# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_a
_database_code_depnum_ccdc_archive 'CCDC 870535'
#TrackingRef 'CCDC870535.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H11 Co N2 O8, 3(H2 O)'
_chemical_formula_sum            'C13 H17 Co N2 O11'
_chemical_formula_weight         436.22
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   8.7712(7)
_cell_length_b                   11.9189(9)
_cell_length_c                   16.7270(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.5216(9)
_cell_angle_gamma                90.00
_cell_volume                     1713.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2855
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      25.00
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2'
_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            11967
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3016
_reflns_number_gt                2427
_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^)+(0.0302P)^2^+0.8631P] 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         3016
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0684
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.27687(4) 0.05668(3) 0.853301(19) 0.02244(11) Uani 1 1 d . . .
C1 C 0.1240(3) 0.0500(2) 0.33234(15) 0.0254(6) Uani 1 1 d . . .
C2 C 0.1922(3) 0.06926(19) 0.42218(14) 0.0216(5) Uani 1 1 d . . .
C3 C 0.0940(3) 0.1134(2) 0.46991(15) 0.0281(6) Uani 1 1 d . . .
H3 H -0.0057 0.1359 0.4451 0.034 Uiso 1 1 calc R . .
C4 C 0.1413(3) 0.1245(2) 0.55356(15) 0.0289(6) Uani 1 1 d . . .
H4 H 0.0738 0.1558 0.5838 0.035 Uiso 1 1 calc R . .
C5 C 0.2878(3) 0.0897(2) 0.59283(14) 0.0229(5) Uani 1 1 d . . .
C6 C 0.3889(3) 0.04433(19) 0.54605(14) 0.0210(5) Uani 1 1 d . . .
C7 C 0.3427(3) 0.03704(19) 0.46071(14) 0.0203(5) Uani 1 1 d . . .
C8 C 0.3357(3) 0.1094(2) 0.68395(15) 0.0264(6) Uani 1 1 d . . .
C9 C 0.5396(3) -0.0054(2) 0.58803(14) 0.0219(5) Uani 1 1 d . . .
O5 O 0.5609(2) -0.02709(15) 0.66022(10) 0.0309(4) Uani 1 1 d . . .
C11 C 0.2027(3) 0.0832(2) 1.03044(16) 0.0324(6) Uani 1 1 d . . .
H11 H 0.1037 0.1064 1.0048 0.039 Uiso 1 1 calc R . .
C12 C 0.2399(3) 0.0806(3) 1.11375(17) 0.0409(7) Uani 1 1 d . . .
H12 H 0.1672 0.0999 1.1450 0.049 Uiso 1 1 calc R . .
C13 C 0.3882(3) 0.0486(2) 1.14991(16) 0.0359(7) Uani 1 1 d . . .
H13 H 0.4167 0.0484 1.2065 0.043 Uiso 1 1 calc R . .
C14 C 0.4440(3) 0.0196(2) 1.02472(14) 0.0211(5) Uani 1 1 d . . .
N1 N 0.3054(2) 0.05303(17) 0.98467(12) 0.0239(5) Uani 1 1 d . . .
N2 N 0.4931(2) 0.01763(17) 1.10560(12) 0.0243(5) Uani 1 1 d . . .
O1 O 0.0643(2) 0.13240(15) 0.29104(10) 0.0347(5) Uani 1 1 d . . .
O2 O 0.1205(2) -0.04923(15) 0.30679(11) 0.0356(5) Uani 1 1 d . . .
O3 O 0.4220(2) 0.19091(16) 0.70719(11) 0.0384(5) Uani 1 1 d . . .
O4 O 0.2743(2) 0.04528(15) 0.72879(10) 0.0300(4) Uani 1 1 d . . .
O1W O 0.06047(19) 0.14058(14) 0.83016(10) 0.0312(4) Uani 1 1 d . . .
H1WA H 0.0678 0.2106 0.8214 0.047 Uiso 1 1 d R . .
H1WB H -0.0017 0.1097 0.7903 0.047 Uiso 1 1 d R . .
O2W O 0.3777(2) 0.21365(14) 0.86247(11) 0.0348(5) Uani 1 1 d . . .
H2WA H 0.4059 0.2166 0.8166 0.052 Uiso 1 1 d R . .
H2WB H 0.4571 0.2221 0.9011 0.052 Uiso 1 1 d R . .
O3W O 0.1500(2) -0.08991(14) 0.84465(10) 0.0289(4) Uani 1 1 d . . .
H3WA H 0.0784 -0.0983 0.8020 0.043 Uiso 1 1 d R . .
H3WB H 0.2060 -0.1489 0.8518 0.043 Uiso 1 1 d R . .
O4W O 0.6469(3) 0.2268(2) 0.97267(14) 0.0711(8) Uani 1 1 d . . .
H4WA H 0.6639 0.2591 1.0192 0.107 Uiso 1 1 d R . .
H4WB H 0.7092 0.2506 0.9436 0.107 Uiso 1 1 d R . .
O5W O 0.3150(2) 0.71798(15) 0.86272(11) 0.0408(5) Uani 1 1 d . . .
H5WA H 0.2509 0.6654 0.8454 0.061 Uiso 1 1 d R . .
H5WB H 0.3921 0.7153 0.8389 0.061 Uiso 1 1 d R . .
O6W O 0.2591(3) 0.8158(2) 0.66124(14) 0.0625(7) Uani 1 1 d . . .
H6WA H 0.2639 0.8838 0.6773 0.094 Uiso 1 1 d R . .
H6WB H 0.1887 0.7844 0.6822 0.094 Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.02319(19) 0.0275(2) 0.01478(18) -0.00067(14) -0.00057(13) 0.00142(15)
C1 0.0196(12) 0.0333(15) 0.0214(13) -0.0006(12) -0.0002(10) -0.0032(11)
C2 0.0217(12) 0.0222(13) 0.0190(13) 0.0024(10) -0.0006(10) -0.0033(10)
C3 0.0203(13) 0.0360(15) 0.0259(15) 0.0000(12) -0.0005(11) 0.0015(11)
C4 0.0265(14) 0.0370(16) 0.0237(14) -0.0032(12) 0.0057(11) 0.0040(12)
C5 0.0265(13) 0.0262(13) 0.0153(13) 0.0019(10) 0.0021(11) -0.0020(10)
C6 0.0231(12) 0.0235(13) 0.0153(12) 0.0003(10) 0.0015(10) -0.0010(10)
C7 0.0249(12) 0.0200(13) 0.0147(12) 0.0013(10) 0.0009(10) -0.0022(10)
C8 0.0244(13) 0.0336(15) 0.0200(14) -0.0004(11) 0.0018(11) 0.0060(12)
C9 0.0245(13) 0.0223(13) 0.0173(13) -0.0020(10) -0.0002(10) -0.0031(10)
O5 0.0309(10) 0.0492(12) 0.0115(9) 0.0042(8) 0.0016(7) 0.0078(8)
C11 0.0248(14) 0.0427(17) 0.0295(15) -0.0012(12) 0.0051(12) 0.0062(12)
C12 0.0368(16) 0.060(2) 0.0289(16) -0.0008(14) 0.0142(13) 0.0114(14)
C13 0.0417(17) 0.0487(18) 0.0184(14) 0.0012(12) 0.0083(12) 0.0082(14)
C14 0.0217(13) 0.0230(13) 0.0174(13) -0.0010(10) 0.0007(10) -0.0023(10)
N1 0.0222(11) 0.0283(12) 0.0198(11) -0.0003(9) 0.0008(9) 0.0021(9)
N2 0.0279(11) 0.0301(12) 0.0137(11) -0.0021(9) 0.0012(9) 0.0019(9)
O1 0.0411(11) 0.0314(10) 0.0232(10) 0.0021(8) -0.0137(8) 0.0024(9)
O2 0.0379(11) 0.0314(11) 0.0301(10) -0.0086(8) -0.0112(8) 0.0030(9)
O3 0.0495(12) 0.0424(12) 0.0225(10) -0.0059(9) 0.0056(9) -0.0155(10)
O4 0.0348(10) 0.0387(11) 0.0169(9) -0.0009(8) 0.0058(8) -0.0038(8)
O1W 0.0293(10) 0.0308(10) 0.0288(10) -0.0027(8) -0.0054(8) 0.0049(8)
O2W 0.0423(11) 0.0329(10) 0.0271(10) -0.0037(8) 0.0023(9) -0.0054(9)
O3W 0.0293(10) 0.0276(10) 0.0249(10) 0.0001(8) -0.0061(8) -0.0010(8)
O4W 0.0825(18) 0.0765(18) 0.0461(15) 0.0038(13) -0.0069(13) -0.0333(15)
O5W 0.0381(11) 0.0324(11) 0.0505(13) -0.0070(9) 0.0051(10) 0.0012(9)
O6W 0.0609(15) 0.0662(16) 0.0647(16) -0.0041(13) 0.0230(13) -0.0022(13)
_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 O3W 2.0610(17) . ?
