 0.0237(6) Uani 1 1 d . . .
C19 C 0.83729(17) 0.59389(19) 0.6454(2) 0.0282(6) Uani 1 1 d . . .
C20 C 0.83566(16) 0.64405(18) 0.8654(2) 0.0257(6) Uani 1 1 d . . .
C21 C 1.0153(2) 0.8309(3) 0.5589(3) 0.0500(9) Uani 1 1 d . . .
H21 H 1.0163 0.8510 0.4928 0.060 Uiso 1 1 calc R . .
C22 C 1.0617(2) 0.8609(3) 0.6452(3) 0.0581(11) Uani 1 1 d . . .
H22 H 1.1001 0.9048 0.6496 0.070 Uiso 1 1 calc R . .
C23 C 0.98414(17) 0.7576(2) 0.6855(2) 0.0306(6) Uani 1 1 d . . .
H23 H 0.9601 0.7175 0.7237 0.037 Uiso 1 1 calc R . .
C24 C 1.0750(2) 0.8210(2) 0.8350(3) 0.0454(8) Uani 1 1 d . . .
H24A H 1.0378 0.8071 0.8750 0.054 Uiso 1 1 calc R . .
H24B H 1.0923 0.8857 0.8506 0.054 Uiso 1 1 calc R . .
C25 C 1.1394(2) 0.7531(2) 0.8654(3) 0.0516(9) Uani 1 1 d . . .
H25A H 1.1763 0.7644 0.8243 0.062 Uiso 1 1 calc R . .
H25B H 1.1626 0.7619 0.9370 0.062 Uiso 1 1 calc R . .
C26 C 1.1657(3) 0.5886(3) 0.8808(3) 0.0621(12) Uani 1 1 d . . .
H26A H 1.1849 0.5935 0.9540 0.075 Uiso 1 1 calc R . .
H26B H 1.2065 0.5975 0.8460 0.075 Uiso 1 1 calc R . .
C27 C 1.1307(3) 0.4919(3) 0.8550(3) 0.0594(12) Uani 1 1 d . . .
H27A H 1.1624 0.4435 0.8936 0.071 Uiso 1 1 calc R . .
H27B H 1.0833 0.4899 0.8759 0.071 Uiso 1 1 calc R . .
C28 C 1.0831(4) 0.5250(3) 0.6676(3) 0.0889(19) Uani 1 1 d . . .
H28 H 1.0604 0.5835 0.6732 0.107 Uiso 1 1 calc R . .
C29 C 1.0862(3) 0.4785(3) 0.5803(3) 0.0779(16) Uani 1 1 d . . .
H29 H 1.0671 0.5009 0.5145 0.093 Uiso 1 1 calc R . .
C30 C 1.13986(19) 0.3909(2) 0.7041(3) 0.0377(7) Uani 1 1 d . . .
H30 H 1.1641 0.3401 0.7416 0.045 Uiso 1 1 calc R . .
N1 N 0.43877(14) -0.12022(16) 0.37090(18) 0.0292(5) Uani 1 1 d . . .
N2 N 0.43228(17) -0.05981(17) 0.21758(19) 0.0374(6) Uani 1 1 d . . .
N3 N 0.41813(15) 0.28235(18) 0.2895(2) 0.0370(6) Uani 1 1 d . . .
N4 N 0.50534(14) 0.25090(17) 0.42458(18) 0.0290(5) Uani 1 1 d . . .
N5 N 0.96612(14) 0.76580(17) 0.58465(19) 0.0317(5) Uani 1 1 d . . .
N6 N 1.04095(15) 0.81395(18) 0.7254(2) 0.0363(6) Uani 1 1 d . . .
N7 N 1.11933(18) 0.46989(19) 0.7462(2) 0.0446(7) Uani 1 1 d . . .
N8 N 1.12190(16) 0.39296(17) 0.6033(2) 0.0360(6) Uani 1 1 d . . .
O1 O 0.38042(13) 0.12181(15) 0.15168(18) 0.0417(5) Uani 1 1 d . . .
O2 O 0.67390(12) 0.28265(14) 0.59673(16) 0.0338(5) Uani 1 1 d . . .
O3 O 0.58210(11) 0.34987(15) 0.65669(16) 0.0356(5) Uani 1 1 d . . .
O4 O 0.66536(14) 0.28170(13) 0.86825(16) 0.0383(5) Uani 1 1 d . . .
O5 O 0.63907(12) 0.40889(14) 0.95059(15) 0.0333(5) Uani 1 1 d . . .
O6 O 0.80789(13) 0.66876(15) 0.60037(17) 0.0395(5) Uani 1 1 d . . .
O7 O 0.89719(13) 0.56066(16) 0.63414(18) 0.0432(6) Uani 1 1 d . . .
O8 O 0.89200(13) 0.67220(16) 0.83850(17) 0.0426(6) Uani 1 1 d . . .
O9 O 0.81103(12) 0.68043(13) 0.94048(16) 0.0334(5) Uani 1 1 d . . .
O10 O 1.11039(14) 0.65938(15) 0.84881(18) 0.0447(6) Uani 1 1 d . . .
Co1 Co 0.59598(2) 0.19769(2) 0.51902(3) 0.02256(10) Uani 1 1 d . . .
Co2 Co 0.87159(2) 0.70927(2) 0.50147(3) 0.02511(11) Uani 1 1 d . . .
O1W O 0.6798(4) 0.5710(5) 1.1054(5) 0.110(2) Uiso 0.60 1 d P . .
O2W O 0.2235(8) -0.1386(10) 0.1081(10) 0.144(5) Uiso 0.40 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.346(5) . ?
C1 N2 1.371(4) . ?
C1 H1 0.9300 . ?
C2 N1 1.383(4) . ?
C2 H2 0.9300 . ?
C3 N1 1.308(4) . ?
C3 N2 1.340(4) . ?
C3 H3 0.9300 . ?
C4 N2 1.464(4) . ?
C4 C5 1.496(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O1 1.404(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O1 1.414(4) . ?
C6 C7 1.500(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.463(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.337(5) . ?
C8 N3 1.366(4) . ?
C8 H8 0.9300 . ?
C9 N4 1.378(4) . ?
C9 H9 0.9300 . ?
C10 N4 1.325(4) . ?
C10 N3 1.337(4) . ?
C10 H10 0.9300 . ?
C11 O3 1.229(3) . ?
C11 O2 1.279(3) . ?
C11 C12 1.514(4) . ?
C12 C13 1.394(3) . ?
C12 C17 1.406(4) . ?
C13 C14 1.395(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(3) . ?
C14 C19 1.506(4) . ?
C15 C16 1.391(4) . ?
C15 C20 1.503(4) . ?
C16 C17 1.382(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.500(3) . ?
C18 O4 1.234(3) . ?
C18 O5 1.282(3) . ?
C19 O7 1.234(4) . ?
C19 O6 1.273(4) . ?
C20 O8 1.229(3) . ?
C20 O9 1.287(3) . ?
C21 C22 1.351(5) . ?
C21 N5 1.377(4) . ?
C21 H21 0.9300 . ?
C22 N6 1.374(4) . ?
C22 H22 0.9300 . ?
C23 N5 1.322(4) . ?
C23 N6 1.330(4) . ?
C23 H23 0.9300 . ?
C24 N6 1.470(4) . ?
C24 C25 1.507(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 O10 1.418(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 O10 1.422(4) . ?
C26 C27 1.509(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N7 1.457(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.346(5) . ?
C28 N7 1.360(5) . ?
C28 H28 0.9300 . ?
C29 N8 1.371(4) . ?
C29 H29 0.9300 . ?
C30 N8 1.317(4) . ?
C30 N7 1.331(4) . ?
C30 H30 0.9300 . ?
N1 Co1 2.033(2) 3_656 ?
N4 Co1 2.014(3) . ?
N5 Co2 2.021(3) . ?
N8 Co2 2.022(3) 3_766 ?
O2 Co1 1.983(2) . ?
O5 Co1 1.9980(19) 4_566 ?
O6 Co2 2.018(2) . ?
O9 Co2 1.980(2) 4_576 ?
Co1 O5 1.9980(19) 4_565 ?
Co1 N1 2.033(2) 3_656 ?
Co2 O9 1.980(2) 4_575 ?
Co2 N8 2.022(3) 3_766 ?

