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

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

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

_publ_section_title              
;
Four-, and six-connected entangled frameworks based on
flexible bis(imidazole) ligands and long dicarboxylate anions
;
loop_
_publ_author_name
'Jian-Fang Ma.'
'Stuart Batten'
'Ying-Ying Liu.'
'Jin Yang.'

# Attachment 'Crystal.cif'

data_compound-1
_database_code_depnum_ccdc_archive 'CCDC 693960'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C24 H22 Cd N4 O5), H2O'
_chemical_formula_sum            'C48 H46 Cd2 N8 O11'
_chemical_formula_weight         1135.73

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   20.008(2)
_cell_length_b                   53.655(6)
_cell_length_c                   8.9809(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9641.1(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4753
_cell_measurement_theta_min      1.52
_cell_measurement_theta_max      26.06

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4592
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'

_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13409
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         26.06
_reflns_number_total             4753
_reflns_number_gt                2919
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'

_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)+(0.0377P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(4)
_refine_ls_number_reflns         4753
_refine_ls_number_parameters     312
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.0959
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_restrained_S_all      0.913
_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 0.2118(4) 0.21090(14) 0.4296(10) 0.071(2) Uani 1 1 d . . .
C2 C 0.1710(3) 0.22960(12) 0.5152(10) 0.0686(17) Uani 1 1 d . . .
C3 C 0.1767(5) 0.23181(18) 0.6640(10) 0.114(3) Uani 1 1 d . . .
H3 H 0.2077 0.2221 0.7148 0.137 Uiso 1 1 calc R . .
C4 C 0.1369(5) 0.24839(16) 0.7425(10) 0.107(3) Uani 1 1 d . . .
H4 H 0.1420 0.2499 0.8450 0.128 Uiso 1 1 calc R . .
C5 C 0.0914(4) 0.26216(13) 0.6723(9) 0.074(2) Uani 1 1 d . . .
C6 C 0.0845(3) 0.26068(11) 0.5196(11) 0.0702(17) Uani 1 1 d . . .
H6 H 0.0532 0.2704 0.4696 0.084 Uiso 1 1 calc R . .
C7 C 0.1256(4) 0.24434(13) 0.4432(8) 0.070(2) Uani 1 1 d . . .
H7 H 0.1221 0.2433 0.3401 0.085 Uiso 1 1 calc R . .
C8 C 0.0366(4) 0.30108(13) 0.7170(7) 0.069(2) Uani 1 1 d . . .
C9 C -0.0027(3) 0.37714(13) 0.6180(7) 0.0570(17) Uani 1 1 d . . .
C10 C 0.0875(3) 0.31592(14) 0.6580(7) 0.066(2) Uani 1 1 d . . .
H10 H 0.1295 0.3093 0.6386 0.079 Uiso 1 1 calc R . .
C11 C 0.0740(3) 0.34032(13) 0.6298(7) 0.0618(18) Uani 1 1 d . . .
H11 H 0.1077 0.3504 0.5914 0.074 Uiso 1 1 calc R . .
C12 C 0.0113(3) 0.35080(12) 0.6567(7) 0.0533(16) Uani 1 1 d . . .
C13 C -0.0385(3) 0.33559(13) 0.7148(7) 0.0629(19) Uani 1 1 d . . .
H13 H -0.0809 0.3421 0.7322 0.075 Uiso 1 1 calc R . .
C14 C -0.0256(4) 0.31119(14) 0.7464(8) 0.076(2) Uani 1 1 d . . .
H14 H -0.0589 0.3013 0.7879 0.091 Uiso 1 1 calc R . .
C15 C 0.2746(4) 0.16995(18) -0.0980(12) 0.098(3) Uani 1 1 d . . .
H15 H 0.3117 0.1804 -0.1023 0.117 Uiso 1 1 calc R . .
C16 C 0.2454(4) 0.15929(16) -0.2163(12) 0.093(3) Uani 1 1 d . . .
H16 H 0.2574 0.1612 -0.3158 0.112 Uiso 1 1 calc R . .
C17 C 0.1951(4) 0.14860(12) -0.0094(9) 0.073(2) Uani 1 1 d . . .
H17 H 0.1650 0.1412 0.0559 0.088 Uiso 1 1 calc R . .
C18 C 0.1466(6) 0.1313(2) -0.2540(15) 0.151(5) Uani 1 1 d D . .
H18A H 0.1701 0.1227 -0.3334 0.181 Uiso 1 1 calc R . .
H18B H 0.1247 0.1188 -0.1929 0.181 Uiso 1 1 calc R . .
C19 C 0.0614(13) 0.1711(4) -0.362(3) 0.331(12) Uani 1 1 d DU . .
H19A H 0.0163 0.1675 -0.3954 0.398 Uiso 1 1 calc R . .
H19B H 0.0853 0.1792 -0.4421 0.398 Uiso 1 1 calc R . .
C20 C 0.0955(8) 0.1481(3) -0.319(2) 0.291(13) Uani 1 1 d D . .
H20A H 0.0572 0.1403 -0.2716 0.349 Uiso 1 1 calc R . .
H20B H 0.0957 0.1407 -0.4179 0.349 Uiso 1 1 calc R . .
C21 C -0.1093(5) 0.20900(16) -0.3624(10) 0.095(3) Uani 1 1 d . . .
H21 H -0.1383 0.2206 -0.4044 0.114 Uiso 1 1 calc R . .
C22 C -0.0755(4) 0.17802(18) -0.2481(13) 0.100(3) Uani 1 1 d . . .
H22 H -0.0723 0.1634 -0.1930 0.120 Uiso 1 1 calc R . .
C23 C -0.0458(6) 0.21000(18) -0.3708(12) 0.108(3) Uani 1 1 d . . .
H23 H -0.0202 0.2222 -0.4176 0.130 Uiso 1 1 calc R . .
C24 C 0.0595(9) 0.1874(4) -0.229(3) 0.282(9) Uani 1 1 d U . .
H24A H 0.0870 0.2023 -0.2339 0.338 Uiso 1 1 calc R . .
H24B H 0.0634 0.1789 -0.1335 0.338 Uiso 1 1 calc R . .
N1 N 0.2423(3) 0.16335(11) 0.0289(8) 0.0728(15) Uani 1 1 d . . .
N2 N 0.1953(3) 0.14531(11) -0.1620(8) 0.0800(18) Uani 1 1 d . . .
N3 N -0.1289(3) 0.18832(11) -0.2821(7) 0.0693(16) Uani 1 1 d . . .
N4 N -0.0242(4) 0.1905(2) -0.3003(14) 0.166(5) Uani 1 1 d . . .
O1 O 0.2484(3) 0.19614(10) 0.4980(6) 0.0934(17) Uani 1 1 d . . .
O2 O 0.2035(2) 0.20995(8) 0.2886(7) 0.0828(14) Uani 1 1 d . . .
O1W O 0.2500 0.2500 0.0896(10) 0.130(4) Uani 1 2 d S . .
O3 O -0.0603(2) 0.38502(8) 0.6128(5) 0.0714(13) Uani 1 1 d . . .
O4 O 0.0463(3) 0.39100(9) 0.5896(6) 0.0885(16) Uani 1 1 d . . .
O5 O 0.0477(3) 0.27659(9) 0.7577(6) 0.0922(15) Uani 1 1 d . . .
Cd1 Cd 0.26791(2) 0.174411(9) 0.26799(7) 0.06741(17) 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 O1 1.242(8) . ?
C1 O2 1.278(9) . ?
C1 C2 1.504(10) . ?
C1 Cd1 2.683(8) . ?
C2 C7 1.368(9) . ?
C2 C3 1.347(11) . ?
C3 C4 1.387(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.331(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(11) . ?
C5 O5 1.397(8) . ?
C6 C7 1.384(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C14 1.384(9) . ?
C8 O5 1.382(7) . ?
C8 C10 1.396(9) . ?
C9 O3 1.230(7) . ?
C9 O4 1.257(7) . ?
C9 C12 1.482(9) . ?
C9 Cd1 2.708(7) 3 ?
C10 C11 1.361(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(9) . ?
C13 C14 1.364(9) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.341(12) . ?
C15 N1 1.357(10) . ?
C15 H15 0.9300 . ?
C16 N2 1.344(9) . ?
C16 H16 0.9300 . ?
C17 N1 1.280(8) . ?
C17 N2 1.382(9) . ?
C17 H17 0.9300 . ?
C18 C20 1.484(9) . ?
C18 N2 1.483(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.461(10) . ?
C19 C24 1.48(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C23 1.274(11) . ?
C21 N3 1.381(9) . ?
C21 H21 0.9300 . ?
C22 N3 1.242(8) . ?
C22 N4 1.311(10) . ?
C22 H22 0.9300 . ?
C23 N4 1.297(11) . ?
C23 H23 0.9300 . ?
C24 N4 1.80(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
N1 Cd1 2.286(7) . ?
N3 Cd1 2.240(6) 9_454 ?
O1 Cd1 2.404(5) . ?
O2 Cd1 2.309(4) . ?
O3 Cd1 2.432(4) 3 ?
O4 Cd1 2.298(5) 3 ?
Cd1 N3 2.240(6) 9 ?
Cd1 O4 2.298(5) 7_544 ?
Cd1 O3 2.432(4) 7_544 ?
Cd1 C9 2.708(7) 7_544 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 122.8(7) . . ?
O1 C1 C2 119.5(7) . . ?
O2 C1 C2 117.5(7) . . ?
O1 C1 Cd1 63.6(4) . . ?
O2 C1 Cd1 59.3(4) . . ?
C2 C1 Cd1 171.9(5) . . ?
C7 C2 C3 118.3(7) . . ?
C7 C2 C1 120.3(8) . . ?
C3 C2 C1 121.4(7) . . ?
C2 C3 C4 120.9(8) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 120.6(8) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.4(7) . . ?
C4 C5 O5 118.4(7) . . ?
C6 C5 O5 121.0(7) . . ?
C5 C6 C7 118.0(7) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
C2 C7 C6 121.8(7) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C14 C8 O5 117.8(7) . . ?
C14 C8 C10 120.3(7) . . ?
O5 C8 C10 121.7(7) . . ?
O3 C9 O4 121.4(7) . . ?
O3 C9 C12 120.9(6) . . ?
O4 C9 C12 117.7(6) . . ?
O3 C9 Cd1 63.9(4) . 3 ?
O4 C9 Cd1 57.8(4) . 3 ?
C12 C9 Cd1 172.8(5) . 3 ?
C11 C10 C8 118.3(7) . . ?
C11 C10 H10 120.9 . . ?
C8 C10 H10 120.9 . . ?
C10 C11 C12 122.3(6) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 118.2(6) . . ?
C13 C12 C9 120.8(6) . . ?
C11 C12 C9 120.9(6) . . ?
C14 C13 C12 120.4(7) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C8 120.4(7) . . ?
C13 C14 H14 119.8 . . ?
C8 C14 H14 119.8 . . ?
C16 C15 N1 110.3(7) . . ?
C16 C15 H15 124.8 . . ?
N1 C15 H15 124.8 . . ?
C15 C16 N2 106.0(8) . . ?
C15 C16 H16 127.0 . . ?
N2 C16 H16 127.0 . . ?
N1 C17 N2 110.1(7) . . ?
N1 C17 H17 125.0 . . ?
N2 C17 H17 125.0 . . ?
C20 C18 N2 111.3(9) . . ?
C20 C18 H18A 109.4 . . ?
N2 C18 H18A 109.4 . . ?
C20 C18 H18B 109.4 . . ?
N2 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C24 107(2) . . ?
C20 C19 H19A 110.2 . . ?
C24 C19 H19A 110.2 . . ?
C20 C19 H19B 110.2 . . ?
C24 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
C18 C20 C19 159.7(16) . . ?
C18 C20 H20A 96.3 . . ?
C19 C20 H20A 96.3 . . ?
C18 C20 H20B 96.3 . . ?
C19 C20 H20B 96.3 . . ?
H20A C20 H20B 103.4 . . ?
C23 C21 N3 110.4(8) . . ?
C23 C21 H21 124.8 . . ?
N3 C21 H21 124.8 . . ?
N3 C22 N4 111.0(9) . . ?
N3 C22 H22 124.5 . . ?
N4 C22 H22 124.5 . . ?
C21 C23 N4 105.6(9) . . ?
C21 C23 H23 127.2 . . ?
N4 C23 H23 127.2 . . ?
C19 C24 N4 77.8(14) . . ?
C19 C24 H24A 115.6 . . ?
N4 C24 H24A 115.6 . . ?
C19 C24 H24B 115.6 . . ?
N4 C24 H24B 115.6 . . ?
H24A C24 H24B 112.6 . . ?
C17 N1 C15 106.7(8) . . ?
C17 N1 Cd1 125.3(6) . . ?
C15 N1 Cd1 127.9(6) . . ?
C16 N2 C17 106.9(7) . . ?
C16 N2 C18 124.8(8) . . ?
C17 N2 C18 128.0(8) . . ?
C22 N3 C21 104.0(7) . . ?
C22 N3 Cd1 126.6(6) . 9_454 ?
C21 N3 Cd1 129.4(6) . 9_454 ?
C23 N4 C22 109.1(9) . . ?
C23 N4 C24 123.9(10) . . ?
C22 N4 C24 123.5(12) . . ?
C1 O1 Cd1 88.8(5) . . ?
C1 O2 Cd1 92.3(4) . . ?
C9 O3 Cd1 89.1(4) . 3 ?
C9 O4 Cd1 94.7(4) . 3 ?
C8 O5 C5 118.8(6) . . ?
N3 Cd1 N1 96.0(2) 9 . ?
N3 Cd1 O4 146.3(2) 9 7_544 ?
N1 Cd1 O4 86.3(2) . 7_544 ?
N3 Cd1 O2 104.78(19) 9 . ?
N1 Cd1 O2 99.5(2) . . ?
O4 Cd1 O2 108.04(18) 7_544 . ?
N3 Cd1 O1 99.23(19) 9 . ?
N1 Cd1 O1 153.75(18) . . ?
O4 Cd1 O1 92.69(19) 7_544 . ?
O2 Cd1 O1 55.96(19) . . ?
N3 Cd1 O3 92.2(2) 9 7_544 ?
N1 Cd1 O3 100.46(19) . 7_544 ?
O4 Cd1 O3 54.50(18) 7_544 7_544 ?
O2 Cd1 O3 152.21(18) . 7_544 ?
O1 Cd1 O3 100.20(17) . 7_544 ?
N3 Cd1 C1 104.5(2) 9 . ?
N1 Cd1 C1 127.2(2) . . ?
O4 Cd1 C1 100.6(2) 7_544 . ?
O2 Cd1 C1 28.4(2) . . ?
O1 Cd1 C1 27.56(19) . . ?
O3 Cd1 C1 126.2(2) 7_544 . ?
N3 Cd1 C9 118.8(2) 9 7_544 ?
N1 Cd1 C9 92.5(2) . 7_544 ?
O4 Cd1 C9 27.56(17) 7_544 7_544 ?
O2 Cd1 C9 133.17(19) . 7_544 ?
O1 Cd1 C9 98.67(19) . 7_544 ?
O3 Cd1 C9 27.01(15) 7_544 7_544 ?
C1 Cd1 C9 117.2(2) . 7_544 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.065

