data_global

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Wei-Yin Sun.'
'Zhengshuai Bai.'
'Shui-Sheng Chen.'
'Man-Sheng Chen.'
'Jian Fan.'
'Gao-Chao Lv.'
'Zhi Su.'

_publ_contact_author_name        'Wei-Yin Sun'
_publ_contact_author_email       SUNWY@NJU.EDU.CN

_publ_section_title              
;
Synthesis and characterization of metal
complexes with mixed 4-imidazole-containing ligand and
varied multi-carboxylic acid
;

# Attachment 'sun-cec.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 761519'
#TrackingRef 'sun-cec.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H20 N4 Ni O5'
_chemical_formula_sum            'C18 H20 N4 Ni O5'
_chemical_formula_weight         431.09

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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'

_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                   9.1481(10)
_cell_length_b                   9.4793(10)
_cell_length_c                   11.1701(12)
_cell_angle_alpha                95.729(2)
_cell_angle_beta                 92.402(2)
_cell_angle_gamma                99.879(2)
_cell_volume                     947.79(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3936
_cell_measurement_theta_min      2.194
_cell_measurement_theta_max      28.303

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             448
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8157
_exptl_absorpt_correction_T_max  0.8832
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5706
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.30
_reflns_number_total             4186
_reflns_number_gt                3920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.3586P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4186
_refine_ls_number_parameters     261
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.19748(2) 0.58241(2) 0.657238(19) 0.02140(10) Uani 1 1 d U . .
C1 C 0.3550(2) 0.1552(2) 0.17866(19) 0.0342(5) Uani 1 1 d . . .
H1 H 0.4477 0.2143 0.1814 0.041 Uiso 1 1 calc R . .
C2 C 0.3193(2) 0.0383(3) 0.0917(2) 0.0364(5) Uani 1 1 d . . .
H2 H 0.3890 0.0197 0.0367 0.044 Uiso 1 1 calc R . .
C3 C 0.1818(2) -0.0523(2) 0.08441(17) 0.0266(4) Uani 1 1 d . . .
C4 C 0.0802(2) -0.0236(2) 0.16863(19) 0.0321(4) Uani 1 1 d . . .
H4 H -0.0120 -0.0834 0.1664 0.039 Uiso 1 1 calc R . .
C5 C 0.1154(2) 0.0932(2) 0.25578(18) 0.0310(4) Uani 1 1 d . . .
H5 H 0.0460 0.1112 0.3113 0.037 Uiso 1 1 calc R . .
C6 C 0.2528(2) 0.1844(2) 0.26186(16) 0.0251(4) Uani 1 1 d . . .
C7 C 0.2816(2) 0.3111(2) 0.35116(17) 0.0244(4) Uani 1 1 d . . .
C8 C 0.2082(2) 0.3418(2) 0.45125(17) 0.0260(4) Uani 1 1 d . . .
H8 H 0.1323 0.2786 0.4806 0.031 Uiso 1 1 calc R . .
C9 C 0.3682(2) 0.5303(2) 0.43413(18) 0.0285(4) Uani 1 1 d . . .
H9 H 0.4255 0.6221 0.4479 0.034 Uiso 1 1 calc R . .
C10 C 0.1447(2) -0.1695(2) -0.01341(17) 0.0266(4) Uani 1 1 d . . .
C11 C 0.2135(2) -0.1992(2) -0.11692(18) 0.0290(4) Uani 1 1 d . . .
H11 H 0.3018 -0.1461 -0.1385 0.035 Uiso 1 1 calc R . .
C12 C 0.0173(2) -0.3601(2) -0.12292(18) 0.0316(4) Uani 1 1 d . . .
H12 H -0.0570 -0.4390 -0.1478 0.038 Uiso 1 1 calc R . .
C13 C 0.4530(3) 1.0347(2) 0.5439(3) 0.0506(7) Uani 1 1 d . . .
H13A H 0.4599 1.1352 0.5308 0.061 Uiso 1 1 calc R . .
H13B H 0.4930 1.0315 0.6252 0.061 Uiso 1 1 calc R . .
C14 C 0.2905(3) 0.9641(3) 0.5339(3) 0.0573(8) Uani 1 1 d . . .
H14A H 0.2352 1.0265 0.5806 0.069 Uiso 1 1 calc R . .
H14B H 0.2542 0.9575 0.4503 0.069 Uiso 1 1 calc R . .
C15 C 0.2571(2) 0.8165(2) 0.57539(18) 0.0280(4) Uani 1 1 d . . .
C16 C 0.5357(3) 0.4516(3) 0.9562(2) 0.0465(6) Uani 1 1 d . . .
H16A H 0.6082 0.4102 1.0007 0.056 Uiso 1 1 calc R . .
H16B H 0.5883 0.5096 0.8994 0.056 Uiso 1 1 calc R . .
C17 C 0.4252(3) 0.3311(3) 0.8869(2) 0.0497(6) Uani 1 1 d . . .
H17A H 0.3818 0.2663 0.9430 0.060 Uiso 1 1 calc R . .
H17B H 0.4779 0.2769 0.8304 0.060 Uiso 1 1 calc R . .
C18 C 0.3011(2) 0.3820(2) 0.81819(18) 0.0315(4) Uani 1 1 d . . .
N1 N 0.13356(19) -0.31887(18) -0.18462(14) 0.0279(3) Uani 1 1 d . . .
N2 N 0.0193(2) -0.27397(18) -0.01943(15) 0.0311(4) Uani 1 1 d . . .
H2A H -0.0462 -0.2827 0.0336 0.037 Uiso 1 1 calc R . .
N3 N 0.26227(18) 0.48006(17) 0.50281(14) 0.0248(3) Uani 1 1 d . . .
N4 N 0.38360(19) 0.43326(18) 0.34207(15) 0.0283(4) Uani 1 1 d . . .
H4A H 0.4462 0.4453 0.2871 0.034 Uiso 1 1 calc R . .
O1 O 0.35132(15) 0.76982(14) 0.63771(12) 0.0278(3) Uani 1 1 d . . .
O2 O 0.12940(15) 0.74133(15) 0.54922(13) 0.0306(3) Uani 1 1 d U . .
O3 O 0.33906(15) 0.48389(15) 0.75531(12) 0.0292(3) Uani 1 1 d . . .
O4 O 0.16983(19) 0.32148(18) 0.82605(15) 0.0437(4) Uani 1 1 d . . .
O1W O 0.00833(17) 0.42537(16) 0.66338(14) 0.0312(3) Uani 1 1 d . . .
H2W H 0.047(3) 0.374(3) 0.707(3) 0.052(9) Uiso 1 1 d . . .
H1W H -0.041(3) 0.372(3) 0.603(3) 0.049(8) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02529(15) 0.01830(13) 0.01670(14) -0.00444(9) 0.00224(9) -0.00366(9)
C1 0.0251(10) 0.0382(11) 0.0328(11) -0.0141(9) 0.0034(8) -0.0025(8)
C2 0.0293(10) 0.0411(12) 0.0332(11) -0.0167(9) 0.0091(8) 0.0004(9)
C3 0.0323(10) 0.0231(9) 0.0217(9) -0.0055(7) 0.0012(7) 0.0017(7)
C4 0.0335(11) 0.0257(9) 0.0314(10) -0.0088(8) 0.0066(8) -0.0053(8)
C5 0.0335(11) 0.0286(10) 0.0268(10) -0.0089(8) 0.0100(8) -0.0012(8)
C6 0.0297(10) 0.0236(9) 0.0193(8) -0.0054(7) -0.0006(7) 0.0023(7)
C7 0.0250(9) 0.0233(9) 0.0215(9) -0.0050(7) 0.0001(7) -0.0006(7)
C8 0.0273(9) 0.0222(9) 0.0239(9) -0.0052(7) 0.0031(7) -0.0040(7)
C9 0.0329(10) 0.0234(9) 0.0239(9) -0.0063(7) 0.0039(7) -0.0055(7)
C10 0.0319(10) 0.0223(9) 0.0226(9) -0.0047(7) 0.0022(7) 0.0000(7)
C11 0.0313(10) 0.0258(9) 0.0249(9) -0.0079(7) 0.0049(8) -0.0041(8)
C12 0.0381(11) 0.0248(9) 0.0260(10) -0.0079(8) 0.0066(8) -0.0058(8)
C13 0.0493(15) 0.0262(11) 0.0729(18) 0.0122(11) 0.0117(13) -0.0087(10)
C14 0.0426(14) 0.0371(13) 0.097(2) 0.0325(15) 0.0124(14) 0.0038(11)
C15 0.0287(10) 0.0232(9) 0.0300(10) 0.0002(7) 0.0063(8) -0.0011(7)
C16 0.0447(14) 0.0598(16) 0.0343(12) 0.0053(11) -0.0085(10) 0.0100(12)
C17 0.0629(17) 0.0427(13) 0.0433(14) 0.0079(11) -0.0110(12) 0.0100(12)
C18 0.0407(12) 0.0293(10) 0.0211(9) -0.0005(8) 0.0007(8) -0.0016(8)
N1 0.0336(9) 0.0247(8) 0.0216(8) -0.0058(6) 0.0043(6) -0.0015(7)
N2 0.0389(10) 0.0261(8) 0.0236(8) -0.0060(7) 0.0100(7) -0.0043(7)
N3 0.0282(8) 0.0226(7) 0.0205(7) -0.0045(6) 0.0025(6) -0.0009(6)
N4 0.0307(9) 0.0283(8) 0.0216(8) -0.0050(6) 0.0075(6) -0.0042(7)
O1 0.0294(7) 0.0232(6) 0.0271(7) -0.0005(5) 0.0012(5) -0.0041(5)
O2 0.0276(7) 0.0294(7) 0.0322(7) 0.0015(5) 0.0005(6) -0.0010(5)
O3 0.0289(7) 0.0317(7) 0.0255(7) 0.0059(6) 0.0024(5) -0.0006(6)
O4 0.0455(10) 0.0437(9) 0.0362(9) 0.0121(7) 0.0031(7) -0.0124(7)
O1W 0.0318(8) 0.0292(7) 0.0260(7) -0.0065(6) 0.0018(6) -0.0078(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 2.0535(15) . ?
Ni1 O3 2.0615(14) . ?
Ni1 N1 2.0694(16) 1_566 ?
Ni1 O1W 2.0884(15) . ?
Ni1 O1 2.1047(13) . ?
Ni1 O2 2.1760(15) . ?
C1 C2 1.383(3) . ?
C1 C6 1.388(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.390(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(3) . ?
C3 C10 1.463(3) . ?
C4 C5 1.384(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.462(2) . ?
C7 C8 1.361(3) . ?
C7 N4 1.372(2) . ?
C8 N3 1.377(2) . ?
C8 H8 0.9300 . ?
C9 N3 1.316(2) . ?
C9 N4 1.338(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.367(3) . ?
C10 N2 1.375(3) . ?
C11 N1 1.375(2) . ?
C11 H11 0.9300 . ?
C12 N1 1.316(3) . ?
C12 N2 1.345(3) . ?
C12 H12 0.9300 . ?
C13 C13 1.507(5) 2_676 ?
C13 C14 1.516(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.504(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O1 1.251(3) . ?
C15 O2 1.266(2) . ?
C16 C16 1.518(5) 2_667 ?
C16 C17 1.513(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.517(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O4 1.250(3) . ?
C18 O3 1.260(2) . ?
N1 Ni1 2.0694(16) 1_544 ?
N2 H2A 0.8600 . ?
N4 H4A 0.8600 . ?
O1W H2W 0.83(3) . ?
O1W H1W 0.86(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 O3 88.56(6) . . ?
N3 Ni1 N1 178.46(6) . 1_566 ?
O3 Ni1 N1 90.06(6) . 1_566 ?
N3 Ni1 O1W 92.84(6) . . ?
O3 Ni1 O1W 96.37(6) . . ?
N1 Ni1 O1W 86.63(6) 1_566 . ?
N3 Ni1 O1 90.90(6) . . ?
O3 Ni1 O1 96.78(6) . . ?
N1 Ni1 O1 89.95(6) 1_566 . ?
O1W Ni1 O1 166.42(6) . . ?
N3 Ni1 O2 88.45(6) . . ?
O3 Ni1 O2 157.78(6) . . ?
N1 Ni1 O2 93.09(6) 1_566 . ?
O1W Ni1 O2 105.77(6) . . ?
O1 Ni1 O2 61.27(5) . . ?
C2 C1 C6 120.09(19) . . ?
C2 C1 H1 120.0 . . ?
C6 C1 H1 120.0 . . ?
C1 C2 C3 121.66(19) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C4 C3 C2 118.12(18) . . ?
C4 C3 C10 121.77(18) . . ?
C2 C3 C10 120.04(18) . . ?
C5 C4 C3 120.45(19) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 121.17(18) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 118.51(17) . . ?
C1 C6 C7 122.27(18) . . ?
C5 C6 C7 119.15(17) . . ?
C8 C7 N4 105.18(16) . . ?
C8 C7 C6 129.54(18) . . ?
N4 C7 C6 124.97(17) . . ?
C7 C8 N3 110.29(16) . . ?
C7 C8 H8 124.9 . . ?
N3 C8 H8 124.9 . . ?
N3 C9 N4 111.77(17) . . ?
N3 C9 H9 124.1 . . ?
N4 C9 H9 124.1 . . ?
C11 C10 N2 104.92(16) . . ?
C11 C10 C3 131.26(18) . . ?
N2 C10 C3 123.75(17) . . ?
C10 C11 N1 110.31(17) . . ?
C10 C11 H11 124.8 . . ?
N1 C11 H11 124.8 . . ?
N1 C12 N2 111.47(18) . . ?
N1 C12 H12 124.3 . . ?
N2 C12 H12 124.3 . . ?
C13 C13 C14 114.0(3) 2_676 . ?
C13 C13 H13A 108.8 2_676 . ?
C14 C13 H13A 108.8 . . ?
C13 C13 H13B 108.8 2_676 . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C15 C14 C13 115.7(2) . . ?
C15 C14 H14A 108.3 . . ?
C13 C14 H14A 108.3 . . ?
C15 C14 H14B 108.3 . . ?
C13 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
O1 C15 O2 120.25(18) . . ?
O1 C15 C14 121.1(2) . . ?
O2 C15 C14 118.6(2) . . ?
C16 C16 C17 113.4(3) 2_667 . ?
C16 C16 H16A 108.9 2_667 . ?
C17 C16 H16A 108.9 . . ?
C16 C16 H16B 108.9 2_667 . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 C18 113.9(2) . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
O4 C18 O3 124.2(2) . . ?
O4 C18 C17 119.2(2) . . ?
O3 C18 C17 116.6(2) . . ?
C12 N1 C11 105.40(16) . . ?
C12 N1 Ni1 128.76(14) . 1_544 ?
C11 N1 Ni1 125.67(13) . 1_544 ?
C12 N2 C10 107.90(16) . . ?
C12 N2 H2A 126.0 . . ?
C10 N2 H2A 126.0 . . ?
C9 N3 C8 105.00(16) . . ?
C9 N3 Ni1 127.51(13) . . ?
C8 N3 Ni1 127.45(13) . . ?
C9 N4 C7 107.76(16) . . ?
C9 N4 H4A 126.1 . . ?
C7 N4 H4A 126.1 . . ?
C15 O1 Ni1 91.01(12) . . ?
C15 O2 Ni1 87.41(12) . . ?
C18 O3 Ni1 126.09(14) . . ?
Ni1 O1W H2W 97(2) . . ?
Ni1 O1W H1W 127.2(19) . . ?
H2W O1W H1W 109(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.2(4) . . . . ?
C1 C2 C3 C4 -0.9(3) . . . . ?
C1 C2 C3 C10 176.2(2) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C10 C3 C4 C5 -176.1(2) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C2 C1 C6 C5 0.4(3) . . . . ?
C2 C1 C6 C7 -176.4(2) . . . . ?
C4 C5 C6 C1 -0.4(3) . . . . ?
C4 C5 C6 C7 176.6(2) . . . . ?
C1 C6 C7 C8 -166.5(2) . . . . ?
C5 C6 C7 C8 16.7(3) . . . . ?
C1 C6 C7 N4 20.9(3) . . . . ?
C5 C6 C7 N4 -155.9(2) . . . . ?
N4 C7 C8 N3 0.4(2) . . . . ?
C6 C7 C8 N3 -173.33(19) . . . . ?
C4 C3 C10 C11 165.6(2) . . . . ?
C2 C3 C10 C11 -11.4(4) . . . . ?
C4 C3 C10 N2 -11.1(3) . . . . ?
C2 C3 C10 N2 172.0(2) . . . . ?
N2 C10 C11 N1 -0.3(2) . . . . ?
C3 C10 C11 N1 -177.4(2) . . . . ?
C13 C13 C14 C15 70.0(4) 2_676 . . . ?
C13 C14 C15 O1 15.1(4) . . . . ?
C13 C14 C15 O2 -167.1(2) . . . . ?
C16 C16 C17 C18 55.8(4) 2_667 . . . ?
C16 C17 C18 O4 -132.7(2) . . . . ?
C16 C17 C18 O3 47.8(3) . . . . ?
N2 C12 N1 C11 -0.4(3) . . . . ?
N2 C12 N1 Ni1 175.06(14) . . . 1_544 ?
C10 C11 N1 C12 0.4(2) . . . . ?
C10 C11 N1 Ni1 -175.20(14) . . . 1_544 ?
N1 C12 N2 C10 0.2(3) . . . . ?
C11 C10 N2 C12 0.1(2) . . . . ?
C3 C10 N2 C12 177.4(2) . . . . ?
N4 C9 N3 C8 0.5(2) . . . . ?
N4 C9 N3 Ni1 178.26(14) . . . . ?
C7 C8 N3 C9 -0.6(2) . . . . ?
C7 C8 N3 Ni1 -178.32(13) . . . . ?
O3 Ni1 N3 C9 -93.95(18) . . . . ?
O1W Ni1 N3 C9 169.75(18) . . . . ?
O1 Ni1 N3 C9 2.81(18) . . . . ?
O2 Ni1 N3 C9 64.03(18) . . . . ?
O3 Ni1 N3 C8 83.27(17) . . . . ?
O1W Ni1 N3 C8 -13.03(17) . . . . ?
O1 Ni1 N3 C8 -179.97(17) . . . . ?
O2 Ni1 N3 C8 -118.74(17) . . . . ?
N3 C9 N4 C7 -0.3(2) . . . . ?
C8 C7 N4 C9 -0.1(2) . . . . ?
C6 C7 N4 C9 174.03(19) . . . . ?
O2 C15 O1 Ni1 -2.53(19) . . . . ?
C14 C15 O1 Ni1 175.2(2) . . . . ?
N3 Ni1 O1 C15 89.19(12) . . . . ?
O3 Ni1 O1 C15 177.84(12) . . . . ?
N1 Ni1 O1 C15 -92.10(12) 1_566 . . . ?
O1W Ni1 O1 C15 -16.8(3) . . . . ?
O2 Ni1 O1 C15 1.45(11) . . . . ?
O1 C15 O2 Ni1 2.45(19) . . . . ?
C14 C15 O2 Ni1 -175.4(2) . . . . ?
N3 Ni1 O2 C15 -93.31(12) . . . . ?
O3 Ni1 O2 C15 -10.9(2) . . . . ?
N1 Ni1 O2 C15 86.81(12) 1_566 . . . ?
O1W Ni1 O2 C15 174.18(11) . . . . ?
O1 Ni1 O2 C15 -1.43(11) . . . . ?
O4 C18 O3 Ni1 3.1(3) . . . . ?
C17 C18 O3 Ni1 -177.45(15) . . . . ?
N3 Ni1 O3 C18 -107.23(17) . . . . ?
N1 Ni1 O3 C18 72.09(17) 1_566 . . . ?
O1W Ni1 O3 C18 -14.52(17) . . . . ?
O1 Ni1 O3 C18 162.04(16) . . . . ?
O2 Ni1 O3 C18 170.43(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.886
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.072

