data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Han, Jianlin'
_publ_contact_author_email       hanjl@nju.edu.cn

_publ_section_title              
;
Hydrogen-Bonding Self-Assembly of Two Dimensional (2D) Layer
Structures Generating Metal-Organic Nanotubes
;
loop_
_publ_author_name
'Hailong Sun'
'Guanghui An'
'Jianlin Han'
'Yi Pan'

data_sune
_database_code_depnum_ccdc_archive 'CCDC 764062'
#TrackingRef 'sunE.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H20 Co N4 O4 S, H0.80 O0.40, 1.6(H2 O)'
_chemical_formula_sum            'C27 H24 Co N4 O6 S'
_chemical_formula_weight         591.49

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c '
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   30.6320(13)
_cell_length_b                   13.6735(15)
_cell_length_c                   14.9266(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.758(2)
_cell_angle_gamma                90.00
_cell_volume                     6220.4(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    1456
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      19.92

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2440
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8263
_exptl_absorpt_correction_T_max  0.8682
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            16743
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6106
_reflns_number_gt                4185
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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^)+(0.05P)^2^] 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         6106
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.19993(9) 0.2718(2) 0.5796(2) 0.0304(6) Uani 1 1 d . . .
C2 C 0.15547(9) 0.3074(2) 0.59677(19) 0.0327(6) Uani 1 1 d . . .
C3 C 0.14959(10) 0.3951(2) 0.6419(2) 0.0361(7) Uani 1 1 d . . .
H3 H 0.1741 0.4317 0.6629 0.043 Uiso 1 1 calc R . .
C4 C 0.10858(10) 0.4290(2) 0.6560(2) 0.0372(7) Uani 1 1 d . . .
H4 H 0.1054 0.4882 0.6853 0.045 Uiso 1 1 calc R . .
C5 C 0.07101(9) 0.3724(2) 0.6254(2) 0.0340(7) Uani 1 1 d . . .
C6 C 0.07657(10) 0.2838(2) 0.5824(2) 0.0401(7) Uani 1 1 d . . .
H6 H 0.0523 0.2446 0.5655 0.048 Uiso 1 1 calc R . .
C7 C 0.11673(10) 0.2542(2) 0.5651(2) 0.0401(7) Uani 1 1 d . . .
H7 H 0.1194 0.1976 0.5316 0.048 Uiso 1 1 calc R . .
C8 C -0.00872(9) 0.4099(2) 0.5936(2) 0.0341(6) Uani 1 1 d . . .
C9 C -0.04415(5) 0.34394(15) 0.44685(10) 0.0375(7) Uani 1 1 d G . .
C10 C -0.08490(6) 0.31593(16) 0.47146(9) 0.0379(7) Uani 1 1 d G . .
H10 H -0.0904 0.3183 0.5316 0.046 Uiso 1 1 calc R . .
C11 C -0.11743(5) 0.28438(16) 0.40623(11) 0.0400(7) Uani 1 1 d G . .
H11 H -0.1447 0.2656 0.4227 0.048 Uiso 1 1 calc R . .
C12 C -0.10920(5) 0.28084(15) 0.31639(10) 0.0330(6) Uani 1 1 d G . .
C13 C -0.06845(6) 0.30885(15) 0.29177(9) 0.0391(7) Uani 1 1 d G . .
H13 H -0.0629 0.3065 0.2317 0.047 Uiso 1 1 calc R . .
C14 C -0.03592(5) 0.34041(16) 0.35701(12) 0.0376(7) Uani 1 1 d G . .
H14 H -0.0087 0.3591 0.3405 0.045 Uiso 1 1 calc R . .
C15 C -0.14414(9) 0.2485(2) 0.2449(2) 0.0331(7) Uani 1 1 d . . .
C16 C 0.17670(10) 0.43479(19) 0.4062(2) 0.0353(7) Uani 1 1 d . . .
H16 H 0.1536 0.4038 0.4307 0.042 Uiso 1 1 calc R . .
C17 C 0.17694(11) 0.5340(2) 0.4023(2) 0.0405(8) Uani 1 1 d . . .
H17 H 0.1542 0.5696 0.4234 0.049 Uiso 1 1 calc R . .
C18 C 0.21170(11) 0.5828(2) 0.3665(2) 0.0380(7) Uani 1 1 d . . .
C19 C 0.24419(11) 0.5246(2) 0.3380(2) 0.0426(8) Uani 1 1 d . . .
H19 H 0.2680 0.5533 0.3144 0.051 Uiso 1 1 calc R . .
C20 C 0.24188(11) 0.4245(2) 0.3441(2) 0.0377(7) Uani 1 1 d . . .
H20 H 0.2647 0.3875 0.3252 0.045 Uiso 1 1 calc R . .
C21 C 0.21618(12) 0.6916(2) 0.3598(2) 0.0429(8) Uani 1 1 d . . .
H21 H 0.2429 0.7204 0.3506 0.051 Uiso 1 1 calc R . .
C22 C 0.17777(11) 0.7501(2) 0.3682(2) 0.0421(8) Uani 1 1 d . . .
H22 H 0.1503 0.7231 0.3734 0.051 Uiso 1 1 calc R . .
C23 C 0.18597(11) 0.8589(2) 0.3678(2) 0.0413(7) Uani 1 1 d . . .
C24 C 0.15785(12) 0.9181(2) 0.3152(2) 0.0442(8) Uani 1 1 d . . .
H24 H 0.1351 0.8914 0.2771 0.053 Uiso 1 1 calc R . .
C25 C 0.16398(11) 1.0197(2) 0.3198(2) 0.0432(8) Uani 1 1 d . . .
H25 H 0.1450 1.0590 0.2830 0.052 Uiso 1 1 calc R . .
C26 C 0.22404(11) 1.0066(2) 0.4095(2) 0.0497(9) Uani 1 1 d . . .
H26 H 0.2493 1.0347 0.4382 0.060 Uiso 1 1 calc R . .
C27 C 0.22212(12) 0.9056(2) 0.4103(2) 0.0484(9) Uani 1 1 d . . .
H27 H 0.2451 0.8695 0.4393 0.058 Uiso 1 1 calc R . .
Co1 Co 0.203583(12) 0.21982(3) 0.37926(2) 0.02598(11) Uani 1 1 d . . .