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

data_compound-2
_database_code_depnum_ccdc_archive 'CCDC 693961'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C24 H22 N4 Ni O5), H2 O'
_chemical_formula_sum            'C48 H46 N8 Ni2 O11'
_chemical_formula_weight         1028.35

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 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'

_cell_length_a                   8.8554(11)
_cell_length_b                   19.877(2)
_cell_length_c                   26.017(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.727(2)
_cell_angle_gamma                90.00
_cell_volume                     4538.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6422
_cell_measurement_theta_min      1.58
_cell_measurement_theta_max      26.05

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'

_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12657
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.1292
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         26.05
_reflns_number_total             6422
_reflns_number_gt                4378
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'

_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)+(0.0243P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(16)
_refine_ls_number_reflns         6422
_refine_ls_number_parameters     628
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0854
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_restrained_S_all      0.897
_refine_ls_shift/su_max          0.005
_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 0.6150(9) 0.5882(4) 0.0316(3) 0.031(2) Uani 1 1 d . . .
H1 H 0.6226 0.5512 0.0537 0.037 Uiso 1 1 calc R . .
C2 C 0.4824(9) 0.6161(4) 0.0096(3) 0.0301(19) Uani 1 1 d . . .
H2 H 0.3843 0.6030 0.0143 0.036 Uiso 1 1 calc R . .
C3 C 0.6762(8) 0.6694(3) -0.0149(3) 0.0263(18) Uani 1 1 d . . .
H3 H 0.7322 0.7006 -0.0311 0.032 Uiso 1 1 calc R . .
C4 C 0.4145(9) 0.7119(4) -0.0523(3) 0.035(2) Uani 1 1 d . . .
H4A H 0.3452 0.6850 -0.0760 0.043 Uiso 1 1 calc R . .
H4B H 0.4697 0.7415 -0.0727 0.043 Uiso 1 1 calc R . .
C5 C 0.3237(9) 0.7537(4) -0.0182(3) 0.036(2) Uani 1 1 d . . .
H5A H 0.2373 0.7734 -0.0399 0.044 Uiso 1 1 calc R . .
H5B H 0.2840 0.7241 0.0064 0.044 Uiso 1 1 calc R . .
C6 C 0.4133(10) 0.8091(4) 0.0112(3) 0.038(2) Uani 1 1 d . . .
H6A H 0.4510 0.8403 -0.0128 0.045 Uiso 1 1 calc R . .
H6B H 0.4997 0.7904 0.0335 0.045 Uiso 1 1 calc R . .
C7 C 0.3069(10) 0.8450(4) 0.0435(3) 0.045(2) Uani 1 1 d . . .
H7A H 0.2107 0.8531 0.0218 0.054 Uiso 1 1 calc R . .
H7B H 0.2866 0.8153 0.0713 0.054 Uiso 1 1 calc R . .
C8 C 0.4194(8) 0.9610(4) 0.0401(3) 0.032(2) Uani 1 1 d . . .
H8 H 0.4438 0.9581 0.0065 0.038 Uiso 1 1 calc R . .
C9 C 0.3404(10) 0.9343(4) 0.1134(3) 0.043(2) Uani 1 1 d . . .
H9 H 0.3025 0.9108 0.1399 0.052 Uiso 1 1 calc R . .
C10 C 0.3827(10) 0.9992(4) 0.1148(3) 0.037(2) Uani 1 1 d . . .
H10 H 0.3776 1.0283 0.1425 0.044 Uiso 1 1 calc R . .
C11 C 1.1430(10) 0.6608(3) 0.1044(3) 0.0279(18) Uani 1 1 d . . .
C12 C 1.2520(9) 0.7032(3) 0.1409(3) 0.0259(18) Uani 1 1 d . . .
C13 C 1.1959(9) 0.7450(4) 0.1757(3) 0.0295(18) Uani 1 1 d . . .
H13 H 1.0916 0.7464 0.1773 0.035 Uiso 1 1 calc R . .
C14 C 1.2933(10) 0.7848(4) 0.2085(3) 0.032(2) Uani 1 1 d . . .
H14 H 1.2543 0.8123 0.2325 0.039 Uiso 1 1 calc R . .
C15 C 1.4463(10) 0.7845(4) 0.2060(3) 0.0294(19) Uani 1 1 d . . .
C16 C 1.5048(10) 0.7422(4) 0.1704(3) 0.035(2) Uani 1 1 d . . .
H16 H 1.6090 0.7409 0.1687 0.042 Uiso 1 1 calc R . .
C17 C 1.4065(9) 0.7026(4) 0.1380(3) 0.033(2) Uani 1 1 d . . .
H17 H 1.4445 0.6751 0.1139 0.039 Uiso 1 1 calc R . .
C18 C 1.5378(8) 0.8364(4) 0.2870(3) 0.0261(18) Uani 1 1 d . . .
C19 C 1.5806(9) 0.8975(4) 0.3090(3) 0.034(2) Uani 1 1 d . . .
H19 H 1.6107 0.9319 0.2884 0.041 Uiso 1 1 calc R . .
C20 C 1.5797(9) 0.9086(3) 0.3610(3) 0.0287(19) Uani 1 1 d . . .
H20 H 1.6127 0.9498 0.3753 0.034 Uiso 1 1 calc R . .
C21 C 1.5308(8) 0.8599(3) 0.3922(3) 0.0234(17) Uani 1 1 d . . .
C22 C 1.4890(8) 0.7971(3) 0.3700(3) 0.0241(17) Uani 1 1 d . . .
H22 H 1.4606 0.7629 0.3911 0.029 Uiso 1 1 calc R . .
C23 C 1.4891(8) 0.7851(3) 0.3184(3) 0.0270(18) Uani 1 1 d . . .
H23 H 1.4575 0.7437 0.3041 0.032 Uiso 1 1 calc R . .
C24 C 1.5156(8) 0.8724(4) 0.4466(3) 0.0265(18) Uani 1 1 d . . .
C25 C 0.7363(9) 0.8730(4) -0.0660(3) 0.0278(18) Uani 1 1 d . . .
C26 C 0.8039(8) 0.8884(4) -0.0121(3) 0.0240(17) Uani 1 1 d . . .
C27 C 0.8779(8) 0.8396(4) 0.0208(3) 0.0296(19) Uani 1 1 d . . .
H27 H 0.8904 0.7963 0.0085 0.036 Uiso 1 1 calc R . .
C28 C 0.9322(8) 0.8555(4) 0.0713(3) 0.0280(19) Uani 1 1 d . . .
H28 H 0.9794 0.8228 0.0934 0.034 Uiso 1 1 calc R . .
C29 C 0.9167(8) 0.9202(4) 0.0890(3) 0.0275(18) Uani 1 1 d . . .
C30 C 0.8413(8) 0.9690(3) 0.0578(3) 0.0290(19) Uani 1 1 d . . .
H30 H 0.8274 1.0119 0.0706 0.035 Uiso 1 1 calc R . .
C31 C 0.7872(8) 0.9529(3) 0.0072(3) 0.0260(17) Uani 1 1 d . . .
H31 H 0.7386 0.9858 -0.0145 0.031 Uiso 1 1 calc R . .
C32 C 0.9120(9) 0.9816(4) 0.1679(3) 0.0302(19) Uani 1 1 d . . .
C33 C 0.9965(10) 1.0331(4) 0.1928(3) 0.035(2) Uani 1 1 d . . .
H33 H 1.0964 1.0407 0.1869 0.042 Uiso 1 1 calc R . .
C34 C 0.9296(10) 1.0730(4) 0.2267(3) 0.036(2) Uani 1 1 d . . .
H34 H 0.9869 1.1074 0.2439 0.044 Uiso 1 1 calc R . .
C35 C 0.7802(9) 1.0642(4) 0.2364(3) 0.0284(19) Uani 1 1 d . . .
C36 C 0.6978(9) 1.0148(4) 0.2086(3) 0.034(2) Uani 1 1 d . . .
H36 H 0.5964 1.0086 0.2131 0.041 Uiso 1 1 calc R . .
C37 C 0.7609(10) 0.9734(4) 0.1739(3) 0.031(2) Uani 1 1 d . . .
H37 H 0.7019 0.9408 0.1550 0.037 Uiso 1 1 calc R . .
C38 C 0.7136(9) 1.1047(4) 0.2752(3) 0.0279(18) Uani 1 1 d . . .
C39 C 0.3584(9) 0.9292(4) -0.1064(3) 0.033(2) Uani 1 1 d . . .
H39 H 0.4298 0.9625 -0.0958 0.040 Uiso 1 1 calc R . .
C40 C 0.2527(9) 0.8401(4) -0.1398(3) 0.036(2) Uani 1 1 d . . .
H40 H 0.2382 0.7984 -0.1559 0.043 Uiso 1 1 calc R . .
C41 C 0.1427(10) 0.8778(4) -0.1236(3) 0.041(2) Uani 1 1 d . . .
H41 H 0.0393 0.8678 -0.1274 0.050 Uiso 1 1 calc R . .
C42 C 0.1341(10) 0.9919(4) -0.0802(3) 0.043(2) Uani 1 1 d . . .
H42A H 0.2111 1.0224 -0.0635 0.052 Uiso 1 1 calc R . .
H42B H 0.0728 0.9768 -0.0543 0.052 Uiso 1 1 calc R . .
C43 C 0.0341(13) 1.0293(5) -0.1220(4) 0.075(3) Uani 1 1 d . . .
H43A H -0.0563 1.0029 -0.1334 0.090 Uiso 1 1 calc R . .
H43B H 0.0019 1.0715 -0.1082 0.090 Uiso 1 1 calc R . .
C44 C 0.1153(18) 1.0424(7) -0.1654(5) 0.140(6) Uani 1 1 d DU . .
H44A H 0.2156 1.0566 -0.1495 0.167 Uiso 1 1 calc R . .
H44B H 0.1299 0.9982 -0.1797 0.167 Uiso 1 1 calc R . .
C45 C 0.0842(15) 1.0850(5) -0.2105(5) 0.099(4) Uani 1 1 d DU . .
H45A H 0.0062 1.0633 -0.2346 0.118 Uiso 1 1 calc R . .
H45B H 0.1758 1.0871 -0.2271 0.118 Uiso 1 1 calc R . .
C46 C -0.0718(12) 1.1775(5) -0.2367(3) 0.063(3) Uani 1 1 d . . .
H46 H -0.1331 1.1547 -0.2629 0.075 Uiso 1 1 calc R . .
C47 C -0.0754(10) 1.2435(4) -0.2256(3) 0.045(2) Uani 1 1 d . . .
H47 H -0.1402 1.2746 -0.2439 0.054 Uiso 1 1 calc R . .
C48 C 0.0965(11) 1.2015(4) -0.1709(3) 0.042(2) Uani 1 1 d . . .
H48 H 0.1748 1.1959 -0.1436 0.050 Uiso 1 1 calc R . .
N1 N 0.7378(7) 0.6225(3) 0.0164(2) 0.0224(14) Uani 1 1 d . . .
N2 N 0.5221(7) 0.6677(3) -0.0210(2) 0.0244(14) Uani 1 1 d . . .
N3 N 0.3630(7) 0.9090(3) 0.0662(2) 0.0364(17) Uani 1 1 d . . .
N4 N 0.4348(7) 1.0159(3) 0.0690(2) 0.0294(16) Uani 1 1 d . . .
N5 N 0.3905(7) 0.8727(3) -0.1289(2) 0.0258(15) Uani 1 1 d . . .
N6 N 0.2103(8) 0.9331(3) -0.1005(2) 0.0324(16) Uani 1 1 d . . .
N7 N 0.0291(7) 1.2582(3) -0.1839(2) 0.0304(15) Uani 1 1 d . . .
N8 N 0.0361(11) 1.1520(3) -0.2028(3) 0.056(2) Uani 1 1 d . . .
O1 O 1.0006(6) 0.6659(2) 0.10429(19) 0.0326(14) Uani 1 1 d . . .
O2 O 1.1960(6) 0.6229(2) 0.07193(17) 0.0297(13) Uani 1 1 d . . .
O1W O 0.8405(7) 0.6299(4) 0.1927(3) 0.0632(19) Uani 1 1 d D . .
HW12 H 0.911(7) 0.615(5) 0.216(2) 0.076 Uiso 1 1 d D . .
HW11 H 0.886(8) 0.644(5) 0.168(2) 0.076 Uiso 1 1 d D . .
O3 O 1.5030(6) 0.8228(2) 0.47777(18) 0.0259(12) Uani 1 1 d . . .
O4 O 1.5076(6) 0.9316(2) 0.46429(17) 0.0313(13) Uani 1 1 d . . .
O5 O 0.7112(6) 0.8123(2) -0.08095(17) 0.0309(13) Uani 1 1 d . . .
O6 O 0.7002(6) 0.9203(2) -0.09847(18) 0.0314(13) Uani 1 1 d . . .
O7 O 0.5741(6) 1.0962(3) 0.28002(19) 0.0351(14) Uani 1 1 d . . .
O8 O 0.7973(6) 1.1424(2) 0.30610(19) 0.0335(13) Uani 1 1 d . . .
O9 O 0.9807(6) 0.9346(3) 0.13952(17) 0.0356(14) Uani 1 1 d . . .
O10 O 1.5476(6) 0.8272(2) 0.23486(18) 0.0417(15) Uani 1 1 d . . .
Ni1 Ni 0.96558(9) 0.60669(4) 0.03678(4) 0.0243(2) Uani 1 1 d . . .
Ni2 Ni 0.59684(10) 0.84850(4) -0.15214(4) 0.0264(2) 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 C2 1.354(10) . ?
C1 N1 1.386(8) . ?
C1 H1 0.9300 . ?
C2 N2 1.373(8) . ?
C2 H2 0.9300 . ?
C3 N1 1.307(8) . ?
C3 N2 1.353(9) . ?
C3 H3 0.9300 . ?
C4 N2 1.460(8) . ?
C4 C5 1.521(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.505(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.523(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.460(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N4 1.323(8) . ?
C8 N3 1.367(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.342(9) . ?
C9 N3 1.366(8) . ?
C9 H9 0.9300 . ?
C10 N4 1.375(8) . ?
C10 H10 0.9300 . ?
C11 O1 1.265(9) . ?
C11 O2 1.268(8) . ?
C11 C12 1.515(9) . ?
C11 Ni1 2.446(7) . ?
C12 C13 1.370(9) . ?
C12 C17 1.380(10) . ?
C13 C14 1.378(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.365(11) . ?
C14 H14 0.9300 . ?
C15 O10 1.382(8) . ?
C15 C16 1.401(10) . ?
C16 C17 1.374(10) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.374(9) . ?
C18 O10 1.382(7) . ?
C18 C23 1.411(9) . ?
C19 C20 1.372(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.370(9) . ?
C20 H20 0.9300 . ?
C21 C22 1.403(9) . ?
C21 C24 1.462(9) . ?
C22 C23 1.365(8) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O4 1.270(7) . ?
C24 O3 1.290(7) . ?
C24 Ni1 2.480(7) 4_565 ?
C25 O6 1.274(8) . ?
C25 O5 1.278(7) . ?
C25 C26 1.481(9) . ?
C25 Ni2 2.457(8) . ?
C26 C31 1.392(9) . ?
C26 C27 1.398(9) . ?
C27 C28 1.373(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.379(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.378(9) . ?
C29 O9 1.390(8) . ?
C30 C31 1.376(9) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C37 1.378(10) . ?
C32 C33 1.376(10) . ?
C32 O9 1.382(8) . ?
C33 C34 1.378(10) . ?
C33 H33 0.9300 . ?
C34 C35 1.390(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.371(10) . ?
C35 C38 1.475(9) . ?
C36 C37 1.392(9) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O8 1.263(8) . ?
C38 O7 1.271(8) . ?
C38 Ni2 2.457(8) 2_575 ?
C39 N5 1.317(8) . ?
C39 N6 1.343(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.342(10) . ?
C40 N5 1.377(9) . ?
C40 H40 0.9300 . ?
C41 N6 1.352(9) . ?
C41 H41 0.9300 . ?
C42 N6 1.483(8) . ?
C42 C43 1.503(11) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.443(13) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.442(9) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 N8 1.420(11) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 N8 1.313(11) . ?
C46 C47 1.344(11) . ?
C46 H46 0.9300 . ?
C47 N7 1.360(9) . ?
C47 H47 0.9300 . ?
C48 N7 1.299(9) . ?
C48 N8 1.351(10) . ?
C48 H48 0.9300 . ?
N1 Ni1 2.040(6) . ?
N4 Ni1 2.023(6) 3_455 ?
N5 Ni2 2.057(6) . ?
N7 Ni2 2.032(6) 3_455 ?
O1 Ni1 2.102(5) . ?
O2 Ni1 2.145(5) . ?
O1W HW12 0.86(6) . ?
O1W HW11 0.85(7) . ?
O3 Ni1 2.137(5) 4_565 ?
O4 Ni1 2.113(5) 4_565 ?
O5 Ni2 2.114(5) . ?
O6 Ni2 2.117(5) . ?
O7 Ni2 2.066(5) 2_575 ?
O8 Ni2 2.210(5) 2_575 ?
Ni1 N4 2.023(6) 3_545 ?
Ni1 O4 2.113(5) 4_464 ?
Ni1 O3 2.137(5) 4_464 ?
Ni1 C24 2.480(7) 4_464 ?
Ni2 N7 2.032(6) 3_545 ?
Ni2 O7 2.066(5) 2_574 ?
Ni2 O8 2.210(5) 2_574 ?
Ni2 C38 2.457(8) 2_574 ?