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
C2 C1 N2 106.6(3) . . ?
C2 C1 H1 126.7 . . ?
N2 C1 H1 126.7 . . ?
C1 C2 N1 109.3(3) . . ?
C1 C2 H2 125.3 . . ?
N1 C2 H2 125.3 . . ?
N1 C3 N2 111.9(3) . . ?
N1 C3 H3 124.1 . . ?
N2 C3 H3 124.1 . . ?
N2 C4 C5 110.5(3) . . ?
N2 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
N2 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
O1 C5 C4 107.9(3) . . ?
O1 C5 H5A 110.1 . . ?
C4 C5 H5A 110.1 . . ?
O1 C5 H5B 110.1 . . ?
C4 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
O1 C6 C7 107.2(3) . . ?
O1 C6 H6A 110.3 . . ?
C7 C6 H6A 110.3 . . ?
O1 C6 H6B 110.3 . . ?
C7 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?
N3 C7 C6 113.7(3) . . ?
N3 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
N3 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 N3 106.7(3) . . ?
C9 C8 H8 126.6 . . ?
N3 C8 H8 126.6 . . ?
C8 C9 N4 109.7(3) . . ?
C8 C9 H9 125.1 . . ?
N4 C9 H9 125.1 . . ?
N4 C10 N3 111.1(3) . . ?
N4 C10 H10 124.5 . . ?
N3 C10 H10 124.5 . . ?
O3 C11 O2 124.6(3) . . ?
O3 C11 C12 119.1(2) . . ?
O2 C11 C12 116.1(2) . . ?
C13 C12 C17 118.8(2) . . ?
C13 C12 C11 119.0(2) . . ?
C17 C12 C11 121.8(2) . . ?
C12 C13 C14 121.6(2) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C13 C14 C15 119.3(2) . . ?
C13 C14 C19 117.1(2) . . ?
C15 C14 C19 123.7(2) . . ?
C16 C15 C14 118.8(2) . . ?
C16 C15 C20 119.5(2) . . ?
C14 C15 C20 121.7(2) . . ?
C17 C16 C15 122.4(2) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C12 118.9(2) . . ?
C16 C17 C18 119.4(2) . . ?
C12 C17 C18 121.6(2) . . ?
O4 C18 O5 121.9(2) . . ?
O4 C18 C17 120.6(2) . . ?
O5 C18 C17 117.5(2) . . ?
O7 C19 O6 123.8(3) . . ?
O7 C19 C14 119.4(3) . . ?
O6 C19 C14 116.6(3) . . ?
O8 C20 O9 123.6(3) . . ?
O8 C20 C15 120.8(2) . . ?
O9 C20 C15 115.6(2) . . ?
C22 C21 N5 109.0(3) . . ?
C22 C21 H21 125.5 . . ?
N5 C21 H21 125.5 . . ?
C21 C22 N6 106.6(3) . . ?
C21 C22 H22 126.7 . . ?
N6 C22 H22 126.7 . . ?
N5 C23 N6 111.5(3) . . ?
N5 C23 H23 124.2 . . ?
N6 C23 H23 124.2 . . ?
N6 C24 C25 112.0(3) . . ?
N6 C24 H24A 109.2 . . ?
C25 C24 H24A 109.2 . . ?
N6 C24 H24B 109.2 . . ?
C25 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
O10 C25 C24 107.1(3) . . ?
O10 C25 H25A 110.3 . . ?
C24 C25 H25A 110.3 . . ?
O10 C25 H25B 110.3 . . ?
C24 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
O10 C26 C27 108.3(4) . . ?
O10 C26 H26A 110.0 . . ?
C27 C26 H26A 110.0 . . ?
O10 C26 H26B 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
N7 C27 C26 112.6(3) . . ?
N7 C27 H27A 109.1 . . ?
C26 C27 H27A 109.1 . . ?
N7 C27 H27B 109.1 . . ?
C26 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C29 C28 N7 106.8(3) . . ?
C29 C28 H28 126.6 . . ?
N7 C28 H28 126.6 . . ?
C28 C29 N8 109.5(3) . . ?
C28 C29 H29 125.3 . . ?
N8 C29 H29 125.3 . . ?
N8 C30 N7 112.3(3) . . ?
N8 C30 H30 123.9 . . ?
N7 C30 H30 123.9 . . ?
C3 N1 C2 105.5(2) . . ?
C3 N1 Co1 121.8(2) . 3_656 ?
C2 N1 Co1 132.6(2) . 3_656 ?
C3 N2 C1 106.8(3) . . ?
C3 N2 C4 125.2(3) . . ?
C1 N2 C4 127.7(3) . . ?
C10 N3 C8 107.3(3) . . ?
C10 N3 C7 126.0(3) . . ?
C8 N3 C7 126.7(3) . . ?
C10 N4 C9 105.2(3) . . ?
C10 N4 Co1 128.85(19) . . ?
C9 N4 Co1 125.9(2) . . ?
C23 N5 C21 105.8(3) . . ?
C23 N5 Co2 122.1(2) . . ?
C21 N5 Co2 131.1(2) . . ?
C23 N6 C22 107.1(3) . . ?
C23 N6 C24 125.2(3) . . ?
C22 N6 C24 127.7(3) . . ?
C30 N7 C28 106.5(3) . . ?
C30 N7 C27 127.0(3) . . ?
C28 N7 C27 126.5(3) . . ?
C30 N8 C29 104.8(3) . . ?
C30 N8 Co2 130.7(2) . 3_766 ?
C29 N8 Co2 124.0(2) . 3_766 ?
C5 O1 C6 112.3(3) . . ?
C11 O2 Co1 112.59(18) . . ?
C18 O5 Co1 105.16(16) . 4_566 ?
C19 O6 Co2 107.05(19) . . ?
C20 O9 Co2 111.76(18) . 4_576 ?
C25 O10 C26 112.2(3) . . ?
O2 Co1 O5 112.09(9) . 4_565 ?
O2 Co1 N4 121.33(10) . . ?
O5 Co1 N4 110.26(9) 4_565 . ?
O2 Co1 N1 104.15(9) . 3_656 ?
O5 Co1 N1 98.28(9) 4_565 3_656 ?
N4 Co1 N1 107.86(10) . 3_656 ?
O9 Co2 O6 97.76(9) 4_575 . ?
O9 Co2 N5 105.45(10) 4_575 . ?
O6 Co2 N5 107.52(10) . . ?
O9 Co2 N8 112.21(10) 4_575 3_766 ?
O6 Co2 N8 112.18(10) . 3_766 ?
N5 Co2 N8 119.36(11) . 3_766 ?