Co1 O2W 2.0621(18) . ?
Co1 O4 2.0827(16) . ?
Co1 O1W 2.1117(17) . ?
Co1 N1 2.162(2) . ?
Co1 N2 2.185(2) 3_657 ?
C1 O1 1.254(3) . ?
C1 O2 1.256(3) . ?
C1 C2 1.520(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.402(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(3) . ?
C5 C8 1.516(3) . ?
C6 C7 1.407(3) . ?
C6 C9 1.490(3) . ?
C7 C9 1.486(3) 3_656 ?
C8 O3 1.245(3) . ?
C8 O4 1.264(3) . ?
C9 O5 1.212(3) . ?
C9 C7 1.486(3) 3_656 ?
C11 N1 1.343(3) . ?
C11 C12 1.367(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.374(4) . ?
C12 H12 0.9300 . ?
C13 N2 1.344(3) . ?
C13 H13 0.9300 . ?
C14 N1 1.326(3) . ?
C14 N2 1.335(3) . ?
C14 C14 1.481(5) 3_657 ?
N2 Co1 2.185(2) 3_657 ?
O1W H1WA 0.8514 . ?
O1W H1WB 0.8555 . ?
O2W H2WA 0.8531 . ?
O2W H2WB 0.8562 . ?
O3W H3WA 0.8565 . ?
O3W H3WB 0.8523 . ?
O4W H4WA 0.8545 . ?
O4W H4WB 0.8492 . ?
O5W H5WA 0.8531 . ?
O5W H5WB 0.8517 . ?
O6W H6WA 0.8518 . ?
O6W H6WB 0.8551 . ?
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
O3W Co1 O2W 172.73(7) . . ?
O3W Co1 O4 88.66(7) . . ?
O2W Co1 O4 93.01(7) . . ?
O3W Co1 O1W 86.31(7) . . ?
O2W Co1 O1W 86.59(7) . . ?
O4 Co1 O1W 91.01(7) . . ?
O3W Co1 N1 90.32(7) . . ?
O2W Co1 N1 88.95(7) . . ?
O4 Co1 N1 172.33(7) . . ?
O1W Co1 N1 96.51(7) . . ?
O3W Co1 N2 97.48(7) . 3_657 ?
O2W Co1 N2 89.37(8) . 3_657 ?
O4 Co1 N2 96.50(7) . 3_657 ?
O1W Co1 N2 171.65(7) . 3_657 ?
N1 Co1 N2 76.09(7) . 3_657 ?
O1 C1 O2 124.8(2) . . ?
O1 C1 C2 117.7(2) . . ?
O2 C1 C2 117.2(2) . . ?
C3 C2 C7 118.3(2) . . ?
C3 C2 C1 117.3(2) . . ?
C7 C2 C1 124.2(2) . . ?
C4 C3 C2 121.5(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 120.9(2) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.7(2) . . ?
C4 C5 C8 118.4(2) . . ?
C6 C5 C8 122.8(2) . . ?
C5 C6 C7 120.3(2) . . ?
C5 C6 C9 119.4(2) . . ?
C7 C6 C9 120.1(2) . . ?
C2 C7 C6 120.2(2) . . ?
C2 C7 C9 120.7(2) . 3_656 ?
C6 C7 C9 118.8(2) . 3_656 ?
O3 C8 O4 126.2(2) . . ?
O3 C8 C5 117.6(2) . . ?
O4 C8 C5 116.0(2) . . ?
O5 C9 C7 120.4(2) . 3_656 ?
O5 C9 C6 120.0(2) . . ?
C7 C9 C6 119.4(2) 3_656 . ?
N1 C11 C12 121.6(2) . . ?
N1 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C13 117.9(3) . . ?
C11 C12 H12 121.1 . . ?
C13 C12 H12 121.1 . . ?
N2 C13 C12 121.7(2) . . ?
N2 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
N1 C14 N2 126.5(2) . . ?
N1 C14 C14 117.1(3) . 3_657 ?
N2 C14 C14 116.4(3) . 3_657 ?
C14 N1 C11 116.4(2) . . ?
C14 N1 Co1 115.34(16) . . ?
C11 N1 Co1 128.27(17) . . ?
C14 N2 C13 115.8(2) . . ?
C14 N2 Co1 114.63(15) . 3_657 ?
C13 N2 Co1 128.98(17) . 3_657 ?
C8 O4 Co1 129.27(16) . . ?
Co1 O1W H1WA 113.5 . . ?
Co1 O1W H1WB 110.4 . . ?
H1WA O1W H1WB 110.3 . . ?
Co1 O2W H2WA 99.6 . . ?
Co1 O2W H2WB 115.8 . . ?
H2WA O2W H2WB 109.7 . . ?
Co1 O3W H3WA 117.0 . . ?
Co1 O3W H3WB 113.6 . . ?
H3WA O3W H3WB 109.1 . . ?
H4WA O4W H4WB 110.9 . . ?
H5WA O5W H5WB 110.2 . . ?
H6WA O6W H6WB 106.3 . . ?
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
O1 C1 C2 C3 56.7(3) . . . . ?
O2 C1 C2 C3 -117.6(3) . . . . ?
O1 C1 C2 C7 -128.7(3) . . . . ?
O2 C1 C2 C7 57.0(3) . . . . ?
C7 C2 C3 C4 -0.7(4) . . . . ?
C1 C2 C3 C4 174.2(2) . . . . ?
C2 C3 C4 C5 -1.3(4) . . . . ?
C3 C4 C5 C6 0.9(4) . . . . ?
C3 C4 C5 C8 177.1(2) . . . . ?
C4 C5 C6 C7 1.5(4) . . . . ?
C8 C5 C6 C7 -174.4(2) . . . . ?
C4 C5 C6 C9 -173.1(2) . . . . ?
C8 C5 C6 C9 11.0(3) . . . . ?
C3 C2 C7 C6 3.2(3) . . . . ?
C1 C2 C7 C6 -171.4(2) . . . . ?
C3 C2 C7 C9 -170.9(2) . . . 3_656 ?
C1 C2 C7 C9 14.6(3) . . . 3_656 ?
C5 C6 C7 C2 -3.6(3) . . . . ?
C9 C6 C7 C2 170.9(2) . . . . ?
C5 C6 C7 C9 170.6(2) . . . 3_656 ?
C9 C6 C7 C9 -14.9(4) . . . 3_656 ?
C4 C5 C8 O3 -100.6(3) . . . . ?
C6 C5 C8 O3 75.4(3) . . . . ?
C4 C5 C8 O4 74.6(3) . . . . ?
C6 C5 C8 O4 -109.5(3) . . . . ?
C5 C6 C9 O5 14.9(3) . . . . ?
C7 C6 C9 O5 -159.7(2) . . . . ?
C5 C6 C9 C7 -170.4(2) . . . 3_656 ?
C7 C6 C9 C7 15.0(4) . . . 3_656 ?
N1 C11 C12 C13 1.6(4) . . . . ?
C11 C12 C13 N2 -1.8(5) . . . . ?
N2 C14 N1 C11 -3.1(4) . . . . ?
C14 C14 N1 C11 176.9(3) 3_657 . . . ?
N2 C14 N1 Co1 175.10(19) . . . . ?
C14 C14 N1 Co1 -4.9(3) 3_657 . . . ?
C12 C11 N1 C14 0.7(4) . . . . ?
C12 C11 N1 Co1 -177.2(2) . . . . ?
O3W Co1 N1 C14 103.16(17) . . . . ?
O2W Co1 N1 C14 -84.07(17) . . . . ?
O4 Co1 N1 C14 20.8(6) . . . . ?
O1W Co1 N1 C14 -170.52(17) . . . . ?
N2 Co1 N1 C14 5.54(16) 3_657 . . . ?
O3W Co1 N1 C11 -78.9(2) . . . . ?
O2W Co1 N1 C11 93.9(2) . . . . ?