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 110.4(6) . . ?
C2 C1 H1 124.8 . . ?
N1 C1 H1 124.8 . . ?
C1 C2 N2 106.0(7) . . ?
C1 C2 H2 127.0 . . ?
N2 C2 H2 127.0 . . ?
N1 C3 N2 112.6(6) . . ?
N1 C3 H3 123.7 . . ?
N2 C3 H3 123.7 . . ?
N2 C4 C5 111.2(6) . . ?
N2 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N2 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C4 114.3(7) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 C7 107.5(7) . . ?
C5 C6 H6A 110.2 . . ?
C7 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
C7 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
N3 C7 C6 115.5(6) . . ?
N3 C7 H7A 108.4 . . ?
C6 C7 H7A 108.4 . . ?
N3 C7 H7B 108.4 . . ?
C6 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
N4 C8 N3 111.0(7) . . ?
N4 C8 H8 124.5 . . ?
N3 C8 H8 124.5 . . ?
C10 C9 N3 107.7(7) . . ?
C10 C9 H9 126.1 . . ?
N3 C9 H9 126.1 . . ?
C9 C10 N4 109.5(7) . . ?
C9 C10 H10 125.2 . . ?
N4 C10 H10 125.2 . . ?
O1 C11 O2 120.2(7) . . ?
O1 C11 C12 120.5(7) . . ?
O2 C11 C12 119.1(7) . . ?
O1 C11 Ni1 59.3(4) . . ?
O2 C11 Ni1 61.2(4) . . ?
C12 C11 Ni1 171.4(5) . . ?
C13 C12 C17 119.4(7) . . ?
C13 C12 C11 119.6(7) . . ?
C17 C12 C11 120.9(7) . . ?
C12 C13 C14 120.3(7) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.7(7) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 O10 123.2(7) . . ?
C14 C15 C16 119.4(7) . . ?
O10 C15 C16 117.2(7) . . ?
C17 C16 C15 119.2(8) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C12 120.9(7) . . ?
C16 C17 H17 119.6 . . ?
C12 C17 H17 119.6 . . ?
C19 C18 O10 118.5(6) . . ?
C19 C18 C23 119.1(6) . . ?
O10 C18 C23 122.5(6) . . ?
C20 C19 C18 121.1(7) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C19 120.9(7) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 118.2(6) . . ?
C20 C21 C24 122.1(6) . . ?
C22 C21 C24 119.7(6) . . ?
C23 C22 C21 121.7(6) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C22 C23 C18 118.9(7) . . ?
C22 C23 H23 120.5 . . ?
C18 C23 H23 120.5 . . ?
O4 C24 O3 117.9(6) . . ?
O4 C24 C21 121.6(6) . . ?
O3 C24 C21 120.4(6) . . ?
O4 C24 Ni1 58.4(4) . 4_565 ?
O3 C24 Ni1 59.5(4) . 4_565 ?
C21 C24 Ni1 175.0(5) . 4_565 ?
O6 C25 O5 118.5(7) . . ?
O6 C25 C26 120.5(7) . . ?
O5 C25 C26 121.0(6) . . ?
O6 C25 Ni2 59.5(4) . . ?
O5 C25 Ni2 59.3(4) . . ?
C26 C25 Ni2 173.7(5) . . ?
C31 C26 C27 118.8(7) . . ?
C31 C26 C25 119.0(6) . . ?
C27 C26 C25 122.2(7) . . ?
C28 C27 C26 120.1(7) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.7(7) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 121.5(7) . . ?
C28 C29 O9 117.5(6) . . ?
C30 C29 O9 121.0(7) . . ?
C31 C30 C29 118.6(7) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
C30 C31 C26 121.3(7) . . ?
C30 C31 H31 119.3 . . ?
C26 C31 H31 119.3 . . ?
C37 C32 C33 120.7(7) . . ?
C37 C32 O9 119.0(7) . . ?
C33 C32 O9 120.2(7) . . ?
C32 C33 C34 118.4(8) . . ?
C32 C33 H33 120.8 . . ?
C34 C33 H33 120.8 . . ?
C33 C34 C35 123.1(8) . . ?
C33 C34 H34 118.5 . . ?
C35 C34 H34 118.5 . . ?
C36 C35 C34 116.5(7) . . ?
C36 C35 C38 121.2(8) . . ?
C34 C35 C38 122.2(7) . . ?
C35 C36 C37 122.3(8) . . ?
C35 C36 H36 118.9 . . ?
C37 C36 H36 118.9 . . ?
C32 C37 C36 118.9(7) . . ?
C32 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
O8 C38 O7 120.7(7) . . ?
O8 C38 C35 120.3(7) . . ?
O7 C38 C35 118.6(7) . . ?
O8 C38 Ni2 63.7(4) . 2_575 ?
O7 C38 Ni2 57.2(4) . 2_575 ?
C35 C38 Ni2 169.1(5) . 2_575 ?
N5 C39 N6 111.8(7) . . ?
N5 C39 H39 124.1 . . ?
N6 C39 H39 124.1 . . ?
C41 C40 N5 109.5(7) . . ?
C41 C40 H40 125.3 . . ?
N5 C40 H40 125.3 . . ?
C40 C41 N6 107.3(8) . . ?
C40 C41 H41 126.4 . . ?
N6 C41 H41 126.4 . . ?
N6 C42 C43 112.7(7) . . ?
N6 C42 H42A 109.1 . . ?
C43 C42 H42A 109.1 . . ?
N6 C42 H42B 109.1 . . ?
C43 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?
C44 C43 C42 110.3(10) . . ?
C44 C43 H43A 109.6 . . ?
C42 C43 H43A 109.6 . . ?
C44 C43 H43B 109.6 . . ?
C42 C43 H43B 109.6 . . ?
H43A C43 H43B 108.1 . . ?
C45 C44 C43 133.0(12) . . ?
C45 C44 H44A 104.0 . . ?
C43 C44 H44A 104.0 . . ?
C45 C44 H44B 104.0 . . ?
C43 C44 H44B 104.0 . . ?
H44A C44 H44B 105.4 . . ?
C44 C45 N8 117.6(10) . . ?
C44 C45 H45A 107.9 . . ?
N8 C45 H45A 107.9 . . ?
C44 C45 H45B 107.9 . . ?
N8 C45 H45B 107.9 . . ?
H45A C45 H45B 107.2 . . ?
N8 C46 C47 105.6(8) . . ?
N8 C46 H46 127.2 . . ?
C47 C46 H46 127.2 . . ?
C46 C47 N7 110.4(8) . . ?
C46 C47 H47 124.8 . . ?
N7 C47 H47 124.8 . . ?
N7 C48 N8 110.0(8) . . ?
N7 C48 H48 125.0 . . ?
N8 C48 H48 125.0 . . ?
C3 N1 C1 104.5(6) . . ?
C3 N1 Ni1 126.0(5) . . ?
C1 N1 Ni1 129.5(5) . . ?
C3 N2 C2 106.5(6) . . ?
C3 N2 C4 128.5(6) . . ?
C2 N2 C4 125.0(6) . . ?
C9 N3 C8 106.0(6) . . ?
C9 N3 C7 127.0(6) . . ?
C8 N3 C7 125.7(7) . . ?
C8 N4 C10 105.8(6) . . ?
C8 N4 Ni1 120.6(5) . 3_455 ?
C10 N4 Ni1 130.9(5) . 3_455 ?
C39 N5 C40 104.8(7) . . ?
C39 N5 Ni2 125.7(5) . . ?
C40 N5 Ni2 128.9(5) . . ?
C39 N6 C41 106.5(7) . . ?
C39 N6 C42 125.7(7) . . ?
C41 N6 C42 127.1(7) . . ?
C48 N7 C47 105.1(7) . . ?
C48 N7 Ni2 124.0(6) . 3_455 ?
C47 N7 Ni2 130.3(6) . 3_455 ?
C46 N8 C48 108.8(8) . . ?
C46 N8 C45 118.2(9) . . ?
C48 N8 C45 132.0(10) . . ?
C11 O1 Ni1 89.6(4) . . ?
C11 O2 Ni1 87.6(4) . . ?
HW12 O1W HW11 106(3) . . ?
C24 O3 Ni1 89.1(4) . 4_565 ?
C24 O4 Ni1 90.8(4) . 4_565 ?
C25 O5 Ni2 89.3(4) . . ?
C25 O6 Ni2 89.3(4) . . ?
C38 O7 Ni2 91.7(5) . 2_575 ?
C38 O8 Ni2 85.4(5) . 2_575 ?
C32 O9 C29 119.5(6) . . ?
C15 O10 C18 119.5(6) . . ?
N4 Ni1 N1 93.6(2) 3_545 . ?
N4 Ni1 O1 99.5(2) 3_545 . ?
N1 Ni1 O1 99.2(2) . . ?
N4 Ni1 O4 95.7(2) 3_545 4_464 ?
N1 Ni1 O4 96.3(2) . 4_464 ?
O1 Ni1 O4 157.5(2) . 4_464 ?
N4 Ni1 O3 157.7(2) 3_545 4_464 ?
N1 Ni1 O3 87.4(2) . 4_464 ?
O1 Ni1 O3 102.30(19) . 4_464 ?
O4 Ni1 O3 62.13(18) 4_464 4_464 ?
N4 Ni1 O2 97.5(2) 3_545 . ?
N1 Ni1 O2 159.74(19) . . ?
O1 Ni1 O2 62.25(19) . . ?
O4 Ni1 O2 99.39(19) 4_464 . ?
O3 Ni1 O2 88.68(18) 4_464 . ?
N4 Ni1 C11 101.7(2) 3_545 . ?
N1 Ni1 C11 129.5(2) . . ?
O1 Ni1 C11 31.1(2) . . ?
O4 Ni1 C11 128.9(2) 4_464 . ?
O3 Ni1 C11 94.7(2) 4_464 . ?
O2 Ni1 C11 31.2(2) . . ?
N4 Ni1 C24 126.4(2) 3_545 4_464 ?
N1 Ni1 C24 91.4(2) . 4_464 ?
O1 Ni1 C24 132.1(2) . 4_464 ?
O4 Ni1 C24 30.81(18) 4_464 4_464 ?
O3 Ni1 C24 31.34(18) 4_464 4_464 ?
O2 Ni1 C24 95.6(2) . 4_464 ?
C11 Ni1 C24 115.3(2) . 4_464 ?
N7 Ni2 N5 95.8(2) 3_545 . ?
N7 Ni2 O7 97.6(2) 3_545 2_574 ?
N5 Ni2 O7 97.9(2) . 2_574 ?
N7 Ni2 O5 97.9(2) 3_545 . ?
N5 Ni2 O5 99.3(2) . . ?
O7 Ni2 O5 155.5(2) 2_574 . ?
N7 Ni2 O6 160.3(2) 3_545 . ?
N5 Ni2 O6 88.4(2) . . ?
O7 Ni2 O6 100.9(2) 2_574 . ?
O5 Ni2 O6 62.46(18) . . ?
N7 Ni2 O8 94.9(2) 3_545 2_574 ?
N5 Ni2 O8 158.31(19) . 2_574 ?
O7 Ni2 O8 61.9(2) 2_574 2_574 ?
O5 Ni2 O8 97.86(19) . 2_574 ?
O6 Ni2 O8 87.94(18) . 2_574 ?
N7 Ni2 C38 98.8(2) 3_545 2_574 ?
N5 Ni2 C38 128.3(2) . 2_574 ?
O7 Ni2 C38 31.1(2) 2_574 2_574 ?
O5 Ni2 C38 127.0(2) . 2_574 ?
O6 Ni2 C38 93.6(2) . 2_574 ?
O8 Ni2 C38 30.8(2) 2_574 2_574 ?
N7 Ni2 C25 129.1(2) 3_545 . ?
N5 Ni2 C25 92.5(2) . . ?
O7 Ni2 C25 130.8(2) 2_574 . ?
O5 Ni2 C25 31.34(19) . . ?
O6 Ni2 C25 31.24(19) . . ?
O8 Ni2 C25 95.4(2) 2_574 . ?
C38 Ni2 C25 114.5(2) 2_574 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.074