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 C1 C2 N1 0.3(4) . . . . ?
N2 C4 C5 O1 60.5(4) . . . . ?
O1 C6 C7 N3 -65.5(4) . . . . ?
N3 C8 C9 N4 -0.7(5) . . . . ?
O3 C11 C12 C13 -124.2(3) . . . . ?
O2 C11 C12 C13 52.3(3) . . . . ?
O3 C11 C12 C17 48.5(4) . . . . ?
O2 C11 C12 C17 -135.0(3) . . . . ?
C17 C12 C13 C14 -3.0(4) . . . . ?
C11 C12 C13 C14 169.9(2) . . . . ?
C12 C13 C14 C15 0.0(4) . . . . ?
C12 C13 C14 C19 -178.9(2) . . . . ?
C13 C14 C15 C16 1.4(4) . . . . ?
C19 C14 C15 C16 -179.8(3) . . . . ?
C13 C14 C15 C20 -179.0(2) . . . . ?
C19 C14 C15 C20 -0.1(4) . . . . ?
C14 C15 C16 C17 0.3(4) . . . . ?
C20 C15 C16 C17 -179.4(2) . . . . ?
C15 C16 C17 C12 -3.3(4) . . . . ?
C15 C16 C17 C18 172.5(2) . . . . ?
C13 C12 C17 C16 4.5(4) . . . . ?
C11 C12 C17 C16 -168.1(2) . . . . ?
C13 C12 C17 C18 -171.1(2) . . . . ?
C11 C12 C17 C18 16.2(4) . . . . ?
C16 C17 C18 O4 -139.6(3) . . . . ?
C12 C17 C18 O4 36.1(4) . . . . ?
C16 C17 C18 O5 37.8(4) . . . . ?
C12 C17 C18 O5 -146.6(3) . . . . ?
C13 C14 C19 O7 -81.1(4) . . . . ?
C15 C14 C19 O7 100.0(3) . . . . ?
C13 C14 C19 O6 94.1(3) . . . . ?
C15 C14 C19 O6 -84.8(3) . . . . ?
C16 C15 C20 O8 154.8(3) . . . . ?
C14 C15 C20 O8 -24.8(4) . . . . ?
C16 C15 C20 O9 -25.1(4) . . . . ?
C14 C15 C20 O9 155.3(3) . . . . ?
N5 C21 C22 N6 -0.1(5) . . . . ?
N6 C24 C25 O10 -63.4(4) . . . . ?
O10 C26 C27 N7 75.5(4) . . . . ?
N7 C28 C29 N8 2.1(7) . . . . ?
N2 C3 N1 C2 0.2(3) . . . . ?
N2 C3 N1 Co1 176.15(19) . . . 3_656 ?
C1 C2 N1 C3 -0.3(3) . . . . ?
C1 C2 N1 Co1 -175.6(2) . . . 3_656 ?
N1 C3 N2 C1 0.0(4) . . . . ?
N1 C3 N2 C4 -174.5(3) . . . . ?
C2 C1 N2 C3 -0.1(4) . . . . ?
C2 C1 N2 C4 174.2(3) . . . . ?
C5 C4 N2 C3 85.1(4) . . . . ?
C5 C4 N2 C1 -88.3(5) . . . . ?
N4 C10 N3 C8 0.1(4) . . . . ?
N4 C10 N3 C7 178.9(3) . . . . ?
C9 C8 N3 C10 0.4(5) . . . . ?
C9 C8 N3 C7 -178.4(3) . . . . ?
C6 C7 N3 C10 85.0(4) . . . . ?
C6 C7 N3 C8 -96.4(4) . . . . ?
N3 C10 N4 C9 -0.6(3) . . . . ?
N3 C10 N4 Co1 176.4(2) . . . . ?
C8 C9 N4 C10 0.8(4) . . . . ?
C8 C9 N4 Co1 -176.3(3) . . . . ?
N6 C23 N5 C21 0.6(4) . . . . ?
N6 C23 N5 Co2 -168.8(2) . . . . ?
C22 C21 N5 C23 -0.3(4) . . . . ?
C22 C21 N5 Co2 167.8(3) . . . . ?
N5 C23 N6 C22 -0.7(4) . . . . ?
N5 C23 N6 C24 -179.3(3) . . . . ?
C21 C22 N6 C23 0.4(4) . . . . ?
C21 C22 N6 C24 179.0(3) . . . . ?
C25 C24 N6 C23 91.9(4) . . . . ?
C25 C24 N6 C22 -86.4(4) . . . . ?
N8 C30 N7 C28 2.6(5) . . . . ?
N8 C30 N7 C27 -179.6(4) . . . . ?
C29 C28 N7 C30 -2.8(6) . . . . ?
C29 C28 N7 C27 179.4(5) . . . . ?
C26 C27 N7 C30 129.3(4) . . . . ?
C26 C27 N7 C28 -53.2(6) . . . . ?
N7 C30 N8 C29 -1.3(5) . . . . ?
N7 C30 N8 Co2 -172.8(2) . . . 3_766 ?
C28 C29 N8 C30 -0.5(6) . . . . ?
C28 C29 N8 Co2 171.7(4) . . . 3_766 ?
C4 C5 O1 C6 -180.0(3) . . . . ?
C7 C6 O1 C5 -168.2(3) . . . . ?
O3 C11 O2 Co1 -2.3(4) . . . . ?
C12 C11 O2 Co1 -178.60(17) . . . . ?
O4 C18 O5 Co1 -1.6(3) . . . 4_566 ?
C17 C18 O5 Co1 -178.9(2) . . . 4_566 ?
O7 C19 O6 Co2 5.7(4) . . . . ?
C14 C19 O6 Co2 -169.25(19) . . . . ?
O8 C20 O9 Co2 3.1(4) . . . 4_576 ?
C15 C20 O9 Co2 -176.99(17) . . . 4_576 ?
C24 C25 O10 C26 -176.5(3) . . . . ?
C27 C26 O10 C25 -177.0(3) . . . . ?
C11 O2 Co1 O5 -170.37(18) . . . 4_565 ?
C11 O2 Co1 N4 56.4(2) . . . . ?
C11 O2 Co1 N1 -65.1(2) . . . 3_656 ?
C10 N4 Co1 O2 116.8(2) . . . . ?
C9 N4 Co1 O2 -66.7(3) . . . . ?
C10 N4 Co1 O5 -17.1(3) . . . 4_565 ?
C9 N4 Co1 O5 159.3(3) . . . 4_565 ?
C10 N4 Co1 N1 -123.4(2) . . . 3_656 ?
C9 N4 Co1 N1 53.0(3) . . . 3_656 ?
C19 O6 Co2 O9 177.44(19) . . . 4_575 ?
C19 O6 Co2 N5 -73.6(2) . . . . ?
C19 O6 Co2 N8 59.6(2) . . . 3_766 ?
C23 N5 Co2 O9 115.0(2) . . . 4_575 ?
C21 N5 Co2 O9 -51.4(3) . . . 4_575 ?
C23 N5 Co2 O6 11.5(3) . . . . ?
C21 N5 Co2 O6 -155.0(3) . . . . ?
C23 N5 Co2 N8 -117.7(2) . . . 3_766 ?
C21 N5 Co2 N8 75.9(3) . . . 3_766 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.074

#=================END

data_Compound-7
_database_code_depnum_ccdc_archive 'CCDC 682071'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H36 Cu5 N8 O22 '
_chemical_formula_sum            'C52 H48 Cu5 N8 O22'
_chemical_formula_weight         1454.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_hall  '-P 2ybc '

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

_cell_length_a                   13.542(5)
_cell_length_b                   16.939(5)
_cell_length_c                   13.351(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.484(13)
_cell_angle_gamma                90.00
_cell_volume                     2829.8(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6417
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1474
_exptl_absorpt_coefficient_mu    1.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25871
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6417
_reflns_number_gt                5369
_reflns_threshold_expression     >2sigma(I)

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

_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.
To obtain a resonable geometry for water molecule, the bond length of
O1W-H1A (O1W-H1B) and the distance of H1A to H1B were
restrained to 0.89 and 1.44 Å, respectively.
Some atoms of the BIE ligand were disordered and
refined with isotropic temperature parameters. The C20, C21 and O10 atoms
have been allowed the same 0.78 occupancies, and the atoms C20', C21'and O10'
have been allowed the same 0.22 occupancies.
;