O4 Co1 N1 C11 -161.2(5) . . . . ?
O1W Co1 N1 C11 7.4(2) . . . . ?
N2 Co1 N1 C11 -176.5(2) 3_657 . . . ?
N1 C14 N2 C13 2.9(4) . . . . ?
C14 C14 N2 C13 -177.1(3) 3_657 . . . ?
N1 C14 N2 Co1 175.17(19) . . . 3_657 ?
C14 C14 N2 Co1 -4.8(3) 3_657 . . 3_657 ?
C12 C13 N2 C14 -0.2(4) . . . . ?
C12 C13 N2 Co1 -171.3(2) . . . 3_657 ?
O3 C8 O4 Co1 5.4(4) . . . . ?
C5 C8 O4 Co1 -169.25(15) . . . . ?
O3W Co1 O4 C8 -178.7(2) . . . . ?
O2W Co1 O4 C8 8.4(2) . . . . ?
O1W Co1 O4 C8 95.0(2) . . . . ?
N1 Co1 O4 C8 -96.3(6) . . . . ?
N2 Co1 O4 C8 -81.3(2) 3_657 . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O2 0.86 1.89 2.739(2) 172.1 3_556
O3W H3WA O1 0.86 1.84 2.690(2) 173.2 3_556
O2W H2WA O3 0.85 1.89 2.716(2) 163.1 .
O2W H2WB O4W 0.86 1.85 2.694(3) 169.9 .
O1W H1WA O1 0.85 1.94 2.786(2) 173.3 4_566
O5W H5WA O2 0.85 1.83 2.682(3) 177.4 4_566
O3W H3WB O5W 0.85 1.84 2.693(3) 175.8 1_545
O4W H4WA O5W 0.85 1.97 2.786(3) 160.5 3_667
O4W H4WB O6W 0.85 1.99 2.750(3) 148.8 2_646
O5W H5WB O3 0.85 1.96 2.806(3) 172.3 2_656
O6W H6WA O4 0.85 2.10 2.952(3) 174.1 1_565
O6W H6WB O1 0.86 2.55 3.157(3) 128.8 3_566
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.058


data_110919c_0m
_database_code_depnum_ccdc_archive 'CCDC 870536'
#TrackingRef 'CCDC870536.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H11 N2 Ni O8, 3(H2 O)'
_chemical_formula_sum            'C13 H17 N2 Ni O11'
_chemical_formula_weight         436.00
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   8.7430(6)
_cell_length_b                   11.8990(8)
_cell_length_c                   16.6418(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8300(10)
_cell_angle_gamma                90.00
_cell_volume                     1694.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3795
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      26.01
_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2'
_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            12321
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3272
_reflns_number_gt                2716
_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^)+(0.0290P)^2^+1.0900P] 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         3272
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.27997(3) 0.05520(2) 0.854811(15) 0.02084(9) Uani 1 1 d . . .
C1 C 0.1215(2) 0.05304(19) 0.33143(13) 0.0244(5) Uani 1 1 d . . .
C2 C 0.1906(2) 0.07041(17) 0.42232(12) 0.0215(4) Uani 1 1 d . . .
C3 C 0.0923(3) 0.11347(19) 0.47063(13) 0.0279(5) Uani 1 1 d . . .
H3 H -0.0079 0.1365 0.4459 0.033 Uiso 1 1 calc R . .
C4 C 0.1409(3) 0.12272(19) 0.55494(14) 0.0286(5) Uani 1 1 d . . .
H4 H 0.0735 0.1533 0.5856 0.034 Uiso 1 1 calc R . .
C5 C 0.2881(2) 0.08729(18) 0.59449(12) 0.0226(5) Uani 1 1 d . . .
C6 C 0.3888(2) 0.04283(17) 0.54685(12) 0.0200(4) Uani 1 1 d . . .
C7 C 0.3419(2) 0.03788(17) 0.46075(12) 0.0201(4) Uani 1 1 d . . .
C8 C 0.3367(2) 0.10610(19) 0.68625(13) 0.0241(5) Uani 1 1 d . . .
C9 C 0.5399(2) -0.00718(17) 0.58830(12) 0.0212(4) Uani 1 1 d . . .
O5 O 0.56208(17) -0.03122(14) 0.66077(9) 0.0305(4) Uani 1 1 d . . .
C11 C 0.2020(3) 0.0849(2) 1.02935(14) 0.0302(5) Uani 1 1 d . . .
H11 H 0.1026 0.1081 1.0034 0.036 Uiso 1 1 calc R . .
C12 C 0.2409(3) 0.0830(2) 1.11369(15) 0.0375(6) Uani 1 1 d . . .
H12 H 0.1685 0.1031 1.1450 0.045 Uiso 1 1 calc R . .
C13 C 0.3900(3) 0.0505(2) 1.15056(14) 0.0336(6) Uani 1 1 d . . .
H13 H 0.4193 0.0510 1.2075 0.040 Uiso 1 1 calc R . .
C14 C 0.4442(2) 0.01994(17) 1.02468(12) 0.0202(4) Uani 1 1 d . . .
N1 N 0.30489(19) 0.05375(15) 0.98397(10) 0.0224(4) Uani 1 1 d . . .
N2 N 0.4938(2) 0.01825(15) 1.10611(10) 0.0235(4) Uani 1 1 d . . .
O1 O 0.06219(19) 0.13641(13) 0.29070(9) 0.0344(4) Uani 1 1 d . . .
O2 O 0.11845(18) -0.04561(13) 0.30480(10) 0.0344(4) Uani 1 1 d . . .
O3 O 0.4246(2) 0.18700(14) 0.70938(9) 0.0377(4) Uani 1 1 d . . .
O4 O 0.27604(17) 0.04142(13) 0.73127(8) 0.0266(3) Uani 1 1 d . . .
O1W O 0.06695(17) 0.13650(13) 0.83277(9) 0.0292(4) Uani 1 1 d . . .
H1WA H 0.0743 0.2065 0.8241 0.044 Uiso 1 1 d R . .
H1WB H 0.0048 0.1056 0.7929 0.044 Uiso 1 1 d R . .
O2W O 0.37832(18) 0.21143(13) 0.86331(9) 0.0325(4) Uani 1 1 d . . .
H2WA H 0.4065 0.2143 0.8174 0.049 Uiso 1 1 d R . .
H2WB H 0.4577 0.2199 0.9020 0.049 Uiso 1 1 d R . .
O3W O 0.15395(17) -0.09106(12) 0.84699(9) 0.0269(3) Uani 1 1 d . . .
H3WA H 0.0823 -0.0995 0.8044 0.040 Uiso 1 1 d R . .
H3WB H 0.2100 -0.1500 0.8541 0.040 Uiso 1 1 d R . .
O4W O 0.6485(3) 0.22601(19) 0.97439(12) 0.0692(7) Uani 1 1 d . . .
H4WA H 0.6655 0.2583 1.0209 0.104 Uiso 1 1 d R . .
H4WB H 0.7108 0.2498 0.9453 0.104 Uiso 1 1 d R . .
O5W O 0.3148(2) 0.71467(14) 0.86121(10) 0.0403(4) Uani 1 1 d . . .
H5WA H 0.2507 0.6621 0.8439 0.060 Uiso 1 1 d R . .
H5WB H 0.3919 0.7120 0.8373 0.060 Uiso 1 1 d R . .
O6W O 0.2586(2) 0.81271(18) 0.66151(12) 0.0582(5) Uani 1 1 d . . .
H6WA H 0.2634 0.8807 0.6776 0.087 Uiso 1 1 d R . .