N1 N 0.03058(8) 0.4103(2) 0.64473(18) 0.0410(6) Uani 1 1 d . . .
H1B H 0.0253 0.3806 0.6963 0.049 Uiso 1 1 d R . .
N2 N -0.00858(8) 0.3726(2) 0.50996(17) 0.0385(6) Uani 1 1 d . . .
H2B H 0.0068 0.4162 0.4807 0.046 Uiso 1 1 d R . .
N3 N 0.20888(8) 0.37860(17) 0.37555(18) 0.0364(6) Uani 1 1 d . . .
N4 N 0.19608(8) 1.06379(17) 0.37504(18) 0.0349(6) Uani 1 1 d . . .
O1 O 0.23139(6) 0.30109(13) 0.62992(13) 0.0297(4) Uani 1 1 d . . .
O2 O 0.20150(7) 0.21424(14) 0.51317(14) 0.0345(5) Uani 1 1 d . . .
O3 O -0.13547(6) 0.24055(15) 0.16594(15) 0.0361(5) Uani 1 1 d . . .
O4 O -0.18201(7) 0.23184(14) 0.26677(14) 0.0348(5) Uani 1 1 d . . .
O1W O 0.16081(18) 1.0193(4) 0.0776(4) 0.0472(15) Uani 0.40 1 d P . .
H1WA H 0.1850 0.9973 0.0627 0.071 Uiso 0.40 1 d PR . .
H1WB H 0.1425 0.9727 0.0788 0.071 Uiso 0.40 1 d PR . .
O2W O 0.4518(2) 0.4508(4) 0.4696(4) 0.0500(15) Uani 0.40 1 d P . .
H2WD H 0.4306 0.4197 0.4413 0.060 Uiso 0.40 1 d PR . .
H2WA H 0.4728 0.4554 0.4366 0.075 Uiso 0.40 1 d PR . .
O3W O 0.98890(18) 0.1477(5) 0.5522(4) 0.0521(16) Uani 0.40 1 d P . .
H3WA H 0.9732 0.0997 0.5320 0.078 Uiso 0.40 1 d PR . .
H3WC H 0.9866 0.1546 0.6081 0.078 Uiso 0.40 1 d PR . .
O4W O 0.5000 0.4393(3) 0.7500 0.0498(10) Uani 0.80 2 d SP . .
H4WA H 0.5111 0.4624 0.8000 0.075 Uiso 0.40 1 d PR . .
H4WB H 0.4747 0.4164 0.7560 0.075 Uiso 0.40 1 d PR . .
O5W O 0.43017(19) 0.6349(4) 0.6163(4) 0.0484(15) Uani 0.40 1 d P . .
H5WD H 0.4455 0.5922 0.6463 0.058 Uiso 0.40 1 d PR . .
H5WC H 0.4298 0.6225 0.5604 0.073 Uiso 0.40 1 d PR . .
S1 S -0.05235(2) 0.46027(6) 0.63469(5) 0.03712(19) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0305(14) 0.0244(13) 0.0354(15) -0.0020(12) -0.0005(12) 0.0091(12)
C2 0.0286(15) 0.0421(16) 0.0272(15) -0.0087(12) 0.0021(11) 0.0011(12)
C3 0.0253(14) 0.0380(16) 0.0425(17) -0.0092(14) -0.0094(12) 0.0043(13)
C4 0.0296(16) 0.0415(16) 0.0391(17) -0.0158(14) -0.0042(13) 0.0065(13)
C5 0.0245(15) 0.0394(16) 0.0370(16) -0.0072(13) -0.0026(12) 0.0058(12)
C6 0.0246(15) 0.0492(18) 0.0460(18) -0.0183(16) 0.0006(12) -0.0056(14)
C7 0.0282(15) 0.0410(17) 0.0499(19) -0.0144(14) -0.0018(14) 0.0051(13)
C8 0.0251(14) 0.0378(15) 0.0391(16) -0.0091(14) 0.0023(12) -0.0026(12)
C9 0.0247(15) 0.0524(19) 0.0356(17) -0.0112(15) 0.0044(13) -0.0065(13)
C10 0.0274(15) 0.0435(17) 0.0427(18) -0.0117(14) 0.0024(13) -0.0109(13)
C11 0.0366(16) 0.0532(19) 0.0307(16) -0.0145(14) 0.0059(12) -0.0145(15)
C12 0.0328(15) 0.0347(15) 0.0302(15) -0.0011(13) -0.0029(12) -0.0106(13)
C13 0.0367(17) 0.0491(18) 0.0316(16) -0.0093(14) 0.0041(13) -0.0128(14)
C14 0.0287(15) 0.0500(18) 0.0341(17) -0.0159(14) 0.0037(12) -0.0046(13)
C15 0.0317(16) 0.0252(14) 0.0404(18) -0.0014(12) -0.0068(13) 0.0045(12)
C16 0.0427(18) 0.0225(13) 0.0413(18) 0.0047(12) 0.0066(14) 0.0029(13)
C17 0.0434(19) 0.0284(15) 0.052(2) -0.0064(14) 0.0173(15) 0.0030(13)
C18 0.0474(19) 0.0241(14) 0.0418(18) 0.0002(13) 0.0013(14) -0.0036(13)
C19 0.051(2) 0.0334(16) 0.0455(19) 0.0090(14) 0.0154(16) -0.0016(14)
C20 0.0449(18) 0.0318(15) 0.0381(17) 0.0119(13) 0.0123(14) 0.0080(13)
C21 0.049(2) 0.0367(16) 0.046(2) 0.0092(14) 0.0203(16) -0.0024(15)
C22 0.0466(19) 0.0283(14) 0.0491(19) 0.0034(13) -0.0064(15) 0.0017(13)
C23 0.0445(18) 0.0345(16) 0.0437(19) 0.0030(14) -0.0010(14) 0.0008(15)
C24 0.0470(19) 0.0322(15) 0.0486(19) -0.0041(15) -0.0191(15) -0.0030(14)
C25 0.0451(19) 0.0350(16) 0.0447(19) -0.0036(14) -0.0196(15) 0.0068(15)
C26 0.045(2) 0.0384(18) 0.061(2) 0.0173(16) -0.0197(17) -0.0089(16)
C27 0.054(2) 0.0301(16) 0.056(2) -0.0238(15) -0.0190(17) 0.0183(15)
Co1 0.0250(2) 0.02217(19) 0.0298(2) 0.00023(15) -0.00193(14) 0.00433(15)
N1 0.0330(14) 0.0514(16) 0.0373(15) -0.0159(13) -0.0036(11) 0.0032(12)
N2 0.0248(13) 0.0487(15) 0.0419(16) -0.0175(12) 0.0034(11) -0.0075(11)
N3 0.0391(15) 0.0232(12) 0.0455(15) 0.0092(11) -0.0022(12) 0.0018(10)
N4 0.0317(13) 0.0243(12) 0.0484(16) -0.0045(11) 0.0031(12) 0.0002(10)
O1 0.0255(10) 0.0243(9) 0.0383(11) -0.0002(8) -0.0020(9) 0.0047(8)
O2 0.0398(12) 0.0322(11) 0.0325(11) -0.0032(9) 0.0086(9) 0.0019(9)
O3 0.0281(10) 0.0386(11) 0.0402(12) -0.0065(9) -0.0027(9) -0.0032(9)
O4 0.0348(11) 0.0330(11) 0.0351(11) -0.0009(9) -0.0038(9) 0.0036(9)
O1W 0.029(3) 0.054(3) 0.057(4) -0.008(3) -0.004(3) 0.019(3)
O2W 0.050(3) 0.049(3) 0.049(4) -0.018(3) -0.003(3) 0.012(3)
O3W 0.034(3) 0.071(4) 0.050(4) 0.001(3) -0.006(3) -0.016(3)
O4W 0.040(2) 0.050(2) 0.059(3) 0.000 -0.001(2) 0.000
O5W 0.051(4) 0.030(3) 0.061(4) 0.004(3) -0.013(3) 0.019(3)
S1 0.0219(4) 0.0457(4) 0.0429(4) -0.0113(4) -0.0012(3) 0.0070(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
C1 O1 1.228(3) . ?