_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)+(0.0456P)²+4.3660P] 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         6417
_refine_ls_number_parameters     383
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
C1 C 0.0423(2) 0.21520(17) 0.3001(3) 0.0261(6) Uani 1 1 d . . .
H1 H -0.0295 0.2061 0.2857 0.031 Uiso 1 1 calc R . .
C2 C 0.0927(2) 0.28022(17) 0.3611(3) 0.0266(6) Uani 1 1 d . . .
C3 C 0.2012(2) 0.29205(17) 0.3852(3) 0.0308(7) Uani 1 1 d . . .
H3 H 0.2361 0.3350 0.4273 0.037 Uiso 1 1 calc R . .
C4 C 0.2571(2) 0.23997(19) 0.3465(3) 0.0341(7) Uani 1 1 d . . .
H4 H 0.3298 0.2475 0.3643 0.041 Uiso 1 1 calc R . .
C5 C 0.2056(2) 0.17658(18) 0.2815(3) 0.0303(7) Uani 1 1 d . . .
H5 H 0.2426 0.1433 0.2526 0.036 Uiso 1 1 calc R . .
C6 C 0.0981(2) 0.16357(16) 0.2602(2) 0.0246(6) Uani 1 1 d . . .
C7 C 0.0381(2) 0.09546(17) 0.1920(2) 0.0252(6) Uani 1 1 d . . .
C8 C 0.0279(3) 0.33739(18) 0.3981(3) 0.0304(7) Uani 1 1 d . . .
C9 C -0.3515(3) 0.3433(2) 0.5162(3) 0.0347(7) Uani 1 1 d . . .
C10 C -0.4013(2) 0.36059(19) 0.5967(3) 0.0301(6) Uani 1 1 d . . .
C11 C -0.4999(2) 0.39744(18) 0.5617(3) 0.0278(6) Uani 1 1 d . . .
H11 H -0.5349 0.4093 0.4886 0.033 Uiso 1 1 calc R . .
C12 C -0.5477(2) 0.41706(18) 0.6339(3) 0.0269(6) Uani 1 1 d . . .
C13 C -0.6509(2) 0.46253(17) 0.5942(2) 0.0260(6) Uani 1 1 d . . .
C14 C -0.4983(3) 0.3950(2) 0.7413(3) 0.0411(8) Uani 1 1 d . . .
H14 H -0.5303 0.4064 0.7901 0.049 Uiso 1 1 calc R . .
C15 C -0.4011(3) 0.3559(3) 0.7763(3) 0.0564(12) Uani 1 1 d . . .
H15 H -0.3691 0.3398 0.8482 0.068 Uiso 1 1 calc R . .
C16 C -0.3513(3) 0.3405(3) 0.7052(3) 0.0471(10) Uani 1 1 d . . .
H16 H -0.2843 0.3167 0.7302 0.057 Uiso 1 1 calc R . .
C17 C -0.2836(3) -0.0528(2) 0.2342(3) 0.0378(8) Uani 1 1 d . . .
H17 H -0.3506 -0.0357 0.1872 0.045 Uiso 1 1 calc R A 1
C18 C -0.1143(3) -0.0694(2) 0.3113(3) 0.0401(8) Uani 1 1 d . . .
H18 H -0.0413 -0.0658 0.3272 0.048 Uiso 1 1 calc R D .
C19 C -0.1598(4) -0.1117(2) 0.3678(3) 0.0505(10) Uani 1 1 d . D .
H19 H -0.1245 -0.1422 0.4290 0.061 Uiso 1 1 calc R B 1
C23 C -0.2218(4) 0.0463(3) 0.6316(4) 0.0613(12) Uani 1 1 d . . .
H23A H -0.2291 0.0739 0.6920 0.074 Uiso 1 1 calc R C 1
H23B H -0.1677 0.0058 0.6609 0.074 Uiso 1 1 calc R C 1
C24 C -0.1445(3) 0.0847(2) 0.4926(3) 0.0405(8) Uani 1 1 d . . .
H24 H -0.1317 0.0346 0.4718 0.049 Uiso 1 1 calc R D .
C25 C -0.1256(3) 0.15402(19) 0.4544(3) 0.0359(7) Uani 1 1 d . D .
H25 H -0.0961 0.1599 0.4023 0.043 Uiso 1 1 calc R . .
C26 C -0.1923(3) 0.1812(2) 0.5727(3) 0.0384(8) Uani 1 1 d . . .
H26 H -0.2182 0.2083 0.6180 0.046 Uiso 1 1 calc R D .
N1 N -0.1925(2) -0.03245(16) 0.2268(2) 0.0306(6) Uani 1 1 d . D .
N3 N -0.1863(3) 0.10244(17) 0.5684(2) 0.0406(7) Uani 1 1 d . D .
N4 N -0.1567(2) 0.21504(15) 0.5042(2) 0.0322(6) Uani 1 1 d . D .
O1 O -0.04746(17) 0.07607(14) 0.20193(18) 0.0334(5) Uani 1 1 d . D .
O2 O 0.07792(17) 0.06357(13) 0.13156(19) 0.0344(5) Uani 1 1 d . . .
O3 O 0.05488(19) 0.40742(12) 0.4111(2) 0.0377(6) Uani 1 1 d . . .
O4 O -0.0522(2) 0.30684(15) 0.4098(3) 0.0579(9) Uani 1 1 d . D .
O5 O -0.13558(15) 0.44545(11) 0.47915(16) 0.0232(4) Uani 1 1 d . . .
O6 O -0.24937(18) 0.34730(13) 0.5539(2) 0.0351(5) Uani 1 1 d . D .
O7 O -0.4093(2) 0.3267(2) 0.4224(2) 0.0668(9) Uani 1 1 d . . .
O8 O -0.69386(16) 0.47141(13) 0.49260(17) 0.0301(5) Uani 1 1 d . . .
O9 O -0.68632(18) 0.48780(15) 0.66188(19) 0.0370(5) Uani 1 1 d . . .
C22 C -0.3253(4) 0.0080(3) 0.5660(4) 0.0633(12) Uiso 0.778(9) 1 d P D 1
H22A H -0.3556 -0.0185 0.6121 0.076 Uiso 0.778(9) 1 calc PR D 1
H22B H -0.3764 0.0463 0.5211 0.076 Uiso 0.778(9) 1 calc PR D 1
C20 C -0.3407(5) -0.1407(4) 0.3555(5) 0.0485(14) Uiso 0.778(9) 1 d P D 1
H20A H -0.3083 -0.1884 0.3944 0.058 Uiso 0.778(9) 1 calc PR D 1
H20B H -0.4045 -0.1555 0.2939 0.058 Uiso 0.778(9) 1 calc PR D 1
C21 C -0.3709(8) -0.0847(5) 0.4311(8) 0.076(2) Uiso 0.778(9) 1 d P D 1
H21A H -0.4217 -0.0461 0.3866 0.091 Uiso 0.778(9) 1 calc PR D 1
H21B H -0.4066 -0.1153 0.4686 0.091 Uiso 0.778(9) 1 calc PR D 1
C22' C -0.3253(4) 0.0080(3) 0.5660(4) 0.0633(12) Uiso 0.222(9) 1 d P D 2
C20' C -0.3734(12) -0.1182(9) 0.3416(12) 0.024(3) Uiso 0.222(9) 1 d P D 2
H20C H -0.4323 -0.1186 0.2716 0.029 Uiso 0.222(9) 1 calc PR D 2
H20D H -0.3668 -0.1717 0.3694 0.029 Uiso 0.222(9) 1 calc PR D 2
C21' C -0.4008(12) -0.0796(8) 0.3983(13) 0.020(3) Uiso 0.222(9) 1 d P D 2
H21C H -0.4084 -0.1170 0.4499 0.024 Uiso 0.222(9) 1 calc PR D 2
H21D H -0.4730 -0.0640 0.3528 0.024 Uiso 0.222(9) 1 calc PR D 2
N2 N -0.2666(3) -0.10116(19) 0.3183(3) 0.0439(7) Uiso 0.778(9) 1 d P D 1
N2' N -0.2666(3) -0.10116(19) 0.3183(3) 0.0439(7) Uiso 0.222(9) 1 d P D 2
O10 O -0.2953(3) -0.0491(2) 0.4993(3) 0.0521(13) Uiso 0.778(9) 1 d P D 1
O10' O -0.3584(13) -0.0132(9) 0.4599(13) 0.062(5) Uiso 0.222(9) 1 d P D 2
Cu1 Cu -0.15447(3) 0.33019(2) 0.47476(3) 0.02895(11) Uani 1 1 d . . .
Cu2 Cu -0.16934(3) 0.01602(2) 0.10217(3) 0.02424(10) Uani 1 1 d . . .
Cu3 Cu 0.0000 0.0000 0.0000 0.02112(12) Uani 1 2 d S . .
O1W O 0.6936(3) 0.1549(2) 0.7909(4) 0.0815(11) Uiso 1 1 d D . .
H1A H 0.630(3) 0.137(4) 0.735(3) 0.122 Uiso 1 1 d D . .
H1B H 0.663(4) 0.177(4) 0.837(4) 0.122 Uiso 1 1 d D . .