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

data_compound-3
_database_code_depnum_ccdc_archive 'CCDC 693962'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H22 Co N4 O4, 0.25(O4)'
_chemical_formula_sum            'C26 H24 Co N4 O5'
_chemical_formula_weight         531.42

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 2/c'
_symmetry_space_group_name_Hall  '-P 2yc'

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

_cell_length_a                   12.999(3)
_cell_length_b                   6.7152(14)
_cell_length_c                   16.547(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.999(4)
_cell_angle_gamma                90.00
_cell_volume                     1436.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2748
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      26.04

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             550
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'

_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7582
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_sigmaI/netI    0.1223
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         26.04
_reflns_number_total             2748
_reflns_number_gt                1802
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'

_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)+(0.1077P)²+3.6704P] 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         2748
_refine_ls_number_parameters     186
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1473
_refine_ls_R_factor_gt           0.0950
_refine_ls_wR_factor_ref         0.2474
_refine_ls_wR_factor_gt          0.2125
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.21765(17) 0.7500 0.0287(4) Uani 1 2 d S . .
N1 N -0.0716(4) 0.3969(8) 0.8254(3) 0.0428(14) Uani 1 1 d . . .
N2 N -0.1041(6) 0.6318(11) 0.9130(4) 0.069(2) Uani 1 1 d . . .
O1 O -0.1384(7) 0.1840(14) 0.6612(4) 0.130(4) Uani 1 1 d . . .
C2 C -0.2406(5) -0.1035(11) 0.6410(4) 0.0491(18) Uani 1 1 d . . .
O2 O -0.1131(8) -0.0333(11) 0.7488(6) 0.161(5) Uani 1 1 d . . .
C3 C -0.2533(7) -0.2996(13) 0.6610(5) 0.067(2) Uani 1 1 d . . .
H3 H -0.2127 -0.3530 0.7054 0.081 Uiso 1 1 calc R . .
C12 C 0.0009(8) 0.9075(13) 0.9749(5) 0.077(3) Uani 1 1 d D . .
H12A H 0.0242 0.9408 0.9227 0.093 Uiso 1 1 calc R . .
H12B H 0.0502 0.8144 1.0019 0.093 Uiso 1 1 calc R . .
C7 C -0.3027(7) -0.0292(13) 0.5756(5) 0.066(2) Uani 1 1 d . . .
H7 H -0.2947 0.1031 0.5607 0.079 Uiso 1 1 calc R . .
C5 C -0.3884(7) -0.3433(17) 0.5529(7) 0.084(3) Uani 1 1 d . . .
C1 C -0.1587(7) 0.0262(14) 0.6877(6) 0.068(3) Uani 1 1 d . . .
C10 C -0.0400(7) 0.5652(12) 0.8597(5) 0.067(2) Uani 1 1 d . . .
H10 H 0.0198 0.6313 0.8487 0.081 Uiso 1 1 calc R . .
C4 C -0.3237(8) -0.4177(14) 0.6176(6) 0.079(3) Uani 1 1 d . . .
H4 H -0.3284 -0.5512 0.6317 0.095 Uiso 1 1 calc R . .
C6 C -0.3766(7) -0.1443(17) 0.5312(6) 0.085(3) Uani 1 1 d . . .
H6 H -0.4179 -0.0899 0.4874 0.102 Uiso 1 1 calc R . .
C9 C -0.1815(8) 0.5039(13) 0.9115(7) 0.085(3) Uani 1 1 d . . .
H9 H -0.2381 0.5106 0.9415 0.102 Uiso 1 1 calc R . .
C11 C -0.1005(9) 0.8120(18) 0.9617(9) 0.131(5) Uani 1 1 d D . .
H11A H -0.1232 0.7800 1.0142 0.157 Uiso 1 1 calc R . .
H11B H -0.1493 0.9069 0.9354 0.157 Uiso 1 1 calc R . .
C8 C -0.1620(7) 0.3635(14) 0.8584(6) 0.081(3) Uani 1 1 d . . .
H8 H -0.2051 0.2551 0.8453 0.097 Uiso 1 1 calc R . .
O1W O -0.432(2) -0.314(5) 0.8037(19) 0.110(9) Uani 0.25 1 d PU . .
O2W O -0.437(2) -0.124(4) 0.3029(16) 0.091(8) Uani 0.25 1 d PU . .
C13' C -0.4799(19) -0.403(3) 0.4899(15) 0.058(5) Uani 0.50 1 d P . .
C13 C -0.4632(17) -0.517(5) 0.5253(13) 0.064(5) Uani 0.50 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
Co1 N1 2.028(5) 2_556 ?
Co1 N1 2.028(5) . ?
Co1 O1 2.212(8) . ?
Co1 O1 2.212(8) 2_556 ?
Co1 O2 2.235(10) . ?
Co1 O2 2.235(10) 2_556 ?
N1 C10 1.312(9) . ?
N1 C8 1.366(10) . ?
N2 C9 1.321(11) . ?
N2 C10 1.351(10) . ?
N2 C11 1.451(11) . ?
O1 C1 1.186(11) . ?
C2 C3 1.373(11) . ?
C2 C7 1.374(11) . ?
C2 C1 1.523(11) . ?
O2 C1 1.186(12) . ?
C3 C4 1.358(11) . ?
C3 H3 0.9300 . ?
C12 C11 1.462(9) . ?
C12 C12 1.496(15) 3_577 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C7 C6 1.384(11) . ?
C7 H7 0.9300 . ?
C5 C4 1.384(14) . ?
C5 C6 1.397(15) . ?
C5 C13' 1.55(3) . ?
C5 C13 1.56(3) . ?
C10 H10 0.9300 . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
C9 C8 1.331(12) . ?
C9 H9 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C8 H8 0.9300 . ?
C13' C13 0.93(2) 3_446 ?
C13' C13 0.97(2) . ?
C13' C13' 1.46(3) 3_446 ?
C13 C13' 0.93(2) 3_446 ?
C13 C13 1.22(4) 3_446 ?

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
N1 Co1 N1 107.2(3) 2_556 . ?
N1 Co1 O1 92.6(2) 2_556 . ?
N1 Co1 O1 94.3(3) . . ?
N1 Co1 O1 94.3(3) 2_556 2_556 ?
N1 Co1 O1 92.6(2) . 2_556 ?
O1 Co1 O1 168.3(5) . 2_556 ?
N1 Co1 O2 141.8(3) 2_556 . ?
N1 Co1 O2 96.3(3) . . ?
O1 Co1 O2 55.1(3) . . ?
O1 Co1 O2 114.7(3) 2_556 . ?
N1 Co1 O2 96.3(3) 2_556 2_556 ?
N1 Co1 O2 141.8(3) . 2_556 ?
O1 Co1 O2 114.7(3) . 2_556 ?
O1 Co1 O2 55.1(3) 2_556 2_556 ?
O2 Co1 O2 82.1(5) . 2_556 ?
C10 N1 C8 102.2(6) . . ?
C10 N1 Co1 129.4(5) . . ?
C8 N1 Co1 128.2(5) . . ?
C9 N2 C10 107.1(7) . . ?
C9 N2 C11 122.2(8) . . ?
C10 N2 C11 130.6(8) . . ?
C1 O1 Co1 92.4(7) . . ?
C3 C2 C7 117.6(7) . . ?
C3 C2 C1 121.4(8) . . ?
C7 C2 C1 120.9(8) . . ?
C1 O2 Co1 91.3(8) . . ?
C4 C3 C2 121.6(9) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C11 C12 C12 112.4(10) . 3_577 ?
C11 C12 H12A 109.1 . . ?
C12 C12 H12A 109.1 3_577 . ?
C11 C12 H12B 109.1 . . ?
C12 C12 H12B 109.1 3_577 . ?
H12A C12 H12B 107.9 . . ?
C2 C7 C6 122.2(9) . . ?
C2 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C4 C5 C6 118.0(8) . . ?
C4 C5 C13' 142.1(12) . . ?
C6 C5 C13' 99.9(13) . . ?
C4 C5 C13 105.6(14) . . ?
C6 C5 C13 136.4(15) . . ?
C13' C5 C13 36.6(9) . . ?
O2 C1 O1 120.3(10) . . ?
O2 C1 C2 120.1(10) . . ?
O1 C1 C2 119.6(10) . . ?
N1 C10 N2 112.4(7) . . ?
N1 C10 H10 123.8 . . ?
N2 C10 H10 123.8 . . ?
C3 C4 C5 121.4(9) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C7 C6 C5 119.2(10) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N2 C9 C8 106.0(8) . . ?
N2 C9 H9 127.0 . . ?
C8 C9 H9 127.0 . . ?
N2 C11 C12 115.2(8) . . ?
N2 C11 H11A 108.5 . . ?
C12 C11 H11A 108.5 . . ?
N2 C11 H11B 108.5 . . ?
C12 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C9 C8 N1 112.3(8) . . ?
C9 C8 H8 123.8 . . ?
N1 C8 H8 123.8 . . ?
C13 C13' C13 80(3) 3_446 . ?
C13 C13' C13' 41.2(19) 3_446 3_446 ?
C13 C13' C13' 38.9(14) . 3_446 ?
C13 C13' C5 150(4) 3_446 . ?
C13 C13' C5 72(3) . . ?
C13' C13' C5 110(3) 3_446 . ?
C13' C13 C13' 100(3) 3_446 . ?
C13' C13 C13 51.6(17) 3_446 3_446 ?
C13' C13 C13 48(2) . 3_446 ?
C13' C13 C5 166(3) 3_446 . ?
C13' C13 C5 71(3) . . ?
C13 C13 C5 119(4) 3_446 . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.097