#====END

data_2
_database_code_depnum_ccdc_archive 'CCDC 761520'
#TrackingRef 'sun-cec.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Co N4 O5'
_chemical_formula_sum            'C18 H18 Co N4 O5'
_chemical_formula_weight         429.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'P2(1)/c '
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.296(2)
_cell_length_b                   18.603(5)
_cell_length_c                   14.049(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 129.493(10)
_cell_angle_gamma                90.00
_cell_volume                     1874.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14361
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4227
_reflns_number_gt                3503
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+3.3191P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4227
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1246
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_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 -0.00279(5) 0.75798(2) 0.24350(3) 0.01082(13) Uani 1 1 d . . .
C1 C 0.4295(4) 1.06421(15) 0.0573(3) 0.0145(6) Uani 1 1 d . . .
C2 C 0.4989(5) 1.02921(18) 0.1669(3) 0.0229(7) Uani 1 1 d . . .
H2 H 0.6149 1.0440 0.2418 0.027 Uiso 1 1 calc R . .
C3 C 0.4024(4) 0.97364(18) 0.1685(3) 0.0210(7) Uani 1 1 d . . .
H3A H 0.4538 0.9502 0.2442 0.025 Uiso 1 1 calc R . .
C4 C 0.2300(4) 0.95123(15) 0.0604(3) 0.0142(6) Uani 1 1 d . . .
C5 C 0.1597(4) 0.98547(15) -0.0495(3) 0.0150(6) Uani 1 1 d . . .
H5 H 0.0433 0.9708 -0.1241 0.018 Uiso 1 1 calc R . .
C6 C 0.2584(4) 1.04124(16) -0.0512(3) 0.0157(6) Uani 1 1 d . . .
H6 H 0.2086 1.0639 -0.1272 0.019 Uiso 1 1 calc R . .
C7 C 0.1317(4) 0.89422(15) 0.0702(3) 0.0135(6) Uani 1 1 d . . .
C8 C 0.1590(4) 0.86838(15) 0.1719(3) 0.0141(6) Uani 1 1 d . . .
H8 H 0.2520 0.8849 0.2539 0.017 Uiso 1 1 calc R . .
C9 C -0.0723(4) 0.80889(16) 0.0159(3) 0.0153(6) Uani 1 1 d . . .
H9 H -0.1725 0.7759 -0.0335 0.018 Uiso 1 1 calc R . .
C10 C 0.5419(4) 1.12235(15) 0.0638(3) 0.0140(6) Uani 1 1 d . . .
C11 C 0.7136(4) 1.14673(15) 0.1623(3) 0.0162(6) Uani 1 1 d . . .
H11 H 0.7856 1.1277 0.2435 0.019 Uiso 1 1 calc R . .
C12 C 0.6300(4) 1.21214(16) 0.0089(3) 0.0156(6) Uani 1 1 d . . .
H12 H 0.6286 1.2477 -0.0403 0.019 Uiso 1 1 calc R . .
C13 C -0.0266(4) 0.85709(15) 0.3615(3) 0.0143(6) Uani 1 1 d . . .
C14 C -0.0840(4) 0.90717(16) 0.4170(3) 0.0173(6) Uani 1 1 d . . .
H14A H -0.0700 0.8815 0.4842 0.021 Uiso 1 1 calc R . .
H14B H -0.2176 0.9190 0.3529 0.021 Uiso 1 1 calc R . .
C15 C 0.0267(4) 0.97703(16) 0.4684(3) 0.0176(6) Uani 1 1 d . . .
H15A H 0.0049 1.0049 0.4003 0.021 Uiso 1 1 calc R . .
H15B H 0.1613 0.9656 0.5284 0.021 Uiso 1 1 calc R . .
C16 C -0.2497(4) 0.64175(15) 0.1278(3) 0.0141(6) Uani 1 1 d . . .
C17 C -0.3992(4) 0.59511(16) 0.0190(3) 0.0163(6) Uani 1 1 d . . .
H17A H -0.5194 0.6212 -0.0295 0.020 Uiso 1 1 calc R . .
H17B H -0.3667 0.5876 -0.0351 0.020 Uiso 1 1 calc R . .
C18 C -0.4245(4) 0.52218(16) 0.0555(3) 0.0177(6) Uani 1 1 d . . .
H18A H -0.3052 0.4955 0.1030 0.021 Uiso 1 1 calc R . .
H18B H -0.4570 0.5293 0.1097 0.021 Uiso 1 1 calc R . .
N1 N 0.4918(3) 1.16501(13) -0.0336(2) 0.0151(5) Uani 1 1 d . . .
H1 H 0.3875 1.1618 -0.1101 0.018 Uiso 1 1 calc R . .
N2 N 0.7679(3) 1.20280(13) 0.1277(2) 0.0141(5) Uani 1 1 d . . .
N3 N -0.0167(3) 0.85537(13) -0.0273(2) 0.0153(5) Uani 1 1 d . . .
H3 H -0.0665 0.8604 -0.1051 0.018 Uiso 1 1 calc R . .
N4 N 0.0319(3) 0.81510(13) 0.1378(2) 0.0140(5) Uani 1 1 d . . .
O1 O -0.1524(3) 0.81297(11) 0.27750(18) 0.0156(4) Uani 1 1 d . . .
O2 O 0.1334(3) 0.85655(12) 0.3953(2) 0.0193(5) Uani 1 1 d . . .
O3 O -0.1754(3) 0.68949(11) 0.1074(2) 0.0201(5) Uani 1 1 d . . .
O4 O -0.2106(4) 0.63183(14) 0.2293(2) 0.0343(6) Uani 1 1 d . . .
O1W O 0.404(3) 0.8491(13) 0.659(2) 0.522(15) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0109(2) 0.0102(2) 0.01075(19) -0.00038(14) 0.00663(16) -0.00055(14)
C1 0.0139(14) 0.0133(14) 0.0167(14) 0.0015(11) 0.0099(12) 0.0006(11)
C2 0.0182(16) 0.0270(17) 0.0143(15) 0.0017(12) 0.0060(13) -0.0077(13)
C3 0.0162(16) 0.0282(17) 0.0142(14) 0.0045(12) 0.0076(13) -0.0042(13)
C4 0.0165(15) 0.0144(14) 0.0155(14) -0.0006(11) 0.0120(12) -0.0007(11)
C5 0.0133(14) 0.0159(14) 0.0131(13) -0.0003(11) 0.0071(12) -0.0007(11)
C6 0.0165(15) 0.0169(14) 0.0124(13) 0.0012(11) 0.0085(12) -0.0004(12)
C7 0.0129(14) 0.0140(13) 0.0123(13) -0.0002(10) 0.0075(12) -0.0007(11)
C8 0.0131(14) 0.0142(14) 0.0140(13) -0.0023(11) 0.0082(12) -0.0041(11)
C9 0.0147(14) 0.0170(14) 0.0122(13) -0.0020(11) 0.0076(12) -0.0034(11)
C10 0.0142(14) 0.0145(14) 0.0128(13) 0.0015(10) 0.0083(12) 0.0016(11)
C11 0.0192(15) 0.0125(13) 0.0158(14) 0.0014(11) 0.0106(13) -0.0015(11)
C12 0.0153(15) 0.0154(14) 0.0148(14) -0.0004(11) 0.0091(12) -0.0024(11)
C13 0.0169(15) 0.0113(13) 0.0142(13) 0.0043(10) 0.0097(12) 0.0023(11)
C14 0.0175(15) 0.0156(15) 0.0200(15) -0.0040(11) 0.0124(13) 0.0000(12)
C15 0.0193(16) 0.0174(15) 0.0177(14) -0.0040(11) 0.0125(13) -0.0010(12)
C16 0.0145(14) 0.0124(14) 0.0126(13) -0.0004(10) 0.0073(12) 0.0006(11)
C17 0.0178(15) 0.0177(15) 0.0116(13) -0.0023(11) 0.0086(12) -0.0049(12)
C18 0.0199(16) 0.0170(15) 0.0148(15) -0.0038(11) 0.0104(13) -0.0078(12)
N1 0.0114(12) 0.0182(13) 0.0112(11) -0.0004(9) 0.0050(10) -0.0030(10)
N2 0.0134(12) 0.0125(12) 0.0146(12) 0.0013(9) 0.0081(10) 0.0004(9)
N3 0.0155(13) 0.0177(13) 0.0100(11) -0.0002(9) 0.0068(10) -0.0021(10)
N4 0.0161(12) 0.0129(12) 0.0118(11) -0.0020(9) 0.0083(10) -0.0027(9)
O1 0.0148(10) 0.0153(10) 0.0145(10) -0.0036(8) 0.0083(9) -0.0015(8)
O2 0.0163(11) 0.0217(11) 0.0197(11) -0.0045(9) 0.0112(9) 0.0013(9)
O3 0.0240(12) 0.0184(11) 0.0197(11) -0.0063(9) 0.0147(10) -0.0093(9)
O4 0.0486(17) 0.0351(14) 0.0128(11) -0.0077(10) 0.0166(12) -0.0219(12)
O1W 0.47(3) 0.70(4) 0.57(3) 0.30(3) 0.41(3) 0.20(3)

_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 1.988(2) . ?
Co1 N4 2.012(2) . ?
Co1 O1 2.013(2) . ?
Co1 N2 2.017(2) 2_645 ?
C1 C2 1.396(4) . ?
C1 C6 1.397(4) . ?
C1 C10 1.466(4) . ?
C2 C3 1.378(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.397(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.390(4) . ?
C4 C7 1.462(4) . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.370(4) . ?
C7 N3 1.378(4) . ?
C8 N4 1.374(4) . ?
C8 H8 0.9500 . ?
C9 N4 1.332(4) . ?
C9 N3 1.336(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.363(4) . ?
C10 N1 1.381(4) . ?
C11 N2 1.375(4) . ?
C11 H11 0.9500 . ?
C12 N2 1.318(4) . ?
C12 N1 1.341(4) . ?
C12 H12 0.9500 . ?
C13 O2 1.240(4) . ?
C13 O1 1.295(4) . ?
C13 C14 1.513(4) . ?
C14 C15 1.524(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C15 1.525(6) 3_576 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 O4 1.241(4) . ?
C16 O3 1.265(4) . ?
C16 C17 1.523(4) . ?
C17 C18 1.521(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C18 1.516(6) 3_465 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
N1 H1 0.8800 . ?
N2 Co1 2.017(2) 2_655 ?
N3 H3 0.8800 . ?

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 N4 92.23(9) . . ?
O3 Co1 O1 107.28(9) . . ?
N4 Co1 O1 111.47(9) . . ?
O3 Co1 N2 106.72(10) . 2_645 ?
N4 Co1 N2 109.90(10) . 2_645 ?
O1 Co1 N2 124.24(9) . 2_645 ?
C2 C1 C6 117.9(3) . . ?
C2 C1 C10 117.7(3) . . ?
C6 C1 C10 124.5(3) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 118.3(3) . . ?
C5 C4 C7 123.8(3) . . ?
C3 C4 C7 117.9(3) . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 120.9(3) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C8 C7 N3 104.9(2) . . ?
C8 C7 C4 129.8(3) . . ?
N3 C7 C4 125.3(3) . . ?
C7 C8 N4 110.0(2) . . ?
C7 C8 H8 125.0 . . ?
N4 C8 H8 125.0 . . ?
N4 C9 N3 110.6(3) . . ?
N4 C9 H9 124.7 . . ?
N3 C9 H9 124.7 . . ?
C11 C10 N1 104.7(3) . . ?
C11 C10 C1 129.6(3) . . ?
N1 C10 C1 125.7(3) . . ?
C10 C11 N2 110.4(3) . . ?
C10 C11 H11 124.8 . . ?
N2 C11 H11 124.8 . . ?
N2 C12 N1 111.2(3) . . ?
N2 C12 H12 124.4 . . ?
N1 C12 H12 124.4 . . ?
O2 C13 O1 120.8(3) . . ?
O2 C13 C14 122.5(3) . . ?
O1 C13 C14 116.7(3) . . ?
C13 C14 C15 114.6(3) . . ?
C13 C14 H14A 108.6 . . ?
C15 C14 H14A 108.6 . . ?
C13 C14 H14B 108.6 . . ?
C15 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 C15 112.5(3) . 3_576 ?
C14 C15 H15A 109.1 . . ?
C15 C15 H15A 109.1 3_576 . ?
C14 C15 H15B 109.1 . . ?
C15 C15 H15B 109.1 3_576 . ?
H15A C15 H15B 107.8 . . ?
O4 C16 O3 124.2(3) . . ?
O4 C16 C17 118.8(3) . . ?
O3 C16 C17 117.0(2) . . ?
C18 C17 C16 114.1(2) . . ?
C18 C17 H17A 108.7 . . ?
C16 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C16 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C18 C18 C17 112.3(3) 3_465 . ?
C18 C18 H18A 109.1 3_465 . ?
C17 C18 H18A 109.1 . . ?
C18 C18 H18B 109.1 3_465 . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.9 . . ?
C12 N1 C10 108.1(2) . . ?
C12 N1 H1 126.0 . . ?
C10 N1 H1 126.0 . . ?
C12 N2 C11 105.5(2) . . ?
C12 N2 Co1 134.0(2) . 2_655 ?
C11 N2 Co1 120.01(19) . 2_655 ?
C9 N3 C7 108.7(2) . . ?
C9 N3 H3 125.7 . . ?
C7 N3 H3 125.7 . . ?
C9 N4 C8 105.8(2) . . ?
C9 N4 Co1 125.2(2) . . ?
C8 N4 Co1 128.99(19) . . ?
C13 O1 Co1 100.30(18) . . ?
C16 O3 Co1 117.10(19) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         2.352
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.093