H6WB H 0.1952 0.7753 0.6835 0.087 Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02235(15) 0.02485(16) 0.01395(14) -0.00087(11) 0.00055(10) 0.00165(11)
C1 0.0204(10) 0.0320(13) 0.0188(11) -0.0009(10) -0.0005(8) -0.0018(9)
C2 0.0249(10) 0.0207(11) 0.0168(10) 0.0014(9) -0.0007(8) -0.0003(8)
C3 0.0230(11) 0.0349(13) 0.0235(12) 0.0004(10) -0.0005(9) 0.0029(9)
C4 0.0292(12) 0.0344(13) 0.0234(12) -0.0018(10) 0.0081(9) 0.0035(10)
C5 0.0252(11) 0.0254(11) 0.0167(10) 0.0009(9) 0.0032(9) -0.0020(9)
C6 0.0228(10) 0.0216(11) 0.0151(10) 0.0002(8) 0.0027(8) -0.0020(8)
C7 0.0231(10) 0.0204(11) 0.0157(10) 0.0017(8) 0.0016(8) -0.0032(8)
C8 0.0244(11) 0.0298(12) 0.0176(11) 0.0007(9) 0.0031(9) 0.0060(9)
C9 0.0252(11) 0.0209(11) 0.0159(10) -0.0025(8) 0.0008(8) -0.0037(9)
O5 0.0321(8) 0.0462(10) 0.0124(7) 0.0054(7) 0.0024(6) 0.0081(7)
C11 0.0240(11) 0.0392(14) 0.0268(12) -0.0006(10) 0.0038(9) 0.0066(10)
C12 0.0352(13) 0.0539(17) 0.0263(13) -0.0019(12) 0.0134(10) 0.0120(12)
C13 0.0398(13) 0.0451(15) 0.0168(11) -0.0004(11) 0.0077(10) 0.0067(11)
C14 0.0233(10) 0.0207(11) 0.0160(10) -0.0013(8) 0.0026(8) -0.0009(8)
N1 0.0215(9) 0.0265(10) 0.0182(9) -0.0003(8) 0.0021(7) 0.0013(7)
N2 0.0254(9) 0.0304(10) 0.0140(9) -0.0006(8) 0.0019(7) 0.0024(8)
O1 0.0419(9) 0.0300(9) 0.0238(9) 0.0041(7) -0.0111(7) 0.0019(7)
O2 0.0360(9) 0.0308(9) 0.0292(9) -0.0072(7) -0.0101(7) 0.0046(7)
O3 0.0486(10) 0.0412(10) 0.0235(9) -0.0059(8) 0.0081(8) -0.0163(8)
O4 0.0308(8) 0.0342(9) 0.0147(7) -0.0001(7) 0.0046(6) -0.0020(7)
O1W 0.0281(8) 0.0290(9) 0.0267(8) -0.0028(7) -0.0033(7) 0.0036(7)
O2W 0.0395(9) 0.0318(9) 0.0250(8) -0.0042(7) 0.0040(7) -0.0052(7)
O3W 0.0273(8) 0.0266(8) 0.0234(8) -0.0001(7) -0.0025(6) -0.0004(6)
O4W 0.0838(16) 0.0734(15) 0.0416(12) 0.0043(11) -0.0075(11) -0.0339(13)
O5W 0.0381(9) 0.0305(9) 0.0516(11) -0.0073(8) 0.0076(8) 0.0016(7)
O6W 0.0570(12) 0.0634(14) 0.0579(13) -0.0022(11) 0.0203(10) -0.0006(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 O2W 2.0410(15) . ?
Ni1 O3W 2.0496(15) . ?
Ni1 O4 2.0558(14) . ?
Ni1 O1W 2.0637(14) . ?
Ni1 N1 2.1157(17) . ?
Ni1 N2 2.1379(17) 3_657 ?
C1 O1 1.252(3) . ?
C1 O2 1.253(3) . ?
C1 C2 1.523(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.401(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.404(3) . ?
C5 C8 1.516(3) . ?
C6 C7 1.409(3) . ?
C6 C9 1.484(3) . ?
C7 C9 1.487(3) 3_656 ?
C8 O3 1.242(3) . ?
C8 O4 1.264(3) . ?
C9 O5 1.216(2) . ?
C9 C7 1.487(3) 3_656 ?
C11 N1 1.339(3) . ?
C11 C12 1.375(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9300 . ?
C13 N2 1.339(3) . ?
C13 H13 0.9300 . ?
C14 N1 1.329(3) . ?
C14 N2 1.336(3) . ?
C14 C14 1.476(4) 3_657 ?
N2 Ni1 2.1379(17) 3_657 ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8501 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8477 . ?
O5W H5WA 0.8499 . ?
O5W H5WB 0.8501 . ?
O6W H6WA 0.8500 . ?
O6W H6WB 0.8499 . ?
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
O2W Ni1 O3W 172.39(6) . . ?
O2W Ni1 O4 93.58(6) . . ?
O3W Ni1 O4 88.29(6) . . ?
O2W Ni1 O1W 86.41(6) . . ?
O3W Ni1 O1W 86.16(6) . . ?
O4 Ni1 O1W 91.73(6) . . ?
O2W Ni1 N1 89.02(6) . . ?
O3W Ni1 N1 89.98(6) . . ?
O4 Ni1 N1 173.01(6) . . ?
O1W Ni1 N1 94.91(6) . . ?
O2W Ni1 N2 90.05(7) . 3_657 ?
O3W Ni1 N2 97.12(6) . 3_657 ?
O4 Ni1 N2 95.53(6) . 3_657 ?
O1W Ni1 N2 172.11(6) . 3_657 ?
N1 Ni1 N2 77.96(6) . 3_657 ?
O1 C1 O2 125.04(19) . . ?
O1 C1 C2 117.77(19) . . ?
O2 C1 C2 116.98(19) . . ?
C3 C2 C7 118.42(19) . . ?
C3 C2 C1 117.27(18) . . ?
C7 C2 C1 124.12(18) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 121.3(2) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 118.40(19) . . ?
C4 C5 C8 118.38(19) . . ?
C6 C5 C8 123.07(18) . . ?
C5 C6 C7 120.31(18) . . ?
C5 C6 C9 119.39(18) . . ?
C7 C6 C9 120.13(18) . . ?
C2 C7 C6 120.24(19) . . ?
C2 C7 C9 120.95(18) . 3_656 ?
C6 C7 C9 118.59(18) . 3_656 ?
O3 C8 O4 126.59(19) . . ?
O3 C8 C5 117.03(19) . . ?
O4 C8 C5 116.24(19) . . ?
O5 C9 C6 120.07(19) . . ?
O5 C9 C7 119.97(18) . 3_656 ?
C6 C9 C7 119.71(17) . 3_656 ?
N1 C11 C12 121.1(2) . . ?
N1 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 118.2(2) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
N2 C13 C12 121.4(2) . . ?
N2 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
N1 C14 N2 126.50(18) . . ?
N1 C14 C14 117.1(2) . 3_657 ?
N2 C14 C14 116.4(2) . 3_657 ?
C14 N1 C11 116.58(18) . . ?
C14 N1 Ni1 114.40(13) . . ?
C11 N1 Ni1 129.00(14) . . ?
C14 N2 C13 116.12(18) . . ?
C14 N2 Ni1 113.74(13) . 3_657 ?
C13 N2 Ni1 129.68(14) . 3_657 ?
C8 O4 Ni1 128.40(14) . . ?
Ni1 O1W H1WA 113.1 . . ?
Ni1 O1W H1WB 110.2 . . ?
H1WA O1W H1WB 110.5 . . ?
Ni1 O2W H2WA 99.8 . . ?
Ni1 O2W H2WB 115.3 . . ?
H2WA O2W H2WB 109.5 . . ?
Ni1 O3W H3WA 116.6 . . ?
Ni1 O3W H3WB 113.9 . . ?
H3WA O3W H3WB 108.9 . . ?
H4WA O4W H4WB 110.9 . . ?
H5WA O5W H5WB 110.2 . . ?
H6WA O6W H6WB 110.9 . . ?
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 57.0(3) . . . . ?
O2 C1 C2 C3 -118.0(2) . . . . ?
O1 C1 C2 C7 -128.1(2) . . . . ?
O2 C1 C2 C7 57.0(3) . . . . ?
C7 C2 C3 C4 -1.0(3) . . . . ?
C1 C2 C3 C4 174.2(2) . . . . ?
C2 C3 C4 C5 -1.3(3) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C3 C4 C5 C8 176.6(2) . . . . ?
C4 C5 C6 C7 1.9(3) . . . . ?
C8 C5 C6 C7 -173.60(19) . . . . ?
C4 C5 C6 C9 -173.30(19) . . . . ?
C8 C5 C6 C9 11.2(3) . . . . ?
C3 C2 C7 C6 3.7(3) . . . . ?
C1 C2 C7 C6 -171.16(19) . . . . ?
C3 C2 C7 C9 -170.91(19) . . . 3_656 ?
C1 C2 C7 C9 14.2(3) . . . 3_656 ?
C5 C6 C7 C2 -4.2(3) . . . . ?
C9 C6 C7 C2 170.92(19) . . . . ?
C5 C6 C7 C9 170.54(19) . . . 3_656 ?