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

data_compound-4
_database_code_depnum_ccdc_archive 'CCDC 693963'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C52 H48 Co2 N8 O8), 3(H2O)'
_chemical_formula_sum            'C104 H99 Co4 N16 O19'
_chemical_formula_weight         2112.71

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           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                   8.6765(9)
_cell_length_b                   11.9414(12)
_cell_length_c                   24.044(2)
_cell_angle_alpha                81.697(2)
_cell_angle_beta                 88.455(2)
_cell_angle_gamma                84.325(2)
_cell_volume                     2452.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9489
_cell_measurement_theta_min      1.71
_cell_measurement_theta_max      26.05

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1095
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'

_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13946
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         26.05
_reflns_number_total             9489
_reflns_number_gt                6468
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'

_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)+(0.0558P)²+0.5759P] 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         9489
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1501
_refine_ls_wR_factor_gt          0.1296
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
Co1 Co 0.77538(6) 0.30717(5) 0.98388(2) 0.02304(16) Uani 1 1 d . . .
Co2 Co -0.38356(7) 0.68205(5) 1.54264(2) 0.02579(17) Uani 1 1 d . . .
O5 O -0.2912(3) 0.7866(3) 1.44583(12) 0.0329(7) Uani 1 1 d . . .
O2 O 0.6266(3) 0.2183(3) 1.06674(13) 0.0354(8) Uani 1 1 d . . .
O6 O -0.2491(3) 0.6091(2) 1.48785(12) 0.0304(7) Uani 1 1 d . . .
O1 O 0.6712(3) 0.3974(3) 1.04045(12) 0.0328(7) Uani 1 1 d . . .
O3 O 0.6212(4) 0.2637(2) 0.93417(12) 0.0331(8) Uani 1 1 d . . .
O4 O 0.8029(4) 0.2143(3) 0.87230(14) 0.0423(8) Uani 1 1 d . . .
N6 N 1.1815(4) 0.1143(3) 1.03697(16) 0.0316(9) Uani 1 1 d . . .
N5 N 0.9456(4) 0.1900(3) 1.01528(14) 0.0256(8) Uani 1 1 d . . .
C21 C 0.3330(5) 0.4214(4) 1.21317(18) 0.0279(10) Uani 1 1 d . . .
N3 N 1.4624(4) 0.4450(3) 0.67188(15) 0.0321(9) Uani 1 1 d . . .
C18 C 0.5162(5) 0.3554(4) 1.12320(18) 0.0290(10) Uani 1 1 d . . .
C28 C -0.0420(5) 0.5484(4) 1.40497(18) 0.0283(10) Uani 1 1 d . . .
H28 H -0.0507 0.4982 1.4380 0.034 Uiso 1 1 calc R . .
N4 N 1.5711(4) 0.5453(3) 0.60015(14) 0.0279(8) Uani 1 1 d . . .
N2 N 1.0095(4) 0.5364(3) 0.87127(14) 0.0309(9) Uani 1 1 d . . .
C38 C 0.8686(6) 0.5447(4) 0.94674(19) 0.0387(12) Uani 1 1 d . . .
H38 H 0.8142 0.5720 0.9766 0.046 Uiso 1 1 calc R . .
C29 C -0.1253(5) 0.6547(4) 1.39976(17) 0.0246(10) Uani 1 1 d . . .
N1 N 0.8842(4) 0.4333(3) 0.93763(14) 0.0284(8) Uani 1 1 d . . .
C25 C 0.1690(5) 0.5572(4) 1.26535(18) 0.0300(10) Uani 1 1 d . . .
H25 H 0.1880 0.6152 1.2365 0.036 Uiso 1 1 calc R . .
C22 C 0.2345(5) 0.4538(4) 1.25995(17) 0.0280(10) Uani 1 1 d . . .
H22 H 0.2159 0.3959 1.2889 0.034 Uiso 1 1 calc R . .
C32 C -0.0125(5) 0.6964(4) 1.30758(17) 0.0304(10) Uani 1 1 d . . .
H32 H -0.0023 0.7476 1.2750 0.037 Uiso 1 1 calc R . .
C23 C 0.3731(5) 0.4996(4) 1.16782(18) 0.0334(11) Uani 1 1 d . . .
H23 H 0.3373 0.5758 1.1670 0.040 Uiso 1 1 calc R . .
C30 C -0.2301(5) 0.6875(4) 1.44659(18) 0.0283(10) Uani 1 1 d . . .
C46 C 1.5255(5) 0.3698(4) 0.63785(19) 0.0377(12) Uani 1 1 d . . .
H46 H 1.5234 0.2912 0.6437 0.045 Uiso 1 1 calc R . .
C24 C 0.4640(5) 0.4671(4) 1.12437(18) 0.0349(11) Uani 1 1 d . . .
H24 H 0.4908 0.5219 1.0951 0.042 Uiso 1 1 calc R . .
C43 C 1.2821(5) 0.5118(4) 0.74486(17) 0.0363(12) Uani 1 1 d . . .
H43A H 1.2089 0.5423 0.7155 0.044 Uiso 1 1 calc R . .
H43B H 1.3445 0.5718 0.7511 0.044 Uiso 1 1 calc R . .
C1 C 0.6668(6) 0.2232(4) 0.8893(2) 0.0327(11) Uani 1 1 d . . .
C13 C -0.1625(5) -0.1535(4) 0.65580(18) 0.0313(11) Uani 1 1 d . . .
C26 C 0.0698(5) 0.5893(4) 1.31201(17) 0.0264(10) Uani 1 1 d . . .
C41 C 1.0993(6) 0.5706(4) 0.81989(19) 0.0399(12) Uani 1 1 d . . .
H41A H 1.1677 0.6260 0.8274 0.048 Uiso 1 1 calc R . .
H41B H 1.0286 0.6071 0.7907 0.048 Uiso 1 1 calc R . .
C44 C 1.3859(6) 0.4137(4) 0.72633(18) 0.0387(12) Uani 1 1 d . . .
H44A H 1.4642 0.3877 0.7545 0.046 Uiso 1 1 calc R . .
H44B H 1.3244 0.3511 0.7237 0.046 Uiso 1 1 calc R . .
C19 C 0.4801(5) 0.2753(4) 1.1684(2) 0.0379(12) Uani 1 1 d . . .
H19 H 0.5159 0.1992 1.1688 0.046 Uiso 1 1 calc R . .
C27 C 0.0537(5) 0.5155(4) 1.36215(17) 0.0278(10) Uani 1 1 d . . .
H27 H 0.1078 0.4437 1.3667 0.033 Uiso 1 1 calc R . .
C34 C 1.0828(5) 0.0502(4) 1.0697(2) 0.0354(11) Uani 1 1 d . . .
H34 H 1.1098 -0.0133 1.0960 0.042 Uiso 1 1 calc R . .
C45 C 1.4928(5) 0.5492(4) 0.64801(17) 0.0290(10) Uani 1 1 d . . .
H45 H 1.4628 0.6156 0.6631 0.035 Uiso 1 1 calc R . .
C35 C 1.0951(5) 0.1961(4) 1.00488(18) 0.0288(10) Uani 1 1 d . . .
H35 H 1.1352 0.2508 0.9784 0.035 Uiso 1 1 calc R . .
C14 C -0.2028(6) -0.0809(4) 0.69478(19) 0.0417(13) Uani 1 1 d . . .
H14 H -0.3068 -0.0599 0.7018 0.050 Uiso 1 1 calc R . .
C42 C 1.1947(5) 0.4725(4) 0.79860(18) 0.0377(12) Uani 1 1 d . . .
H42A H 1.1272 0.4162 0.7916 0.045 Uiso 1 1 calc R . .
H42B H 1.2680 0.4370 0.8271 0.045 Uiso 1 1 calc R . .
C17 C 0.6101(5) 0.3193(4) 1.07438(18) 0.0286(10) Uani 1 1 d . . .
C40 C 0.9696(5) 0.4315(4) 0.89147(17) 0.0292(10) Uani 1 1 d . . .
H40 H 0.9984 0.3666 0.8750 0.035 Uiso 1 1 calc R . .
C37 C 1.4123(4) 0.0071(4) 1.00073(19) 0.0293(10) Uani 1 1 d . . .
H37A H 1.3742 0.0280 0.9627 0.035 Uiso 1 1 calc R . .
H37B H 1.3740 -0.0647 1.0161 0.035 Uiso 1 1 calc R . .
C12 C -0.0068(6) -0.1852(4) 0.64693(19) 0.0402(12) Uani 1 1 d . . .
H12 H 0.0224 -0.2348 0.6212 0.048 Uiso 1 1 calc R . .
C31 C -0.1092(5) 0.7287(4) 1.35044(17) 0.0282(10) Uani 1 1 d . . .
H31 H -0.1636 0.8005 1.3461 0.034 Uiso 1 1 calc R . .
C7 C 0.3853(6) 0.1973(4) 0.8746(2) 0.0415(13) Uani 1 1 d . . .
H7 H 0.3590 0.2375 0.9043 0.050 Uiso 1 1 calc R . .
C5 C 0.3064(7) 0.0937(5) 0.8037(2) 0.0491(14) Uani 1 1 d . . .
C2 C 0.5405(6) 0.1832(4) 0.85704(18) 0.0343(11) Uani 1 1 d . . .
C20 C 0.3910(6) 0.3086(4) 1.2128(2) 0.0413(12) Uani 1 1 d . . .
H20 H 0.3694 0.2544 1.2431 0.050 Uiso 1 1 calc R . .
C33 C 0.9374(5) 0.0973(4) 1.05621(19) 0.0330(11) Uani 1 1 d . . .
H33 H 0.8464 0.0711 1.0721 0.040 Uiso 1 1 calc R . .
C47 C 1.5919(5) 0.4326(4) 0.59392(19) 0.0352(11) Uani 1 1 d . . .
H47 H 1.6438 0.4035 0.5640 0.042 Uiso 1 1 calc R . .
C11 C 0.1060(6) -0.1437(4) 0.6760(2) 0.0460(13) Uani 1 1 d . . .
H11 H 0.2098 -0.1665 0.6696 0.055 Uiso 1 1 calc R . .
C39 C 0.9437(6) 0.6086(4) 0.90597(19) 0.0429(13) Uani 1 1 d . . .
H39 H 0.9495 0.6867 0.9023 0.052 Uiso 1 1 calc R . .
C8 C 0.1777(7) 0.0425(4) 0.7788(2) 0.0523(15) Uani 1 1 d . . .
H8 H 0.0779 0.0597 0.7922 0.063 Uiso 1 1 calc R . .
C36 C 1.3515(5) 0.0971(4) 1.0360(2) 0.0371(12) Uani 1 1 d . . .
H36A H 1.3882 0.0752 1.0741 0.044 Uiso 1 1 calc R . .
H36B H 1.3923 0.1683 1.0211 0.044 Uiso 1 1 calc R . .
C6 C 0.2708(6) 0.1523(4) 0.8483(2) 0.0459(14) Uani 1 1 d . . .
H6 H 0.1687 0.1617 0.8610 0.055 Uiso 1 1 calc R . .
C10 C 0.0676(6) -0.0696(4) 0.7140(2) 0.0445(13) Uani 1 1 d . . .
C4 C 0.4569(7) 0.0847(5) 0.7845(2) 0.0602(17) Uani 1 1 d . . .
H4 H 0.4814 0.0486 0.7532 0.072 Uiso 1 1 calc R . .
C9 C 0.1926(7) -0.0221(5) 0.7410(2) 0.0546(15) Uani 1 1 d . . .
H9 H 0.2932 -0.0418 0.7290 0.065 Uiso 1 1 calc R . .
C15 C -0.0897(7) -0.0389(4) 0.7235(2) 0.0499(14) Uani 1 1 d . . .
H15 H -0.1188 0.0101 0.7495 0.060 Uiso 1 1 calc R . .
C3 C 0.5746(7) 0.1289(5) 0.8111(2) 0.0553(15) Uani 1 1 d . . .
H3 H 0.6760 0.1214 0.7976 0.066 Uiso 1 1 calc R . .
O7 O -0.4237(4) -0.1821(3) 0.63683(14) 0.0501(9) Uani 1 1 d . . .
C16 C -0.2850(6) -0.1937(4) 0.62252(19) 0.0331(11) Uani 1 1 d . . .
O8 O -0.2358(4) -0.2408(3) 0.58012(13) 0.0396(8) Uani 1 1 d . . .
N7 N -0.6043(4) 0.7329(3) 1.51862(14) 0.0262(8) Uani 1 1 d . . .
C48 C -0.6604(5) 0.8215(4) 1.48280(19) 0.0332(11) Uani 1 1 d . . .
H48 H -0.6010 0.8760 1.4638 0.040 Uiso 1 1 calc R . .
C49 C -0.7305(5) 0.6747(4) 1.53653(18) 0.0288(10) Uani 1 1 d . . .
H49 H -0.7272 0.6084 1.5623 0.035 Uiso 1 1 calc R . .
N8 N -0.8139(4) 0.8222(3) 1.47753(15) 0.0295(9) Uani 1 1 d . . .
C50 C -0.8578(5) 0.7280(4) 1.51132(18) 0.0318(11) Uani 1 1 d . . .
H50 H -0.9575 0.7054 1.5158 0.038 Uiso 1 1 calc R . .
C51 C -0.9173(6) 0.9090(4) 1.44351(19) 0.0386(12) Uani 1 1 d . . .
H51A H -0.9705 0.8735 1.4168 0.046 Uiso 1 1 calc R . .
H51B H -0.8560 0.9648 1.4225 0.046 Uiso 1 1 calc R . .
C52 C -1.0355(5) 0.9684(4) 1.47927(19) 0.0351(11) Uani 1 1 d . . .
H52A H -1.0975 0.9125 1.4998 0.042 Uiso 1 1 calc R . .
H52B H -1.1041 1.0218 1.4549 0.042 Uiso 1 1 calc R . .
O1W O -0.4649(5) 0.9433(3) 1.36749(15) 0.0667(11) Uani 1 1 d . . .
O2W O 0.3305(12) 0.3754(9) 0.9555(5) 0.115(4) Uani 0.50 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
Co1 O3 1.972(3) . ?
Co1 O1 1.998(3) . ?
Co1 N5 2.014(3) . ?
Co1 N1 2.035(3) . ?
Co2 O8 1.960(3) 1_566 ?
Co2 O6 1.976(3) . ?
Co2 N7 2.025(3) . ?
Co2 N4 2.044(4) 1_356 ?
O5 C30 1.246(5) . ?
O2 C17 1.240(5) . ?
O6 C30 1.281(5) . ?
O1 C17 1.293(5) . ?
O3 C1 1.282(5) . ?
O4 C1 1.239(5) . ?
N6 C35 1.335(5) . ?
N6 C34 1.363(5) . ?
N6 C36 1.469(5) . ?
N5 C35 1.322(5) . ?
N5 C33 1.377(5) . ?
C21 C23 1.390(6) . ?
C21 C20 1.392(6) . ?
C21 C22 1.468(6) . ?
N3 C45 1.341(5) . ?
N3 C46 1.367(6) . ?
N3 C44 1.468(5) . ?
C18 C24 1.370(6) . ?
C18 C19 1.392(6) . ?
C18 C17 1.501(6) . ?
C28 C27 1.382(6) . ?
C28 C29 1.388(6) . ?
C28 H28 0.9300 . ?
N4 C45 1.325(5) . ?
N4 C47 1.370(5) . ?
N4 Co2 2.044(3) 1_754 ?
N2 C40 1.352(5) . ?
N2 C39 1.361(6) . ?
N2 C41 1.472(5) . ?
C38 C39 1.348(6) . ?
C38 N1 1.372(5) . ?
C38 H38 0.9300 . ?
C29 C31 1.385(5) . ?
C29 C30 1.500(6) . ?
N1 C40 1.319(5) . ?
C25 C22 1.329(6) . ?
C25 C26 1.467(6) . ?
C25 H25 0.9300 . ?
C22 H22 0.9300 . ?
C32 C31 1.385(6) . ?
C32 C26 1.394(6) . ?
C32 H32 0.9300 . ?
C23 C24 1.370(6) . ?
C23 H23 0.9300 . ?
C46 C47 1.354(6) . ?
C46 H46 0.9300 . ?
C24 H24 0.9300 . ?
C43 C44 1.517(6) . ?
C43 C42 1.519(6) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C1 C2 1.512(6) . ?
C13 C14 1.382(6) . ?
C13 C12 1.386(6) . ?
C13 C16 1.503(6) . ?
C26 C27 1.399(6) . ?
C41 C42 1.509(7) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C19 C20 1.383(6) . ?
C19 H19 0.9300 . ?
C27 H27 0.9300 . ?
C34 C33 1.358(6) . ?
C34 H34 0.9300 . ?
C45 H45 0.9300 . ?
C35 H35 0.9300 . ?
C14 C15 1.388(6) . ?
C14 H14 0.9300 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C40 H40 0.9300 . ?
C37 C36 1.510(6) . ?
C37 C37 1.514(8) 2_857 ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C12 C11 1.387(6) . ?
C12 H12 0.9300 . ?
C31 H31 0.9300 . ?
C7 C6 1.383(6) . ?
C7 C2 1.401(7) . ?
C7 H7 0.9300 . ?
C5 C4 1.373(8) . ?
C5 C6 1.376(7) . ?
C5 C8 1.503(7) . ?
C2 C3 1.370(6) . ?
C20 H20 0.9300 . ?
C33 H33 0.9300 . ?
C47 H47 0.9300 . ?
C11 C10 1.374(7) . ?
C11 H11 0.9300 . ?
C39 H39 0.9300 . ?
C8 C9 1.271(7) . ?
C8 H8 0.9300 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C6 H6 0.9300 . ?
C10 C15 1.399(7) . ?
C10 C9 1.478(7) . ?
C4 C3 1.405(7) . ?
C4 H4 0.9300 . ?
C9 H9 0.9300 . ?
C15 H15 0.9300 . ?
C3 H3 0.9300 . ?
O7 C16 1.243(6) . ?
C16 O8 1.278(5) . ?
O8 Co2 1.960(3) 1_544 ?
N7 C48 1.324(5) . ?
N7 C49 1.381(5) . ?
C48 N8 1.341(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.333(6) . ?
C49 H49 0.9300 . ?
N8 C50 1.369(5) . ?
N8 C51 1.470(5) . ?
C50 H50 0.9300 . ?
C51 C52 1.510(6) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C52 1.511(8) 2_378 ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?