#====END

data_3
_database_code_depnum_ccdc_archive 'CCDC 761521'
#TrackingRef 'sun-cec.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 Cd2 N4 O8'
_chemical_formula_sum            'C24 H26 Cd2 N4 O8'
_chemical_formula_weight         723.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Cd Cd -0.8075 1.2024 '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                   10.0234(16)
_cell_length_b                   11.8495(19)
_cell_length_c                   12.210(2)
_cell_angle_alpha                110.104(3)
_cell_angle_beta                 107.980(2)
_cell_angle_gamma                95.921(3)
_cell_volume                     1259.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5566
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      28.25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_T_max  0.8179
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7532
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         28.29
_reflns_number_total             5536
_reflns_number_gt                5155
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.6972P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5536
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.1018
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.42140(2) 0.327255(16) 0.874327(18) 0.02463(9) Uani 1 1 d . . .
Cd2 Cd 0.59945(2) 0.176243(17) 0.639469(18) 0.02343(9) Uani 1 1 d . . .
C1 C 0.9507(3) -0.1506(2) 0.7536(3) 0.0247(5) Uani 1 1 d . . .
C2 C 1.0766(3) -0.1471(3) 0.8467(3) 0.0340(7) Uani 1 1 d . . .
H2 H 1.1250 -0.0733 0.9160 0.041 Uiso 1 1 calc R . .
C3 C 1.1300(3) -0.2515(3) 0.8373(3) 0.0331(6) Uani 1 1 d . . .
H3 H 1.2139 -0.2473 0.9001 0.040 Uiso 1 1 calc R . .
C4 C 1.0592(3) -0.3631(2) 0.7344(3) 0.0242(5) Uani 1 1 d . . .
C5 C 0.9340(3) -0.3668(3) 0.6408(3) 0.0326(6) Uani 1 1 d . . .
H5 H 0.8861 -0.4404 0.5712 0.039 Uiso 1 1 calc R . .
C6 C 0.8804(3) -0.2620(3) 0.6503(3) 0.0320(6) Uani 1 1 d . . .
H6 H 0.7969 -0.2661 0.5872 0.038 Uiso 1 1 calc R . .
C7 C 0.8933(3) -0.0407(2) 0.7633(3) 0.0238(5) Uani 1 1 d . . .
C8 C 0.7596(3) -0.0287(3) 0.7023(3) 0.0250(5) Uani 1 1 d . . .
H8 H 0.6811 -0.0937 0.6454 0.030 Uiso 1 1 calc R . .
C9 C 0.8907(3) 0.1555(3) 0.8197(3) 0.0297(6) Uani 1 1 d . . .
H9 H 0.9213 0.2412 0.8589 0.036 Uiso 1 1 calc R . .
C10 C 1.1140(3) -0.4736(3) 0.7294(3) 0.0245(5) Uani 1 1 d . . .
C11 C 1.2470(3) -0.4853(3) 0.7921(3) 0.0274(6) Uani 1 1 d . . .
H11 H 1.3274 -0.4202 0.8436 0.033 Uiso 1 1 calc R . .
C12 C 1.1106(3) -0.6691(3) 0.6911(3) 0.0294(6) Uani 1 1 d . . .
H12 H 1.0773 -0.7544 0.6599 0.035 Uiso 1 1 calc R . .
C13 C 0.6191(3) 0.3159(3) 0.5067(3) 0.0305(6) Uani 1 1 d . . .
C14 C 0.6111(4) 0.3797(3) 0.4167(3) 0.0390(8) Uani 1 1 d . . .
H14A H 0.7019 0.3878 0.4040 0.047 Uiso 1 1 calc R . .
H14B H 0.5979 0.4623 0.4543 0.047 Uiso 1 1 calc R . .
C15 C 0.4885(4) 0.3100(3) 0.2896(3) 0.0373(7) Uani 1 1 d . . .
H15A H 0.3981 0.2982 0.3023 0.045 Uiso 1 1 calc R . .
H15B H 0.4818 0.3592 0.2398 0.045 Uiso 1 1 calc R . .
C16 C 0.5111(4) 0.1851(3) 0.2185(3) 0.0358(7) Uani 1 1 d . . .
H16A H 0.5152 0.1352 0.2675 0.043 Uiso 1 1 calc R . .
H16B H 0.6028 0.1968 0.2079 0.043 Uiso 1 1 calc R . .
C17 C 0.3911(4) 0.1163(3) 0.0900(3) 0.0371(7) Uani 1 1 d . . .
H17A H 0.4053 0.0342 0.0524 0.045 Uiso 1 1 calc R . .
H17B H 0.2993 0.1072 0.1009 0.045 Uiso 1 1 calc R . .
C18 C 0.3847(3) 0.1809(3) 0.0010(3) 0.0266(6) Uani 1 1 d . . .
C19 C 0.3054(3) 0.5392(3) 1.1002(3) 0.0272(6) Uani 1 1 d . . .
C20 C 0.1718(4) 0.4446(3) 1.0705(4) 0.0403(8) Uani 1 1 d . . .
H20A H 0.1917 0.4129 1.1359 0.048 Uiso 1 1 calc R . .
H20B H 0.1570 0.3761 0.9927 0.048 Uiso 1 1 calc R . .
C21 C 0.0305(3) 0.4857(3) 1.0575(3) 0.0345(6) Uani 1 1 d . . .
H21A H -0.0403 0.4210 1.0541 0.041 Uiso 1 1 calc R . .
H21B H 0.0460 0.5588 1.1316 0.041 Uiso 1 1 calc R . .
C22 C 0.3379(3) 0.0503(3) 0.6220(2) 0.0235(5) Uani 1 1 d . . .
C23 C 0.1887(3) -0.0013(3) 0.6112(3) 0.0338(6) Uani 1 1 d . . .
H23A H 0.1741 0.0432 0.6881 0.041 Uiso 1 1 calc R . .
H23B H 0.1777 -0.0877 0.5987 0.041 Uiso 1 1 calc R . .
C24 C 0.0760(3) 0.0111(3) 0.4997(3) 0.0291(6) Uani 1 1 d . . .
H24A H 0.1022 0.0934 0.5023 0.035 Uiso 1 1 calc R . .
H24B H 0.0773 -0.0478 0.4220 0.035 Uiso 1 1 calc R . .
N1 N 0.7595(3) 0.0949(2) 0.7386(2) 0.0260(5) Uani 1 1 d . . .
N2 N 0.9739(3) 0.0777(2) 0.8382(2) 0.0283(5) Uani 1 1 d . . .
H2A H 1.0625 0.0982 0.8883 0.034 Uiso 1 1 calc R . .
N3 N 1.0297(3) -0.5922(2) 0.6648(2) 0.0271(5) Uani 1 1 d . . .
H3A H 0.9405 -0.6132 0.6160 0.033 Uiso 1 1 calc R . .
N4 N 1.2438(3) -0.6083(2) 0.7673(2) 0.0289(5) Uani 1 1 d . . .
O1 O 0.7391(3) 0.3088(2) 0.5733(2) 0.0396(5) Uani 1 1 d . . .
O2 O 0.5038(2) 0.2706(2) 0.5120(2) 0.0335(5) Uani 1 1 d . . .
O3 O 0.2654(2) 0.1808(2) -0.0727(2) 0.0334(5) Uani 1 1 d . . .
O4 O 0.5022(2) 0.2342(2) 0.0038(2) 0.0327(5) Uani 1 1 d . . .
O5 O 0.3975(2) 0.16265(19) 0.6935(2) 0.0368(5) Uani 1 1 d . . .
O6 O 0.4001(3) -0.0120(2) 0.5588(2) 0.0375(5) Uani 1 1 d . . .
O7 O 0.4043(2) 0.5001(2) 1.0653(2) 0.0353(5) Uani 1 1 d . . .
O8 O 0.3161(3) 0.65089(19) 1.1582(2) 0.0445(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.02628(13) 0.02087(13) 0.02464(13) 0.00815(9) 0.00720(9) 0.00688(9)
Cd2 0.02093(13) 0.02256(13) 0.02503(13) 0.00782(9) 0.00754(9) 0.00641(8)
C1 0.0227(13) 0.0207(12) 0.0284(13) 0.0096(10) 0.0068(10) 0.0048(10)
C2 0.0304(15) 0.0200(13) 0.0361(16) 0.0058(11) -0.0012(12) 0.0037(11)
C3 0.0267(14) 0.0246(13) 0.0350(15) 0.0090(12) -0.0021(12) 0.0043(11)
C4 0.0243(13) 0.0192(12) 0.0284(13) 0.0096(10) 0.0080(11) 0.0064(10)
C5 0.0308(15) 0.0216(13) 0.0307(15) 0.0046(11) -0.0007(12) 0.0042(11)
C6 0.0293(14) 0.0249(14) 0.0315(15) 0.0089(12) 0.0001(12) 0.0079(11)
C7 0.0237(13) 0.0204(12) 0.0261(13) 0.0093(10) 0.0077(10) 0.0048(10)
C8 0.0213(12) 0.0219(12) 0.0274(13) 0.0075(10) 0.0065(10) 0.0031(10)
C9 0.0259(14) 0.0221(13) 0.0300(14) 0.0039(11) 0.0029(11) 0.0052(11)
C10 0.0227(13) 0.0215(12) 0.0264(13) 0.0086(10) 0.0070(10) 0.0036(10)
C11 0.0248(13) 0.0201(12) 0.0331(14) 0.0092(11) 0.0073(11) 0.0039(10)
C12 0.0314(15) 0.0189(12) 0.0293(14) 0.0043(11) 0.0062(12) 0.0052(11)
C13 0.0349(16) 0.0243(13) 0.0211(13) 0.0034(11) 0.0044(11) -0.0001(12)
C14 0.0402(18) 0.0411(18) 0.0299(16) 0.0167(14) 0.0073(13) -0.0065(14)
C15 0.0365(17) 0.0433(18) 0.0292(15) 0.0182(14) 0.0054(13) 0.0043(14)
C16 0.0343(16) 0.0427(18) 0.0299(15) 0.0200(14) 0.0063(13) 0.0045(13)
C17 0.0377(17) 0.0373(17) 0.0308(16) 0.0165(13) 0.0063(13) -0.0044(14)
C18 0.0307(14) 0.0217(12) 0.0204(12) 0.0049(10) 0.0056(11) 0.0015(11)
C19 0.0323(15) 0.0254(13) 0.0230(13) 0.0078(10) 0.0113(11) 0.0062(11)
C20 0.0337(17) 0.0331(16) 0.056(2) 0.0170(15) 0.0193(15) 0.0095(13)
C21 0.0318(16) 0.0343(15) 0.0400(17) 0.0133(13) 0.0189(14) 0.0052(12)
C22 0.0216(12) 0.0265(13) 0.0212(12) 0.0078(10) 0.0082(10) 0.0055(10)
C23 0.0229(14) 0.0422(17) 0.0387(16) 0.0189(14) 0.0126(12) 0.0034(12)
C24 0.0218(14) 0.0317(14) 0.0272(13) 0.0043(11) 0.0107(11) -0.0001(11)
N1 0.0224(11) 0.0196(11) 0.0310(12) 0.0065(9) 0.0068(9) 0.0059(9)
N2 0.0226(11) 0.0222(11) 0.0293(12) 0.0052(9) 0.0017(9) 0.0030(9)
N3 0.0241(12) 0.0225(11) 0.0268(12) 0.0044(9) 0.0051(9) 0.0051(9)
N4 0.0296(12) 0.0213(11) 0.0333(13) 0.0098(10) 0.0084(10) 0.0094(9)
O1 0.0295(11) 0.0435(13) 0.0395(13) 0.0187(11) 0.0047(10) -0.0010(10)
O2 0.0297(11) 0.0381(12) 0.0323(11) 0.0168(9) 0.0093(9) 0.0026(9)
O3 0.0275(11) 0.0351(11) 0.0316(11) 0.0121(9) 0.0051(9) 0.0050(9)
O4 0.0279(11) 0.0377(12) 0.0324(11) 0.0186(9) 0.0070(9) 0.0029(9)
O5 0.0358(12) 0.0275(10) 0.0391(12) 0.0017(9) 0.0185(10) 0.0014(9)
O6 0.0319(12) 0.0317(11) 0.0377(12) -0.0015(9) 0.0163(10) 0.0036(9)
O7 0.0281(11) 0.0344(12) 0.0391(12) 0.0073(9) 0.0156(9) 0.0049(9)
O8 0.0546(15) 0.0247(10) 0.0388(12) 0.0004(9) 0.0127(11) 0.0042(10)

_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 O4 2.228(2) 1_556 ?
Cd1 N4 2.234(2) 1_465 ?
Cd1 O7 2.283(2) 2_667 ?
Cd1 O5 2.314(2) . ?
Cd1 O7 2.588(2) . ?
Cd1 O3 2.591(2) 1_556 ?
Cd1 C18 2.757(3) 1_556 ?
Cd2 N1 2.212(2) . ?
Cd2 O2 2.256(2) . ?
Cd2 O5 2.322(2) . ?
Cd2 O8 2.427(2) 2_667 ?
Cd2 O1 2.489(2) . ?
Cd2 O6 2.509(2) . ?
Cd2 O6 2.533(2) 2_656 ?
C1 C6 1.395(4) . ?
C1 C2 1.400(4) . ?
C1 C7 1.460(4) . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(4) . ?
C4 C10 1.461(4) . ?
C5 C6 1.385(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.366(4) . ?
C7 N2 1.374(3) . ?
C8 N1 1.377(4) . ?
C8 H8 0.9300 . ?
C9 N1 1.318(4) . ?
C9 N2 1.334(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.365(4) . ?
C10 N3 1.375(3) . ?
C11 N4 1.378(4) . ?
C11 H11 0.9300 . ?
C12 N4 1.320(4) . ?
C12 N3 1.336(4) . ?
C12 H12 0.9300 . ?
C13 O2 1.254(4) . ?
C13 O1 1.256(4) . ?
C13 C14 1.521(4) . ?
C14 C15 1.528(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.518(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.525(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.520(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O3 1.254(4) . ?
C18 O4 1.262(4) . ?
C18 Cd1 2.757(3) 1_554 ?
C19 O8 1.242(3) . ?
C19 O7 1.265(4) . ?
C19 C20 1.514(4) . ?
C20 C21 1.525(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C21 1.516(6) 2_567 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O6 1.237(4) . ?
C22 O5 1.267(3) . ?
C22 C23 1.503(4) . ?
C23 C24 1.542(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C24 1.522(5) 2_556 ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
N2 H2A 0.8600 . ?
N3 H3A 0.8600 . ?
N4 Cd1 2.234(2) 1_645 ?
O3 Cd1 2.591(2) 1_554 ?
O4 Cd1 2.228(2) 1_554 ?
O6 Cd2 2.533(2) 2_656 ?
O7 Cd1 2.283(2) 2_667 ?
O8 Cd2 2.427(2) 2_667 ?