C9 C6 C7 C9 -14.3(3) . . . 3_656 ?
C4 C5 C8 O3 -101.1(2) . . . . ?
C6 C5 C8 O3 74.4(3) . . . . ?
C4 C5 C8 O4 75.0(3) . . . . ?
C6 C5 C8 O4 -109.6(2) . . . . ?
C5 C6 C9 O5 15.5(3) . . . . ?
C7 C6 C9 O5 -159.6(2) . . . . ?
C5 C6 C9 C7 -170.34(18) . . . 3_656 ?
C7 C6 C9 C7 14.5(3) . . . 3_656 ?
N1 C11 C12 C13 1.4(4) . . . . ?
C11 C12 C13 N2 -2.0(4) . . . . ?
N2 C14 N1 C11 -2.9(3) . . . . ?
C14 C14 N1 C11 177.0(2) 3_657 . . . ?
N2 C14 N1 Ni1 175.31(17) . . . . ?
C14 C14 N1 Ni1 -4.8(3) 3_657 . . . ?
C12 C11 N1 C14 0.9(3) . . . . ?
C12 C11 N1 Ni1 -177.05(18) . . . . ?
O2W Ni1 N1 C14 -84.86(15) . . . . ?
O3W Ni1 N1 C14 102.69(15) . . . . ?
O4 Ni1 N1 C14 27.0(6) . . . . ?
O1W Ni1 N1 C14 -171.17(15) . . . . ?
N2 Ni1 N1 C14 5.41(14) 3_657 . . . ?
O2W Ni1 N1 C11 93.1(2) . . . . ?
O3W Ni1 N1 C11 -79.3(2) . . . . ?
O4 Ni1 N1 C11 -155.0(5) . . . . ?
O1W Ni1 N1 C11 6.8(2) . . . . ?
N2 Ni1 N1 C11 -176.6(2) 3_657 . . . ?
N1 C14 N2 C13 2.4(3) . . . . ?
C14 C14 N2 C13 -177.6(2) 3_657 . . . ?
N1 C14 N2 Ni1 175.33(17) . . . 3_657 ?
C14 C14 N2 Ni1 -4.6(3) 3_657 . . 3_657 ?
C12 C13 N2 C14 0.2(3) . . . . ?
C12 C13 N2 Ni1 -171.39(19) . . . 3_657 ?
O3 C8 O4 Ni1 7.2(3) . . . . ?
C5 C8 O4 Ni1 -168.42(13) . . . . ?
O2W Ni1 O4 C8 8.13(17) . . . . ?
O3W Ni1 O4 C8 -179.25(17) . . . . ?
O1W Ni1 O4 C8 94.65(17) . . . . ?
N1 Ni1 O4 C8 -103.5(5) . . . . ?
N2 Ni1 O4 C8 -82.27(18) 3_657 . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O2 0.85 1.90 2.742(2) 172.6 3_556
O3W H3WA O1 0.85 1.86 2.709(2) 172.3 3_556
O2W H2WA O3 0.85 1.87 2.690(2) 163.0 .
O2W H2WB O4W 0.85 1.85 2.690(3) 170.3 .
O1W H1WA O1 0.85 1.95 2.790(2) 171.1 4_566
O5W H5WA O2 0.85 1.84 2.686(2) 177.6 4_566
O3W H3WB O5W 0.85 1.84 2.691(2) 173.7 1_545
O4W H4WA O5W 0.85 1.96 2.780(3) 161.6 3_667
O4W H4WB O6W 0.85 2.00 2.755(3) 148.5 2_646
O5W H5WB O3 0.85 1.94 2.789(2) 172.3 2_656
O6W H6WA O4 0.85 2.10 2.950(3) 173.3 1_565
O6W H6WB O1 0.85 2.60 3.127(3) 121.5 3_566
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.055


data_1
_database_code_depnum_ccdc_archive 'CCDC 903428'
#TrackingRef '14296_web_deposit_cif_file_0_WeihongYan_1348726269.Co.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H16 Co2 O16, 6(H2 O)'
_chemical_formula_sum            'C18 H28 Co2 O22'
_chemical_formula_weight         714.26
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   10.5379(12)
_cell_length_b                   32.858(4)
_cell_length_c                   7.9030(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6070(10)
_cell_angle_gamma                90.00
_cell_volume                     2698.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5
_exptl_crystal_description       block
_exptl_crystal_colour            .pink'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(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            21199
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5268
_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^)+(0.0436P)^2^+6.7639P] 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         5268
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1292
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
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 -0.48049(4) 0.749817(13) -0.05326(6) 0.00896(14) Uani 1 1 d . . .
Co2 Co 0.5000 0.5000 0.5000 0.00978(17) Uani 1 2 d S . .
Co3 Co 0.5000 0.5000 1.0000 0.01025(17) Uani 1 2 d S . .
C1 C -0.1028(3) 0.70106(10) 0.0924(4) 0.0112(7) Uani 1 1 d . . .
C2 C -0.0343(3) 0.73709(10) 0.1296(5) 0.0150(7) Uani 1 1 d . . .
H2 H -0.0699 0.7616 0.0862 0.018 Uiso 1 1 calc R . .
C3 C 0.0862(3) 0.73667(10) 0.2306(5) 0.0149(7) Uani 1 1 d . . .
H3 H 0.1300 0.7611 0.2565 0.018 Uiso 1 1 calc R . .
C4 C 0.1430(3) 0.70029(10) 0.2942(4) 0.0116(7) Uani 1 1 d . . .
C5 C 0.0767(3) 0.66372(10) 0.2533(4) 0.0113(7) Uani 1 1 d . . .
C6 C 0.1414(3) 0.62433(10) 0.2986(4) 0.0113(7) Uani 1 1 d . . .
C7 C 0.0637(3) 0.58634(10) 0.2813(4) 0.0108(7) Uani 1 1 d . . .
C8 C 0.1185(3) 0.54982(10) 0.3485(4) 0.0116(7) Uani 1 1 d . . .
C9 C 0.0483(3) 0.51397(10) 0.3162(5) 0.0163(7) Uani 1 1 d . . .
H9 H 0.0836 0.4895 0.3611 0.020 Uiso 1 1 calc R . .
C10 C -0.0737(3) 0.51430(10) 0.2179(5) 0.0160(7) Uani 1 1 d . . .
H10 H -0.1188 0.4900 0.1963 0.019 Uiso 1 1 calc R . .
C11 C -0.1291(3) 0.55043(10) 0.1514(4) 0.0119(7) Uani 1 1 d . . .
C12 C -0.0614(3) 0.58687(10) 0.1857(4) 0.0117(7) Uani 1 1 d . . .
C13 C -0.1250(3) 0.62616(10) 0.1293(4) 0.0113(7) Uani 1 1 d . . .
C14 C -0.0480(3) 0.66423(10) 0.1556(4) 0.0104(7) Uani 1 1 d . . .
C15 C -0.2339(3) 0.70400(9) -0.0196(4) 0.0099(7) Uani 1 1 d . . .
C16 C 0.2730(3) 0.70258(9) 0.4093(4) 0.0110(7) Uani 1 1 d . . .
C17 C 0.2497(3) 0.54681(10) 0.4588(5) 0.0130(7) Uani 1 1 d . . .
C18 C -0.2582(3) 0.54709(9) 0.0358(4) 0.0121(7) Uani 1 1 d . . .
O1 O 0.2584(2) 0.62229(7) 0.3400(3) 0.0165(5) Uani 1 1 d . . .
O2 O -0.2391(2) 0.62746(7) 0.0712(4) 0.0207(6) Uani 1 1 d . . .
O3 O -0.3224(2) 0.71804(7) 0.0560(3) 0.0133(5) Uani 1 1 d . . .
O4 O -0.2464(2) 0.69549(8) -0.1738(3) 0.0160(5) Uani 1 1 d . . .
O5 O 0.3621(2) 0.71745(7) 0.3374(3) 0.0138(5) Uani 1 1 d . . .
O6 O 0.2848(2) 0.69334(7) 0.5628(3) 0.0157(5) Uani 1 1 d . . .
O7 O 0.2654(2) 0.55941(7) 0.6092(3) 0.0161(5) Uani 1 1 d . . .
O8 O 0.3339(2) 0.52821(7) 0.3889(3) 0.0146(5) Uani 1 1 d . . .
O9 O -0.2658(2) 0.55153(8) -0.1199(3) 0.0201(6) Uani 1 1 d . . .