C1 O2 1.271(3) . ?
C1 C2 1.493(4) . ?
C2 C3 1.395(4) . ?
C2 C7 1.431(4) . ?
C3 C4 1.375(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.423(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(4) . ?
C5 N1 1.399(4) . ?
C6 C7 1.344(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N2 1.349(4) . ?
C8 N1 1.359(4) . ?
C8 S1 1.673(3) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C9 N2 1.422(3) . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 C15 1.500(3) . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O3 1.238(4) . ?
C15 O4 1.257(4) . ?
C15 Co1 2.495(3) 2 ?
C16 C17 1.357(4) . ?
C16 N3 1.364(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.408(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(5) . ?
C18 C21 1.498(4) . ?
C19 C20 1.374(4) . ?
C19 H19 0.9300 . ?
C20 N3 1.316(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.438(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.509(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.370(4) . ?
C23 C27 1.377(4) . ?
C24 C25 1.402(4) . ?
C24 H24 0.9300 . ?
C25 N4 1.359(4) . ?
C25 H25 0.9300 . ?
C26 N4 1.233(4) . ?
C26 C27 1.383(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
Co1 O2 2.008(2) . ?
Co1 O1 2.0306(19) 7_556 ?
Co1 N4 2.146(2) 1_545 ?
Co1 O3 2.146(2) 2 ?
Co1 N3 2.178(2) . ?
Co1 O4 2.219(2) 2 ?
Co1 C15 2.495(3) 2 ?
N1 H1B 0.8999 . ?
N2 H2B 0.8998 . ?
N4 Co1 2.146(2) 1_565 ?
O1 Co1 2.0306(19) 7_556 ?
O3 Co1 2.146(2) 2 ?
O4 Co1 2.219(2) 2 ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8498 . ?
O2W H2WD 0.8501 . ?
O2W H2WA 0.8501 . ?
O3W H3WA 0.8500 . ?
O3W H3WC 0.8501 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8500 . ?
O5W H5WD 0.8500 . ?
O5W H5WC 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 126.2(3) . . ?
O1 C1 C2 117.5(2) . . ?
O2 C1 C2 116.3(2) . . ?
C3 C2 C7 117.0(3) . . ?
C3 C2 C1 121.8(3) . . ?
C7 C2 C1 121.2(3) . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.3(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 N1 124.8(3) . . ?
C6 C5 C4 119.3(3) . . ?
N1 C5 C4 115.9(3) . . ?
C7 C6 C5 120.5(3) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 121.9(3) . . ?
C6 C7 H7 119.1 . . ?
C2 C7 H7 119.1 . . ?
N2 C8 N1 115.9(3) . . ?
N2 C8 S1 124.9(2) . . ?
N1 C8 S1 119.2(2) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 N2 123.34(15) . . ?
C14 C9 N2 116.59(15) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C15 120.73(17) . . ?
C13 C12 C15 119.26(17) . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
O3 C15 O4 121.5(3) . . ?
O3 C15 C12 119.8(3) . . ?
O4 C15 C12 118.7(3) . . ?
O3 C15 Co1 59.31(14) . 2 ?
O4 C15 Co1 62.67(15) . 2 ?
C12 C15 Co1 171.87(19) . 2 ?
C17 C16 N3 122.8(3) . . ?
C17 C16 H16 118.6 . . ?
N3 C16 H16 118.6 . . ?
C16 C17 C18 119.9(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 116.2(3) . . ?
C19 C18 C21 118.7(3) . . ?
C17 C18 C21 125.1(3) . . ?
C20 C19 C18 120.9(3) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
N3 C20 C19 123.0(3) . . ?
N3 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
C22 C21 C18 117.7(3) . . ?
C22 C21 H21 121.2 . . ?
C18 C21 H21 121.2 . . ?
C21 C22 C23 114.2(3) . . ?
C21 C22 H22 122.9 . . ?
C23 C22 H22 122.9 . . ?
C24 C23 C27 114.8(3) . . ?
C24 C23 C22 119.3(3) . . ?
C27 C23 C22 125.6(3) . . ?
C23 C24 C25 119.0(3) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N4 C25 C24 123.7(3) . . ?
N4 C25 H25 118.2 . . ?
C24 C25 H25 118.2 . . ?
N4 C26 C27 127.5(3) . . ?
N4 C26 H26 116.3 . . ?
C27 C26 H26 116.3 . . ?
C23 C27 C26 119.5(3) . . ?
C23 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
O2 Co1 O1 101.02(8) . 7_556 ?