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
O4 Cd1 N4 150.47(9) 1_556 1_465 ?
O4 Cd1 O7 107.35(9) 1_556 2_667 ?
N4 Cd1 O7 94.93(9) 1_465 2_667 ?
O4 Cd1 O5 95.65(9) 1_556 . ?
N4 Cd1 O5 91.35(9) 1_465 . ?
O7 Cd1 O5 116.33(8) 2_667 . ?
O4 Cd1 O7 86.31(8) 1_556 . ?
N4 Cd1 O7 82.73(9) 1_465 . ?
O7 Cd1 O7 71.24(9) 2_667 . ?
O5 Cd1 O7 170.92(7) . . ?
O4 Cd1 O3 53.56(8) 1_556 1_556 ?
N4 Cd1 O3 98.03(9) 1_465 1_556 ?
O7 Cd1 O3 150.95(8) 2_667 1_556 ?
O5 Cd1 O3 89.31(8) . 1_556 ?
O7 Cd1 O3 84.72(8) . 1_556 ?
O4 Cd1 C18 26.74(9) 1_556 1_556 ?
N4 Cd1 C18 124.22(10) 1_465 1_556 ?
O7 Cd1 C18 130.16(9) 2_667 1_556 ?
O5 Cd1 C18 94.29(8) . 1_556 ?
O7 Cd1 C18 83.46(8) . 1_556 ?
O3 Cd1 C18 26.89(8) 1_556 1_556 ?
N1 Cd2 O2 158.22(9) . . ?
N1 Cd2 O5 109.97(9) . . ?
O2 Cd2 O5 91.80(9) . . ?
N1 Cd2 O8 84.16(9) . 2_667 ?
O2 Cd2 O8 100.29(8) . 2_667 ?
O5 Cd2 O8 79.03(8) . 2_667 ?
N1 Cd2 O1 104.86(9) . . ?
O2 Cd2 O1 54.63(8) . . ?
O5 Cd2 O1 140.49(8) . . ?
O8 Cd2 O1 86.66(8) 2_667 . ?
N1 Cd2 O6 92.49(9) . . ?
O2 Cd2 O6 101.23(9) . . ?
O5 Cd2 O6 53.08(7) . . ?
O8 Cd2 O6 127.52(8) 2_667 . ?
O1 Cd2 O6 143.50(8) . . ?
N1 Cd2 O6 85.08(9) . 2_656 ?
O2 Cd2 O6 84.28(9) . 2_656 ?
O5 Cd2 O6 119.61(8) . 2_656 ?
O8 Cd2 O6 160.88(9) 2_667 2_656 ?
O1 Cd2 O6 80.88(8) . 2_656 ?
O6 Cd2 O6 68.70(9) . 2_656 ?
C6 C1 C2 118.5(3) . . ?
C6 C1 C7 120.3(3) . . ?
C2 C1 C7 121.2(3) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 118.6(3) . . ?
C3 C4 C10 119.6(3) . . ?
C5 C4 C10 121.8(3) . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C8 C7 N2 105.6(2) . . ?
C8 C7 C1 130.7(3) . . ?
N2 C7 C1 123.7(2) . . ?
C7 C8 N1 109.2(2) . . ?
C7 C8 H8 125.4 . . ?
N1 C8 H8 125.4 . . ?
N1 C9 N2 111.1(3) . . ?
N1 C9 H9 124.4 . . ?
N2 C9 H9 124.4 . . ?
C11 C10 N3 105.4(2) . . ?
C11 C10 C4 130.3(3) . . ?
N3 C10 C4 124.0(2) . . ?
C10 C11 N4 109.5(3) . . ?
C10 C11 H11 125.3 . . ?
N4 C11 H11 125.3 . . ?
N4 C12 N3 111.2(3) . . ?
N4 C12 H12 124.4 . . ?
N3 C12 H12 124.4 . . ?
O2 C13 O1 121.3(3) . . ?
O2 C13 C14 118.5(3) . . ?
O1 C13 C14 120.3(3) . . ?
C13 C14 C15 112.9(3) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C16 C15 C14 111.9(3) . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
C14 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 C17 112.3(3) . . ?
C15 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C16 113.5(3) . . ?
C18 C17 H17A 108.9 . . ?
C16 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C16 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
O3 C18 O4 121.5(3) . . ?
O3 C18 C17 120.4(3) . . ?
O4 C18 C17 118.1(3) . . ?
O3 C18 Cd1 69.15(16) . 1_554 ?
O4 C18 Cd1 52.57(14) . 1_554 ?
C17 C18 Cd1 169.1(2) . 1_554 ?
O8 C19 O7 122.1(3) . . ?
O8 C19 C20 120.2(3) . . ?
O7 C19 C20 117.7(3) . . ?
C19 C20 C21 118.1(3) . . ?
C19 C20 H20A 107.8 . . ?
C21 C20 H20A 107.8 . . ?
C19 C20 H20B 107.8 . . ?
C21 C20 H20B 107.8 . . ?
H20A C20 H20B 107.1 . . ?
C21 C21 C20 114.1(3) 2_567 . ?
C21 C21 H21A 108.7 2_567 . ?
C20 C21 H21A 108.7 . . ?
C21 C21 H21B 108.7 2_567 . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
O6 C22 O5 119.6(3) . . ?
O6 C22 C23 121.8(3) . . ?
O5 C22 C23 118.5(2) . . ?
C22 C23 C24 109.5(2) . . ?
C22 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?
C24 C24 C23 112.6(3) 2_556 . ?
C24 C24 H24A 109.1 2_556 . ?
C23 C24 H24A 109.1 . . ?
C24 C24 H24B 109.1 2_556 . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C9 N1 C8 106.1(2) . . ?
C9 N1 Cd2 125.1(2) . . ?
C8 N1 Cd2 126.26(19) . . ?
C9 N2 C7 108.0(2) . . ?
C9 N2 H2A 126.0 . . ?
C7 N2 H2A 126.0 . . ?
C12 N3 C10 108.0(2) . . ?
C12 N3 H3A 126.0 . . ?
C10 N3 H3A 126.0 . . ?
C12 N4 C11 105.9(2) . . ?
C12 N4 Cd1 129.8(2) . 1_645 ?
C11 N4 Cd1 123.1(2) . 1_645 ?
C13 O1 Cd2 86.39(19) . . ?
C13 O2 Cd2 97.34(19) . . ?
C18 O3 Cd1 83.95(18) . 1_554 ?
C18 O4 Cd1 100.68(18) . 1_554 ?
C22 O5 Cd1 146.54(19) . . ?
C22 O5 Cd2 97.63(16) . . ?
Cd1 O5 Cd2 112.77(9) . . ?
C22 O6 Cd2 89.54(17) . . ?
C22 O6 Cd2 152.1(2) . 2_656 ?
Cd2 O6 Cd2 111.30(9) . 2_656 ?
C19 O7 Cd1 105.37(19) . 2_667 ?
C19 O7 Cd1 137.1(2) . . ?
Cd1 O7 Cd1 108.76(9) 2_667 . ?
C19 O8 Cd2 146.8(2) . 2_667 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.4(5) . . . . ?
C7 C1 C2 C3 179.7(3) . . . . ?
C1 C2 C3 C4 -0.1(5) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C2 C3 C4 C10 -177.1(3) . . . . ?
C3 C4 C5 C6 -0.6(5) . . . . ?
C10 C4 C5 C6 177.0(3) . . . . ?
C4 C5 C6 C1 0.2(5) . . . . ?
C2 C1 C6 C5 0.3(5) . . . . ?
C7 C1 C6 C5 -179.7(3) . . . . ?
C6 C1 C7 C8 17.5(5) . . . . ?
C2 C1 C7 C8 -162.6(3) . . . . ?
C6 C1 C7 N2 -159.7(3) . . . . ?
C2 C1 C7 N2 20.2(4) . . . . ?
N2 C7 C8 N1 0.6(3) . . . . ?
C1 C7 C8 N1 -176.9(3) . . . . ?
C3 C4 C10 C11 -19.8(5) . . . . ?
C5 C4 C10 C11 162.6(3) . . . . ?
C3 C4 C10 N3 153.4(3) . . . . ?
C5 C4 C10 N3 -24.3(4) . . . . ?
N3 C10 C11 N4 -0.6(3) . . . . ?
C4 C10 C11 N4 173.5(3) . . . . ?
O2 C13 C14 C15 -41.9(4) . . . . ?
O1 C13 C14 C15 137.8(3) . . . . ?
C13 C14 C15 C16 -65.2(4) . . . . ?
C14 C15 C16 C17 -178.5(2) . . . . ?
C15 C16 C17 C18 64.4(4) . . . . ?
C16 C17 C18 O3 -142.4(3) . . . . ?
C16 C17 C18 O4 37.5(4) . . . . ?
C16 C17 C18 Cd1 8.2(14) . . . 1_554 ?
O8 C19 C20 C21 27.1(5) . . . . ?
O7 C19 C20 C21 -153.6(3) . . . . ?
C19 C20 C21 C21 68.9(4) . . . 2_567 ?
O6 C22 C23 C24 -83.8(4) . . . . ?
O5 C22 C23 C24 92.7(3) . . . . ?
C22 C23 C24 C24 -166.8(3) . . . 2_556 ?
N2 C9 N1 C8 -0.7(4) . . . . ?
N2 C9 N1 Cd2 -163.4(2) . . . . ?
C7 C8 N1 C9 0.0(3) . . . . ?
C7 C8 N1 Cd2 162.5(2) . . . . ?
O2 Cd2 N1 C9 61.1(4) . . . . ?
O5 Cd2 N1 C9 -118.1(3) . . . . ?
O8 Cd2 N1 C9 -42.0(3) 2_667 . . . ?
O1 Cd2 N1 C9 42.9(3) . . . . ?
O6 Cd2 N1 C9 -169.5(3) . . . . ?
O6 Cd2 N1 C9 122.1(3) 2_656 . . . ?
O2 Cd2 N1 C8 -98.2(3) . . . . ?
O5 Cd2 N1 C8 82.6(2) . . . . ?
O8 Cd2 N1 C8 158.7(2) 2_667 . . . ?
O1 Cd2 N1 C8 -116.4(2) . . . . ?
O6 Cd2 N1 C8 31.2(2) . . . . ?
O6 Cd2 N1 C8 -37.2(2) 2_656 . . . ?
N1 C9 N2 C7 1.1(4) . . . . ?
C8 C7 N2 C9 -1.0(3) . . . . ?
C1 C7 N2 C9 176.8(3) . . . . ?
N4 C12 N3 C10 -1.3(4) . . . . ?
C11 C10 N3 C12 1.1(3) . . . . ?
C4 C10 N3 C12 -173.5(3) . . . . ?
N3 C12 N4 C11 0.9(4) . . . . ?
N3 C12 N4 Cd1 167.9(2) . . . 1_645 ?
C10 C11 N4 C12 -0.2(4) . . . . ?
C10 C11 N4 Cd1 -168.3(2) . . . 1_645 ?
O2 C13 O1 Cd2 5.9(3) . . . . ?
C14 C13 O1 Cd2 -173.8(3) . . . . ?
N1 Cd2 O1 C13 168.38(18) . . . . ?
O2 Cd2 O1 C13 -3.45(17) . . . . ?
O5 Cd2 O1 C13 -40.3(2) . . . . ?
O8 Cd2 O1 C13 -108.56(19) 2_667 . . . ?
O6 Cd2 O1 C13 52.7(2) . . . . ?
O6 Cd2 O1 C13 85.99(19) 2_656 . . . ?
O1 C13 O2 Cd2 -6.6(3) . . . . ?
C14 C13 O2 Cd2 173.1(2) . . . . ?
N1 Cd2 O2 C13 -18.3(3) . . . . ?
O5 Cd2 O2 C13 161.04(18) . . . . ?
O8 Cd2 O2 C13 81.86(19) 2_667 . . . ?
O1 Cd2 O2 C13 3.48(17) . . . . ?
O6 Cd2 O2 C13 -146.30(18) . . . . ?
O6 Cd2 O2 C13 -79.38(18) 2_656 . . . ?
O4 C18 O3 Cd1 -5.6(3) . . . 1_554 ?
C17 C18 O3 Cd1 174.3(3) . . . 1_554 ?
O3 C18 O4 Cd1 6.6(3) . . . 1_554 ?
C17 C18 O4 Cd1 -173.3(2) . . . 1_554 ?
O6 C22 O5 Cd1 -152.0(3) . . . . ?
C23 C22 O5 Cd1 31.4(5) . . . . ?
O6 C22 O5 Cd2 3.6(3) . . . . ?
C23 C22 O5 Cd2 -173.0(2) . . . . ?
O4 Cd1 O5 C22 59.7(4) 1_556 . . . ?
N4 Cd1 O5 C22 -91.6(4) 1_465 . . . ?
O7 Cd1 O5 C22 172.2(3) 2_667 . . . ?
O3 Cd1 O5 C22 6.4(4) 1_556 . . . ?
C18 Cd1 O5 C22 32.9(4) 1_556 . . . ?
O4 Cd1 O5 Cd2 -93.97(11) 1_556 . . . ?
N4 Cd1 O5 Cd2 114.75(11) 1_465 . . . ?
O7 Cd1 O5 Cd2 18.57(14) 2_667 . . . ?
O3 Cd1 O5 Cd2 -147.23(10) 1_556 . . . ?
C18 Cd1 O5 Cd2 -120.78(11) 1_556 . . . ?
N1 Cd2 O5 C22 -79.49(19) . . . . ?
O2 Cd2 O5 C22 100.79(18) . . . . ?
O8 Cd2 O5 C22 -159.1(2) 2_667 . . . ?
O1 Cd2 O5 C22 130.09(17) . . . . ?
O6 Cd2 O5 C22 -1.92(16) . . . . ?
O6 Cd2 O5 C22 16.3(2) 2_656 . . . ?
N1 Cd2 O5 Cd1 86.23(12) . . . . ?
O2 Cd2 O5 Cd1 -93.49(11) . . . . ?
O8 Cd2 O5 Cd1 6.64(9) 2_667 . . . ?
O1 Cd2 O5 Cd1 -64.20(17) . . . . ?
O6 Cd2 O5 Cd1 163.79(17) . . . . ?
O6 Cd2 O5 Cd1 -177.94(8) 2_656 . . . ?
O5 C22 O6 Cd2 -3.3(3) . . . . ?
C23 C22 O6 Cd2 173.2(2) . . . . ?
O5 C22 O6 Cd2 -142.9(4) . . . 2_656 ?
C23 C22 O6 Cd2 33.5(6) . . . 2_656 ?
N1 Cd2 O6 C22 115.22(19) . . . . ?
O2 Cd2 O6 C22 -81.79(19) . . . . ?
O5 Cd2 O6 C22 1.95(16) . . . . ?
O8 Cd2 O6 C22 30.7(2) 2_667 . . . ?
O1 Cd2 O6 C22 -125.42(18) . . . . ?
O6 Cd2 O6 C22 -161.0(3) 2_656 . . . ?
N1 Cd2 O6 Cd2 -83.74(11) . . . 2_656 ?
O2 Cd2 O6 Cd2 79.26(11) . . . 2_656 ?
O5 Cd2 O6 Cd2 162.99(17) . . . 2_656 ?
O8 Cd2 O6 Cd2 -168.29(9) 2_667 . . 2_656 ?
O1 Cd2 O6 Cd2 35.62(19) . . . 2_656 ?
O6 Cd2 O6 Cd2 0.0 2_656 . . 2_656 ?
O8 C19 O7 Cd1 -1.9(3) . . . 2_667 ?
C20 C19 O7 Cd1 178.9(2) . . . 2_667 ?
O8 C19 O7 Cd1 -143.6(3) . . . . ?
C20 C19 O7 Cd1 37.1(4) . . . . ?
O4 Cd1 O7 C19 -109.4(3) 1_556 . . . ?
N4 Cd1 O7 C19 43.1(3) 1_465 . . . ?
O7 Cd1 O7 C19 140.9(4) 2_667 . . . ?
O3 Cd1 O7 C19 -55.7(3) 1_556 . . . ?
C18 Cd1 O7 C19 -82.7(3) 1_556 . . . ?
O4 Cd1 O7 Cd1 109.72(10) 1_556 . . 2_667 ?
N4 Cd1 O7 Cd1 -97.75(11) 1_465 . . 2_667 ?
O7 Cd1 O7 Cd1 0.0 2_667 . . 2_667 ?
O3 Cd1 O7 Cd1 163.44(10) 1_556 . . 2_667 ?
C18 Cd1 O7 Cd1 136.43(11) 1_556 . . 2_667 ?
O7 C19 O8 Cd2 -86.8(5) . . . 2_667 ?
C20 C19 O8 Cd2 92.5(5) . . . 2_667 ?

_diffrn_measured_fraction_theta_max 0.882
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.149

#====END

data_4
_database_code_depnum_ccdc_archive 'CCDC 761522'
#TrackingRef 'sun-cec.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H18 N4 Ni O6'
_chemical_formula_sum            'C26 H18 N4 Ni O6'
_chemical_formula_weight         541.15