O10 O -0.3518(2) 0.53595(7) 0.1095(3) 0.0154(5) Uani 1 1 d . . .
O1W O -0.4808(2) 0.77842(7) 0.1963(3) 0.0113(5) Uani 1 1 d . . .
H1C H -0.5453 0.7941 0.1715 0.017 Uiso 1 1 d R . .
H1D H -0.4106 0.7913 0.2263 0.017 Uiso 1 1 d R . .
O2W O -0.3604(2) 0.79493(7) -0.1181(3) 0.0151(5) Uani 1 1 d . . .
H2C H -0.3505 0.7917 -0.2218 0.023 Uiso 1 1 d R . .
H2D H -0.3819 0.8195 -0.1049 0.023 Uiso 1 1 d R . .
O3W O -0.6064(2) 0.70665(7) 0.0123(3) 0.0179(5) Uani 1 1 d . . .
H3C H -0.5989 0.6816 -0.0110 0.027 Uiso 1 1 d R . .
H3D H -0.6229 0.7092 0.1135 0.027 Uiso 1 1 d R . .
O4W O 0.6082(2) 0.54806(7) 0.4247(3) 0.0154(5) Uani 1 1 d . . .
H4C H 0.6755 0.5536 0.4962 0.023 Uiso 1 1 d R . .
H4D H 0.6248 0.5457 0.3235 0.023 Uiso 1 1 d R . .
O5W O 0.4946(2) 0.52865(7) 0.7476(3) 0.0117(5) Uani 1 1 d . . .
H5C H 0.5624 0.5431 0.7685 0.018 Uiso 1 1 d R . .
H5D H 0.4272 0.5430 0.7192 0.018 Uiso 1 1 d R . .
O6W O 0.3663(2) 0.54133(8) 1.0615(3) 0.0185(5) Uani 1 1 d . . .
H6C H 0.3717 0.5666 1.0401 0.028 Uiso 1 1 d R . .
H6D H 0.3536 0.5376 1.1638 0.028 Uiso 1 1 d R . .
O7W O 0.8247(2) 0.57638(8) 0.5991(3) 0.0234(6) Uani 1 1 d . . .
H7C H 0.8513 0.6008 0.5968 0.035 Uiso 1 1 d R . .
H7D H 0.8226 0.5700 0.7028 0.035 Uiso 1 1 d R . .
O8W O 0.3752(3) 0.62214(9) 0.9815(4) 0.0370(8) Uani 1 1 d . . .
H8C H 0.4401 0.6209 0.9309 0.056 Uiso 1 1 d R . .
H8D H 0.3085 0.6219 0.9042 0.056 Uiso 1 1 d R . .
O9W O 0.0963(3) 0.34472(8) 0.3919(4) 0.0298(7) Uani 1 1 d . . .
H9C H 0.1338 0.3308 0.3240 0.045 Uiso 1 1 d R . .
H9F H 0.0219 0.3490 0.3348 0.045 Uiso 1 1 d R . .
O10W O 0.4723(3) 0.36931(9) 0.5760(4) 0.0351(7) Uani 1 1 d . . .
H10C H 0.5540 0.3698 0.5998 0.053 Uiso 1 1 d R . .
H10D H 0.4391 0.3920 0.5960 0.053 Uiso 1 1 d R . .
O11W O 0.8370(3) 0.13240(8) 0.7801(4) 0.0276(7) Uani 1 1 d . . .
H11C H 0.8198 0.1499 0.8520 0.041 Uiso 1 1 d R . .
H11D H 0.8306 0.1084 0.8175 0.041 Uiso 1 1 d R . .
O12W O 0.4485(3) 0.37743(11) 0.2253(5) 0.0483(9) Uani 1 1 d . . .
H12C H 0.4477 0.3729 0.3310 0.073 Uiso 1 1 d R . .
H12D H 0.3952 0.3597 0.1769 0.073 Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0062(2) 0.0075(2) 0.0126(3) 0.00008(17) -0.00040(18) 0.00150(16)
Co2 0.0063(3) 0.0063(3) 0.0158(3) 0.0003(2) -0.0009(3) 0.0016(2)
Co3 0.0062(3) 0.0071(3) 0.0166(4) 0.0005(2) -0.0006(3) -0.0013(2)
C1 0.0097(16) 0.0096(16) 0.0137(16) 0.0010(13) 0.0009(13) 0.0024(12)
C2 0.0154(17) 0.0083(16) 0.0206(19) 0.0027(13) 0.0009(15) 0.0019(13)
C3 0.0141(17) 0.0077(16) 0.0228(19) 0.0016(14) 0.0033(15) -0.0032(13)
C4 0.0083(16) 0.0116(17) 0.0147(17) -0.0002(13) 0.0011(13) -0.0018(12)
C5 0.0085(15) 0.0086(16) 0.0161(17) 0.0011(13) 0.0001(13) -0.0016(12)
C6 0.0086(16) 0.0120(17) 0.0132(17) -0.0010(13) 0.0014(13) -0.0019(12)
C7 0.0078(15) 0.0089(16) 0.0155(17) -0.0001(13) 0.0016(13) 0.0012(12)
C8 0.0079(15) 0.0098(16) 0.0176(17) 0.0000(13) 0.0033(13) 0.0005(12)
C9 0.0160(18) 0.0071(17) 0.025(2) 0.0010(14) 0.0006(15) 0.0015(13)
C10 0.0148(17) 0.0081(17) 0.025(2) 0.0004(14) 0.0033(15) -0.0020(13)
C11 0.0076(15) 0.0118(17) 0.0162(17) -0.0013(13) 0.0019(13) -0.0018(12)
C12 0.0094(16) 0.0097(17) 0.0158(17) -0.0006(13) 0.0020(13) -0.0015(12)
C13 0.0101(17) 0.0097(17) 0.0142(17) 0.0011(13) 0.0020(14) -0.0011(12)
C14 0.0087(15) 0.0079(16) 0.0151(17) -0.0001(13) 0.0030(13) 0.0016(12)
C15 0.0090(16) 0.0047(15) 0.0154(17) 0.0028(12) 0.0005(13) 0.0026(12)
C16 0.0123(17) 0.0031(15) 0.0172(18) -0.0024(12) 0.0012(14) -0.0009(12)
C17 0.0108(16) 0.0059(16) 0.0217(19) 0.0026(13) 0.0013(14) 0.0014(12)
C18 0.0124(17) 0.0027(15) 0.0208(19) -0.0001(13) 0.0011(14) -0.0014(12)
O1 0.0083(12) 0.0125(13) 0.0272(14) 0.0023(10) -0.0015(10) 0.0008(9)
O2 0.0067(12) 0.0128(13) 0.0390(16) 0.0035(11) -0.0071(11) -0.0002(9)
O3 0.0107(12) 0.0143(12) 0.0143(12) 0.0011(10) 0.0002(10) 0.0065(9)
O4 0.0109(12) 0.0235(14) 0.0136(13) -0.0005(10) 0.0018(10) 0.0057(10)
O5 0.0074(11) 0.0142(12) 0.0188(12) -0.0005(10) -0.0006(10) -0.0054(9)
O6 0.0125(12) 0.0155(13) 0.0173(13) 0.0026(10) -0.0030(10) -0.0047(10)
O7 0.0133(12) 0.0147(13) 0.0192(13) -0.0022(10) -0.0006(10) 0.0041(10)
O8 0.0111(12) 0.0134(12) 0.0182(13) 0.0009(10) -0.0004(10) 0.0046(9)
O9 0.0157(13) 0.0249(14) 0.0189(14) -0.0001(11) 0.0004(11) -0.0100(11)
O10 0.0103(12) 0.0182(13) 0.0169(13) -0.0028(10) 0.0003(10) -0.0064(10)
O1W 0.0082(11) 0.0095(12) 0.0154(12) -0.0004(9) 0.0002(9) 0.0007(9)
O2W 0.0180(13) 0.0114(12) 0.0162(12) -0.0013(9) 0.0036(10) -0.0009(9)
O3W 0.0199(13) 0.0127(12) 0.0211(13) -0.0014(10) 0.0039(11) -0.0052(10)
O4W 0.0134(12) 0.0129(12) 0.0189(13) -0.0017(10) 0.0001(10) -0.0025(9)
O5W 0.0079(11) 0.0078(12) 0.0181(12) -0.0003(9) -0.0019(10) -0.0013(8)
O6W 0.0197(13) 0.0187(14) 0.0174(13) 0.0018(10) 0.0039(11) 0.0069(10)
O7W 0.0268(14) 0.0187(14) 0.0244(14) 0.0010(11) 0.0029(12) -0.0039(11)
O8W 0.0403(19) 0.0336(18) 0.0374(18) -0.0010(14) 0.0076(15) 0.0014(14)
O9W 0.0262(15) 0.0231(15) 0.0422(18) -0.0053(13) 0.0124(13) 0.0005(12)
O10W 0.0204(15) 0.0245(16) 0.058(2) -0.0015(14) 0.0005(14) -0.0002(12)
O11W 0.0270(15) 0.0188(15) 0.0398(17) -0.0016(12) 0.0140(13) 0.0013(11)
O12W 0.036(2) 0.064(3) 0.041(2) 0.0019(17) -0.0017(16) -0.0135(16)
_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 2.032(2) . ?