O2 Co1 N4 88.71(9) . 1_545 ?
O1 Co1 N4 87.76(9) 7_556 1_545 ?
O2 Co1 O3 101.01(9) . 2 ?
O1 Co1 O3 157.93(8) 7_556 2 ?
N4 Co1 O3 91.39(9) 1_545 2 ?
O2 Co1 N3 94.19(9) . . ?
O1 Co1 N3 93.59(9) 7_556 . ?
N4 Co1 N3 176.51(10) 1_545 . ?
O3 Co1 N3 86.15(9) 2 . ?
O2 Co1 O4 160.82(8) . 2 ?
O1 Co1 O4 98.15(8) 7_556 2 ?
N4 Co1 O4 91.39(9) 1_545 2 ?
O3 Co1 O4 59.81(8) 2 2 ?
N3 Co1 O4 85.23(9) . 2 ?
O2 Co1 C15 130.66(10) . 2 ?
O1 Co1 C15 128.30(9) 7_556 2 ?
N4 Co1 C15 93.81(9) 1_545 2 ?
O3 Co1 C15 29.75(9) 2 2 ?
N3 Co1 C15 82.83(9) . 2 ?
O4 Co1 C15 30.21(9) 2 2 ?
C8 N1 C5 129.4(3) . . ?
C8 N1 H1B 104.7 . . ?
C5 N1 H1B 104.4 . . ?
C8 N2 C9 130.1(2) . . ?
C8 N2 H2B 104.4 . . ?
C9 N2 H2B 105.3 . . ?
C20 N3 C16 117.2(3) . . ?
C20 N3 Co1 123.1(2) . . ?
C16 N3 Co1 119.6(2) . . ?
C26 N4 C25 113.7(3) . . ?
C26 N4 Co1 123.4(2) . 1_565 ?
C25 N4 Co1 121.9(2) . 1_565 ?
C1 O1 Co1 128.89(19) . 7_556 ?
C1 O2 Co1 139.54(18) . . ?
C15 O3 Co1 90.93(17) . 2 ?
C15 O4 Co1 87.13(18) . 2 ?
H1WA O1W H1WB 109.5 . . ?
H2WD O2W H2WA 109.5 . . ?
H3WA O3W H3WC 109.5 . . ?
H4WA O4W H4WB 109.5 . . ?
H5WD O5W H5WC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 24.1(4) . . . . ?
O2 C1 C2 C3 -155.3(3) . . . . ?
O1 C1 C2 C7 -157.8(3) . . . . ?
O2 C1 C2 C7 22.8(4) . . . . ?
C7 C2 C3 C4 0.4(5) . . . . ?
C1 C2 C3 C4 178.6(3) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C3 C4 C5 N1 178.2(3) . . . . ?
N1 C5 C6 C7 178.7(3) . . . . ?
C4 C5 C6 C7 -3.9(5) . . . . ?
C5 C6 C7 C2 5.7(5) . . . . ?
C3 C2 C7 C6 -3.9(5) . . . . ?
C1 C2 C7 C6 177.9(3) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
N2 C9 C10 C11 -176.9(2) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C15 -179.0(2) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C15 C12 C13 C14 179.0(2) . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
N2 C9 C14 C13 177.1(2) . . . . ?
C11 C12 C15 O3 -176.0(2) . . . . ?
C13 C12 C15 O3 5.0(3) . . . . ?
C11 C12 C15 O4 5.4(3) . . . . ?
C13 C12 C15 O4 -173.6(2) . . . . ?
N3 C16 C17 C18 -0.7(5) . . . . ?
C16 C17 C18 C19 -0.8(5) . . . . ?
C16 C17 C18 C21 -179.0(3) . . . . ?
C17 C18 C19 C20 0.6(5) . . . . ?
C21 C18 C19 C20 179.0(3) . . . . ?
C18 C19 C20 N3 1.1(5) . . . . ?
C19 C18 C21 C22 164.8(3) . . . . ?
C17 C18 C21 C22 -17.0(5) . . . . ?
C18 C21 C22 C23 175.6(3) . . . . ?
C21 C22 C23 C24 133.9(4) . . . . ?
C21 C22 C23 C27 -40.1(5) . . . . ?
C27 C23 C24 C25 -9.7(6) . . . . ?
C22 C23 C24 C25 175.7(3) . . . . ?
C23 C24 C25 N4 -1.1(6) . . . . ?
C24 C23 C27 C26 10.2(6) . . . . ?
C22 C23 C27 C26 -175.6(4) . . . . ?
N4 C26 C27 C23 1.1(7) . . . . ?
N2 C8 N1 C5 -4.1(5) . . . . ?
S1 C8 N1 C5 179.4(3) . . . . ?
C6 C5 N1 C8 -40.6(5) . . . . ?
C4 C5 N1 C8 142.0(3) . . . . ?
N1 C8 N2 C9 166.3(3) . . . . ?
S1 C8 N2 C9 -17.4(5) . . . . ?
C10 C9 N2 C8 -24.8(4) . . . . ?
C14 C9 N2 C8 158.2(3) . . . . ?
C19 C20 N3 C16 -2.5(5) . . . . ?
C19 C20 N3 Co1 176.9(3) . . . . ?
C17 C16 N3 C20 2.4(5) . . . . ?
C17 C16 N3 Co1 -177.1(3) . . . . ?
O2 Co1 N3 C20 121.4(2) . . . . ?
O1 Co1 N3 C20 20.1(3) 7_556 . . . ?
O3 Co1 N3 C20 -137.8(3) 2 . . . ?
O4 Co1 N3 C20 -77.8(2) 2 . . . ?
C15 Co1 N3 C20 -108.1(3) 2 . . . ?
O2 Co1 N3 C16 -59.1(2) . . . . ?
O1 Co1 N3 C16 -160.5(2) 7_556 . . . ?
O3 Co1 N3 C16 41.6(2) 2 . . . ?
O4 Co1 N3 C16 101.6(2) 2 . . . ?
C15 Co1 N3 C16 71.3(2) 2 . . . ?
C27 C26 N4 C25 -11.9(6) . . . . ?
C27 C26 N4 Co1 179.9(3) . . . 1_565 ?
C24 C25 N4 C26 11.8(5) . . . . ?
C24 C25 N4 Co1 -179.8(3) . . . 1_565 ?
O2 C1 O1 Co1 6.0(4) . . . 7_556 ?