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   'P21/n '
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   10.563(2)
_cell_length_b                   22.256(5)
_cell_length_c                   10.562(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.040(8)
_cell_angle_gamma                90.00
_cell_volume                     2473.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3489
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8645
_exptl_absorpt_correction_T_max  0.9066
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12294
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4406
_reflns_number_gt                3495
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4406
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1588
_refine_ls_wR_factor_gt          0.1524
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Ni1 Ni 0.70024(4) 0.238935(19) 0.18566(4) 0.02688(19) Uani 1 1 d . . .
C1 C 0.9504(4) 0.00271(16) 0.3751(4) 0.0348(9) Uani 1 1 d . . .
H1 H 0.9174 0.0039 0.2906 0.042 Uiso 1 1 calc R . .
C2 C 0.9689(3) 0.05543(15) 0.4422(3) 0.0302(8) Uani 1 1 d . . .
C3 C 1.0195(4) 0.05184(17) 0.5679(4) 0.0380(10) Uani 1 1 d . . .
H3 H 1.0335 0.0870 0.6146 0.046 Uiso 1 1 calc R . .
C4 C 0.9333(4) 0.11305(16) 0.3838(4) 0.0346(9) Uani 1 1 d . . .
C5 C 0.8453(3) 0.12831(15) 0.2881(4) 0.0320(9) Uani 1 1 d . . .
H5 H 0.7931 0.1010 0.2418 0.038 Uiso 1 1 calc R . .
C6 C 0.9285(5) 0.21014(18) 0.3519(5) 0.0639(16) Uani 1 1 d . . .
H6 H 0.9471 0.2508 0.3611 0.077 Uiso 1 1 calc R . .
C7 C 0.8804(4) 0.48997(17) 0.0347(4) 0.0484(12) Uani 1 1 d . . .
H7 H 0.7986 0.4839 0.0584 0.058 Uiso 1 1 calc R . .
C8 C 0.9555(4) 0.44093(16) 0.0142(4) 0.0356(9) Uani 1 1 d . . .
C9 C 1.0764(4) 0.45167(17) -0.0208(5) 0.0486(12) Uani 1 1 d . . .
H9 H 1.1294 0.4195 -0.0352 0.058 Uiso 1 1 calc R . .
C10 C 0.9070(4) 0.37954(16) 0.0305(4) 0.0347(9) Uani 1 1 d . . .
C11 C 0.8261(3) 0.35717(16) 0.1114(4) 0.0333(9) Uani 1 1 d . . .
H11 H 0.7877 0.3797 0.1716 0.040 Uiso 1 1 calc R . .
C12 C 0.8774(4) 0.28354(17) -0.0007(4) 0.0466(11) Uani 1 1 d . . .
H12 H 0.8830 0.2453 -0.0354 0.056 Uiso 1 1 calc R . .
C13 C 0.5529(3) 0.15731(15) 0.1195(4) 0.0306(8) Uani 1 1 d . . .
C14 C 0.4626(3) 0.10880(16) 0.0748(4) 0.0318(9) Uani 1 1 d . . .
C15 C 0.4527(3) 0.08991(17) -0.0490(4) 0.0371(9) Uani 1 1 d . . .
H15 H 0.5006 0.1089 -0.1071 0.045 Uiso 1 1 calc R . .
C16 C 0.3723(4) 0.04280(18) -0.0897(4) 0.0390(9) Uani 1 1 d . . .
H16 H 0.3682 0.0295 -0.1734 0.047 Uiso 1 1 calc R . .
C17 C 0.2987(3) 0.01620(17) -0.0035(4) 0.0357(9) Uani 1 1 d . . .
C18 C 0.3032(4) 0.03568(18) 0.1203(4) 0.0421(10) Uani 1 1 d . . .
H18 H 0.2518 0.0184 0.1774 0.051 Uiso 1 1 calc R . .
C19 C 0.3862(4) 0.08162(18) 0.1577(4) 0.0392(10) Uani 1 1 d . . .
H19 H 0.3908 0.0947 0.2416 0.047 Uiso 1 1 calc R . .
C20 C 0.1479(4) -0.06466(17) 0.0176(4) 0.0407(10) Uani 1 1 d . . .
C21 C 0.0254(4) -0.07626(18) -0.0303(4) 0.0423(10) Uani 1 1 d . . .
H21 H -0.0084 -0.0571 -0.1039 0.051 Uiso 1 1 calc R . .
C22 C -0.0475(4) -0.11650(17) 0.0311(4) 0.0386(10) Uani 1 1 d . . .
H22 H -0.1296 -0.1254 -0.0028 0.046 Uiso 1 1 calc R . .
C23 C 0.0005(4) -0.14349(16) 0.1420(4) 0.0333(9) Uani 1 1 d . . .
C24 C 0.1259(4) -0.13193(18) 0.1881(4) 0.0415(10) Uani 1 1 d . . .
H24 H 0.1596 -0.1506 0.2623 0.050 Uiso 1 1 calc R . .
C25 C 0.2003(4) -0.09319(19) 0.1249(4) 0.0447(10) Uani 1 1 d . . .
H25 H 0.2846 -0.0865 0.1545 0.054 Uiso 1 1 calc R . .
C26 C -0.0786(4) -0.18493(16) 0.2108(4) 0.0340(9) Uani 1 1 d . . .
N1 N 0.8086(3) 0.29663(12) 0.0921(3) 0.0329(7) Uani 1 1 d . . .
N2 N 0.9391(3) 0.33166(14) -0.0400(3) 0.0466(9) Uani 1 1 d . . .
H2 H 0.9899 0.3322 -0.0993 0.056 Uiso 1 1 calc R . .
N3 N 0.8433(3) 0.18854(13) 0.2688(3) 0.0333(7) Uani 1 1 d . . .
N4 N 0.9864(4) 0.16679(15) 0.4230(4) 0.0681(14) Uani 1 1 d . . .
H4 H 1.0463 0.1718 0.4827 0.082 Uiso 1 1 calc R . .
O1 O 0.5639(2) 0.17258(11) 0.2351(2) 0.0354(6) Uani 1 1 d . . .
O2 O 0.6203(2) 0.18240(11) 0.0424(2) 0.0373(6) Uani 1 1 d . . .
O3 O -0.1817(2) -0.20526(11) 0.1574(3) 0.0375(6) Uani 1 1 d . . .
O4 O -0.0441(3) -0.20026(11) 0.3230(3) 0.0391(7) Uani 1 1 d . . .
O5 O 0.2166(3) -0.02746(13) -0.0558(3) 0.0525(8) Uani 1 1 d . . .
O1W O 0.7607(11) 0.2433(5) 0.5979(9) 0.296(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0287(3) 0.0176(3) 0.0347(3) 0.00215(19) 0.0048(2) -0.00004(17)
C1 0.041(2) 0.028(2) 0.034(2) 0.0002(17) -0.0046(17) 0.0013(16)
C2 0.029(2) 0.0230(19) 0.039(2) -0.0001(16) 0.0035(16) 0.0010(14)
C3 0.046(2) 0.024(2) 0.042(2) -0.0050(17) -0.0034(19) 0.0036(17)
C4 0.040(2) 0.023(2) 0.040(2) 0.0019(17) -0.0041(17) 0.0005(16)
C5 0.032(2) 0.023(2) 0.040(2) -0.0029(16) 0.0000(16) 0.0024(15)
C6 0.085(4) 0.019(2) 0.080(4) 0.010(2) -0.034(3) -0.007(2)
C7 0.040(2) 0.026(2) 0.083(3) 0.001(2) 0.028(2) -0.0043(18)
C8 0.041(2) 0.024(2) 0.044(2) -0.0003(17) 0.0120(18) -0.0081(16)
C9 0.041(2) 0.023(2) 0.085(3) -0.001(2) 0.025(2) 0.0011(17)
C10 0.038(2) 0.0199(19) 0.047(2) 0.0002(17) 0.0111(18) -0.0027(16)
C11 0.036(2) 0.0208(19) 0.045(2) -0.0022(17) 0.0115(17) -0.0028(15)
C12 0.063(3) 0.020(2) 0.061(3) -0.001(2) 0.033(2) -0.0064(19)
C13 0.028(2) 0.024(2) 0.040(2) 0.0030(17) 0.0063(16) 0.0040(15)
C14 0.028(2) 0.026(2) 0.041(2) 0.0015(17) 0.0051(16) -0.0024(15)
C15 0.032(2) 0.034(2) 0.047(2) 0.0054(19) 0.0117(18) -0.0074(17)
C16 0.039(2) 0.040(2) 0.038(2) -0.0024(19) 0.0050(18) -0.0081(18)
C17 0.032(2) 0.031(2) 0.044(2) 0.0011(18) 0.0035(17) -0.0123(16)
C18 0.036(2) 0.045(3) 0.046(2) -0.001(2) 0.0109(19) -0.0176(18)
C19 0.038(2) 0.039(2) 0.041(2) -0.0031(19) 0.0057(18) -0.0084(18)
C20 0.045(2) 0.033(2) 0.046(2) -0.0053(19) 0.0153(19) -0.0174(18)
C21 0.042(2) 0.040(2) 0.045(2) 0.003(2) 0.0025(19) -0.0120(18)
C22 0.034(2) 0.034(2) 0.048(2) -0.0019(19) 0.0031(18) -0.0095(17)
C23 0.038(2) 0.0193(19) 0.044(2) -0.0058(17) 0.0099(17) -0.0024(16)
C24 0.035(2) 0.040(2) 0.049(3) 0.001(2) 0.0020(19) -0.0046(18)
C25 0.030(2) 0.046(3) 0.058(3) 0.001(2) 0.0004(19) -0.0108(18)
C26 0.037(2) 0.0214(19) 0.044(2) -0.0042(17) 0.0114(18) 0.0024(16)
N1 0.0398(18) 0.0170(16) 0.0430(19) 0.0018(14) 0.0099(15) -0.0029(13)
N2 0.059(2) 0.0282(19) 0.058(2) -0.0012(17) 0.0332(18) -0.0033(16)
N3 0.0380(18) 0.0211(16) 0.0396(18) 0.0002(14) -0.0040(15) -0.0002(13)
N4 0.089(3) 0.0244(19) 0.081(3) 0.005(2) -0.050(3) -0.0048(19)
O1 0.0356(15) 0.0310(15) 0.0404(16) 0.0013(12) 0.0088(12) -0.0052(11)
O2 0.0387(15) 0.0323(15) 0.0415(16) 0.0008(12) 0.0073(12) -0.0130(12)
O3 0.0345(15) 0.0303(15) 0.0476(16) 0.0043(12) 0.0031(12) -0.0078(11)
O4 0.0468(17) 0.0294(15) 0.0414(17) 0.0012(12) 0.0061(13) -0.0084(12)
O5 0.056(2) 0.057(2) 0.0449(17) -0.0039(15) 0.0082(14) -0.0350(16)
O1W 0.277(12) 0.402(13) 0.210(10) 0.124(9) 0.024(9) 0.060(10)

_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 N3 2.020(3) . ?
Ni1 N1 2.033(3) . ?
Ni1 O2 2.088(3) . ?
Ni1 O3 2.094(3) 2 ?
Ni1 O4 2.129(3) 2 ?
Ni1 O1 2.158(2) . ?
Ni1 C26 2.442(4) 2 ?
C1 C2 1.376(5) . ?
C1 C3 1.380(5) 3_756 ?
C1 H1 0.9300 . ?
C2 C3 1.389(5) . ?
C2 C4 1.458(5) . ?
C3 C1 1.380(5) 3_756 ?
C3 H3 0.9300 . ?
C4 C5 1.354(5) . ?
C4 N4 1.370(5) . ?
C5 N3 1.356(4) . ?
C5 H5 0.9300 . ?
C6 N3 1.293(5) . ?
C6 N4 1.338(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.378(5) . ?
C7 C9 1.389(5) 3_765 ?
C7 H7 0.9300 . ?
C8 C9 1.381(5) . ?
C8 C10 1.474(5) . ?
C9 C7 1.389(5) 3_765 ?
C9 H9 0.9300 . ?
C10 C11 1.355(5) . ?
C10 N2 1.360(5) . ?
C11 N1 1.373(4) . ?
C11 H11 0.9300 . ?
C12 N1 1.303(5) . ?
C12 N2 1.338(5) . ?
C12 H12 0.9300 . ?
C13 O2 1.259(4) . ?
C13 O1 1.263(4) . ?
C13 C14 1.490(5) . ?
C14 C15 1.369(5) . ?
C14 C19 1.381(5) . ?
C15 C16 1.393(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.381(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(5) . ?
C17 O5 1.384(4) . ?
C18 C19 1.381(5) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.372(6) . ?
C20 C25 1.372(6) . ?
C20 O5 1.383(5) . ?
C21 C22 1.379(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.394(5) . ?
C23 C26 1.477(5) . ?
C24 C25 1.378(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O4 1.255(5) . ?
C26 O3 1.265(4) . ?
C26 Ni1 2.442(4) 2_545 ?
N2 H2 0.8600 . ?
N4 H4 0.8600 . ?
O3 Ni1 2.094(3) 2_545 ?
O4 Ni1 2.129(3) 2_545 ?

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
N3 Ni1 N1 97.48(13) . . ?
N3 Ni1 O2 102.69(11) . . ?
N1 Ni1 O2 103.73(11) . . ?
N3 Ni1 O3 95.95(11) . 2 ?
N1 Ni1 O3 96.08(11) . 2 ?
O2 Ni1 O3 150.57(11) . 2 ?
N3 Ni1 O4 156.74(12) . 2 ?
N1 Ni1 O4 92.58(11) . 2 ?
O2 Ni1 O4 95.14(10) . 2 ?
O3 Ni1 O4 62.03(10) 2 2 ?
N3 Ni1 O1 90.25(11) . . ?
N1 Ni1 O1 164.94(11) . . ?
O2 Ni1 O1 61.79(10) . . ?
O3 Ni1 O1 95.94(10) 2 . ?
O4 Ni1 O1 85.09(10) 2 . ?
N3 Ni1 C26 126.42(13) . 2 ?
N1 Ni1 C26 96.91(12) . 2 ?
O2 Ni1 C26 123.18(12) . 2 ?
O3 Ni1 C26 31.21(11) 2 2 ?
O4 Ni1 C26 30.92(11) 2 2 ?
O1 Ni1 C26 88.74(11) . 2 ?
C2 C1 C3 120.6(3) . 3_756 ?
C2 C1 H1 119.7 . . ?
C3 C1 H1 119.7 3_756 . ?
C1 C2 C3 117.9(3) . . ?
C1 C2 C4 120.8(3) . . ?
C3 C2 C4 121.2(3) . . ?
C1 C3 C2 121.5(3) 3_756 . ?
C1 C3 H3 119.3 3_756 . ?
C2 C3 H3 119.3 . . ?
C5 C4 N4 104.0(3) . . ?
C5 C4 C2 132.1(3) . . ?
N4 C4 C2 123.8(3) . . ?
C4 C5 N3 111.2(3) . . ?
C4 C5 H5 124.4 . . ?
N3 C5 H5 124.4 . . ?
N3 C6 N4 111.7(4) . . ?
N3 C6 H6 124.1 . . ?
N4 C6 H6 124.1 . . ?
C8 C7 C9 121.7(4) . 3_765 ?
C8 C7 H7 119.2 . . ?
C9 C7 H7 119.2 3_765 . ?
C7 C8 C9 117.6(4) . . ?
C7 C8 C10 120.3(4) . . ?
C9 C8 C10 122.0(4) . . ?
C8 C9 C7 120.7(4) . 3_765 ?
C8 C9 H9 119.6 . . ?
C7 C9 H9 119.6 3_765 . ?
C11 C10 N2 105.0(3) . . ?
C11 C10 C8 131.2(4) . . ?
N2 C10 C8 123.8(4) . . ?
C10 C11 N1 110.5(3) . . ?
C10 C11 H11 124.7 . . ?
N1 C11 H11 124.7 . . ?
N1 C12 N2 111.9(3) . . ?
N1 C12 H12 124.0 . . ?
N2 C12 H12 124.0 . . ?
O2 C13 O1 119.8(3) . . ?
O2 C13 C14 120.0(3) . . ?
O1 C13 C14 120.3(3) . . ?
C15 C14 C19 118.1(3) . . ?
C15 C14 C13 121.2(3) . . ?
C19 C14 C13 120.6(3) . . ?
C14 C15 C16 121.3(4) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 118.9(4) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C18 C17 C16 121.1(3) . . ?
C18 C17 O5 124.7(3) . . ?
C16 C17 O5 114.0(3) . . ?
C17 C18 C19 118.2(4) . . ?
C17 C18 H18 120.9 . . ?
C19 C18 H18 120.9 . . ?
C14 C19 C18 122.3(4) . . ?
C14 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C21 C20 C25 121.1(4) . . ?
C21 C20 O5 115.5(4) . . ?
C25 C20 O5 123.2(4) . . ?
C20 C21 C22 119.8(4) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 120.4(4) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 119.0(4) . . ?
C22 C23 C26 120.7(4) . . ?
C24 C23 C26 120.3(4) . . ?
C25 C24 C23 120.7(4) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C20 C25 C24 118.9(4) . . ?
C20 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
O4 C26 O3 119.4(4) . . ?
O4 C26 C23 120.3(3) . . ?
O3 C26 C23 120.4(4) . . ?
O4 C26 Ni1 60.64(19) . 2_545 ?
O3 C26 Ni1 59.03(19) . 2_545 ?
C23 C26 Ni1 174.7(3) . 2_545 ?
C12 N1 C11 104.8(3) . . ?
C12 N1 Ni1 126.8(3) . . ?
C11 N1 Ni1 128.4(3) . . ?
C12 N2 C10 107.8(3) . . ?
C12 N2 H2 126.1 . . ?
C10 N2 H2 126.1 . . ?
C6 N3 C5 105.3(3) . . ?
C6 N3 Ni1 122.5(3) . . ?
C5 N3 Ni1 128.0(2) . . ?
C6 N4 C4 107.7(3) . . ?
C6 N4 H4 126.1 . . ?
C4 N4 H4 126.1 . . ?
C13 O1 Ni1 87.6(2) . . ?
C13 O2 Ni1 90.8(2) . . ?
C26 O3 Ni1 89.8(2) . 2_545 ?
C26 O4 Ni1 88.4(2) . 2_545 ?
C20 O5 C17 122.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 C2 C3 0.6(6) 3_756 . . . ?
C3 C1 C2 C4 -177.9(4) 3_756 . . . ?
C1 C2 C3 C1 -0.6(6) . . . 3_756 ?
C4 C2 C3 C1 177.8(4) . . . 3_756 ?
C1 C2 C4 C5 26.3(7) . . . . ?
C3 C2 C4 C5 -152.1(4) . . . . ?
C1 C2 C4 N4 -155.9(4) . . . . ?
C3 C2 C4 N4 25.7(6) . . . . ?
N4 C4 C5 N3 -0.2(5) . . . . ?
C2 C4 C5 N3 178.0(4) . . . . ?
C9 C7 C8 C9 0.1(8) 3_765 . . . ?
C9 C7 C8 C10 179.6(4) 3_765 . . . ?
C7 C8 C9 C7 -0.1(8) . . . 3_765 ?
C10 C8 C9 C7 -179.6(4) . . . 3_765 ?
C7 C8 C10 C11 -33.0(7) . . . . ?
C9 C8 C10 C11 146.5(5) . . . . ?
C7 C8 C10 N2 146.8(4) . . . . ?
C9 C8 C10 N2 -33.6(6) . . . . ?
N2 C10 C11 N1 0.3(4) . . . . ?
C8 C10 C11 N1 -179.8(4) . . . . ?
O2 C13 C14 C15 1.1(6) . . . . ?
O1 C13 C14 C15 -177.4(3) . . . . ?
O2 C13 C14 C19 -178.8(3) . . . . ?
O1 C13 C14 C19 2.7(5) . . . . ?
C19 C14 C15 C16 -2.8(6) . . . . ?
C13 C14 C15 C16 177.2(3) . . . . ?
C14 C15 C16 C17 2.0(6) . . . . ?
C15 C16 C17 C18 0.4(6) . . . . ?
C15 C16 C17 O5 176.1(3) . . . . ?
C16 C17 C18 C19 -1.8(6) . . . . ?
O5 C17 C18 C19 -177.1(4) . . . . ?
C15 C14 C19 C18 1.4(6) . . . . ?
C13 C14 C19 C18 -178.7(4) . . . . ?
C17 C18 C19 C14 0.9(6) . . . . ?
C25 C20 C21 C22 1.0(7) . . . . ?
O5 C20 C21 C22 175.0(4) . . . . ?
C20 C21 C22 C23 2.1(6) . . . . ?
C21 C22 C23 C24 -3.2(6) . . . . ?
C21 C22 C23 C26 177.8(4) . . . . ?
C22 C23 C24 C25 1.2(6) . . . . ?
C26 C23 C24 C25 -179.8(4) . . . . ?
C21 C20 C25 C24 -3.0(7) . . . . ?
O5 C20 C25 C24 -176.6(4) . . . . ?
C23 C24 C25 C20 1.9(6) . . . . ?
C22 C23 C26 O4 -166.2(3) . . . . ?
C24 C23 C26 O4 14.8(6) . . . . ?
C22 C23 C26 O3 13.7(6) . . . . ?
C24 C23 C26 O3 -165.3(4) . . . . ?
N2 C12 N1 C11 1.1(5) . . . . ?
N2 C12 N1 Ni1 -179.0(3) . . . . ?
C10 C11 N1 C12 -0.8(5) . . . . ?
C10 C11 N1 Ni1 179.2(3) . . . . ?
N3 Ni1 N1 C12 66.2(4) . . . . ?
O2 Ni1 N1 C12 -38.9(4) . . . . ?
O3 Ni1 N1 C12 163.0(4) 2 . . . ?
O4 Ni1 N1 C12 -134.8(4) 2 . . . ?
O1 Ni1 N1 C12 -54.2(6) . . . . ?
C26 Ni1 N1 C12 -165.6(4) 2 . . . ?
N3 Ni1 N1 C11 -113.8(3) . . . . ?
O2 Ni1 N1 C11 141.1(3) . . . . ?
O3 Ni1 N1 C11 -17.0(3) 2 . . . ?
O4 Ni1 N1 C11 45.1(3) 2 . . . ?
O1 Ni1 N1 C11 125.8(4) . . . . ?
C26 Ni1 N1 C11 14.4(3) 2 . . . ?
N1 C12 N2 C10 -0.9(5) . . . . ?
C11 C10 N2 C12 0.3(5) . . . . ?
C8 C10 N2 C12 -179.5(4) . . . . ?
N4 C6 N3 C5 0.7(6) . . . . ?
N4 C6 N3 Ni1 159.5(4) . . . . ?
C4 C5 N3 C6 -0.3(5) . . . . ?
C4 C5 N3 Ni1 -157.6(3) . . . . ?
N1 Ni1 N3 C6 64.3(4) . . . . ?
O2 Ni1 N3 C6 170.2(4) . . . . ?
O3 Ni1 N3 C6 -32.7(4) 2 . . . ?
O4 Ni1 N3 C6 -50.6(5) 2 . . . ?
O1 Ni1 N3 C6 -128.7(4) . . . . ?
C26 Ni1 N3 C6 -40.1(4) 2 . . . ?
N1 Ni1 N3 C5 -142.0(3) . . . . ?
O2 Ni1 N3 C5 -36.0(4) . . . . ?
O3 Ni1 N3 C5 121.1(3) 2 . . . ?
O4 Ni1 N3 C5 103.1(4) 2 . . . ?
O1 Ni1 N3 C5 25.1(3) . . . . ?
C26 Ni1 N3 C5 113.7(3) 2 . . . ?
N3 C6 N4 C4 -0.8(7) . . . . ?
C5 C4 N4 C6 0.6(6) . . . . ?
C2 C4 N4 C6 -177.8(4) . . . . ?
O2 C13 O1 Ni1 2.6(3) . . . . ?
C14 C13 O1 Ni1 -178.8(3) . . . . ?
N3 Ni1 O1 C13 -105.9(2) . . . . ?
N1 Ni1 O1 C13 15.3(5) . . . . ?
O2 Ni1 O1 C13 -1.6(2) . . . . ?
O3 Ni1 O1 C13 158.1(2) 2 . . . ?
O4 Ni1 O1 C13 97.0(2) 2 . . . ?
C26 Ni1 O1 C13 127.7(2) 2 . . . ?
O1 C13 O2 Ni1 -2.7(3) . . . . ?
C14 C13 O2 Ni1 178.7(3) . . . . ?
N3 Ni1 O2 C13 84.9(2) . . . . ?
N1 Ni1 O2 C13 -174.0(2) . . . . ?
O3 Ni1 O2 C13 -43.1(3) 2 . . . ?
O4 Ni1 O2 C13 -80.0(2) 2 . . . ?
O1 Ni1 O2 C13 1.6(2) . . . . ?
C26 Ni1 O2 C13 -66.0(2) 2 . . . ?
O4 C26 O3 Ni1 -6.2(4) . . . 2_545 ?
C23 C26 O3 Ni1 173.9(3) . . . 2_545 ?
O3 C26 O4 Ni1 6.1(3) . . . 2_545 ?
C23 C26 O4 Ni1 -174.0(3) . . . 2_545 ?
C21 C20 O5 C17 140.2(4) . . . . ?
C25 C20 O5 C17 -45.9(6) . . . . ?
C18 C17 O5 C20 -13.4(6) . . . . ?
C16 C17 O5 C20 171.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.097