Co1 O5 2.044(2) 4_475 ?
Co1 O3W 2.066(2) . ?
Co1 O2W 2.069(2) . ?
Co1 O1W 2.185(2) . ?
Co1 O1W 2.186(2) 4_575 ?
Co2 O8 2.045(2) 3_666 ?
Co2 O8 2.045(2) . ?
Co2 O4W 2.092(2) . ?
Co2 O4W 2.092(2) 3_666 ?
Co2 O5W 2.181(2) 3_666 ?
Co2 O5W 2.181(2) . ?
Co3 O10 2.033(2) 1_656 ?
Co3 O10 2.033(2) 3_566 ?
Co3 O6W 2.073(2) . ?
Co3 O6W 2.073(2) 3_667 ?
Co3 O5W 2.198(2) 3_667 ?
Co3 O5W 2.198(2) . ?
C1 C2 1.392(5) . ?
C1 C14 1.397(4) . ?
C1 C15 1.515(4) . ?
C2 C3 1.383(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(5) . ?
C4 C16 1.514(5) . ?
C5 C14 1.409(5) . ?
C5 C6 1.479(5) . ?
C6 O1 1.223(4) . ?
C6 C7 1.486(4) . ?
C7 C8 1.397(5) . ?
C7 C12 1.407(5) . ?
C8 C9 1.392(5) . ?
C8 C17 1.509(5) . ?
C9 C10 1.386(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.397(5) . ?
C11 C18 1.511(5) . ?
C12 C13 1.488(4) . ?
C13 O2 1.214(4) . ?
C13 C14 1.487(4) . ?
C15 O4 1.236(4) . ?
C15 O3 1.275(4) . ?
C16 O6 1.237(4) . ?
C16 O5 1.273(4) . ?
C17 O7 1.243(4) . ?
C17 O8 1.277(4) . ?
C18 O9 1.229(4) . ?
C18 O10 1.280(4) . ?
O5 Co1 2.044(2) 4_676 ?
O10 Co3 2.033(2) 1_454 ?
O1W Co1 2.186(2) 4_576 ?
O1W H1C 0.8500 . ?
O1W H1D 0.8500 . ?
O2W H2C 0.8500 . ?
O2W H2D 0.8501 . ?
O3W H3C 0.8500 . ?
O3W H3D 0.8500 . ?
O4W H4C 0.8499 . ?
O4W H4D 0.8499 . ?
O5W H5C 0.8500 . ?
O5W H5D 0.8500 . ?
O6W H6C 0.8500 . ?
O6W H6D 0.8500 . ?
O7W H7C 0.8501 . ?
O7W H7D 0.8500 . ?
O8W H8C 0.8497 . ?
O8W H8D 0.8505 . ?
O9W H9C 0.8501 . ?
O9W H9F 0.8483 . ?
O10W H10C 0.8503 . ?
O10W H10D 0.8500 . ?
O11W H11C 0.8500 . ?
O11W H11D 0.8500 . ?
O12W H12C 0.8501 . ?
O12W H12D 0.8546 . ?
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 O5 179.16(10) . 4_475 ?
O3 Co1 O3W 93.20(10) . . ?
O5 Co1 O3W 87.56(10) 4_475 . ?
O3 Co1 O2W 88.93(10) . . ?
O5 Co1 O2W 90.30(10) 4_475 . ?
O3W Co1 O2W 177.54(10) . . ?
O3 Co1 O1W 87.83(9) . . ?
O5 Co1 O1W 91.83(9) 4_475 . ?
O3W Co1 O1W 88.35(9) . . ?
O2W Co1 O1W 90.50(9) . . ?
O3 Co1 O1W 92.50(9) . 4_575 ?
O5 Co1 O1W 87.83(9) 4_475 4_575 ?
O3W Co1 O1W 91.83(9) . 4_575 ?
O2W Co1 O1W 89.31(9) . 4_575 ?
O1W Co1 O1W 179.61(7) . 4_575 ?
O8 Co2 O8 180.00(13) 3_666 . ?
O8 Co2 O4W 89.78(9) 3_666 . ?
O8 Co2 O4W 90.22(9) . . ?
O8 Co2 O4W 90.22(9) 3_666 3_666 ?
O8 Co2 O4W 89.78(9) . 3_666 ?
O4W Co2 O4W 180.0 . 3_666 ?
O8 Co2 O5W 92.34(9) 3_666 3_666 ?
O8 Co2 O5W 87.66(9) . 3_666 ?
O4W Co2 O5W 88.49(9) . 3_666 ?
O4W Co2 O5W 91.50(9) 3_666 3_666 ?
O8 Co2 O5W 87.66(9) 3_666 . ?
O8 Co2 O5W 92.34(9) . . ?
O4W Co2 O5W 91.51(9) . . ?
O4W Co2 O5W 88.50(9) 3_666 . ?
O5W Co2 O5W 180.000(1) 3_666 . ?
O10 Co3 O10 180.0 1_656 3_566 ?
O10 Co3 O6W 91.35(10) 1_656 . ?
O10 Co3 O6W 88.65(10) 3_566 . ?
O10 Co3 O6W 88.65(10) 1_656 3_667 ?
O10 Co3 O6W 91.35(10) 3_566 3_667 ?
O6W Co3 O6W 179.999(2) . 3_667 ?
O10 Co3 O5W 87.76(9) 1_656 3_667 ?
O10 Co3 O5W 92.24(9) 3_566 3_667 ?
O6W Co3 O5W 89.04(9) . 3_667 ?
O6W Co3 O5W 90.96(9) 3_667 3_667 ?
O10 Co3 O5W 92.24(9) 1_656 . ?
O10 Co3 O5W 87.76(9) 3_566 . ?
O6W Co3 O5W 90.96(9) . . ?
O6W Co3 O5W 89.04(9) 3_667 . ?
O5W Co3 O5W 180.0 3_667 . ?
C2 C1 C14 119.5(3) . . ?
C2 C1 C15 117.3(3) . . ?
C14 C1 C15 123.1(3) . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 C16 117.7(3) . . ?
C5 C4 C16 123.2(3) . . ?
C4 C5 C14 120.0(3) . . ?
C4 C5 C6 120.2(3) . . ?
C14 C5 C6 119.6(3) . . ?
O1 C6 C5 121.0(3) . . ?
O1 C6 C7 119.6(3) . . ?
C5 C6 C7 119.2(3) . . ?
C8 C7 C12 120.4(3) . . ?
C8 C7 C6 120.0(3) . . ?
C12 C7 C6 119.4(3) . . ?
C9 C8 C7 119.0(3) . . ?
C9 C8 C17 117.2(3) . . ?
C7 C8 C17 123.8(3) . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.8(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 C18 116.5(3) . . ?
C12 C11 C18 124.0(3) . . ?
C11 C12 C7 119.8(3) . . ?
C11 C12 C13 119.7(3) . . ?
C7 C12 C13 120.4(3) . . ?
O2 C13 C14 120.4(3) . . ?
O2 C13 C12 120.8(3) . . ?
C14 C13 C12 118.7(3) . . ?
C1 C14 C5 119.9(3) . . ?
C1 C14 C13 119.7(3) . . ?
C5 C14 C13 120.3(3) . . ?
O4 C15 O3 125.3(3) . . ?
O4 C15 C1 119.9(3) . . ?
O3 C15 C1 114.6(3) . . ?
O6 C16 O5 124.8(3) . . ?
O6 C16 C4 120.6(3) . . ?
O5 C16 C4 114.3(3) . . ?
O7 C17 O8 125.6(3) . . ?
O7 C17 C8 119.6(3) . . ?