_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 C2 1.385(4) . ?
C1 C6 1.388(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.393(4) . ?
C2 C8 1.511(4) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.501(4) . ?
C7 O2 1.252(3) . ?
C7 O1 1.259(3) . ?
C8 O3 1.234(4) . ?
C8 O4 1.263(4) . ?
C9 O7 1.229(4) . ?
C9 O6 1.280(4) . ?
C9 C10 1.501(4) . ?
C10 C11 1.383(4) . ?
C10 C16 1.387(5) . ?
C11 C12 1.391(4) . ?
C11 H11 0.9300 . ?
C12 C14 1.382(5) . ?
C12 C13 1.504(4) . ?
C13 O9 1.249(4) . ?
C13 O8 1.264(4) . ?
C14 C15 1.386(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.383(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 N1 1.320(4) . ?
C17 N2 1.338(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.348(5) . ?
C18 N1 1.368(4) . ?
C18 H18 0.9300 . ?
C19 N2 1.353(5) . ?
C19 H19 0.9300 . ?
C23 N3 1.469(5) . ?
C23 C22 1.487(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.344(5) . ?
C24 N3 1.368(4) . ?
C24 H24 0.9300 . ?
C25 N4 1.379(4) . ?
C25 H25 0.9300 . ?
C26 N4 1.317(4) . ?
C26 N3 1.338(4) . ?
C26 H26 0.9300 . ?
N1 Cu2 1.985(3) . ?
N4 Cu1 1.992(3) . ?
O1 Cu2 1.962(2) . ?
O2 Cu3 1.985(2) . ?
O3 Cu3 2.257(2) 2 ?
O4 Cu1 1.936(2) . ?
O5 Cu1 1.967(2) . ?
O5 Cu2 1.9766(19) 4_566 ?
O5 Cu3 1.978(2) 2 ?
O6 Cu1 1.973(2) . ?
O8 Cu2 1.952(2) 2_455 ?
C22 O10 1.474(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C20 N2 1.443(6) . ?
C20 C21 1.550(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 O10 1.236(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C20' C21' 1.16(2) . ?
C20' H20C 0.9700 . ?
C20' H20D 0.9700 . ?
C21' O10' 1.38(2) . ?
C21' H21C 0.9700 . ?
C21' H21D 0.9700 . ?
Cu2 O8 1.952(2) 2_445 ?
Cu2 O5 1.9766(19) 4_565 ?
Cu3 O5 1.978(2) 4_565 ?
Cu3 O5 1.978(2) 2_545 ?
Cu3 O2 1.985(2) 3 ?
Cu3 O3 2.257(2) 4_565 ?
Cu3 O3 2.257(2) 2_545 ?
O1W H1A 0.95(4) . ?
O1W H1B 0.94(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
C2 C1 C6 120.6(3) . . ?
C2 C1 H1 119.7 . . ?
C6 C1 H1 119.7 . . ?
C1 C2 C3 119.3(3) . . ?
C1 C2 C8 119.0(3) . . ?
C3 C2 C8 121.7(3) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.1(3) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 120.2(3) . . ?
C1 C6 C7 118.0(3) . . ?
C5 C6 C7 121.8(3) . . ?
O2 C7 O1 126.6(3) . . ?
O2 C7 C6 117.1(3) . . ?
O1 C7 C6 116.3(2) . . ?
O3 C8 O4 126.8(3) . . ?
O3 C8 C2 119.0(3) . . ?
O4 C8 C2 114.3(3) . . ?
O7 C9 O6 125.8(3) . . ?
O7 C9 C10 119.3(3) . . ?
O6 C9 C10 115.0(3) . . ?
C11 C10 C16 119.1(3) . . ?
C11 C10 C9 119.1(3) . . ?
C16 C10 C9 121.7(3) . . ?
C10 C11 C12 121.2(3) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C14 C12 C11 119.1(3) . . ?
C14 C12 C13 121.3(3) . . ?
C11 C12 C13 119.6(3) . . ?
O9 C13 O8 126.1(3) . . ?
O9 C13 C12 118.9(3) . . ?
O8 C13 C12 115.1(2) . . ?
C12 C14 C15 119.9(3) . . ?
C12 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C10 119.9(3) . . ?
C15 C16 H16 120.1 . . ?
C10 C16 H16 120.1 . . ?
N1 C17 N2 110.9(3) . . ?
N1 C17 H17 124.5 . . ?
N2 C17 H17 124.5 . . ?
C19 C18 N1 109.2(3) . . ?
C19 C18 H18 125.4 . . ?
N1 C18 H18 125.4 . . ?
C18 C19 N2 106.8(3) . . ?
C18 C19 H19 126.6 . . ?
N2 C19 H19 126.6 . . ?
N3 C23 C22 112.7(4) . . ?
N3 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 . . ?
N3 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C25 C24 N3 106.4(3) . . ?
C25 C24 H24 126.8 . . ?
N3 C24 H24 126.8 . . ?
C24 C25 N4 109.5(3) . . ?
C24 C25 H25 125.3 . . ?
N4 C25 H25 125.3 . . ?
N4 C26 N3 111.1(3) . . ?
N4 C26 H26 124.5 . . ?
N3 C26 H26 124.5 . . ?
C17 N1 C18 105.7(3) . . ?
C17 N1 Cu2 128.5(2) . . ?
C18 N1 Cu2 124.0(2) . . ?
C26 N3 C24 107.4(3) . . ?
C26 N3 C23 125.6(3) . . ?
C24 N3 C23 127.0(3) . . ?
C26 N4 C25 105.6(3) . . ?
C26 N4 Cu1 126.9(2) . . ?
C25 N4 Cu1 127.5(2) . . ?
C7 O1 Cu2 129.3(2) . . ?
C7 O2 Cu3 126.2(2) . . ?
C8 O3 Cu3 127.06(19) . 2 ?
C8 O4 Cu1 140.0(2) . . ?
Cu1 O5 Cu2 106.49(9) . 4_566 ?
Cu1 O5 Cu3 124.82(9) . 2 ?
Cu2 O5 Cu3 103.07(9) 4_566 2 ?
C9 O6 Cu1 127.5(2) . . ?
C13 O8 Cu2 132.44(19) . 2_455 ?
O10 C22 C23 103.1(4) . . ?
O10 C22 H22A 111.1 . . ?
C23 C22 H22A 111.1 . . ?
O10 C22 H22B 111.1 . . ?
C23 C22 H22B 111.1 . . ?
H22A C22 H22B 109.1 . . ?
N2 C20 C21 109.3(5) . . ?
N2 C20 H20A 109.8 . . ?
C21 C20 H20A 109.8 . . ?
N2 C20 H20B 109.8 . . ?
C21 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
O10 C21 C20 115.3(7) . . ?
O10 C21 H21A 108.4 . . ?
C20 C21 H21A 108.4 . . ?
O10 C21 H21B 108.4 . . ?
C20 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C21' C20' H20C 106.4 . . ?
C21' C20' H20D 106.4 . . ?
H20C C20' H20D 106.5 . . ?