C2 C1 O1 Co1 -173.32(19) . . . 7_556 ?
O1 C1 O2 Co1 -95.0(4) . . . . ?
C2 C1 O2 Co1 84.3(4) . . . . ?
O1 Co1 O2 C1 99.8(3) 7_556 . . . ?
N4 Co1 O2 C1 -172.7(3) 1_545 . . . ?
O3 Co1 O2 C1 -81.6(3) 2 . . . ?
N3 Co1 O2 C1 5.3(3) . . . . ?
O4 Co1 O2 C1 -82.2(4) 2 . . . ?
C15 Co1 O2 C1 -78.8(3) 2 . . . ?
O4 C15 O3 Co1 8.0(3) . . . 2 ?
C12 C15 O3 Co1 -170.6(2) . . . 2 ?
O3 C15 O4 Co1 -7.7(3) . . . 2 ?
C12 C15 O4 Co1 170.9(2) . . . 2 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.066

data_290402a
_database_code_depnum_ccdc_archive 'CCDC 771360'
#TrackingRef 'sunD.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H20 Co N4 O5 S'
_chemical_formula_weight         547.44

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c '
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   31.561(3)
_cell_length_b                   11.4596(10)
_cell_length_c                   14.6190(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1150(10)
_cell_angle_gamma                90.00
_cell_volume                     5257.3(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    1296
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      21.29

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2248
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8125
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            14145
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5151
_reflns_number_gt                3603
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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^)+(0.04P)^2^+1.22P] 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         5151
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.20032(8) 0.2366(2) 0.58125(18) 0.0207(6) Uani 1 1 d . . .
C2 C 0.15600(8) 0.2042(2) 0.59933(18) 0.0226(5) Uani 1 1 d . . .
C3 C 0.12221(9) 0.2701(3) 0.5620(2) 0.0356(8) Uani 1 1 d . . .
H3 H 0.1272 0.3357 0.5272 0.043 Uiso 1 1 calc R . .
C4 C 0.08061(9) 0.2407(3) 0.5752(3) 0.0427(9) Uani 1 1 d . . .
H4 H 0.0580 0.2878 0.5516 0.051 Uiso 1 1 calc R . .
C5 C 0.07322(9) 0.1420(3) 0.6231(2) 0.0336(7) Uani 1 1 d . . .
C6 C 0.10689(9) 0.0741(3) 0.6622(2) 0.0350(7) Uani 1 1 d . . .
H6 H 0.1016 0.0074 0.6954 0.042 Uiso 1 1 calc R . .
C7 C 0.14758(9) 0.1060(3) 0.6515(2) 0.0300(6) Uani 1 1 d . . .
H7 H 0.1702 0.0620 0.6793 0.036 Uiso 1 1 calc R . .
C8 C -0.00659(10) 0.1079(3) 0.5898(2) 0.0343(7) Uani 1 1 d . . .
C9 C -0.04160(9) 0.1902(3) 0.4436(2) 0.0332(7) Uani 1 1 d . . .
C10 C -0.08032(9) 0.2254(3) 0.4716(2) 0.0391(8) Uani 1 1 d . . .
H10 H -0.0844 0.2274 0.5337 0.047 Uiso 1 1 calc R . .
C11 C -0.11282(9) 0.2573(3) 0.4048(2) 0.0401(8) Uani 1 1 d . . .
H11 H -0.1390 0.2798 0.4228 0.048 Uiso 1 1 calc R . .
C12 C -0.10742(9) 0.2567(2) 0.3123(2) 0.0260(6) Uani 1 1 d . . .
C13 C -0.06899(9) 0.2237(2) 0.2861(2) 0.0301(7) Uani 1 1 d . . .
H13 H -0.0648 0.2246 0.2241 0.036 Uiso 1 1 calc R . .
C14 C -0.03622(9) 0.1891(3) 0.3503(2) 0.0357(7) Uani 1 1 d . . .
H14 H -0.0104 0.1649 0.3313 0.043 Uiso 1 1 calc R . .
C15 C -0.14430(8) 0.2844(2) 0.2415(2) 0.0242(6) Uani 1 1 d . . .
C16 C 0.16849(10) 0.5515(3) 0.3596(3) 0.0477(9) Uani 1 1 d . . .
H16 H 0.1432 0.5098 0.3475 0.057 Uiso 1 1 calc R . .
C17 C 0.16636(10) 0.6698(3) 0.3571(3) 0.0464(9) Uani 1 1 d . . .
H17 H 0.1401 0.7067 0.3443 0.056 Uiso 1 1 calc R . .
C18 C 0.20386(9) 0.7370(2) 0.3740(2) 0.0258(6) Uani 1 1 d . . .
C19 C 0.24138(9) 0.6742(3) 0.3919(2) 0.0344(7) Uani 1 1 d . . .
H19 H 0.2673 0.7132 0.4025 0.041 Uiso 1 1 calc R . .
C20 C 0.24034(9) 0.5563(3) 0.3941(2) 0.0342(7) Uani 1 1 d . . .
H20 H 0.2661 0.5174 0.4073 0.041 Uiso 1 1 calc R . .
C21 C 0.20354(10) 0.8669(2) 0.3727(2) 0.0266(6) Uani 1 1 d . . .
C22 C 0.16988(9) 0.9288(2) 0.4034(2) 0.0287(6) Uani 1 1 d . . .
H22 H 0.1468 0.8901 0.4242 0.034 Uiso 1 1 calc R . .
C23 C 0.17159(9) 1.0505(2) 0.4022(2) 0.0274(6) Uani 1 1 d . . .
H23 H 0.1489 1.0915 0.4223 0.033 Uiso 1 1 calc R . .
C24 C 0.23527(9) 1.0485(2) 0.34451(19) 0.0247(6) Uani 1 1 d . . .
H24 H 0.2580 1.0883 0.3232 0.030 Uiso 1 1 calc R . .
C25 C 0.23619(9) 0.9280(2) 0.3436(2) 0.0278(6) Uani 1 1 d . . .
H25 H 0.2592 0.8891 0.3230 0.033 Uiso 1 1 calc R . .
Co1 Co 0.205870(11) 0.30070(3) 0.37984(3) 0.01946(10) Uani 1 1 d . . .
N1 N -0.00670(8) 0.1565(3) 0.50642(19) 0.0426(7) Uani 1 1 d . . .
