# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Xian-Ming Zhang'
'Guo-Xin Wu'
'Hai-Shun Wu'
'Ming-Hua Zeng'

_publ_contact_author_name        'Xian-Ming Zhang'
_publ_contact_author_email       ZHANGXM@DNS.SXNU.EDU.CN

_publ_section_title              
;
A Hybrid Cobalt Hydroxyacetate Magnet: Ionothermal
Synthesis, 3-D Co-O-Co Connectivity and Free Disordered Spin Glass Behavior
;

# Attachment 'B919966G_zhang.cif'

data_sad
_database_code_depnum_ccdc_archive 'CCDC 752623'
#TrackingRef 'B919966G_zhang.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 Co3 O10'
_chemical_formula_weight         446.98

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           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   8.6768(6)
_cell_length_b                   8.6768(6)
_cell_length_c                   17.3688(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1307.64(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892
_exptl_absorpt_coefficient_mu    3.810
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.6578
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3430
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         25.93
_reflns_number_total             628
_reflns_number_gt                586
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0361P)^2^+7.8509P] 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     SHELXL
_refine_ls_extinction_coef       0.0035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         628
_refine_ls_number_parameters     51
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.7500 0.1250 0.0128(3) Uani 1 4 d S . .
Co2 Co 0.5000 0.5000 0.0000 0.0141(3) Uani 1 2 d S . .
O1 O 0.5000 0.7500 0.00743(17) 0.0074(7) Uani 1 2 d S . .
O2 O 0.2772(3) 0.5085(3) 0.03604(15) 0.0204(6) Uani 1 1 d . . .
O3 O 0.2762(3) 0.6696(3) 0.13593(14) 0.0179(6) Uani 1 1 d . . .
C1 C 0.0461(5) 0.5329(6) 0.1067(3) 0.0324(11) Uani 1 1 d . . .
H1A H 0.0098 0.5912 0.1500 0.049 Uiso 1 1 calc R . .
H1B H 0.0375 0.4248 0.1176 0.049 Uiso 1 1 calc R . .
H1C H -0.0150 0.5575 0.0622 0.049 Uiso 1 1 calc R . .
C2 C 0.2110(4) 0.5724(4) 0.0913(2) 0.0167(8) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0135(4) 0.0135(4) 0.0113(5) 0.000 0.000 0.000
Co2 0.0151(4) 0.0151(4) 0.0120(4) -0.0029(2) -0.0002(3) 0.0001(3)
O1 0.0134(17) 0.0066(15) 0.0021(14) 0.000 0.000 0.0003(13)
O2 0.0173(14) 0.0245(14) 0.0195(13) -0.0064(11) 0.0022(11) -0.0012(11)
O3 0.0169(13) 0.0214(14) 0.0156(13) -0.0036(11) 0.0034(10) -0.0030(11)
C1 0.022(2) 0.038(3) 0.037(3) -0.015(2) 0.0051(19) -0.0052(19)
C2 0.0177(19) 0.0159(18) 0.0164(17) -0.0005(14) -0.0007(14) 0.0007(14)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.042(3) 15_565 ?
Co1 O1 2.042(3) . ?
Co1 O3 2.072(3) 6_564 ?
Co1 O3 2.072(3) . ?
Co1 O3 2.072(2) 12_766 ?
Co1 O3 2.072(2) 15_565 ?
Co2 O2 2.034(3) 9_665 ?
Co2 O2 2.034(3) . ?
Co2 O3 2.113(2) 12_766 ?
Co2 O3 2.113(2) 4_454 ?
Co2 O1 2.1730(2) 9_665 ?
Co2 O1 2.1730(2) . ?
O1 Co2 2.1730(2) 6_564 ?
O2 C2 1.248(5) . ?
O3 C2 1.277(5) . ?
O3 Co2 2.113(2) 3 ?
C1 C2 1.496(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 180.0 15_565 . ?
O1 Co1 O3 84.74(7) 15_565 6_564 ?
O1 Co1 O3 95.26(7) . 6_564 ?
O1 Co1 O3 84.74(7) 15_565 . ?
O1 Co1 O3 95.26(7) . . ?
O3 Co1 O3 169.49(14) 6_564 . ?
O1 Co1 O3 95.26(7) 15_565 12_766 ?
O1 Co1 O3 84.74(7) . 12_766 ?
O3 Co1 O3 90.481(13) 6_564 12_766 ?
O3 Co1 O3 90.481(13) . 12_766 ?
O1 Co1 O3 95.26(7) 15_565 15_565 ?
O1 Co1 O3 84.74(7) . 15_565 ?
O3 Co1 O3 90.481(13) 6_564 15_565 ?
O3 Co1 O3 90.481(13) . 15_565 ?
O3 Co1 O3 169.49(14) 12_766 15_565 ?
O2 Co2 O2 180.0(2) 9_665 . ?
O2 Co2 O3 88.77(10) 9_665 12_766 ?
O2 Co2 O3 91.23(10) . 12_766 ?
O2 Co2 O3 91.23(10) 9_665 4_454 ?
O2 Co2 O3 88.77(10) . 4_454 ?
O3 Co2 O3 180.0 12_766 4_454 ?
O2 Co2 O1 86.88(8) 9_665 9_665 ?
O2 Co2 O1 93.12(8) . 9_665 ?
O3 Co2 O1 99.38(10) 12_766 9_665 ?
O3 Co2 O1 80.62(10) 4_454 9_665 ?
O2 Co2 O1 93.12(8) 9_665 . ?
O2 Co2 O1 86.88(8) . . ?
O3 Co2 O1 80.62(10) 12_766 . ?
O3 Co2 O1 99.38(10) 4_454 . ?
O1 Co2 O1 180.00(15) 9_665 . ?
Co1 O1 Co2 93.40(8) . . ?
Co1 O1 Co2 93.40(8) . 6_564 ?
Co2 O1 Co2 173.19(15) . 6_564 ?
C2 O2 Co2 133.6(3) . . ?
C2 O3 Co1 125.5(2) . . ?
C2 O3 Co2 137.7(2) . 3 ?
Co1 O3 Co2 94.32(10) . 3 ?
O2 C2 O3 123.8(4) . . ?
O2 C2 C1 118.4(3) . . ?
O3 C2 C1 117.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.93
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.108
#======================================