C20' C21' O10' 133.0(15) . . ?
C20' C21' H21C 104.0 . . ?
O10' C21' H21C 104.0 . . ?
C20' C21' H21D 104.0 . . ?
O10' C21' H21D 104.0 . . ?
H21C C21' H21D 105.4 . . ?
C17 N2 C19 107.4(3) . . ?
C17 N2 C20 130.9(4) . . ?
C19 N2 C20 121.7(4) . . ?
C21 O10 C22 115.0(5) . . ?
O4 Cu1 O5 96.26(9) . . ?
O4 Cu1 O6 174.05(13) . . ?
O5 Cu1 O6 86.68(8) . . ?
O4 Cu1 N4 87.46(11) . . ?
O5 Cu1 N4 167.84(11) . . ?
O6 Cu1 N4 88.63(10) . . ?
O8 Cu2 O1 169.68(10) 2_445 . ?
O8 Cu2 O5 93.04(9) 2_445 4_565 ?
O1 Cu2 O5 89.49(9) . 4_565 ?
O8 Cu2 N1 88.16(10) 2_445 . ?
O1 Cu2 N1 90.42(10) . . ?
O5 Cu2 N1 173.73(10) 4_565 . ?
O5 Cu3 O5 180 4_565 2_545 ?
O5 Cu3 O2 88.75(9) 4_565 3 ?
O5 Cu3 O2 91.25(9) 2_545 3 ?
O5 Cu3 O2 91.25(9) 4_565 . ?
O5 Cu3 O2 88.75(9) 2_545 . ?
O2 Cu3 O2 180 3 . ?
O5 Cu3 O3 94.36(8) 4_565 4_565 ?
O5 Cu3 O3 85.64(8) 2_545 4_565 ?
O2 Cu3 O3 94.72(10) 3 4_565 ?
O2 Cu3 O3 85.28(10) . 4_565 ?
O5 Cu3 O3 85.64(8) 4_565 2_545 ?
O5 Cu3 O3 94.36(8) 2_545 2_545 ?
O2 Cu3 O3 85.28(10) 3 2_545 ?
O2 Cu3 O3 94.72(10) . 2_545 ?
O3 Cu3 O3 180 4_565 2_545 ?
H1A O1W H1B 99(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
C6 C1 C2 C3 -2.0(5) . . . . ?
C6 C1 C2 C8 176.8(3) . . . . ?
C1 C2 C3 C4 1.2(5) . . . . ?
C8 C2 C3 C4 -177.6(3) . . . . ?
C2 C3 C4 C5 1.5(5) . . . . ?
C3 C4 C5 C6 -3.3(5) . . . . ?
C2 C1 C6 C5 0.2(5) . . . . ?
C2 C1 C6 C7 -178.3(3) . . . . ?
C4 C5 C6 C1 2.5(5) . . . . ?
C4 C5 C6 C7 -179.1(3) . . . . ?
C1 C6 C7 O2 159.7(3) . . . . ?
C5 C6 C7 O2 -18.8(5) . . . . ?
C1 C6 C7 O1 -20.5(4) . . . . ?
C5 C6 C7 O1 161.0(3) . . . . ?
C1 C2 C8 O3 -150.5(3) . . . . ?
C3 C2 C8 O3 28.4(5) . . . . ?
C1 C2 C8 O4 27.8(5) . . . . ?
C3 C2 C8 O4 -153.4(3) . . . . ?
O7 C9 C10 C11 -33.5(5) . . . . ?
O6 C9 C10 C11 146.7(3) . . . . ?
O7 C9 C10 C16 146.4(4) . . . . ?
O6 C9 C10 C16 -33.4(5) . . . . ?
C16 C10 C11 C12 2.3(5) . . . . ?
C9 C10 C11 C12 -177.8(3) . . . . ?
C10 C11 C12 C14 -3.8(5) . . . . ?
C10 C11 C12 C13 175.4(3) . . . . ?
C14 C12 C13 O9 7.6(5) . . . . ?
C11 C12 C13 O9 -171.6(3) . . . . ?
C14 C12 C13 O8 -172.4(3) . . . . ?
C11 C12 C13 O8 8.3(4) . . . . ?
C11 C12 C14 C15 1.8(6) . . . . ?
C13 C12 C14 C15 -177.5(4) . . . . ?
C12 C14 C15 C16 1.8(7) . . . . ?
C14 C15 C16 C10 -3.4(7) . . . . ?
C11 C10 C16 C15 1.4(6) . . . . ?
C9 C10 C16 C15 -178.5(4) . . . . ?
N1 C18 C19 N2 0.0(4) . . . . ?
N3 C24 C25 N4 -0.9(4) . . . . ?
N2 C17 N1 C18 -0.6(4) . . . . ?
N2 C17 N1 Cu2 164.2(2) . . . . ?
C19 C18 N1 C17 0.3(4) . . . . ?
C19 C18 N1 Cu2 -165.4(3) . . . . ?
N4 C26 N3 C24 -0.1(4) . . . . ?
N4 C26 N3 C23 -178.2(4) . . . . ?
C25 C24 N3 C26 0.6(4) . . . . ?
C25 C24 N3 C23 178.7(4) . . . . ?
C22 C23 N3 C26 103.5(5) . . . . ?
C22 C23 N3 C24 -74.3(5) . . . . ?
N3 C26 N4 C25 -0.5(4) . . . . ?
N3 C26 N4 Cu1 177.2(2) . . . . ?
C24 C25 N4 C26 0.9(4) . . . . ?
C24 C25 N4 Cu1 -176.7(3) . . . . ?
O2 C7 O1 Cu2 -21.0(5) . . . . ?
C6 C7 O1 Cu2 159.2(2) . . . . ?
O1 C7 O2 Cu3 22.4(5) . . . . ?
C6 C7 O2 Cu3 -157.9(2) . . . . ?
O4 C8 O3 Cu3 17.0(6) . . . 2 ?
C2 C8 O3 Cu3 -165.0(2) . . . 2 ?
O3 C8 O4 Cu1 -16.3(7) . . . . ?
C2 C8 O4 Cu1 165.6(3) . . . . ?
O7 C9 O6 Cu1 1.0(5) . . . . ?
C10 C9 O6 Cu1 -179.2(2) . . . . ?
O9 C13 O8 Cu2 -6.2(5) . . . 2_455 ?
C12 C13 O8 Cu2 173.9(2) . . . 2_455 ?
N3 C23 C22 O10 74.7(5) . . . . ?
N2 C20 C21 O10 -45.0(9) . . . . ?
N1 C17 N2 C19 0.7(4) . . . . ?
N1 C17 N2 C20 -177.2(4) . . . . ?
C18 C19 N2 C17 -0.4(4) . . . . ?
C18 C19 N2 C20 177.7(4) . . . . ?
C21 C20 N2 C17 -86.1(7) . . . . ?
C21 C20 N2 C19 96.3(6) . . . . ?
C20 C21 O10 C22 176.1(5) . . . . ?
C23 C22 O10 C21 -174.8(6) . . . . ?
C8 O4 Cu1 O5 21.4(5) . . . . ?
C8 O4 Cu1 N4 -146.9(5) . . . . ?
Cu2 O5 Cu1 O4 -151.98(13) 4_566 . . . ?
Cu3 O5 Cu1 O4 -32.44(16) 2 . . . ?
Cu2 O5 Cu1 O6 22.82(10) 4_566 . . . ?
Cu3 O5 Cu1 O6 142.36(14) 2 . . . ?
Cu2 O5 Cu1 N4 -44.7(5) 4_566 . . . ?
Cu3 O5 Cu1 N4 74.9(5) 2 . . . ?
C9 O6 Cu1 O5 105.2(3) . . . . ?
C9 O6 Cu1 N4 -86.0(3) . . . . ?
C26 N4 Cu1 O4 162.9(3) . . . . ?
C25 N4 Cu1 O4 -20.0(3) . . . . ?
C26 N4 Cu1 O5 54.7(6) . . . . ?
C25 N4 Cu1 O5 -128.2(4) . . . . ?
C26 N4 Cu1 O6 -12.7(3) . . . . ?
C25 N4 Cu1 O6 164.5(3) . . . . ?
C7 O1 Cu2 O8 -132.5(5) . . . 2_445 ?
C7 O1 Cu2 O5 -28.2(3) . . . 4_565 ?
C7 O1 Cu2 N1 145.5(3) . . . . ?
C17 N1 Cu2 O8 -24.0(3) . . . 2_445 ?
C18 N1 Cu2 O8 138.4(3) . . . 2_445 ?
C17 N1 Cu2 O1 145.8(3) . . . . ?
C18 N1 Cu2 O1 -51.9(3) . . . . ?
C7 O2 Cu3 O5 25.3(3) . . . 4_565 ?
C7 O2 Cu3 O5 -154.7(3) . . . 2_545 ?
C7 O2 Cu3 O3 119.6(3) . . . 4_565 ?
C7 O2 Cu3 O3 -60.4(3) . . . 2_545 ?