H1A H 0.0082 0.1067 0.4747 0.051 Uiso 1 1 d R . .
N2 N 0.03169(7) 0.1036(3) 0.64118(18) 0.0413(7) Uani 1 1 d . . .
H2B H 0.0273 0.1398 0.6940 0.050 Uiso 1 1 d R . .
N3 N 0.20492(8) 0.4907(2) 0.37867(18) 0.0292(5) Uani 1 1 d . . .
N4 N 0.20370(7) 1.11183(18) 0.37426(17) 0.0264(5) Uani 1 1 d . . .
O1 O -0.13808(5) 0.29184(16) 0.15901(13) 0.0254(4) Uani 1 1 d . . .
O2 O -0.18108(6) 0.29659(19) 0.26638(13) 0.0309(5) Uani 1 1 d . . .
O3 O 0.23059(6) 0.19129(16) 0.63387(13) 0.0259(4) Uani 1 1 d . . .
O4 O 0.20529(6) 0.30767(16) 0.51704(12) 0.0239(4) Uani 1 1 d . . .
O1W O 1.03227(13) 0.4993(5) 0.6749(3) 0.0489(13) Uani 0.50 1 d P . .
H1WD H 1.0054 0.4908 0.6719 0.059 Uiso 0.50 1 d PR . .
H1WC H 1.0441 0.4327 0.6748 0.073 Uiso 0.50 1 d PR . .
O2W O 0.95951(13) 0.4991(3) 0.5711(3) 0.0360(10) Uani 0.50 1 d P . .
H2WA H 0.9638 0.5136 0.5159 0.054 Uiso 0.50 1 d PR . .
H2WC H 0.9433 0.5509 0.5900 0.054 Uiso 0.50 1 d PR . .
S1 S -0.04932(2) 0.05037(8) 0.63261(6) 0.0408(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0210(13) 0.0187(13) 0.0229(14) -0.0073(10) 0.0047(11) 0.0006(10)
C2 0.0182(12) 0.0241(13) 0.0263(14) 0.0003(12) 0.0051(10) -0.0013(11)
C3 0.0190(14) 0.0342(18) 0.053(2) 0.0195(14) -0.0004(13) 0.0026(12)
C4 0.0127(14) 0.050(2) 0.066(2) 0.0275(17) 0.0057(14) 0.0005(13)
C5 0.0188(14) 0.0520(19) 0.0303(16) 0.0077(15) 0.0046(12) -0.0023(14)
C6 0.0266(15) 0.0372(17) 0.0410(19) 0.0135(14) 0.0028(13) 0.0011(13)
C7 0.0223(14) 0.0346(16) 0.0317(16) 0.0066(13) -0.0031(12) -0.0024(12)
C8 0.0278(16) 0.050(2) 0.0247(15) 0.0093(13) 0.0012(12) 0.0059(14)
C9 0.0217(14) 0.0446(18) 0.0323(16) 0.0129(15) -0.0010(12) 0.0066(13)
C10 0.0259(16) 0.070(2) 0.0221(15) 0.0056(15) 0.0042(12) 0.0028(15)
C11 0.0192(15) 0.065(2) 0.0380(18) 0.0010(16) 0.0112(13) 0.0096(15)
C12 0.0217(14) 0.0251(14) 0.0298(15) 0.0046(12) -0.0033(11) 0.0063(11)
C13 0.0294(15) 0.0309(17) 0.0297(16) 0.0108(12) 0.0014(12) 0.0013(12)
C14 0.0250(15) 0.0498(19) 0.0322(16) 0.0158(15) 0.0021(12) 0.0125(14)
C15 0.0175(14) 0.0195(14) 0.0347(16) 0.0002(11) -0.0006(11) -0.0016(11)
C16 0.0255(16) 0.0168(14) 0.100(3) 0.0004(17) 0.0022(18) 0.0016(12)
C17 0.0274(17) 0.0242(16) 0.084(3) -0.0044(16) -0.0123(17) 0.0010(13)
C18 0.0295(15) 0.0213(14) 0.0266(14) 0.0035(12) 0.0028(12) 0.0004(12)
C19 0.0221(15) 0.0292(17) 0.050(2) -0.0118(13) -0.0055(13) -0.0048(12)
C20 0.0239(15) 0.0235(15) 0.053(2) -0.0042(14) -0.0061(13) 0.0077(12)
C21 0.0416(17) 0.0143(13) 0.0244(14) 0.0001(11) 0.0058(12) -0.0015(12)
C22 0.0222(14) 0.0181(14) 0.0471(19) 0.0069(12) 0.0094(13) -0.0016(11)
C23 0.0235(14) 0.0195(13) 0.0396(17) -0.0045(12) 0.0049(12) -0.0024(11)
C24 0.0284(15) 0.0183(13) 0.0279(15) -0.0021(11) 0.0061(12) -0.0052(11)
C25 0.0263(15) 0.0160(14) 0.0407(18) -0.0071(12) 0.0025(12) 0.0000(11)
Co1 0.01706(18) 0.01552(17) 0.02503(19) 0.00055(15) -0.00139(13) -0.00189(15)
N1 0.0167(12) 0.075(2) 0.0355(15) 0.0128(14) 0.0009(10) 0.0019(13)
N2 0.0102(11) 0.080(2) 0.0327(15) 0.0232(14) 0.0004(10) 0.0012(13)
N3 0.0274(13) 0.0208(12) 0.0389(14) -0.0003(11) 0.0013(10) 0.0049(10)
N4 0.0261(13) 0.0141(11) 0.0376(14) 0.0041(10) -0.0032(11) -0.0016(9)
O1 0.0152(9) 0.0279(10) 0.0324(11) 0.0044(9) -0.0012(8) 0.0000(8)
O2 0.0154(9) 0.0435(12) 0.0323(11) 0.0038(10) -0.0042(8) 0.0050(9)
O3 0.0185(9) 0.0238(10) 0.0347(11) 0.0107(9) -0.0004(8) -0.0017(8)
O4 0.0269(10) 0.0233(9) 0.0207(9) 0.0016(8) -0.0008(7) -0.0021(8)
O1W 0.021(2) 0.090(4) 0.034(3) 0.016(2) -0.0046(18) -0.004(2)
O2W 0.039(2) 0.022(2) 0.049(3) 0.0049(19) 0.018(2) -0.0070(19)
S1 0.0179(4) 0.0694(6) 0.0344(4) 0.0115(4) -0.0001(3) -0.0045(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O4 1.265(3) . ?