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 Co1 O1 110.48(13) . . ?
O3 Co1 N5 119.11(13) . . ?
O1 Co1 N5 114.30(13) . . ?
O3 Co1 N1 106.36(13) . . ?
O1 Co1 N1 98.38(13) . . ?
N5 Co1 N1 105.57(14) . . ?
O8 Co2 O6 102.00(13) 1_566 . ?
O8 Co2 N7 130.50(14) 1_566 . ?
O6 Co2 N7 116.12(13) . . ?
O8 Co2 N4 104.40(13) 1_566 1_356 ?
O6 Co2 N4 101.69(13) . 1_356 ?
N7 Co2 N4 97.76(14) . 1_356 ?
C30 O6 Co2 105.7(3) . . ?
C17 O1 Co1 101.5(3) . . ?
C1 O3 Co1 119.5(3) . . ?
C35 N6 C34 107.3(4) . . ?
C35 N6 C36 125.6(4) . . ?
C34 N6 C36 127.1(4) . . ?
C35 N5 C33 105.2(4) . . ?
C35 N5 Co1 125.1(3) . . ?
C33 N5 Co1 129.2(3) . . ?
C23 C21 C20 117.0(4) . . ?
C23 C21 C22 122.7(4) . . ?
C20 C21 C22 120.3(4) . . ?
C45 N3 C46 107.3(4) . . ?
C45 N3 C44 127.4(4) . . ?
C46 N3 C44 125.1(4) . . ?
C24 C18 C19 118.5(4) . . ?
C24 C18 C17 121.1(4) . . ?
C19 C18 C17 120.3(4) . . ?
C27 C28 C29 121.5(4) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C45 N4 C47 105.4(4) . . ?
C45 N4 Co2 126.0(3) . 1_754 ?
C47 N4 Co2 127.8(3) . 1_754 ?
C40 N2 C39 107.1(4) . . ?
C40 N2 C41 127.8(4) . . ?
C39 N2 C41 125.0(4) . . ?
C39 C38 N1 110.0(4) . . ?
C39 C38 H38 125.0 . . ?
N1 C38 H38 125.0 . . ?
C31 C29 C28 118.3(4) . . ?
C31 C29 C30 121.3(4) . . ?
C28 C29 C30 120.3(4) . . ?
C40 N1 C38 105.4(4) . . ?
C40 N1 Co1 129.9(3) . . ?
C38 N1 Co1 124.5(3) . . ?
C22 C25 C26 126.8(4) . . ?
C22 C25 H25 116.6 . . ?
C26 C25 H25 116.6 . . ?
C25 C22 C21 126.9(4) . . ?
C25 C22 H22 116.6 . . ?
C21 C22 H22 116.6 . . ?
C31 C32 C26 121.8(4) . . ?
C31 C32 H32 119.1 . . ?
C26 C32 H32 119.1 . . ?
C24 C23 C21 121.6(4) . . ?
C24 C23 H23 119.2 . . ?
C21 C23 H23 119.2 . . ?
O5 C30 O6 122.2(4) . . ?
O5 C30 C29 121.4(4) . . ?
O6 C30 C29 116.3(4) . . ?
C47 C46 N3 106.2(4) . . ?
C47 C46 H46 126.9 . . ?
N3 C46 H46 126.9 . . ?
C23 C24 C18 121.2(4) . . ?
C23 C24 H24 119.4 . . ?
C18 C24 H24 119.4 . . ?
C44 C43 C42 110.6(4) . . ?
C44 C43 H43A 109.5 . . ?
C42 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
O4 C1 O3 124.8(4) . . ?
O4 C1 C2 120.2(4) . . ?
O3 C1 C2 115.0(4) . . ?
C14 C13 C12 118.5(4) . . ?
C14 C13 C16 120.5(4) . . ?
C12 C13 C16 121.0(4) . . ?
C32 C26 C27 117.4(4) . . ?
C32 C26 C25 120.3(4) . . ?
C27 C26 C25 122.3(4) . . ?
N2 C41 C42 113.4(4) . . ?
N2 C41 H41A 108.9 . . ?
C42 C41 H41A 108.9 . . ?
N2 C41 H41B 108.9 . . ?
C42 C41 H41B 108.9 . . ?
H41A C41 H41B 107.7 . . ?
N3 C44 C43 112.7(4) . . ?
N3 C44 H44A 109.1 . . ?
C43 C44 H44A 109.1 . . ?
N3 C44 H44B 109.1 . . ?
C43 C44 H44B 109.1 . . ?
H44A C44 H44B 107.8 . . ?
C20 C19 C18 120.2(4) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C28 C27 C26 120.6(4) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C33 C34 N6 106.4(4) . . ?
C33 C34 H34 126.8 . . ?
N6 C34 H34 126.8 . . ?
N4 C45 N3 111.2(4) . . ?
N4 C45 H45 124.4 . . ?
N3 C45 H45 124.4 . . ?
N5 C35 N6 111.8(4) . . ?
N5 C35 H35 124.1 . . ?
N6 C35 H35 124.1 . . ?
C13 C14 C15 120.7(5) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C41 C42 C43 111.4(4) . . ?
C41 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
C41 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
O2 C17 O1 121.5(4) . . ?
O2 C17 C18 120.9(4) . . ?
O1 C17 C18 117.6(4) . . ?
N1 C40 N2 111.0(4) . . ?
N1 C40 H40 124.5 . . ?
N2 C40 H40 124.5 . . ?
C36 C37 C37 111.4(4) . 2_857 ?
C36 C37 H37A 109.3 . . ?
C37 C37 H37A 109.3 2_857 . ?
C36 C37 H37B 109.3 . . ?
C37 C37 H37B 109.3 2_857 . ?
H37A C37 H37B 108.0 . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C32 C31 C29 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C29 C31 H31 119.8 . . ?
C6 C7 C2 121.1(5) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C4 C5 C6 118.6(5) . . ?
C4 C5 C8 123.5(5) . . ?
C6 C5 C8 117.9(5) . . ?
C3 C2 C7 118.1(4) . . ?
C3 C2 C1 121.2(5) . . ?
C7 C2 C1 120.7(4) . . ?
C19 C20 C21 121.4(4) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C34 C33 N5 109.3(4) . . ?
C34 C33 H33 125.3 . . ?
N5 C33 H33 125.3 . . ?
C46 C47 N4 109.8(4) . . ?
C46 C47 H47 125.1 . . ?
N4 C47 H47 125.1 . . ?
C10 C11 C12 121.4(5) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C38 C39 N2 106.4(4) . . ?
C38 C39 H39 126.8 . . ?
N2 C39 H39 126.8 . . ?
C9 C8 C5 126.0(6) . . ?
C9 C8 H8 117.0 . . ?
C5 C8 H8 117.0 . . ?
N6 C36 C37 112.4(3) . . ?
N6 C36 H36A 109.1 . . ?
C37 C36 H36A 109.1 . . ?
N6 C36 H36B 109.1 . . ?
C37 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C5 C6 C7 120.6(5) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C11 C10 C15 117.9(5) . . ?
C11 C10 C9 119.1(5) . . ?
C15 C10 C9 122.9(5) . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C8 C9 C10 127.1(6) . . ?
C8 C9 H9 116.4 . . ?
C10 C9 H9 116.4 . . ?
C14 C15 C10 120.8(5) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
C2 C3 C4 120.1(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
O7 C16 O8 123.7(4) . . ?
O7 C16 C13 120.8(4) . . ?
O8 C16 C13 115.5(4) . . ?
C16 O8 Co2 117.5(3) . 1_544 ?
C48 N7 C49 105.3(4) . . ?
C48 N7 Co2 130.2(3) . . ?
C49 N7 Co2 124.5(3) . . ?
N7 C48 N8 111.1(4) . . ?
N7 C48 H48 124.5 . . ?
N8 C48 H48 124.5 . . ?
C50 C49 N7 109.6(4) . . ?
C50 C49 H49 125.2 . . ?
N7 C49 H49 125.2 . . ?
C48 N8 C50 107.0(4) . . ?
C48 N8 C51 126.9(4) . . ?
C50 N8 C51 126.1(4) . . ?
C49 C50 N8 107.0(4) . . ?
C49 C50 H50 126.5 . . ?
N8 C50 H50 126.5 . . ?
N8 C51 C52 112.0(4) . . ?
N8 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
N8 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 C52 113.5(5) . 2_378 ?
C51 C52 H52A 108.9 . . ?
C52 C52 H52A 108.9 2_378 . ?
C51 C52 H52B 108.9 . . ?
C52 C52 H52B 108.9 2_378 . ?
H52A C52 H52B 107.7 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.083