#====END

data_5
_database_code_depnum_ccdc_archive 'CCDC 761523'
#TrackingRef 'sun-cec.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Co N4 O5'
_chemical_formula_sum            'C22 H20 Co N4 O5'
_chemical_formula_weight         479.35

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'
Co Co 0.3494 0.9721 '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'
H H 0.0000 0.0000 '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                   10.654(5)
_cell_length_b                   10.711(5)
_cell_length_c                   11.681(5)
_cell_angle_alpha                110.143(7)
_cell_angle_beta                 102.356(7)
_cell_angle_gamma                109.812(7)
_cell_volume                     1091.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2128
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      25.93

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             494
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8790
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5664
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3966
_reflns_number_gt                3295
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3966
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0775
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.72817(4) 0.25781(3) 0.83296(3) 0.02292(11) Uani 1 1 d . . .
C1 C 0.5527(3) -0.4637(3) 0.6315(3) 0.0352(7) Uani 1 1 d . . .
H1 H 0.5877 -0.4401 0.7201 0.042 Uiso 1 1 calc R . .
C2 C 0.5668(3) -0.3502(3) 0.5949(3) 0.0296(6) Uani 1 1 d . . .
C3 C 0.5125(3) -0.3902(3) 0.4619(3) 0.0350(7) Uani 1 1 d . . .
H3 H 0.5204 -0.3163 0.4353 0.042 Uiso 1 1 calc R . .
C4 C 0.6376(3) -0.1931(3) 0.6907(2) 0.0284(6) Uani 1 1 d . . .
C5 C 0.6246(3) -0.0754(2) 0.6811(2) 0.0301(6) Uani 1 1 d . . .
H5 H 0.5627 -0.0809 0.6081 0.036 Uiso 1 1 calc R . .
C6 C 0.7839(3) 0.0132(3) 0.8724(3) 0.0372(7) Uani 1 1 d . . .
H6 H 0.8530 0.0782 0.9566 0.045 Uiso 1 1 calc R . .
C7 C 0.0329(3) 0.1057(3) 0.6247(2) 0.0275(6) Uani 1 1 d . . .
H7 H 0.0542 0.1765 0.7086 0.033 Uiso 1 1 calc R . .
C8 C 0.1418(3) 0.0789(2) 0.5915(2) 0.0239(6) Uani 1 1 d . . .
C9 C 0.1067(3) -0.0285(3) 0.4655(2) 0.0277(6) Uani 1 1 d . . .
H9 H 0.1783 -0.0485 0.4419 0.033 Uiso 1 1 calc R . .
C10 C 0.2902(3) 0.1562(3) 0.6844(2) 0.0250(6) Uani 1 1 d . . .
C11 C 0.4050(3) 0.1291(3) 0.6816(2) 0.0282(6) Uani 1 1 d . . .
H11 H 0.4029 0.0493 0.6143 0.034 Uiso 1 1 calc R . .
C12 C 0.4814(3) 0.3259(3) 0.8598(3) 0.0380(7) Uani 1 1 d . . .
H12 H 0.5405 0.4096 0.9401 0.046 Uiso 1 1 calc R . .
C13 C 0.8824(3) 0.6236(3) 0.5953(3) 0.0432(8) Uani 1 1 d . . .
H13 H 0.7892 0.5787 0.5341 0.052 Uiso 1 1 calc R . .
C14 C 0.9601(4) 0.7759(4) 0.6528(3) 0.0547(9) Uani 1 1 d . . .
H14 H 0.9190 0.8331 0.6318 0.066 Uiso 1 1 calc R . .
C15 C 1.0989(4) 0.8429(3) 0.7417(3) 0.0540(10) Uani 1 1 d . . .
H15 H 1.1524 0.9459 0.7818 0.065 Uiso 1 1 calc R . .
C16 C 1.1577(4) 0.7567(3) 0.7706(3) 0.0436(8) Uani 1 1 d . . .
H16 H 1.2524 0.8026 0.8293 0.052 Uiso 1 1 calc R . .
C17 C 1.0803(3) 0.6025(3) 0.7149(2) 0.0320(7) Uani 1 1 d . . .
C18 C 0.9387(3) 0.5353(3) 0.6257(2) 0.0315(7) Uani 1 1 d . . .
C19 C 0.8442(3) 0.3700(3) 0.5617(3) 0.0360(7) Uani 1 1 d . . .
H19A H 0.8994 0.3195 0.5307 0.043 Uiso 1 1 calc R . .
H19B H 0.7646 0.3444 0.4853 0.043 Uiso 1 1 calc R . .
C20 C 0.7835(3) 0.3106(3) 0.6480(3) 0.0303(6) Uani 1 1 d . . .
C21 C 1.1511(3) 0.5151(3) 0.7523(2) 0.0345(7) Uani 1 1 d . . .
H21A H 1.2413 0.5420 0.7387 0.041 Uiso 1 1 calc R . .
H21B H 1.0901 0.4102 0.6930 0.041 Uiso 1 1 calc R . .
C22 C 1.1817(3) 0.5359(3) 0.8919(2) 0.0269(6) Uani 1 1 d . . .
N1 N 0.7403(3) -0.1344(2) 0.8142(2) 0.0372(6) Uani 1 1 d . . .
H1A H 0.7708 -0.1835 0.8478 0.045 Uiso 1 1 calc R . .
N2 N 0.7166(2) 0.0540(2) 0.7952(2) 0.0294(5) Uani 1 1 d . . .
N3 N 0.3418(2) 0.2834(2) 0.8002(2) 0.0355(6) Uani 1 1 d . . .
H3A H 0.2929 0.3276 0.8289 0.043 Uiso 1 1 calc R . .
N4 N 0.5251(2) 0.2356(2) 0.7917(2) 0.0293(5) Uani 1 1 d . . .
O1 O 1.18240(19) 0.64905(18) 0.97402(16) 0.0325(4) Uani 1 1 d . . .
O2 O 1.2120(2) 0.44362(18) 0.91880(16) 0.0340(5) Uani 1 1 d . . .
O3 O 0.8468(2) 0.38850(19) 0.77217(17) 0.0379(5) Uani 1 1 d . . .
O4 O 0.6766(2) 0.18754(18) 0.59873(18) 0.0363(5) Uani 1 1 d . . .
O1W O 0.1378(3) 0.2986(3) 0.0821(3) 0.0555(7) Uani 1 1 d . . .
H1W H 0.154(4) 0.332(4) 0.033(4) 0.096(17) Uiso 1 1 d . . .
H2W H 0.116(4) 0.354(4) 0.129(4) 0.087(16) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0241(2) 0.01900(18) 0.0220(2) 0.00768(15) 0.00590(15) 0.00905(15)
C1 0.0429(19) 0.0277(15) 0.0280(15) 0.0119(13) 0.0049(14) 0.0142(14)
C2 0.0315(16) 0.0203(13) 0.0308(16) 0.0087(12) 0.0070(13) 0.0108(12)
C3 0.0448(19) 0.0218(14) 0.0376(17) 0.0160(13) 0.0108(14) 0.0142(14)
C4 0.0307(16) 0.0235(13) 0.0277(15) 0.0112(12) 0.0064(13) 0.0116(12)
C5 0.0333(16) 0.0235(14) 0.0244(14) 0.0068(12) 0.0022(13) 0.0123(13)
C6 0.0450(19) 0.0259(15) 0.0269(15) 0.0063(12) 0.0020(14) 0.0138(14)
C7 0.0309(16) 0.0220(13) 0.0251(14) 0.0080(11) 0.0071(13) 0.0118(12)
C8 0.0224(14) 0.0204(13) 0.0277(14) 0.0121(11) 0.0052(12) 0.0095(11)
C9 0.0260(15) 0.0264(14) 0.0349(16) 0.0142(12) 0.0124(13) 0.0154(12)
C10 0.0246(15) 0.0209(13) 0.0259(14) 0.0092(11) 0.0065(12) 0.0096(12)
C11 0.0283(16) 0.0241(13) 0.0257(14) 0.0070(12) 0.0072(12) 0.0109(12)
C12 0.0250(16) 0.0342(16) 0.0327(16) 0.0001(13) -0.0005(13) 0.0116(14)
C13 0.048(2) 0.058(2) 0.0455(19) 0.0361(17) 0.0254(16) 0.0299(17)
C14 0.081(3) 0.059(2) 0.067(2) 0.048(2) 0.043(2) 0.048(2)
C15 0.091(3) 0.0304(17) 0.051(2) 0.0267(16) 0.035(2) 0.0252(19)
C16 0.055(2) 0.0367(17) 0.0308(16) 0.0163(14) 0.0140(15) 0.0125(16)
C17 0.0466(19) 0.0325(15) 0.0238(15) 0.0167(13) 0.0178(14) 0.0186(14)
C18 0.0419(18) 0.0378(16) 0.0263(15) 0.0208(13) 0.0186(14) 0.0204(14)
C19 0.0388(18) 0.0409(16) 0.0261(15) 0.0165(13) 0.0102(13) 0.0156(15)
C20 0.0328(17) 0.0322(15) 0.0325(16) 0.0165(13) 0.0125(14) 0.0198(14)
C21 0.0419(18) 0.0334(15) 0.0254(15) 0.0095(12) 0.0113(14) 0.0186(14)
C22 0.0223(15) 0.0262(14) 0.0239(14) 0.0077(12) 0.0045(12) 0.0082(12)
N1 0.0509(16) 0.0238(12) 0.0309(13) 0.0115(10) 0.0035(12) 0.0186(12)
N2 0.0339(14) 0.0209(11) 0.0274(12) 0.0073(10) 0.0069(11) 0.0121(11)
N3 0.0265(14) 0.0364(13) 0.0339(13) 0.0034(11) 0.0059(11) 0.0198(11)
N4 0.0254(13) 0.0279(12) 0.0276(12) 0.0078(10) 0.0041(11) 0.0129(11)
O1 0.0418(12) 0.0288(10) 0.0190(9) 0.0051(8) 0.0054(9) 0.0169(9)
O2 0.0421(12) 0.0353(10) 0.0293(10) 0.0143(9) 0.0099(9) 0.0251(10)
O3 0.0399(12) 0.0360(10) 0.0244(10) 0.0138(9) 0.0092(9) 0.0042(9)
O4 0.0377(12) 0.0262(10) 0.0383(11) 0.0108(9) 0.0146(10) 0.0109(9)
O1W 0.082(2) 0.0509(15) 0.0488(16) 0.0287(13) 0.0246(14) 0.0401(15)