C1 O3 1.272(3) . ?
C1 C2 1.498(3) . ?
C2 C3 1.372(4) . ?
C2 C7 1.400(4) . ?
C3 C4 1.389(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.363(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(4) . ?
C5 N2 1.434(3) . ?
C6 C7 1.360(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.340(4) . ?
C8 N2 1.354(4) . ?
C8 S1 1.681(3) . ?
C9 C10 1.389(4) . ?
C9 C14 1.391(4) . ?
C9 N1 1.411(4) . ?
C10 C11 1.388(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.364(4) . ?
C12 C15 1.507(4) . ?
C13 C14 1.379(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O1 1.245(3) . ?
C15 O2 1.261(3) . ?
C15 Co1 2.494(3) 2 ?
C16 N3 1.348(4) . ?
C16 C17 1.358(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.412(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(4) . ?
C18 C21 1.488(3) . ?
C19 C20 1.352(4) . ?
C19 H19 0.9300 . ?
C20 N3 1.346(4) . ?
C20 H20 0.9300 . ?
C21 C25 1.352(4) . ?
C21 C22 1.391(4) . ?
C22 C23 1.396(4) . ?
C22 H22 0.9300 . ?
C23 N4 1.333(3) . ?
C23 H23 0.9300 . ?
C24 N4 1.342(3) . ?
C24 C25 1.381(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
Co1 O4 2.0093(18) . ?
Co1 O3 2.0386(18) 7_556 ?
Co1 O1 2.1567(18) 2 ?
Co1 N4 2.167(2) 1_545 ?
Co1 N3 2.177(2) . ?
Co1 O2 2.197(2) 2 ?
Co1 C15 2.494(3) 2 ?
N1 H1A 0.9000 . ?
N2 H2B 0.9000 . ?
N4 Co1 2.167(2) 1_565 ?
O1 Co1 2.1567(17) 2 ?
O2 Co1 2.197(2) 2 ?
O3 Co1 2.0386(18) 7_556 ?
O1W H1WD 0.8500 . ?
O1W H1WC 0.8499 . ?
O2W H2WA 0.8499 . ?
O2W H2WC 0.8500 . ?

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 C1 O3 124.5(2) . . ?
O4 C1 C2 118.8(2) . . ?
O3 C1 C2 116.6(2) . . ?
C3 C2 C7 118.3(3) . . ?
C3 C2 C1 119.6(2) . . ?
C7 C2 C1 122.0(2) . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 N2 124.0(3) . . ?
C6 C5 N2 115.2(3) . . ?
C7 C6 C5 119.4(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C2 121.0(3) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
N1 C8 N2 115.8(3) . . ?
N1 C8 S1 125.3(2) . . ?
N2 C8 S1 118.9(2) . . ?
C10 C9 C14 119.6(3) . . ?
C10 C9 N1 122.5(3) . . ?
C14 C9 N1 117.8(3) . . ?
C11 C10 C9 118.4(3) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C12 C11 C10 121.9(3) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 C15 120.6(3) . . ?
C11 C12 C15 120.3(3) . . ?
C12 C13 C14 120.9(3) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C9 120.2(3) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
O1 C15 O2 121.1(2) . . ?
O1 C15 C12 119.4(2) . . ?
O2 C15 C12 119.5(3) . . ?
O1 C15 Co1 59.84(13) . 2 ?
O2 C15 Co1 61.68(14) . 2 ?
C12 C15 Co1 172.10(19) . 2 ?
N3 C16 C17 124.1(3) . . ?
N3 C16 H16 117.9 . . ?
C17 C16 H16 117.9 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C17 115.6(3) . . ?
C19 C18 C21 121.7(3) . . ?
C17 C18 C21 122.6(3) . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
N3 C20 C19 125.2(3) . . ?
N3 C20 H20 117.4 . . ?
C19 C20 H20 117.4 . . ?
C25 C21 C22 118.1(2) . . ?
C25 C21 C18 121.2(3) . . ?
C22 C21 C18 120.7(2) . . ?
C21 C22 C23 118.3(2) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 H22 120.9 . . ?
N4 C23 C22 124.2(3) . . ?
N4 C23 H23 117.9 . . ?
C22 C23 H23 117.9 . . ?
N4 C24 C25 124.1(2) . . ?
N4 C24 H24 117.9 . . ?
C25 C24 H24 117.9 . . ?
C21 C25 C24 119.8(3) . . ?
C21 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
O4 Co1 O3 102.12(8) . 7_556 ?
O4 Co1 O1 98.65(7) . 2 ?
O3 Co1 O1 159.21(8) 7_556 2 ?
O4 Co1 N4 94.23(9) . 1_545 ?
O3 Co1 N4 93.94(8) 7_556 1_545 ?
O1 Co1 N4 85.21(8) 2 1_545 ?
O4 Co1 N3 88.08(9) . . ?
O3 Co1 N3 88.11(8) 7_556 . ?
O1 Co1 N3 91.87(8) 2 . ?
N4 Co1 N3 176.52(9) 1_545 . ?
O4 Co1 O2 158.72(7) . 2 ?
O3 Co1 O2 99.06(7) 7_556 2 ?
O1 Co1 O2 60.15(7) 2 2 ?
N4 Co1 O2 86.30(9) 1_545 2 ?
N3 Co1 O2 90.61(9) . 2 ?
O4 Co1 C15 128.57(8) . 2 ?
O3 Co1 C15 129.31(8) 7_556 2 ?
O1 Co1 C15 29.94(8) 2 2 ?
N4 Co1 C15 83.07(9) 1_545 2 ?
N3 Co1 C15 93.45(9) . 2 ?
O2 Co1 C15 30.34(8) 2 2 ?
C8 N1 C9 129.2(3) . . ?
C8 N1 H1A 104.7 . . ?
C9 N1 H1A 104.7 . . ?
C8 N2 C5 131.7(3) . . ?
C8 N2 H2B 104.4 . . ?
C5 N2 H2B 104.2 . . ?
C20 N3 C16 114.9(2) . . ?
C20 N3 Co1 123.13(19) . . ?
C16 N3 Co1 122.0(2) . . ?
C23 N4 C24 115.4(2) . . ?