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

data_compound-5
_database_code_depnum_ccdc_archive 'CCDC 693964'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H22 Cd N4 O5'
_chemical_formula_sum            'C28 H22 Cd N4 O5'
_chemical_formula_weight         606.90

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'
Cd Cd -0.8075 1.2024 '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 n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   14.7584(10)
_cell_length_b                   14.2630(9)
_cell_length_c                   12.1990(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2567.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2643
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'

_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13791
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         26.02
_reflns_number_total             2643
_reflns_number_gt                2436
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'

_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)+(0.0331P)²+1.0110P] 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         2643
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0575
_refine_ls_wR_factor_gt          0.0561
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Cd1 Cd 0.720054(11) 0.2500 0.854893(14) 0.02450(8) Uani 1 2 d S . .
N2 N 0.77853(11) 0.00466(13) 0.65217(14) 0.0369(4) Uani 1 1 d . . .
O2 O 0.62294(11) 0.2500 0.99282(14) 0.0270(4) Uani 1 2 d S . .
O4 O -0.15563(9) 0.32750(11) 0.94707(11) 0.0426(3) Uani 1 1 d . . .
O1 O 0.54938(12) 0.2500 0.83440(14) 0.0334(4) Uani 1 2 d S . .
O3 O 0.22290(12) 0.2500 1.17865(18) 0.0682(9) Uani 1 2 d S . .
N1 N 0.72623(9) 0.12614(11) 0.74242(13) 0.0305(3) Uani 1 1 d . . .
C11 C 0.38156(18) 0.2500 1.1715(2) 0.0338(6) Uani 1 2 d S . .
H11 H 0.3819 0.2500 1.2477 0.041 Uiso 1 2 calc SR . .
C15 C 0.13937(19) 0.2500 1.1253(2) 0.0489(9) Uani 1 2 d S . .
C5 C 0.92285(14) -0.03220(13) 0.55523(16) 0.0365(4) Uani 1 1 d . . .
C8 C 0.54948(16) 0.2500 0.9368(2) 0.0253(5) Uani 1 2 d S . .
C13 C 0.29875(18) 0.2500 1.0007(2) 0.0379(7) Uani 1 2 d S . .
H13 H 0.2439 0.2500 0.9631 0.045 Uiso 1 2 calc SR . .
C18 C -0.02929(17) 0.2500 1.0271(2) 0.0341(6) Uani 1 2 d S . .
C9 C 0.46229(16) 0.2500 0.99947(19) 0.0242(5) Uani 1 2 d S . .
C14 C 0.38040(16) 0.2500 0.9444(2) 0.0295(5) Uani 1 2 d S . .
H14 H 0.3801 0.2500 0.8681 0.035 Uiso 1 2 calc SR . .
C1 C 0.65914(14) 0.09180(16) 0.67568(16) 0.0398(5) Uani 1 1 d . . .
H1 H 0.6009 0.1163 0.6698 0.048 Uiso 1 1 calc R . .
C10 C 0.46189(17) 0.2500 1.1134(2) 0.0285(5) Uani 1 2 d S . .
H10 H 0.5166 0.2500 1.1512 0.034 Uiso 1 2 calc SR . .
C7 C 0.99553(15) 0.02193(14) 0.39066(17) 0.0405(5) Uani 1 1 d . . .
H7 H 0.9918 0.0368 0.3166 0.049 Uiso 1 1 calc R . .
C6 C 0.91925(14) -0.01012(14) 0.44477(17) 0.0408(5) Uani 1 1 d . . .
H6 H 0.8651 -0.0169 0.4067 0.049 Uiso 1 1 calc R . .
C12 C 0.30074(19) 0.2500 1.1145(2) 0.0382(7) Uani 1 2 d S . .
C3 C 0.79715(13) 0.07164(13) 0.72611(16) 0.0351(4) Uani 1 1 d . . .
H3 H 0.8527 0.0787 0.7612 0.042 Uiso 1 1 calc R . .
C19 C -0.11946(17) 0.2500 0.9702(2) 0.0341(6) Uani 1 2 d S . .
C17 C 0.01376(14) 0.16644(17) 1.05205(17) 0.0455(5) Uani 1 1 d . . .
H17 H -0.0144 0.1098 1.0355 0.055 Uiso 1 1 calc R . .
C4 C 0.84020(16) -0.06979(15) 0.6138(2) 0.0474(5) Uani 1 1 d . . .
H4A H 0.8074 -0.1110 0.5646 0.057 Uiso 1 1 calc R . .
H4B H 0.8597 -0.1067 0.6763 0.057 Uiso 1 1 calc R . .
C2 C 0.69067(16) 0.01711(17) 0.62000(18) 0.0448(5) Uani 1 1 d . . .
H2 H 0.6589 -0.0190 0.5695 0.054 Uiso 1 1 calc R . .
C16 C 0.09828(14) 0.1663(2) 1.10139(18) 0.0527(6) Uani 1 1 d . . .
H16 H 0.1268 0.1099 1.1181 0.063 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.2102(17) . ?
Cd1 N1 2.2387(15) . ?
Cd1 N1 2.2387(15) 8_565 ?
Cd1 O4 2.4191(14) 1_655 ?
Cd1 O4 2.4191(14) 8_665 ?
Cd1 O1 2.5313(18) . ?
Cd1 C8 2.709(2) . ?
Cd1 C19 2.755(3) 1_655 ?
N2 C3 1.342(3) . ?
N2 C2 1.366(3) . ?
N2 C4 1.475(3) . ?
O2 C8 1.281(3) . ?
O4 C19 1.2596(19) . ?
O4 Cd1 2.4191(14) 1_455 ?
O1 C8 1.250(3) . ?
O3 C12 1.390(3) . ?
O3 C15 1.394(3) . ?
N1 C3 1.319(2) . ?
N1 C1 1.372(2) . ?
C11 C12 1.381(4) . ?
C11 C10 1.381(4) . ?
C11 H11 0.9300 . ?
C15 C16 1.371(3) 8_565 ?
C15 C16 1.371(3) . ?
C5 C7 1.381(3) 5_756 ?
C5 C6 1.385(3) . ?
C5 C4 1.512(3) . ?
C8 C9 1.497(3) . ?
C13 C14 1.387(4) . ?
C13 C12 1.388(4) . ?
C13 H13 0.9300 . ?
C18 C17 1.385(3) 8_565 ?
C18 C17 1.385(3) . ?
C18 C19 1.501(4) . ?
C9 C14 1.383(3) . ?
C9 C10 1.390(3) . ?
C14 H14 0.9300 . ?
C1 C2 1.346(3) . ?
C1 H1 0.9300 . ?
C10 H10 0.9300 . ?
C7 C5 1.381(3) 5_756 ?
C7 C6 1.383(3) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C3 H3 0.9300 . ?
C19 O4 1.2596(19) 8_565 ?
C19 Cd1 2.755(3) 1_455 ?
C17 C16 1.385(3) . ?
C17 H17 0.9300 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?

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 Cd1 N1 119.53(4) . . ?
O2 Cd1 N1 119.53(4) . 8_565 ?
N1 Cd1 N1 104.21(8) . 8_565 ?
O2 Cd1 O4 97.93(5) . 1_655 ?
N1 Cd1 O4 127.92(5) . 1_655 ?
N1 Cd1 O4 83.88(5) 8_565 1_655 ?
O2 Cd1 O4 97.93(5) . 8_665 ?
N1 Cd1 O4 83.88(5) . 8_665 ?
N1 Cd1 O4 127.92(5) 8_565 8_665 ?
O4 Cd1 O4 54.38(7) 1_655 8_665 ?
O2 Cd1 O1 55.24(6) . . ?
N1 Cd1 O1 88.85(4) . . ?
N1 Cd1 O1 88.85(4) 8_565 . ?
O4 Cd1 O1 143.19(4) 1_655 . ?
O4 Cd1 O1 143.19(4) 8_665 . ?
O2 Cd1 C8 27.92(7) . . ?
N1 Cd1 C8 105.31(5) . . ?
N1 Cd1 C8 105.31(5) 8_565 . ?
O4 Cd1 C8 122.23(6) 1_655 . ?
O4 Cd1 C8 122.23(6) 8_665 . ?
O1 Cd1 C8 27.33(6) . . ?
O2 Cd1 C19 99.71(7) . 1_655 ?
N1 Cd1 C19 106.14(5) . 1_655 ?
N1 Cd1 C19 106.14(5) 8_565 1_655 ?
O4 Cd1 C19 27.20(4) 1_655 1_655 ?
O4 Cd1 C19 27.20(4) 8_665 1_655 ?
O1 Cd1 C19 154.96(7) . 1_655 ?
C8 Cd1 C19 127.63(8) . 1_655 ?
C3 N2 C2 107.15(17) . . ?
C3 N2 C4 126.81(18) . . ?
C2 N2 C4 126.03(18) . . ?
C8 O2 Cd1 98.22(14) . . ?
C19 O4 Cd1 91.41(13) . 1_455 ?
C8 O1 Cd1 84.26(14) . . ?
C12 O3 C15 117.9(2) . . ?
C3 N1 C1 105.83(16) . . ?
C3 N1 Cd1 126.15(12) . . ?
C1 N1 Cd1 128.02(13) . . ?
C12 C11 C10 118.9(2) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C16 C15 C16 121.2(3) 8_565 . ?
C16 C15 O3 119.38(14) 8_565 . ?
C16 C15 O3 119.38(14) . . ?
C7 C5 C6 118.31(19) 5_756 . ?
C7 C5 C4 121.01(19) 5_756 . ?
C6 C5 C4 120.6(2) . . ?
O1 C8 O2 122.3(2) . . ?
O1 C8 C9 120.6(2) . . ?
O2 C8 C9 117.1(2) . . ?
O1 C8 Cd1 68.41(13) . . ?
O2 C8 Cd1 53.86(11) . . ?
C9 C8 Cd1 170.96(17) . . ?
C14 C13 C12 118.5(2) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C17 C18 C17 118.8(3) 8_565 . ?
C17 C18 C19 120.57(13) 8_565 . ?
C17 C18 C19 120.57(13) . . ?
C14 C9 C10 118.8(2) . . ?
C14 C9 C8 120.2(2) . . ?
C10 C9 C8 120.9(2) . . ?
C9 C14 C13 121.2(2) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C2 C1 N1 109.41(19) . . ?
C2 C1 H1 125.3 . . ?
N1 C1 H1 125.3 . . ?
C11 C10 C9 121.1(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C5 C7 C6 121.13(19) 5_756 . ?
C5 C7 H7 119.4 5_756 . ?
C6 C7 H7 119.4 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C11 C12 C13 121.5(3) . . ?
C11 C12 O3 115.5(2) . . ?
C13 C12 O3 123.1(3) . . ?
N1 C3 N2 111.00(17) . . ?
N1 C3 H3 124.5 . . ?
N2 C3 H3 124.5 . . ?
O4 C19 O4 122.7(2) . 8_565 ?
O4 C19 C18 118.65(12) . . ?
O4 C19 C18 118.65(12) 8_565 . ?
O4 C19 Cd1 61.39(12) . 1_455 ?
O4 C19 Cd1 61.39(12) 8_565 1_455 ?
C18 C19 Cd1 176.81(17) . 1_455 ?
C18 C17 C16 120.7(2) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N2 C4 C5 113.11(17) . . ?
N2 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C1 C2 N2 106.61(18) . . ?
C1 C2 H2 126.7 . . ?
N2 C2 H2 126.7 . . ?
C15 C16 C17 119.3(2) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.064