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 H1B O7 0.94(6) 1.77(3) 2.643(5) 155(6) 4_666

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.085

#================END

data_Compound-8
_database_code_depnum_ccdc_archive 'CCDC 682072'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H40 Cu3 N8 O17'
_chemical_formula_sum            'C38 H40 Cu3 N8 O17'
_chemical_formula_weight         1071.40

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           orthorhombic
_symmetry_space_group_name_H-M   'P b c n '
_symmetry_space_group_name_hall  '-P 2n 2ab '

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

_cell_length_a                   11.7668(16)
_cell_length_b                   16.821(3)
_cell_length_c                   20.579(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4073.1(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4672
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2188
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_process_details   
;
Higashi,T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37393
_diffrn_reflns_av_R_equivalents  0.2328
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4672
_reflns_number_gt                2418
_reflns_threshold_expression     >2sigma(I)

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

_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.
To obtain a reasonable geometry for water molecule, the bond length of
O1W-H1A (O1W-H1B) and the distance of H1A to H1B were
restrained to 0.89 and 1.44 Å respectively.
;

_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)+(0.0605P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4672
_refine_ls_number_parameters     308
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1442
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      0.954
_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
C1 C 0.5979(4) 0.9372(3) 0.6618(3) 0.0231(12) Uani 1 1 d . . .
C2 C 0.5212(4) 0.8649(3) 0.6644(3) 0.0200(12) Uani 1 1 d . . .
C3 C 0.4053(4) 0.8738(3) 0.6755(2) 0.0201(12) Uani 1 1 d . . .
H3 H 0.3742 0.9246 0.6771 0.024 Uiso 1 1 calc R . .
C4 C 0.3348(4) 0.8082(3) 0.6845(2) 0.0164(11) Uani 1 1 d . . .
C5 C 0.2097(4) 0.8190(3) 0.7018(3) 0.0240(12) Uani 1 1 d . . .
C7 C 0.4951(4) 0.7222(3) 0.6649(2) 0.0184(11) Uani 1 1 d . . .
C6 C 0.3811(4) 0.7332(3) 0.6790(3) 0.0219(12) Uani 1 1 d . . .
H6 H 0.3348 0.6890 0.6850 0.026 Uiso 1 1 calc R . .
C9 C 0.5427(4) 0.6388(3) 0.6613(3) 0.0199(11) Uani 1 1 d . . .
C10 C 0.7879(6) 0.4764(4) 0.5242(3) 0.0432(16) Uani 1 1 d . . .
H10 H 0.8526 0.4519 0.5408 0.052 Uiso 1 1 calc R . .
C11 C 0.6346(6) 0.5413(4) 0.5167(3) 0.0477(18) Uani 1 1 d . . .
H11 H 0.5709 0.5715 0.5271 0.057 Uiso 1 1 calc R . .
C12 C 0.6618(6) 0.5158(4) 0.4566(3) 0.054(2) Uani 1 1 d . . .
H12 H 0.6206 0.5247 0.4187 0.064 Uiso 1 1 calc R . .
C13 C 0.8169(6) 0.4306(4) 0.4091(3) 0.0460(18) Uani 1 1 d . . .
H13A H 0.8860 0.4583 0.3968 0.055 Uiso 1 1 calc R . .
H13B H 0.7675 0.4289 0.3714 0.055 Uiso 1 1 calc R . .
C14 C 0.8456(7) 0.3480(4) 0.4291(4) 0.058(2) Uani 1 1 d . . .
H14A H 0.8723 0.3184 0.3917 0.069 Uiso 1 1 calc R . .
H14B H 0.9063 0.3493 0.4610 0.069 Uiso 1 1 calc R . .
C15 C 0.7792(7) 0.2343(4) 0.4824(4) 0.062(2) Uani 1 1 d . . .
H15A H 0.8328 0.2393 0.5179 0.075 Uiso 1 1 calc R . .
H15B H 0.8112 0.1992 0.4497 0.075 Uiso 1 1 calc R . .
C16 C 0.6678(6) 0.2033(4) 0.5061(3) 0.0506(19) Uani 1 1 d . . .
H16A H 0.6130 0.2057 0.4709 0.061 Uiso 1 1 calc R . .
H16B H 0.6767 0.1479 0.5183 0.061 Uiso 1 1 calc R . .
C17 C 0.5856(6) 0.3254(4) 0.5610(3) 0.0414(17) Uani 1 1 d . . .
H17 H 0.5858 0.3600 0.5257 0.050 Uiso 1 1 calc R . .
C18 C 0.5477(5) 0.3406(4) 0.6222(3) 0.0382(16) Uani 1 1 d . . .
H18 H 0.5180 0.3889 0.6362 0.046 Uiso 1 1 calc R . .
C19 C 0.6071(5) 0.2211(4) 0.6233(3) 0.0387(16) Uani 1 1 d . . .
H19 H 0.6272 0.1705 0.6374 0.046 Uiso 1 1 calc R . .
C8 C 0.5665(4) 0.7889(3) 0.6594(2) 0.0202(11) Uani 1 1 d . . .
H8 H 0.6440 0.7822 0.6524 0.024 Uiso 1 1 calc R . .
N1 N 0.7157(4) 0.5158(3) 0.5604(2) 0.0333(11) Uani 1 1 d . . .
N2 N 0.7601(4) 0.4748(3) 0.4616(2) 0.0361(12) Uani 1 1 d . . .
N3 N 0.6234(4) 0.2482(3) 0.5622(2) 0.0360(12) Uani 1 1 d . . .
N4 N 0.5597(4) 0.2746(3) 0.6601(2) 0.0296(11) Uani 1 1 d . . .
O1 O 0.1577(3) 0.7552(2) 0.71703(19) 0.0310(9) Uani 1 1 d . . .
O2 O 0.1656(3) 0.8860(2) 0.6994(2) 0.0379(11) Uani 1 1 d . . .
O1W O 0.6947(4) 0.5249(2) 0.7502(2) 0.0383(10) Uani 1 1 d D . .
O3 O 0.5560(3) 1.0044(2) 0.6551(2) 0.0370(10) Uani 1 1 d . . .
O2W O 0.0000 0.6232(4) 0.7500 0.060(2) Uani 1 2 d S . .
O4 O 0.7037(3) 0.9246(2) 0.66451(18) 0.0267(9) Uani 1 1 d . . .
O5 O 0.6500(3) 0.6319(2) 0.6502(2) 0.0317(10) Uani 1 1 d . . .
O6 O 0.4798(3) 0.5803(2) 0.6690(2) 0.0358(11) Uani 1 1 d . . .
O7 O 0.7536(4) 0.3108(3) 0.4550(2) 0.0629(15) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.76113(6) 0.7500 0.0241(2) Uani 1 2 d S . .
Cu2 Cu 0.71275(6) 0.52499(4) 0.65565(3) 0.02547(19) Uani 1 1 d . . .
H1A H 0.634(3) 0.551(2) 0.762(3) 0.038 Uiso 1 1 d D . .
H1B H 0.687(4) 0.4745(14) 0.762(3) 0.038 Uiso 1 1 d D . .
H2A H -0.006(6) 0.588(3) 0.725(3) 0.038 Uiso 1 1 d . . .


_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 O3 1.242(6) . ?
C1 O4 1.263(6) . ?
C1 C2 1.515(7) . ?
C2 C8 1.388(7) . ?
C2 C3 1.392(7) . ?
C3 C4 1.393(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.378(7) . ?
C4 C5 1.526(7) . ?
C5 O2 1.242(6) . ?
C5 O1 1.274(6) . ?
C7 C6 1.385(7) . ?
C7 C8 1.406(7) . ?
C7 C9 1.513(7) . ?
C6 H6 0.9300 . ?
C9 O6 1.241(6) . ?
C9 O5 1.288(6) . ?
C10 N1 1.310(8) . ?
C10 N2 1.330(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.348(9) . ?
C11 N1 1.379(8) . ?
C11 H11 0.9300 . ?
C12 N2 1.350(8) . ?
C12 H12 0.9300 . ?
C13 N2 1.472(7) . ?
C13 C14 1.488(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O7 1.359(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O7 1.437(8) . ?
C15 C16 1.493(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N3 1.475(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.362(9) . ?
C17 N3 1.373(7) . ?
C17 H17 0.9300 . ?
C18 N4 1.363(7) . ?
C18 H18 0.9300 . ?
C19 N4 1.302(7) . ?
C19 N3 1.352(8) . ?
C19 H19 0.9300 . ?
C8 H8 0.9300 . ?
N1 Cu2 1.966(5) . ?
N4 Cu1 1.992(5) 6_657 ?
O1 Cu1 1.979(3) . ?
O1W Cu2 1.957(4) . ?
O1W H1A 0.87(4) . ?
O1W H1B 0.886(19) . ?
O2W Cu1 2.320(6) . ?
O2W H2A 0.78(5) . ?
O4 Cu2 1.963(3) 7_765 ?
O5 Cu2 1.948(4) . ?
Cu1 O1 1.979(4) 4_556 ?
Cu1 N4 1.992(5) 7_665 ?
Cu1 N4 1.992(5) 6_567 ?
Cu2 O4 1.963(3) 7_755 ?