C23 N4 Co1 122.48(18) . 1_565 ?
C24 N4 Co1 122.06(18) . 1_565 ?
C15 O1 Co1 90.22(15) . 2 ?
C15 O2 Co1 87.98(17) . 2 ?
C1 O3 Co1 127.28(17) . 7_556 ?
C1 O4 Co1 136.88(18) . . ?
H1WD O1W H1WC 109.5 . . ?
H2WA O2W H2WC 109.5 . . ?

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
O4 C1 C2 C3 -14.9(4) . . . . ?
O3 C1 C2 C3 163.7(3) . . . . ?
O4 C1 C2 C7 163.3(3) . . . . ?
O3 C1 C2 C7 -18.1(4) . . . . ?
C7 C2 C3 C4 -0.1(5) . . . . ?
C1 C2 C3 C4 178.1(3) . . . . ?
C2 C3 C4 C5 -2.6(6) . . . . ?
C3 C4 C5 C6 3.0(5) . . . . ?
C3 C4 C5 N2 179.6(3) . . . . ?
C4 C5 C6 C7 -0.8(5) . . . . ?
N2 C5 C6 C7 -177.7(3) . . . . ?
C5 C6 C7 C2 -2.0(5) . . . . ?
C3 C2 C7 C6 2.4(5) . . . . ?
C1 C2 C7 C6 -175.8(3) . . . . ?
C14 C9 C10 C11 0.7(5) . . . . ?
N1 C9 C10 C11 179.8(3) . . . . ?
C9 C10 C11 C12 -1.0(5) . . . . ?
C10 C11 C12 C13 0.0(5) . . . . ?
C10 C11 C12 C15 176.0(3) . . . . ?
C11 C12 C13 C14 1.3(5) . . . . ?
C15 C12 C13 C14 -174.6(3) . . . . ?
C12 C13 C14 C9 -1.7(5) . . . . ?
C10 C9 C14 C13 0.6(5) . . . . ?
N1 C9 C14 C13 -178.5(3) . . . . ?
C13 C12 C15 O1 -9.3(4) . . . . ?
C11 C12 C15 O1 174.8(3) . . . . ?
C13 C12 C15 O2 168.8(3) . . . . ?
C11 C12 C15 O2 -7.1(4) . . . . ?
C13 C12 C15 Co1 72.6(15) . . . 2 ?
C11 C12 C15 Co1 -103.3(14) . . . 2 ?
N3 C16 C17 C18 0.8(6) . . . . ?
C16 C17 C18 C19 0.4(5) . . . . ?
C16 C17 C18 C21 -179.7(4) . . . . ?
C17 C18 C19 C20 -1.2(5) . . . . ?
C21 C18 C19 C20 178.8(3) . . . . ?
C18 C19 C20 N3 1.0(5) . . . . ?
C19 C18 C21 C25 33.3(5) . . . . ?
C17 C18 C21 C25 -146.6(3) . . . . ?
C19 C18 C21 C22 -145.3(3) . . . . ?
C17 C18 C21 C22 34.8(5) . . . . ?
C25 C21 C22 C23 0.2(5) . . . . ?
C18 C21 C22 C23 178.9(3) . . . . ?
C21 C22 C23 N4 -0.7(5) . . . . ?
C22 C21 C25 C24 -0.4(5) . . . . ?
C18 C21 C25 C24 -179.0(3) . . . . ?
N4 C24 C25 C21 1.0(5) . . . . ?
N2 C8 N1 C9 -168.9(3) . . . . ?
S1 C8 N1 C9 12.7(6) . . . . ?
C10 C9 N1 C8 29.2(6) . . . . ?
C14 C9 N1 C8 -151.7(4) . . . . ?
N1 C8 N2 C5 -0.1(6) . . . . ?
S1 C8 N2 C5 178.4(3) . . . . ?
C4 C5 N2 C8 36.7(6) . . . . ?
C6 C5 N2 C8 -146.5(4) . . . . ?
C19 C20 N3 C16 0.2(5) . . . . ?
C19 C20 N3 Co1 178.4(3) . . . . ?
C17 C16 N3 C20 -1.1(6) . . . . ?
C17 C16 N3 Co1 -179.3(3) . . . . ?
O4 Co1 N3 C20 84.8(2) . . . . ?
O3 Co1 N3 C20 -17.4(2) 7_556 . . . ?
O1 Co1 N3 C20 -176.6(2) 2 . . . ?
N4 Co1 N3 C20 -143.6(14) 1_545 . . . ?
O2 Co1 N3 C20 -116.4(2) 2 . . . ?
C15 Co1 N3 C20 -146.6(2) 2 . . . ?
O4 Co1 N3 C16 -97.1(3) . . . . ?
O3 Co1 N3 C16 160.7(3) 7_556 . . . ?
O1 Co1 N3 C16 1.5(3) 2 . . . ?
N4 Co1 N3 C16 34.4(16) 1_545 . . . ?
O2 Co1 N3 C16 61.6(3) 2 . . . ?
C15 Co1 N3 C16 31.4(3) 2 . . . ?
C22 C23 N4 C24 1.2(4) . . . . ?
C22 C23 N4 Co1 -177.1(2) . . . 1_565 ?
C25 C24 N4 C23 -1.4(4) . . . . ?
C25 C24 N4 Co1 177.0(2) . . . 1_565 ?
O2 C15 O1 Co1 -7.2(3) . . . 2 ?
C12 C15 O1 Co1 171.0(2) . . . 2 ?
O1 C15 O2 Co1 7.0(3) . . . 2 ?
C12 C15 O2 Co1 -171.1(2) . . . 2 ?
O4 C1 O3 Co1 -9.6(4) . . . 7_556 ?
C2 C1 O3 Co1 171.89(17) . . . 7_556 ?
O3 C1 O4 Co1 99.0(3) . . . . ?
C2 C1 O4 Co1 -82.5(3) . . . . ?
O3 Co1 O4 C1 -102.9(3) 7_556 . . . ?
O1 Co1 O4 C1 77.8(3) 2 . . . ?
N4 Co1 O4 C1 -8.0(3) 1_545 . . . ?
N3 Co1 O4 C1 169.4(3) . . . . ?
O2 Co1 O4 C1 82.7(3) 2 . . . ?
C15 Co1 O4 C1 76.5(3) 2 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.072