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

data_compound-6
_database_code_depnum_ccdc_archive 'CCDC 693965'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H68 N8 Ni4 O24'
_chemical_formula_sum            'C84 H68 N8 Ni4 O24'
_chemical_formula_weight         1808.30

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                   28.442(3)
_cell_length_b                   5.7468(6)
_cell_length_c                   24.666(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.039(2)
_cell_angle_gamma                90.00
_cell_volume                     3737.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3669
_cell_measurement_theta_min      1.54
_cell_measurement_theta_max      26.07

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1864
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'

_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9981
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         26.07
_reflns_number_total             3669
_reflns_number_gt                2982
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'

_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)+(0.0465P)²+0.8848P] 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         3669
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.0962
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Ni1 Ni 0.728997(13) 0.11371(6) 0.543759(15) 0.01606(12) Uani 1 1 d . . .
O3 O 0.44205(7) 0.1505(3) 0.29013(8) 0.0217(5) Uani 1 1 d . . .
O4 O 0.29970(7) -0.6064(3) 0.11393(8) 0.0199(4) Uani 1 1 d . . .
O2 O 0.64580(7) -0.3159(3) 0.46398(9) 0.0249(5) Uani 1 1 d . . .
O1 O 0.66460(7) 0.0652(3) 0.47603(8) 0.0240(5) Uani 1 1 d . . .
O5 O 0.25172(7) -0.2954(3) 0.08955(8) 0.0194(4) Uani 1 1 d . . .
O1W O 0.73130(8) 0.4546(3) 0.51156(9) 0.0168(4) Uani 1 1 d . . .
N2 N 0.63325(9) 0.4355(4) 0.61282(10) 0.0235(6) Uani 1 1 d . . .
C19 C 0.54450(11) 0.5433(5) 0.54901(13) 0.0219(6) Uani 1 1 d . . .
C6 C 0.52861(10) 0.2277(5) 0.34070(12) 0.0200(6) Uani 1 1 d . . .
H6 H 0.5237 0.3681 0.3206 0.024 Uiso 1 1 calc R . .
C21 C 0.49430(11) 0.2936(5) 0.46998(13) 0.0253(7) Uani 1 1 d . . .
H011 H 0.4908 0.1539 0.4498 0.030 Uiso 1 1 calc R . .
N1 N 0.69037(9) 0.2295(4) 0.59380(10) 0.0209(5) Uani 1 1 d . . .
C5 C 0.48885(10) 0.0722(5) 0.32882(12) 0.0177(6) Uani 1 1 d . . .
C17 C 0.65668(11) 0.3979(5) 0.57575(13) 0.0264(7) Uani 1 1 d . . .
H17 H 0.6500 0.4809 0.5413 0.032 Uiso 1 1 calc R . .
C8 C 0.40715(10) -0.0007(5) 0.25162(11) 0.0178(6) Uani 1 1 d . . .
C13 C 0.32071(10) -0.0457(5) 0.18711(12) 0.0196(6) Uani 1 1 d . . .
H13 H 0.2877 0.0111 0.1711 0.024 Uiso 1 1 calc R . .
C3 C 0.54329(10) -0.1951(5) 0.39847(12) 0.0179(6) Uani 1 1 d . . .
H3 H 0.5483 -0.3387 0.4172 0.022 Uiso 1 1 calc R . .
C1 C 0.63575(10) -0.1052(5) 0.45386(11) 0.0169(6) Uani 1 1 d . . .
C7 C 0.57567(10) 0.1735(5) 0.38257(12) 0.0196(6) Uani 1 1 d . . .
H7 H 0.6020 0.2809 0.3918 0.023 Uiso 1 1 calc R . .
C20 C 0.53797(11) 0.3349(5) 0.51825(14) 0.0260(7) Uani 1 1 d . . .
H20 H 0.5633 0.2224 0.5303 0.031 Uiso 1 1 calc R . .
C9 C 0.41941(10) -0.2112(5) 0.23348(12) 0.0197(6) Uani 1 1 d . . .
H9 H 0.4527 -0.2652 0.2486 0.024 Uiso 1 1 calc R . .
C4 C 0.49560(10) -0.1378(5) 0.35857(12) 0.0186(6) Uani 1 1 d . . .
H4 H 0.4684 -0.2387 0.3518 0.022 Uiso 1 1 calc R . .
C11 C 0.33221(10) -0.2594(5) 0.16844(11) 0.0177(6) Uani 1 1 d . . .
C15 C 0.68810(12) 0.1567(6) 0.64572(14) 0.0341(8) Uani 1 1 d . . .
H15 H 0.7078 0.0388 0.6692 0.041 Uiso 1 1 calc R . .
C2 C 0.58383(10) -0.0416(5) 0.41111(11) 0.0152(6) Uani 1 1 d . . .
C10 C 0.38184(10) -0.3407(5) 0.19265(12) 0.0192(6) Uani 1 1 d . . .
H10 H 0.3898 -0.4847 0.1811 0.023 Uiso 1 1 calc R . .
C14 C 0.35765(10) 0.0829(5) 0.22908(12) 0.0199(6) Uani 1 1 d . . .
H14 H 0.3496 0.2235 0.2421 0.024 Uiso 1 1 calc R . .
C16 C 0.65282(12) 0.2823(6) 0.65770(14) 0.0349(8) Uani 1 1 d . . .
H16 H 0.6438 0.2668 0.6901 0.042 Uiso 1 1 calc R . .
C18 C 0.59136(11) 0.5994(5) 0.60254(14) 0.0273(7) Uani 1 1 d . . .
H18A H 0.6029 0.7544 0.5981 0.033 Uiso 1 1 calc R . .
H18B H 0.5822 0.6008 0.6366 0.033 Uiso 1 1 calc R . .
C12 C 0.29301(10) -0.3948(5) 0.12193(12) 0.0184(6) Uani 1 1 d . . .
HW11 H 0.7439(14) 0.564(7) 0.5385(16) 0.051(12) Uiso 1 1 d . . .
HW12 H 0.7048(14) 0.514(7) 0.4930(16) 0.049(12) 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
Ni1 O1 1.9816(19) . ?
Ni1 N1 2.047(2) . ?
Ni1 O4 2.1046(18) 8_546 ?
Ni1 O1W 2.109(2) 7_656 ?
Ni1 O5 2.1194(19) 8_546 ?
Ni1 O1W 2.124(2) . ?
Ni1 C12 2.446(3) 8_546 ?
O3 C5 1.390(3) . ?
O3 C8 1.391(3) . ?
O4 C12 1.257(3) . ?
O4 Ni1 2.1046(18) 8_445 ?
O2 C1 1.248(3) . ?
O1 C1 1.263(3) . ?
O5 C12 1.281(3) . ?
O5 Ni1 2.1194(19) 8_445 ?
O1W Ni1 2.109(2) 7_656 ?
O1W HW11 0.89(4) . ?
O1W HW12 0.80(4) . ?
N2 C17 1.336(4) . ?
N2 C16 1.359(4) . ?
N2 C18 1.464(4) . ?
C19 C21 1.388(4) 5_666 ?
C19 C20 1.392(4) . ?
C19 C18 1.518(4) . ?
C6 C5 1.384(4) . ?
C6 C7 1.385(4) . ?
C6 H6 0.9300 . ?
C21 C20 1.381(4) . ?
C21 C19 1.388(4) 5_666 ?
C21 H011 0.9300 . ?
N1 C17 1.316(4) . ?
N1 C15 1.372(4) . ?
C5 C4 1.388(4) . ?
C17 H17 0.9300 . ?
C8 C9 1.379(4) . ?
C8 C14 1.391(4) . ?
C13 C14 1.380(4) . ?
C13 C11 1.393(4) . ?
C13 H13 0.9300 . ?
C3 C4 1.384(4) . ?
C3 C2 1.391(4) . ?
C3 H3 0.9300 . ?
C1 C2 1.503(4) . ?
C7 C2 1.398(4) . ?
C7 H7 0.9300 . ?
C20 H20 0.9300 . ?
C9 C10 1.379(4) . ?
C9 H9 0.9300 . ?
C4 H4 0.9300 . ?
C11 C10 1.391(4) . ?
C11 C12 1.485(4) . ?
C15 C16 1.356(4) . ?
C15 H15 0.9300 . ?
C10 H10 0.9300 . ?
C14 H14 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C12 Ni1 2.446(3) 8_445 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N1 91.07(9) . . ?
O1 Ni1 O4 170.45(8) . 8_546 ?
N1 Ni1 O4 94.25(8) . 8_546 ?
O1 Ni1 O1W 88.76(8) . 7_656 ?
N1 Ni1 O1W 171.64(9) . 7_656 ?
O4 Ni1 O1W 87.13(8) 8_546 7_656 ?
O1 Ni1 O5 109.17(8) . 8_546 ?
N1 Ni1 O5 94.85(8) . 8_546 ?
O4 Ni1 O5 62.50(7) 8_546 8_546 ?
O1W Ni1 O5 93.09(8) 7_656 8_546 ?
O1 Ni1 O1W 87.87(8) . . ?
N1 Ni1 O1W 91.40(9) . . ?
O4 Ni1 O1W 99.91(8) 8_546 . ?
O1W Ni1 O1W 80.24(8) 7_656 . ?
O5 Ni1 O1W 161.67(8) 8_546 . ?
O1 Ni1 C12 140.49(9) . 8_546 ?
N1 Ni1 C12 95.80(9) . 8_546 ?
O4 Ni1 C12 30.94(8) 8_546 8_546 ?
O1W Ni1 C12 89.62(8) 7_656 8_546 ?
O5 Ni1 C12 31.56(8) 8_546 8_546 ?
O1W Ni1 C12 130.61(9) . 8_546 ?
C5 O3 C8 121.4(2) . . ?
C12 O4 Ni1 89.68(16) . 8_445 ?
C1 O1 Ni1 135.98(18) . . ?
C12 O5 Ni1 88.40(16) . 8_445 ?
Ni1 O1W Ni1 99.76(8) 7_656 . ?
Ni1 O1W HW11 117(2) 7_656 . ?
Ni1 O1W HW11 116(2) . . ?
Ni1 O1W HW12 109(3) 7_656 . ?
Ni1 O1W HW12 117(3) . . ?
HW11 O1W HW12 99(3) . . ?
C17 N2 C16 107.2(2) . . ?
C17 N2 C18 124.6(3) . . ?
C16 N2 C18 128.0(3) . . ?
C21 C19 C20 118.0(3) 5_666 . ?
C21 C19 C18 118.5(3) 5_666 . ?
C20 C19 C18 123.4(3) . . ?
C5 C6 C7 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C20 C21 C19 121.3(3) . 5_666 ?
C20 C21 H011 119.4 . . ?
C19 C21 H011 119.4 5_666 . ?
C17 N1 C15 104.9(3) . . ?
C17 N1 Ni1 121.49(19) . . ?
C15 N1 Ni1 133.4(2) . . ?
C6 C5 C4 120.6(3) . . ?
C6 C5 O3 115.6(2) . . ?
C4 C5 O3 123.5(2) . . ?
N1 C17 N2 112.0(3) . . ?
N1 C17 H17 124.0 . . ?
N2 C17 H17 124.0 . . ?
C9 C8 C14 121.0(3) . . ?
C9 C8 O3 124.5(2) . . ?
C14 C8 O3 114.4(2) . . ?
C14 C13 C11 120.8(2) . . ?
C14 C13 H13 119.6 . . ?
C11 C13 H13 119.6 . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
O2 C1 O1 127.1(3) . . ?
O2 C1 C2 117.9(2) . . ?
O1 C1 C2 115.0(2) . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C3 C4 C5 119.2(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C10 C11 C13 118.7(3) . . ?
C10 C11 C12 120.1(3) . . ?
C13 C11 C12 121.1(2) . . ?
C16 C15 N1 109.8(3) . . ?
C16 C15 H15 125.1 . . ?
N1 C15 H15 125.1 . . ?
C3 C2 C7 118.7(2) . . ?
C3 C2 C1 121.1(2) . . ?
C7 C2 C1 120.1(2) . . ?
C9 C10 C11 121.0(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C13 C14 C8 119.1(3) . . ?
C13 C14 H14 120.5 . . ?
C8 C14 H14 120.5 . . ?
C15 C16 N2 106.1(3) . . ?
C15 C16 H16 126.9 . . ?
N2 C16 H16 126.9 . . ?
N2 C18 C19 113.9(2) . . ?
N2 C18 H18A 108.8 . . ?
C19 C18 H18A 108.8 . . ?
N2 C18 H18B 108.8 . . ?
C19 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
O4 C12 O5 119.4(2) . . ?
O4 C12 C11 120.9(2) . . ?
O5 C12 C11 119.7(2) . . ?
O4 C12 Ni1 59.38(14) . 8_445 ?
O5 C12 Ni1 60.03(14) . 8_445 ?
C11 C12 Ni1 178.76(19) . 8_445 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.076

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