_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 O1 1.9682(19) 2_767 ?
Co1 O3 1.9828(18) . ?
Co1 N4 2.024(2) . ?
Co1 N2 2.026(2) . ?
C1 C3 1.373(3) 2_646 ?
C1 C2 1.394(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.386(4) . ?
C2 C4 1.461(3) . ?
C3 C1 1.373(3) 2_646 ?
C3 H3 0.9300 . ?
C4 C5 1.353(3) . ?
C4 N1 1.380(3) . ?
C5 N2 1.381(3) . ?
C5 H5 0.9300 . ?
C6 N2 1.313(3) . ?
C6 N1 1.343(3) . ?
C6 H6 0.9300 . ?
C7 C9 1.379(3) 2_556 ?
C7 C8 1.386(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(3) . ?
C8 C10 1.457(3) . ?
C9 C7 1.379(3) 2_556 ?
C9 H9 0.9300 . ?
C10 C11 1.354(4) . ?
C10 N3 1.376(3) . ?
C11 N4 1.374(3) . ?
C11 H11 0.9300 . ?
C12 N4 1.311(3) . ?
C12 N3 1.336(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.374(4) . ?
C13 C18 1.380(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.370(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.392(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.398(4) . ?
C17 C21 1.502(4) . ?
C18 C19 1.505(3) . ?
C19 C20 1.510(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 O4 1.243(3) . ?
C20 O3 1.273(3) . ?
C21 C22 1.512(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O2 1.252(3) . ?
C22 O1 1.257(3) . ?
N1 H1A 0.8600 . ?
N3 H3A 0.8600 . ?
O1 Co1 1.9682(19) 2_767 ?
O1W H1W 0.80(4) . ?
O1W H2W 0.80(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O3 107.72(8) 2_767 . ?
O1 Co1 N4 105.80(8) 2_767 . ?
O3 Co1 N4 113.84(9) . . ?
O1 Co1 N2 97.87(8) 2_767 . ?
O3 Co1 N2 121.94(9) . . ?
N4 Co1 N2 107.43(9) . . ?
C3 C1 C2 120.7(2) 2_646 . ?
C3 C1 H1 119.6 2_646 . ?
C2 C1 H1 119.6 . . ?
C3 C2 C1 117.8(2) . . ?
C3 C2 C4 119.7(2) . . ?
C1 C2 C4 122.6(2) . . ?
C1 C3 C2 121.5(2) 2_646 . ?
C1 C3 H3 119.2 2_646 . ?
C2 C3 H3 119.2 . . ?
C5 C4 N1 105.3(2) . . ?
C5 C4 C2 130.3(2) . . ?
N1 C4 C2 124.4(2) . . ?
C4 C5 N2 110.2(2) . . ?
C4 C5 H5 124.9 . . ?
N2 C5 H5 124.9 . . ?
N2 C6 N1 111.4(2) . . ?
N2 C6 H6 124.3 . . ?
N1 C6 H6 124.3 . . ?
C9 C7 C8 120.7(2) 2_556 . ?
C9 C7 H7 119.7 2_556 . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 118.5(2) . . ?
C7 C8 C10 122.5(2) . . ?
C9 C8 C10 119.1(2) . . ?
C7 C9 C8 120.8(2) 2_556 . ?
C7 C9 H9 119.6 2_556 . ?
C8 C9 H9 119.6 . . ?
C11 C10 N3 104.9(2) . . ?
C11 C10 C8 131.8(2) . . ?
N3 C10 C8 123.3(2) . . ?
C10 C11 N4 110.7(2) . . ?
C10 C11 H11 124.6 . . ?
N4 C11 H11 124.6 . . ?
N4 C12 N3 112.0(2) . . ?
N4 C12 H12 124.0 . . ?
N3 C12 H12 124.0 . . ?
C14 C13 C18 122.0(3) . . ?
C14 C13 H13 119.0 . . ?
C18 C13 H13 119.0 . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 119.4(3) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 122.1(3) . . ?
C15 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C16 C17 C18 118.1(3) . . ?
C16 C17 C21 119.2(3) . . ?
C18 C17 C21 122.7(2) . . ?
C13 C18 C17 119.0(3) . . ?
C13 C18 C19 118.4(3) . . ?
C17 C18 C19 122.6(3) . . ?
C18 C19 C20 115.7(2) . . ?
C18 C19 H19A 108.4 . . ?
C20 C19 H19A 108.4 . . ?
C18 C19 H19B 108.4 . . ?
C20 C19 H19B 108.4 . . ?
H19A C19 H19B 107.4 . . ?
O4 C20 O3 121.2(2) . . ?
O4 C20 C19 120.7(2) . . ?
O3 C20 C19 118.1(2) . . ?
C17 C21 C22 116.0(2) . . ?
C17 C21 H21A 108.3 . . ?
C22 C21 H21A 108.3 . . ?
C17 C21 H21B 108.3 . . ?
C22 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
O2 C22 O1 124.7(2) . . ?
O2 C22 C21 117.6(2) . . ?
O1 C22 C21 117.6(2) . . ?
C6 N1 C4 107.7(2) . . ?
C6 N1 H1A 126.2 . . ?
C4 N1 H1A 126.2 . . ?
C6 N2 C5 105.5(2) . . ?
C6 N2 Co1 129.27(17) . . ?
C5 N2 Co1 125.14(18) . . ?
C12 N3 C10 107.6(2) . . ?
C12 N3 H3A 126.2 . . ?
C10 N3 H3A 126.2 . . ?
C12 N4 C11 104.8(2) . . ?
C12 N4 Co1 127.42(18) . . ?
C11 N4 Co1 127.60(17) . . ?
C22 O1 Co1 127.81(17) . 2_767 ?
C20 O3 Co1 100.75(16) . . ?
H1W O1W H2W 104(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 C2 C3 0.3(5) 2_646 . . . ?
C3 C1 C2 C4 -178.9(3) 2_646 . . . ?
C1 C2 C3 C1 -0.3(5) . . . 2_646 ?
C4 C2 C3 C1 178.9(3) . . . 2_646 ?
C3 C2 C4 C5 23.5(5) . . . . ?
C1 C2 C4 C5 -157.4(3) . . . . ?
C3 C2 C4 N1 -154.1(3) . . . . ?
C1 C2 C4 N1 25.0(4) . . . . ?
N1 C4 C5 N2 0.0(3) . . . . ?
C2 C4 C5 N2 -177.9(3) . . . . ?
C9 C7 C8 C9 -0.5(4) 2_556 . . . ?
C9 C7 C8 C10 -179.0(2) 2_556 . . . ?
C7 C8 C9 C7 0.5(4) . . . 2_556 ?
C10 C8 C9 C7 179.0(2) . . . 2_556 ?
C7 C8 C10 C11 166.0(3) . . . . ?
C9 C8 C10 C11 -12.4(4) . . . . ?
C7 C8 C10 N3 -15.3(4) . . . . ?
C9 C8 C10 N3 166.2(2) . . . . ?
N3 C10 C11 N4 -0.1(3) . . . . ?
C8 C10 C11 N4 178.8(2) . . . . ?
C18 C13 C14 C15 1.2(4) . . . . ?
C13 C14 C15 C16 0.4(5) . . . . ?
C14 C15 C16 C17 -1.4(5) . . . . ?
C15 C16 C17 C18 0.7(4) . . . . ?
C15 C16 C17 C21 -179.3(3) . . . . ?
C14 C13 C18 C17 -1.8(4) . . . . ?
C14 C13 C18 C19 177.8(2) . . . . ?
C16 C17 C18 C13 0.9(4) . . . . ?
C21 C17 C18 C13 -179.1(2) . . . . ?
C16 C17 C18 C19 -178.7(2) . . . . ?
C21 C17 C18 C19 1.3(4) . . . . ?
C13 C18 C19 C20 -103.7(3) . . . . ?
C17 C18 C19 C20 75.9(3) . . . . ?
C18 C19 C20 O4 160.5(3) . . . . ?
C18 C19 C20 O3 -20.9(4) . . . . ?
C16 C17 C21 C22 69.0(3) . . . . ?
C18 C17 C21 C22 -111.0(3) . . . . ?
C17 C21 C22 O2 165.3(2) . . . . ?
C17 C21 C22 O1 -18.4(4) . . . . ?
N2 C6 N1 C4 0.0(3) . . . . ?
C5 C4 N1 C6 -0.1(3) . . . . ?
C2 C4 N1 C6 178.1(2) . . . . ?
N1 C6 N2 C5 0.0(3) . . . . ?
N1 C6 N2 Co1 175.85(17) . . . . ?
C4 C5 N2 C6 0.0(3) . . . . ?
C4 C5 N2 Co1 -176.11(17) . . . . ?
O1 Co1 N2 C6 -16.4(3) 2_767 . . . ?
O3 Co1 N2 C6 100.2(3) . . . . ?
N4 Co1 N2 C6 -125.8(2) . . . . ?
O1 Co1 N2 C5 158.7(2) 2_767 . . . ?
O3 Co1 N2 C5 -84.7(2) . . . . ?
N4 Co1 N2 C5 49.3(2) . . . . ?
N4 C12 N3 C10 -0.1(3) . . . . ?
C11 C10 N3 C12 0.1(3) . . . . ?
C8 C10 N3 C12 -178.9(2) . . . . ?
N3 C12 N4 C11 0.1(3) . . . . ?
N3 C12 N4 Co1 175.72(17) . . . . ?
C10 C11 N4 C12 0.0(3) . . . . ?
C10 C11 N4 Co1 -175.64(17) . . . . ?
O1 Co1 N4 C12 34.5(2) 2_767 . . . ?
O3 Co1 N4 C12 -83.6(2) . . . . ?
N2 Co1 N4 C12 138.3(2) . . . . ?
O1 Co1 N4 C11 -150.8(2) 2_767 . . . ?
O3 Co1 N4 C11 91.1(2) . . . . ?
N2 Co1 N4 C11 -47.0(2) . . . . ?
O2 C22 O1 Co1 15.9(4) . . . 2_767 ?
C21 C22 O1 Co1 -160.03(18) . . . 2_767 ?
O4 C20 O3 Co1 0.1(3) . . . . ?
C19 C20 O3 Co1 -178.4(2) . . . . ?
O1 Co1 O3 C20 175.52(16) 2_767 . . . ?
N4 Co1 O3 C20 -67.51(18) . . . . ?
N2 Co1 O3 C20 63.89(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.060

#====END

data_6
_database_code_depnum_ccdc_archive 'CCDC 761524'
#TrackingRef 'sun-cec.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H42 Mn3 N8 O14'
_chemical_formula_sum            'C48 H42 Mn3 N8 O14'
_chemical_formula_weight         1119.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.2547(12)
_cell_length_b                   10.1947(14)
_cell_length_c                   12.9233(17)
_cell_angle_alpha                98.955(3)
_cell_angle_beta                 93.424(3)
_cell_angle_gamma                104.368(2)
_cell_volume                     1160.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2005
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      26.06

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             573
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8716
_exptl_absorpt_correction_T_max  0.9091
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7029
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         28.32
_reflns_number_total             5163
_reflns_number_gt                3500
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5163
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1166
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_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
Mn1 Mn 0.0000 0.0000 0.5000 0.02433(16) Uani 1 2 d S . .
Mn2 Mn 0.74458(5) 1.05465(5) 0.27358(4) 0.02998(15) Uani 1 1 d . . .
C1 C -0.1252(3) 0.4175(3) 0.8176(2) 0.0280(7) Uani 1 1 d . . .
C2 C 0.0006(3) 0.5275(3) 0.8321(2) 0.0367(8) Uani 1 1 d . . .
H2A H 0.0801 0.5207 0.7926 0.044 Uiso 1 1 calc R . .
C3 C 0.0126(4) 0.6457(3) 0.9020(3) 0.0395(8) Uani 1 1 d . . .
H3A H 0.0976 0.7188 0.9075 0.047 Uiso 1 1 calc R . .
C4 C -0.1031(3) 0.6571(3) 0.9657(2) 0.0298(7) Uani 1 1 d . . .
C5 C -0.2291(4) 0.5471(3) 0.9508(2) 0.0362(8) Uani 1 1 d . . .
H5A H -0.3084 0.5535 0.9905 0.043 Uiso 1 1 calc R . .
C6 C -0.2419(4) 0.4294(3) 0.8802(2) 0.0363(8) Uani 1 1 d . . .
H6A H -0.3279 0.3571 0.8735 0.044 Uiso 1 1 calc R . .
C7 C -0.0325(3) 0.2488(3) 0.6847(2) 0.0326(7) Uani 1 1 d . . .
H7A H 0.0682 0.2958 0.6898 0.039 Uiso 1 1 calc R . .
C8 C -0.2370(3) 0.0952(3) 0.6398(2) 0.0366(8) Uani 1 1 d . . .
H8A H -0.3084 0.0152 0.6083 0.044 Uiso 1 1 calc R . .
C9 C -0.1356(3) 0.2943(3) 0.7398(2) 0.0300(7) Uani 1 1 d . . .
C10 C -0.2014(4) 0.8277(3) 1.0925(2) 0.0371(8) Uani 1 1 d . . .
H10A H -0.3031 0.7827 1.0830 0.044 Uiso 1 1 calc R . .
C11 C 0.0042(4) 0.9770(3) 1.1485(2) 0.0366(8) Uani 1 1 d . . .
H11A H 0.0748 1.0548 1.1846 0.044 Uiso 1 1 calc R . .
C12 C -0.0941(3) 0.7811(3) 1.0422(2) 0.0325(7) Uani 1 1 d . . .
C13 C 0.2611(3) 0.4454(3) 0.3817(2) 0.0257(6) Uani 1 1 d . . .
C14 C 0.3611(3) 0.5704(3) 0.4244(2) 0.0291(7) Uani 1 1 d . . .
H14A H 0.3328 0.6293 0.4772 0.035 Uiso 1 1 calc R . .
C15 C 0.5002(3) 0.6095(3) 0.3910(2) 0.0316(7) Uani 1 1 d . . .
C16 C 0.5404(3) 0.5206(3) 0.3116(2) 0.0343(8) Uani 1 1 d . . .
H16A H 0.6339 0.5463 0.2870 0.041 Uiso 1 1 calc R . .
C17 C 0.4427(3) 0.3941(3) 0.2687(2) 0.0301(7) Uani 1 1 d . . .
C18 C 0.3038(3) 0.3592(3) 0.3053(2) 0.0309(7) Uani 1 1 d . . .
H18A H 0.2376 0.2747 0.2771 0.037 Uiso 1 1 calc R . .
C19 C 0.1066(3) 0.4123(3) 0.4227(3) 0.0329(7) Uani 1 1 d . . .
H19A H 0.1197 0.4345 0.4991 0.039 Uiso 1 1 calc R . .
H19B H 0.0491 0.4708 0.3976 0.039 Uiso 1 1 calc R . .
C20 C 0.0171(3) 0.2633(3) 0.3898(3) 0.0302(7) Uani 1 1 d . . .
C21 C 0.6102(4) 0.7430(3) 0.4422(2) 0.0404(8) Uani 1 1 d . . .
H21A H 0.7000 0.7220 0.4697 0.048 Uiso 1 1 calc R . .
H21B H 0.5669 0.7834 0.5016 0.048 Uiso 1 1 calc R . .
C22 C 0.6558(3) 0.8498(3) 0.3728(2) 0.0273(7) Uani 1 1 d . . .
C23 C 0.4873(4) 0.2962(3) 0.1836(3) 0.0404(8) Uani 1 1 d . . .
H23A H 0.3989 0.2474 0.1357 0.048 Uiso 1 1 calc R . .
H23B H 0.5581 0.3495 0.1438 0.048 Uiso 1 1 calc R . .
C24 C 0.5567(3) 0.1918(3) 0.2237(3) 0.0349(7) Uani 1 1 d . . .
N1 N -0.0957(3) 0.1242(3) 0.6201(2) 0.0350(6) Uani 1 1 d . . .
N2 N -0.2660(3) 0.1925(3) 0.7095(2) 0.0360(6) Uani 1 1 d . . .
H2B H -0.3517 0.1920 0.7320 0.043 Uiso 1 1 calc R . .
N3 N -0.1391(3) 0.9499(3) 1.1593(2) 0.0382(7) Uani 1 1 d . . .
N4 N 0.0369(3) 0.8799(3) 1.0799(2) 0.0373(7) Uani 1 1 d . . .
H4A H 0.1247 0.8789 1.0621 0.045 Uiso 1 1 calc R . .
O1 O 0.0646(2) 0.1746(2) 0.42544(19) 0.0449(6) Uani 1 1 d . . .
O1W O 0.6578(3) 0.1079(3) 0.9471(3) 0.0601(8) Uani 1 1 d . . .
O2 O -0.0989(3) 0.2396(2) 0.3286(2) 0.0560(7) Uani 1 1 d . . .
O3 O 0.7756(2) 0.94432(19) 0.40347(16) 0.0312(5) Uani 1 1 d . . .
O4 O 0.5783(2) 0.8512(2) 0.29203(17) 0.0338(5) Uani 1 1 d . . .
O5 O 0.5655(3) 0.1790(2) 0.31670(18) 0.0481(6) Uani 1 1 d . . .
O6 O 0.6083(2) 0.1163(2) 0.15611(17) 0.0428(6) Uani 1 1 d . . .
H1WA H 0.642(3) 0.109(3) 1.019(3) 0.037(9) Uiso 1 1 d . . .
H1WB H 0.609(5) 0.053(4) 0.907(3) 0.057(15) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0213(3) 0.0198(3) 0.0288(4) 0.0008(3) 0.0010(3) 0.0022(3)
Mn2 0.0301(3) 0.0260(3) 0.0321(3) 0.0031(2) 0.0007(2) 0.0059(2)
C1 0.0322(17) 0.0300(16) 0.0223(16) 0.0028(13) 0.0009(13) 0.0103(14)
C2 0.0293(17) 0.0418(19) 0.0348(19) -0.0055(15) 0.0071(14) 0.0082(15)
C3 0.0341(18) 0.0329(18) 0.043(2) -0.0063(15) -0.0011(16) 0.0025(15)
C4 0.0354(17) 0.0304(17) 0.0232(16) -0.0002(13) 0.0029(14) 0.0109(14)
C5 0.0394(19) 0.0366(18) 0.0341(19) 0.0012(15) 0.0117(15) 0.0138(15)
C6 0.0341(18) 0.0316(18) 0.040(2) 0.0021(15) 0.0036(15) 0.0045(14)
C7 0.0276(16) 0.0319(17) 0.0336(18) -0.0029(14) 0.0015(14) 0.0045(14)
C8 0.0316(17) 0.0355(18) 0.0351(19) -0.0084(14) 0.0036(15) 0.0032(14)
C9 0.0280(16) 0.0281(16) 0.0324(18) 0.0027(13) -0.0029(14) 0.0077(13)
C10 0.0340(18) 0.0406(19) 0.0315(18) -0.0062(14) 0.0017(15) 0.0086(15)
C11 0.044(2) 0.0312(17) 0.0275(17) -0.0053(13) 0.0057(15) 0.0032(15)
C12 0.0345(18) 0.0310(17) 0.0304(18) 0.0026(14) -0.0017(14) 0.0086(14)
C13 0.0250(15) 0.0217(15) 0.0302(17) 0.0054(12) 0.0039(13) 0.0050(12)
C14 0.0328(17) 0.0223(15) 0.0286(17) 0.0026(12) 0.0007(14) 0.0022(13)
C15 0.0262(16) 0.0287(17) 0.0349(18) 0.0121(14) -0.0052(14) -0.0041(13)
C16 0.0233(16) 0.045(2) 0.0358(19) 0.0160(16) 0.0058(14) 0.0046(14)
C17 0.0345(17) 0.0360(18) 0.0268(16) 0.0120(14) 0.0073(14) 0.0172(14)
C18 0.0287(16) 0.0181(15) 0.0432(19) 0.0053(13) 0.0018(14) 0.0017(12)
C19 0.0268(16) 0.0272(16) 0.0413(19) 0.0014(14) 0.0063(14) 0.0032(13)
C20 0.0243(16) 0.0266(16) 0.0380(19) 0.0062(14) 0.0105(14) 0.0016(13)
C21 0.0383(19) 0.041(2) 0.0308(18) 0.0090(15) -0.0030(15) -0.0110(15)
C22 0.0194(15) 0.0266(16) 0.0327(18) 0.0002(13) 0.0049(13) 0.0025(12)
C23 0.045(2) 0.043(2) 0.039(2) 0.0083(16) 0.0082(16) 0.0194(16)
C24 0.0253(16) 0.0341(18) 0.043(2) 0.0028(15) -0.0005(15) 0.0075(14)
N1 0.0292(14) 0.0297(14) 0.0415(17) -0.0055(12) 0.0004(13) 0.0071(12)
N2 0.0230(13) 0.0359(15) 0.0437(17) -0.0051(13) 0.0002(12) 0.0057(12)
N3 0.0382(16) 0.0333(15) 0.0405(17) -0.0019(13) 0.0014(13) 0.0102(13)
N4 0.0330(15) 0.0325(15) 0.0438(17) 0.0008(13) 0.0046(13) 0.0072(12)
O1 0.0304(12) 0.0328(13) 0.0721(18) 0.0246(12) 0.0039(12) 0.0004(10)
O1W 0.0487(18) 0.070(2) 0.0463(19) -0.0011(16) 0.0107(15) -0.0075(15)
O2 0.0425(15) 0.0392(14) 0.0744(19) 0.0154(13) -0.0218(14) -0.0083(12)
O3 0.0232(11) 0.0274(11) 0.0364(12) 0.0069(9) -0.0046(9) -0.0045(9)
O4 0.0247(11) 0.0380(13) 0.0351(13) 0.0099(10) -0.0034(10) 0.0007(9)
O5 0.0659(17) 0.0566(16) 0.0349(14) 0.0137(12) 0.0131(12) 0.0349(13)
O6 0.0500(14) 0.0511(15) 0.0319(13) -0.0026(11) 0.0032(11) 0.0280(12)

_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
Mn1 O1 2.128(2) 2_556 ?
Mn1 O1 2.128(2) . ?
Mn1 N1 2.215(3) . ?
Mn1 N1 2.215(3) 2_556 ?
Mn1 O3 2.2534(19) 2_666 ?
Mn1 O3 2.2534(19) 1_445 ?
Mn2 O2 2.065(2) 1_665 ?
Mn2 N3 2.180(3) 1_654 ?
Mn2 O6 2.180(2) 1_565 ?
Mn2 O3 2.204(2) . ?
Mn2 O4 2.311(2) . ?
Mn2 O5 2.366(2) 1_565 ?
Mn2 C24 2.597(3) 1_565 ?
Mn2 C22 2.606(3) . ?
C1 C2 1.381(4) . ?
C1 C6 1.405(4) . ?
C1 C9 1.460(4) . ?
C2 C3 1.365(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.406(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(4) . ?
C4 C12 1.460(4) . ?
C5 C6 1.364(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C9 1.353(4) . ?
C7 N1 1.377(4) . ?
C7 H7A 0.9300 . ?
C8 N1 1.316(4) . ?
C8 N2 1.323(4) . ?
C8 H8A 0.9300 . ?
C9 N2 1.371(4) . ?
C10 C12 1.360(4) . ?
C10 N3 1.370(4) . ?
C10 H10A 0.9300 . ?
C11 N3 1.306(4) . ?
C11 N4 1.329(4) . ?
C11 H11A 0.9300 . ?
C12 N4 1.375(4) . ?
C13 C18 1.361(4) . ?
C13 C14 1.385(4) . ?
C13 C19 1.531(4) . ?
C14 C15 1.367(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.391(4) . ?
C15 C21 1.509(4) . ?
C16 C17 1.389(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.379(4) . ?
C17 C23 1.514(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.518(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 O1 1.235(3) . ?
C20 O2 1.244(4) . ?
C21 C22 1.513(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O4 1.235(3) . ?
C22 O3 1.270(3) . ?
C23 C24 1.512(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 O5 1.229(4) . ?
C24 O6 1.267(4) . ?
C24 Mn2 2.597(3) 1_545 ?
N2 H2B 0.8600 . ?
N3 Mn2 2.180(3) 1_456 ?
N4 H4A 0.8600 . ?
O1W H1WA 0.94(3) . ?
O1W H1WB 0.74(4) . ?
O2 Mn2 2.065(2) 1_445 ?
O3 Mn1 2.2534(19) 1_665 ?
O5 Mn2 2.366(2) 1_545 ?
O6 Mn2 2.180(2) 1_545 ?