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
O3 C1 O4 123.3(5) . . ?
O3 C1 C2 119.9(5) . . ?
O4 C1 C2 116.8(4) . . ?
C8 C2 C3 119.2(5) . . ?
C8 C2 C1 120.5(4) . . ?
C3 C2 C1 120.2(4) . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C6 C4 C3 118.7(4) . . ?
C6 C4 C5 120.6(5) . . ?
C3 C4 C5 120.7(4) . . ?
O2 C5 O1 125.0(5) . . ?
O2 C5 C4 120.1(5) . . ?
O1 C5 C4 114.9(5) . . ?
C6 C7 C8 119.3(4) . . ?
C6 C7 C9 119.5(4) . . ?
C8 C7 C9 121.0(4) . . ?
C4 C6 C7 121.4(5) . . ?
C4 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
O6 C9 O5 122.4(5) . . ?
O6 C9 C7 120.5(5) . . ?
O5 C9 C7 117.0(4) . . ?
N1 C10 N2 113.7(6) . . ?
N1 C10 H10 123.2 . . ?
N2 C10 H10 123.2 . . ?
C12 C11 N1 109.6(6) . . ?
C12 C11 H11 125.2 . . ?
N1 C11 H11 125.2 . . ?
C11 C12 N2 107.2(6) . . ?
C11 C12 H12 126.4 . . ?
N2 C12 H12 126.4 . . ?
N2 C13 C14 111.7(5) . . ?
N2 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
N2 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
O7 C14 C13 111.0(6) . . ?
O7 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
O7 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
O7 C15 C16 104.9(6) . . ?
O7 C15 H15A 110.8 . . ?
C16 C15 H15A 110.8 . . ?
O7 C15 H15B 110.8 . . ?
C16 C15 H15B 110.8 . . ?
H15A C15 H15B 108.8 . . ?
N3 C16 C15 112.8(6) . . ?
N3 C16 H16A 109.0 . . ?
C15 C16 H16A 109.0 . . ?
N3 C16 H16B 109.0 . . ?
C15 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 N3 105.5(5) . . ?
C18 C17 H17 127.2 . . ?
N3 C17 H17 127.2 . . ?
C17 C18 N4 109.9(6) . . ?
C17 C18 H18 125.0 . . ?
N4 C18 H18 125.0 . . ?
N4 C19 N3 111.6(5) . . ?
N4 C19 H19 124.2 . . ?
N3 C19 H19 124.2 . . ?
C2 C8 C7 119.9(4) . . ?
C2 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 N1 C11 103.6(5) . . ?
C10 N1 Cu2 128.2(4) . . ?
C11 N1 Cu2 127.8(5) . . ?
C10 N2 C12 105.9(6) . . ?
C10 N2 C13 127.6(6) . . ?
C12 N2 C13 126.2(6) . . ?
C19 N3 C17 106.8(5) . . ?
C19 N3 C16 127.3(5) . . ?
C17 N3 C16 125.8(5) . . ?
C19 N4 C18 106.0(5) . . ?
C19 N4 Cu1 127.7(4) . 6_657 ?
C18 N4 Cu1 125.9(4) . 6_657 ?
C5 O1 Cu1 119.5(4) . . ?
Cu2 O1W H1A 111(4) . . ?
Cu2 O1W H1B 107(4) . . ?
H1A O1W H1B 109(3) . . ?
Cu1 O2W H2A 139(4) . . ?
C1 O4 Cu2 110.2(3) . 7_765 ?
C9 O5 Cu2 116.4(3) . . ?
C14 O7 C15 113.5(6) . . ?
O1 Cu1 O1 174.2(2) 4_556 . ?
O1 Cu1 N4 89.62(17) 4_556 7_665 ?
O1 Cu1 N4 91.04(17) . 7_665 ?
O1 Cu1 N4 91.04(17) 4_556 6_567 ?
O1 Cu1 N4 89.62(17) . 6_567 ?
N4 Cu1 N4 166.9(3) 7_665 6_567 ?
O1 Cu1 O2W 87.10(12) 4_556 . ?
O1 Cu1 O2W 87.10(12) . . ?
N4 Cu1 O2W 96.55(14) 7_665 . ?
N4 Cu1 O2W 96.55(14) 6_567 . ?
O5 Cu2 O1W 91.00(17) . . ?
O5 Cu2 O4 171.88(16) . 7_755 ?
O1W Cu2 O4 87.76(16) . 7_755 ?
O5 Cu2 N1 91.25(18) . . ?
O1W Cu2 N1 173.1(2) . . ?
O4 Cu2 N1 90.92(18) 7_755 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C1 C2 C8 167.7(5) . . . . ?
O4 C1 C2 C8 -10.0(8) . . . . ?
O3 C1 C2 C3 -16.0(8) . . . . ?
O4 C1 C2 C3 166.3(5) . . . . ?
C8 C2 C3 C4 2.7(8) . . . . ?
C1 C2 C3 C4 -173.6(5) . . . . ?
C2 C3 C4 C6 -3.0(8) . . . . ?
C2 C3 C4 C5 175.3(5) . . . . ?
C6 C4 C5 O2 -171.9(5) . . . . ?
C3 C4 C5 O2 9.9(8) . . . . ?
C6 C4 C5 O1 7.0(7) . . . . ?
C3 C4 C5 O1 -171.2(5) . . . . ?
C3 C4 C6 C7 -0.1(8) . . . . ?
C5 C4 C6 C7 -178.4(5) . . . . ?
C8 C7 C6 C4 3.4(8) . . . . ?
C9 C7 C6 C4 178.3(5) . . . . ?
C6 C7 C9 O6 2.1(8) . . . . ?
C8 C7 C9 O6 176.9(5) . . . . ?
C6 C7 C9 O5 -177.7(5) . . . . ?
C8 C7 C9 O5 -3.0(7) . . . . ?
N1 C11 C12 N2 -0.5(8) . . . . ?
N2 C13 C14 O7 50.7(8) . . . . ?
O7 C15 C16 N3 -68.6(7) . . . . ?
N3 C17 C18 N4 -1.0(7) . . . . ?
C3 C2 C8 C7 0.7(8) . . . . ?
C1 C2 C8 C7 177.0(5) . . . . ?
C6 C7 C8 C2 -3.7(8) . . . . ?
C9 C7 C8 C2 -178.5(5) . . . . ?
N2 C10 N1 C11 0.1(8) . . . . ?
N2 C10 N1 Cu2 173.2(4) . . . . ?
C12 C11 N1 C10 0.2(8) . . . . ?
C12 C11 N1 Cu2 -172.9(5) . . . . ?
N1 C10 N2 C12 -0.4(8) . . . . ?
N1 C10 N2 C13 -174.5(6) . . . . ?
C11 C12 N2 C10 0.5(8) . . . . ?
C11 C12 N2 C13 174.7(6) . . . . ?
C14 C13 N2 C10 43.8(9) . . . . ?
C14 C13 N2 C12 -129.2(7) . . . . ?
N4 C19 N3 C17 1.4(7) . . . . ?
N4 C19 N3 C16 -175.8(6) . . . . ?
C18 C17 N3 C19 -0.2(7) . . . . ?
C18 C17 N3 C16 177.1(6) . . . . ?
C15 C16 N3 C19 -115.1(7) . . . . ?
C15 C16 N3 C17 68.1(9) . . . . ?
N3 C19 N4 C18 -2.0(7) . . . . ?
N3 C19 N4 Cu1 171.6(4) . . . 6_657 ?
C17 C18 N4 C19 1.8(7) . . . . ?
C17 C18 N4 Cu1 -172.0(4) . . . 6_657 ?
O2 C5 O1 Cu1 -7.9(7) . . . . ?
C4 C5 O1 Cu1 173.3(3) . . . . ?
O3 C1 O4 Cu2 -0.7(7) . . . 7_765 ?
C2 C1 O4 Cu2 176.9(4) . . . 7_765 ?
O6 C9 O5 Cu2 -6.7(7) . . . . ?
C7 C9 O5 Cu2 173.2(3) . . . . ?
C13 C14 O7 C15 -172.9(6) . . . . ?
C16 C15 O7 C14 -178.5(6) . . . . ?
C5 O1 Cu1 N4 79.1(4) . . . 7_665 ?
C5 O1 Cu1 N4 -87.8(4) . . . 6_567 ?
C5 O1 Cu1 O2W 175.6(4) . . . . ?
C9 O5 Cu2 O1W -71.1(4) . . . . ?
C9 O5 Cu2 N1 102.4(4) . . . . ?
C10 N1 Cu2 O5 148.0(6) . . . . ?
C11 N1 Cu2 O5 -40.5(5) . . . . ?
C10 N1 Cu2 O4 -24.2(6) . . . 7_755 ?
C11 N1 Cu2 O4 147.3(5) . . . 7_755 ?

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 H1A O6 0.87(4) 2.01(3) 2.803(5) 149(5) 4_656
O2W H2A O3 0.78(5) 2.10(6) 2.870(6) 168(7) 7_655

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.113

#================END