O8 C17 C8 114.7(3) . . ?
O9 C18 O10 124.3(3) . . ?
O9 C18 C11 119.9(3) . . ?
O10 C18 C11 115.5(3) . . ?
C15 O3 Co1 126.8(2) . . ?
C16 O5 Co1 128.4(2) . 4_676 ?
C17 O8 Co2 129.7(2) . . ?
C18 O10 Co3 124.6(2) . 1_454 ?
Co1 O1W Co1 129.41(11) . 4_576 ?
Co1 O1W H1C 100.0 . . ?
Co1 O1W H1C 110.3 4_576 . ?
Co1 O1W H1D 109.5 . . ?
Co1 O1W H1D 95.1 4_576 . ?
H1C O1W H1D 112.8 . . ?
Co1 O2W H2C 109.1 . . ?
Co1 O2W H2D 117.6 . . ?
H2C O2W H2D 108.5 . . ?
Co1 O3W H3C 121.6 . . ?
Co1 O3W H3D 114.2 . . ?
H3C O3W H3D 109.9 . . ?
Co2 O4W H4C 114.1 . . ?
Co2 O4W H4D 113.9 . . ?
H4C O4W H4D 111.4 . . ?
Co2 O5W Co3 128.96(11) . . ?
Co2 O5W H5C 105.5 . . ?
Co3 O5W H5C 99.7 . . ?
Co2 O5W H5D 98.5 . . ?
Co3 O5W H5D 111.7 . . ?
H5C O5W H5D 112.4 . . ?
Co3 O6W H6C 121.5 . . ?
Co3 O6W H6D 110.4 . . ?
H6C O6W H6D 110.9 . . ?
H7C O7W H7D 108.3 . . ?
H8C O8W H8D 107.2 . . ?
H9C O9W H9F 103.8 . . ?
H10C O10W H10D 112.1 . . ?
H11C O11W H11D 111.1 . . ?
H12C O12W H12D 102.0 . . ?
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
C14 C1 C2 C3 -1.0(5) . . . . ?
C15 C1 C2 C3 -179.8(3) . . . . ?
C1 C2 C3 C4 1.4(6) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C2 C3 C4 C16 -177.8(3) . . . . ?
C3 C4 C5 C14 -2.8(5) . . . . ?
C16 C4 C5 C14 175.4(3) . . . . ?
C3 C4 C5 C6 171.6(3) . . . . ?
C16 C4 C5 C6 -10.2(5) . . . . ?
C4 C5 C6 O1 -14.8(5) . . . . ?
C14 C5 C6 O1 159.7(3) . . . . ?
C4 C5 C6 C7 169.7(3) . . . . ?
C14 C5 C6 C7 -15.8(5) . . . . ?
O1 C6 C7 C8 14.5(5) . . . . ?
C5 C6 C7 C8 -169.9(3) . . . . ?
O1 C6 C7 C12 -160.6(3) . . . . ?
C5 C6 C7 C12 15.0(5) . . . . ?
C12 C7 C8 C9 1.3(5) . . . . ?
C6 C7 C8 C9 -173.8(3) . . . . ?
C12 C7 C8 C17 -177.2(3) . . . . ?
C6 C7 C8 C17 7.7(5) . . . . ?
C7 C8 C9 C10 0.5(5) . . . . ?
C17 C8 C9 C10 179.1(3) . . . . ?
C8 C9 C10 C11 -0.9(6) . . . . ?
C9 C10 C11 C12 -0.6(5) . . . . ?
C9 C10 C11 C18 175.8(3) . . . . ?
C10 C11 C12 C7 2.4(5) . . . . ?
C18 C11 C12 C7 -173.7(3) . . . . ?
C10 C11 C12 C13 -174.1(3) . . . . ?
C18 C11 C12 C13 9.7(5) . . . . ?
C8 C7 C12 C11 -2.8(5) . . . . ?
C6 C7 C12 C11 172.3(3) . . . . ?
C8 C7 C12 C13 173.7(3) . . . . ?
C6 C7 C12 C13 -11.1(5) . . . . ?
C11 C12 C13 O2 8.3(5) . . . . ?
C7 C12 C13 O2 -168.2(3) . . . . ?
C11 C12 C13 C14 -175.5(3) . . . . ?
C7 C12 C13 C14 8.0(5) . . . . ?
C2 C1 C14 C5 -1.3(5) . . . . ?
C15 C1 C14 C5 177.4(3) . . . . ?
C2 C1 C14 C13 174.7(3) . . . . ?
C15 C1 C14 C13 -6.7(5) . . . . ?
C4 C5 C14 C1 3.2(5) . . . . ?
C6 C5 C14 C1 -171.3(3) . . . . ?
C4 C5 C14 C13 -172.7(3) . . . . ?
C6 C5 C14 C13 12.8(5) . . . . ?
O2 C13 C14 C1 -8.5(5) . . . . ?
C12 C13 C14 C1 175.3(3) . . . . ?
O2 C13 C14 C5 167.4(3) . . . . ?
C12 C13 C14 C5 -8.8(5) . . . . ?
C2 C1 C15 O4 100.3(4) . . . . ?
C14 C1 C15 O4 -78.4(4) . . . . ?
C2 C1 C15 O3 -75.4(4) . . . . ?
C14 C1 C15 O3 106.0(4) . . . . ?
C3 C4 C16 O6 112.7(4) . . . . ?
C5 C4 C16 O6 -65.5(5) . . . . ?
C3 C4 C16 O5 -62.1(4) . . . . ?
C5 C4 C16 O5 119.7(4) . . . . ?
C9 C8 C17 O7 -106.0(4) . . . . ?
C7 C8 C17 O7 72.6(5) . . . . ?
C9 C8 C17 O8 69.1(4) . . . . ?
C7 C8 C17 O8 -112.4(4) . . . . ?
C10 C11 C18 O9 -105.8(4) . . . . ?
C12 C11 C18 O9 70.5(5) . . . . ?
C10 C11 C18 O10 68.1(4) . . . . ?
C12 C11 C18 O10 -115.7(4) . . . . ?
O4 C15 O3 Co1 -24.7(5) . . . . ?
C1 C15 O3 Co1 150.7(2) . . . . ?
O5 Co1 O3 C15 -87(7) 4_475 . . . ?
O3W Co1 O3 C15 118.9(3) . . . . ?
O2W Co1 O3 C15 -62.4(3) . . . . ?
O1W Co1 O3 C15 -152.9(3) . . . . ?
O1W Co1 O3 C15 26.9(3) 4_575 . . . ?
O6 C16 O5 Co1 -25.4(5) . . . 4_676 ?
C4 C16 O5 Co1 149.2(2) . . . 4_676 ?
O7 C17 O8 Co2 17.0(5) . . . . ?
C8 C17 O8 Co2 -157.7(2) . . . . ?
O8 Co2 O8 C17 91(7) 3_666 . . . ?
O4W Co2 O8 C17 -105.9(3) . . . . ?
O4W Co2 O8 C17 74.1(3) 3_666 . . . ?
O5W Co2 O8 C17 165.6(3) 3_666 . . . ?
O5W Co2 O8 C17 -14.4(3) . . . . ?
O9 C18 O10 Co3 29.0(5) . . . 1_454 ?
C11 C18 O10 Co3 -144.6(2) . . . 1_454 ?
O3 Co1 O1W Co1 -53.81(14) . . . 4_576 ?
O5 Co1 O1W Co1 126.96(14) 4_475 . . 4_576 ?
O3W Co1 O1W Co1 39.45(14) . . . 4_576 ?
O2W Co1 O1W Co1 -142.72(14) . . . 4_576 ?
O1W Co1 O1W Co1 157(17) 4_575 . . 4_576 ?
O8 Co2 O5W Co3 -54.73(13) 3_666 . . . ?
O8 Co2 O5W Co3 125.27(13) . . . . ?
O4W Co2 O5W Co3 -144.44(13) . . . . ?
O4W Co2 O5W Co3 35.55(13) 3_666 . . . ?
O5W Co2 O5W Co3 -175(25) 3_666 . . . ?
O10 Co3 O5W Co2 127.70(14) 1_656 . . . ?
O10 Co3 O5W Co2 -52.30(14) 3_566 . . . ?
O6W Co3 O5W Co2 -140.91(14) . . . . ?
O6W Co3 O5W Co2 39.09(14) 3_667 . . . ?
O5W Co3 O5W Co2 174(35) 3_667 . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.106