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 Mn1 O1 180.0 2_556 . ?
O1 Mn1 N1 91.06(9) 2_556 . ?
O1 Mn1 N1 88.94(9) . . ?
O1 Mn1 N1 88.94(9) 2_556 2_556 ?
O1 Mn1 N1 91.06(9) . 2_556 ?
N1 Mn1 N1 180.0 . 2_556 ?
O1 Mn1 O3 88.36(7) 2_556 2_666 ?
O1 Mn1 O3 91.64(7) . 2_666 ?
N1 Mn1 O3 92.57(8) . 2_666 ?
N1 Mn1 O3 87.43(8) 2_556 2_666 ?
O1 Mn1 O3 91.64(7) 2_556 1_445 ?
O1 Mn1 O3 88.36(7) . 1_445 ?
N1 Mn1 O3 87.43(8) . 1_445 ?
N1 Mn1 O3 92.57(8) 2_556 1_445 ?
O3 Mn1 O3 180.0 2_666 1_445 ?
O2 Mn2 N3 102.71(11) 1_665 1_654 ?
O2 Mn2 O6 100.19(9) 1_665 1_565 ?
N3 Mn2 O6 94.96(9) 1_654 1_565 ?
O2 Mn2 O3 99.71(8) 1_665 . ?
N3 Mn2 O3 97.84(9) 1_654 . ?
O6 Mn2 O3 153.29(8) 1_565 . ?
O2 Mn2 O4 154.33(9) 1_665 . ?
N3 Mn2 O4 92.67(9) 1_654 . ?
O6 Mn2 O4 98.78(8) 1_565 . ?
O3 Mn2 O4 57.39(7) . . ?
O2 Mn2 O5 85.03(10) 1_665 1_565 ?
N3 Mn2 O5 151.62(9) 1_654 1_565 ?
O6 Mn2 O5 56.67(8) 1_565 1_565 ?
O3 Mn2 O5 107.83(8) . 1_565 ?
O4 Mn2 O5 91.13(8) . 1_565 ?
O2 Mn2 C24 88.57(10) 1_665 1_565 ?
N3 Mn2 C24 123.74(11) 1_654 1_565 ?
O6 Mn2 C24 29.11(9) 1_565 1_565 ?
O3 Mn2 C24 134.77(10) . 1_565 ?
O4 Mn2 C24 99.92(9) . 1_565 ?
O5 Mn2 C24 28.18(9) 1_565 1_565 ?
O2 Mn2 C22 127.87(10) 1_665 . ?
N3 Mn2 C22 96.37(9) 1_654 . ?
O6 Mn2 C22 126.08(9) 1_565 . ?
O3 Mn2 C22 29.12(8) . . ?
O4 Mn2 C22 28.28(7) . . ?
O5 Mn2 C22 100.18(9) 1_565 . ?
C24 Mn2 C22 119.38(10) 1_565 . ?
C2 C1 C6 117.4(3) . . ?
C2 C1 C9 120.9(3) . . ?
C6 C1 C9 121.7(3) . . ?
C3 C2 C1 122.5(3) . . ?
C3 C2 H2A 118.7 . . ?
C1 C2 H2A 118.7 . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C12 120.9(3) . . ?
C3 C4 C12 121.9(3) . . ?
C6 C5 C4 122.7(3) . . ?
C6 C5 H5A 118.6 . . ?
C4 C5 H5A 118.6 . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 H6A 120.0 . . ?
C1 C6 H6A 120.0 . . ?
C9 C7 N1 111.4(3) . . ?
C9 C7 H7A 124.3 . . ?
N1 C7 H7A 124.3 . . ?
N1 C8 N2 112.5(3) . . ?
N1 C8 H8A 123.8 . . ?
N2 C8 H8A 123.8 . . ?
C7 C9 N2 104.3(3) . . ?
C7 C9 C1 132.5(3) . . ?
N2 C9 C1 123.3(3) . . ?
C12 C10 N3 110.6(3) . . ?
C12 C10 H10A 124.7 . . ?
N3 C10 H10A 124.7 . . ?
N3 C11 N4 111.8(3) . . ?
N3 C11 H11A 124.1 . . ?
N4 C11 H11A 124.1 . . ?
C10 C12 N4 104.3(3) . . ?
C10 C12 C4 131.5(3) . . ?
N4 C12 C4 124.2(3) . . ?
C18 C13 C14 118.8(3) . . ?
C18 C13 C19 123.4(3) . . ?
C14 C13 C19 117.8(3) . . ?
C15 C14 C13 121.7(3) . . ?
C15 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
C14 C15 C16 118.4(3) . . ?
C14 C15 C21 120.8(3) . . ?
C16 C15 C21 120.7(3) . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C18 C17 C16 118.5(3) . . ?
C18 C17 C23 120.6(3) . . ?
C16 C17 C23 120.9(3) . . ?
C13 C18 C17 121.7(3) . . ?
C13 C18 H18A 119.2 . . ?
C17 C18 H18A 119.2 . . ?
C20 C19 C13 114.3(2) . . ?
C20 C19 H19A 108.7 . . ?
C13 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C13 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
O1 C20 O2 124.7(3) . . ?
O1 C20 C19 117.9(3) . . ?
O2 C20 C19 117.4(3) . . ?
C15 C21 C22 116.4(3) . . ?
C15 C21 H21A 108.2 . . ?
C22 C21 H21A 108.2 . . ?
C15 C21 H21B 108.2 . . ?
C22 C21 H21B 108.2 . . ?
H21A C21 H21B 107.3 . . ?
O4 C22 O3 120.1(3) . . ?
O4 C22 C21 122.7(3) . . ?
O3 C22 C21 117.2(3) . . ?
O4 C22 Mn2 62.48(15) . . ?
O3 C22 Mn2 57.60(14) . . ?
C21 C22 Mn2 173.3(2) . . ?
C24 C23 C17 114.6(3) . . ?
C24 C23 H23A 108.6 . . ?
C17 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C17 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
O5 C24 O6 120.3(3) . . ?
O5 C24 C23 123.2(3) . . ?
O6 C24 C23 116.6(3) . . ?
O5 C24 Mn2 65.41(17) . 1_545 ?
O6 C24 Mn2 56.88(15) . 1_545 ?
C23 C24 Mn2 163.4(2) . 1_545 ?
C8 N1 C7 103.6(3) . . ?
C8 N1 Mn1 125.2(2) . . ?
C7 N1 Mn1 131.0(2) . . ?
C8 N2 C9 108.2(3) . . ?
C8 N2 H2B 125.9 . . ?
C9 N2 H2B 125.9 . . ?
C11 N3 C10 105.1(3) . . ?
C11 N3 Mn2 128.7(2) . 1_456 ?
C10 N3 Mn2 125.6(2) . 1_456 ?
C11 N4 C12 108.2(3) . . ?
C11 N4 H4A 125.9 . . ?
C12 N4 H4A 125.9 . . ?
C20 O1 Mn1 143.2(2) . . ?
H1WA O1W H1WB 119(4) . . ?
C20 O2 Mn2 128.9(2) . 1_445 ?
C22 O3 Mn2 93.29(17) . . ?
C22 O3 Mn1 144.75(19) . 1_665 ?
Mn2 O3 Mn1 119.32(8) . 1_665 ?
C22 O4 Mn2 89.24(16) . . ?
C24 O5 Mn2 86.41(19) . 1_545 ?
C24 O6 Mn2 94.01(19) . 1_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.6(5) . . . . ?
C9 C1 C2 C3 178.2(3) . . . . ?
C1 C2 C3 C4 2.5(5) . . . . ?
C2 C3 C4 C5 -2.6(5) . . . . ?
C2 C3 C4 C12 179.4(3) . . . . ?
C3 C4 C5 C6 2.0(5) . . . . ?
C12 C4 C5 C6 -179.9(3) . . . . ?
C4 C5 C6 C1 -1.2(5) . . . . ?
C2 C1 C6 C5 0.9(4) . . . . ?
C9 C1 C6 C5 -178.9(3) . . . . ?
N1 C7 C9 N2 1.3(3) . . . . ?
N1 C7 C9 C1 179.5(3) . . . . ?
C2 C1 C9 C7 13.4(5) . . . . ?
C6 C1 C9 C7 -166.8(3) . . . . ?
C2 C1 C9 N2 -168.6(3) . . . . ?
C6 C1 C9 N2 11.1(4) . . . . ?
N3 C10 C12 N4 -0.4(3) . . . . ?
N3 C10 C12 C4 179.2(3) . . . . ?
C5 C4 C12 C10 -15.7(5) . . . . ?
C3 C4 C12 C10 162.3(3) . . . . ?
C5 C4 C12 N4 163.8(3) . . . . ?
C3 C4 C12 N4 -18.2(5) . . . . ?
C18 C13 C14 C15 0.7(4) . . . . ?
C19 C13 C14 C15 -178.7(3) . . . . ?
C13 C14 C15 C16 0.3(4) . . . . ?
C13 C14 C15 C21 -177.0(3) . . . . ?
C14 C15 C16 C17 -1.2(4) . . . . ?
C21 C15 C16 C17 176.1(3) . . . . ?
C15 C16 C17 C18 1.0(4) . . . . ?
C15 C16 C17 C23 -178.9(3) . . . . ?
C14 C13 C18 C17 -0.9(4) . . . . ?
C19 C13 C18 C17 178.5(3) . . . . ?
C16 C17 C18 C13 0.0(4) . . . . ?
C23 C17 C18 C13 180.0(3) . . . . ?
C18 C13 C19 C20 13.1(4) . . . . ?
C14 C13 C19 C20 -167.6(3) . . . . ?
C13 C19 C20 O1 66.8(4) . . . . ?
C13 C19 C20 O2 -113.1(3) . . . . ?
C14 C15 C21 C22 -116.6(3) . . . . ?
C16 C15 C21 C22 66.1(4) . . . . ?
C15 C21 C22 O4 22.4(5) . . . . ?
C15 C21 C22 O3 -161.0(3) . . . . ?
O2 Mn2 C22 O4 164.68(16) 1_665 . . . ?
N3 Mn2 C22 O4 -83.78(17) 1_654 . . . ?
O6 Mn2 C22 O4 17.1(2) 1_565 . . . ?
O3 Mn2 C22 O4 -178.5(3) . . . . ?
O5 Mn2 C22 O4 73.06(17) 1_565 . . . ?
C24 Mn2 C22 O4 51.0(2) 1_565 . . . ?
O2 Mn2 C22 O3 -16.9(2) 1_665 . . . ?
N3 Mn2 C22 O3 94.69(17) 1_654 . . . ?
O6 Mn2 C22 O3 -164.42(15) 1_565 . . . ?
O4 Mn2 C22 O3 178.5(3) . . . . ?
O5 Mn2 C22 O3 -108.47(17) 1_565 . . . ?
C24 Mn2 C22 O3 -130.55(17) 1_565 . . . ?
C18 C17 C23 C24 -87.0(4) . . . . ?
C16 C17 C23 C24 92.9(3) . . . . ?
C17 C23 C24 O5 5.8(5) . . . . ?
C17 C23 C24 O6 -173.7(3) . . . . ?
C17 C23 C24 Mn2 -111.0(8) . . . 1_545 ?
N2 C8 N1 C7 1.1(4) . . . . ?
N2 C8 N1 Mn1 -174.9(2) . . . . ?
C9 C7 N1 C8 -1.5(4) . . . . ?
C9 C7 N1 Mn1 174.2(2) . . . . ?
O1 Mn1 N1 C8 -59.5(3) 2_556 . . . ?
O1 Mn1 N1 C8 120.5(3) . . . . ?
O3 Mn1 N1 C8 -147.9(3) 2_666 . . . ?
O3 Mn1 N1 C8 32.1(3) 1_445 . . . ?
O1 Mn1 N1 C7 125.6(3) 2_556 . . . ?
O1 Mn1 N1 C7 -54.4(3) . . . . ?
O3 Mn1 N1 C7 37.2(3) 2_666 . . . ?
O3 Mn1 N1 C7 -142.8(3) 1_445 . . . ?
N1 C8 N2 C9 -0.4(4) . . . . ?
C7 C9 N2 C8 -0.6(3) . . . . ?
C1 C9 N2 C8 -179.0(3) . . . . ?
N4 C11 N3 C10 -0.3(4) . . . . ?
N4 C11 N3 Mn2 171.2(2) . . . 1_456 ?
C12 C10 N3 C11 0.4(4) . . . . ?
C12 C10 N3 Mn2 -171.4(2) . . . 1_456 ?
N3 C11 N4 C12 0.0(4) . . . . ?
C10 C12 N4 C11 0.3(3) . . . . ?
C4 C12 N4 C11 -179.4(3) . . . . ?
O2 C20 O1 Mn1 -48.8(6) . . . . ?
C19 C20 O1 Mn1 131.3(3) . . . . ?
N1 Mn1 O1 C20 -52.1(4) . . . . ?
N1 Mn1 O1 C20 127.9(4) 2_556 . . . ?
O3 Mn1 O1 C20 -144.6(4) 2_666 . . . ?
O3 Mn1 O1 C20 35.4(4) 1_445 . . . ?
O1 C20 O2 Mn2 4.2(5) . . . 1_445 ?
C19 C20 O2 Mn2 -175.9(2) . . . 1_445 ?
O4 C22 O3 Mn2 1.6(3) . . . . ?
C21 C22 O3 Mn2 -175.1(2) . . . . ?
O4 C22 O3 Mn1 -157.0(2) . . . 1_665 ?
C21 C22 O3 Mn1 26.3(5) . . . 1_665 ?
Mn2 C22 O3 Mn1 -158.6(3) . . . 1_665 ?
O2 Mn2 O3 C22 166.57(18) 1_665 . . . ?
N3 Mn2 O3 C22 -89.02(18) 1_654 . . . ?
O6 Mn2 O3 C22 28.9(3) 1_565 . . . ?
O4 Mn2 O3 C22 -0.86(16) . . . . ?
O5 Mn2 O3 C22 78.71(18) 1_565 . . . ?
C24 Mn2 O3 C22 68.9(2) 1_565 . . . ?
O2 Mn2 O3 Mn1 -27.41(13) 1_665 . . 1_665 ?
N3 Mn2 O3 Mn1 77.00(12) 1_654 . . 1_665 ?
O6 Mn2 O3 Mn1 -165.10(14) 1_565 . . 1_665 ?
O4 Mn2 O3 Mn1 165.15(14) . . . 1_665 ?
O5 Mn2 O3 Mn1 -115.28(11) 1_565 . . 1_665 ?
C24 Mn2 O3 Mn1 -125.13(12) 1_565 . . 1_665 ?
C22 Mn2 O3 Mn1 166.0(2) . . . 1_665 ?
O3 C22 O4 Mn2 -1.5(3) . . . . ?
C21 C22 O4 Mn2 175.0(3) . . . . ?
O2 Mn2 O4 C22 -28.8(3) 1_665 . . . ?
N3 Mn2 O4 C22 98.48(18) 1_654 . . . ?
O6 Mn2 O4 C22 -166.07(17) 1_565 . . . ?
O3 Mn2 O4 C22 0.89(16) . . . . ?
O5 Mn2 O4 C22 -109.65(17) 1_565 . . . ?
C24 Mn2 O4 C22 -136.58(18) 1_565 . . . ?
O6 C24 O5 Mn2 15.7(3) . . . 1_545 ?
C23 C24 O5 Mn2 -163.7(3) . . . 1_545 ?
O5 C24 O6 Mn2 -17.1(3) . . . 1_545 ?
C23 C24 O6 Mn2 162.3(2) . . . 1_545 ?

_diffrn_measured_fraction_theta_max 0.893
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.085

#====END