# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Hui-Zhong Kou'
'Osamu Sato'
'Jun Tao'

_publ_contact_author_name        'Hui-Zhong Kou'
_publ_contact_author_address     
;
Department of Chemistry
Tsinghua University
Beijing
100084
CHINA
;

_publ_contact_author_email       KOUHZ@MAIL.TSINGHUA.EDU.CN

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Assembly of a two-dimensional oxalate-bridged
heterometallic CoII3CrIII2 antiferromagnet
;

data_3
_database_code_depnum_ccdc_archive 'CCDC 674833'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H48 Co3 Cr2 O36'
_chemical_formula_weight         1193.41

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'
Cr Cr 0.3209 0.6236 '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   C2/c

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                   25.654(5)
_cell_length_b                   14.893(3)
_cell_length_c                   14.821(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.78(3)
_cell_angle_gamma                90.00
_cell_volume                     4706.8(23)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3063
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2436
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_process_details   'ABSCOR; Higashi, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku IP'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 0.66
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7808
_diffrn_reflns_av_R_equivalents  0.1612
_diffrn_reflns_av_sigmaI/netI    0.1521
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4095
_reflns_number_gt                3063
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'crystalstructure 3.6.0 (Rigaku/MSC, 2004)'
_computing_cell_refinement       'crystalstructure 3.6.0 (Rigaku/MSC, 2004)'
_computing_data_reduction        'Crystalstructure 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XP (Sheldrick, 1998)'

_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^)+(0.0100P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00028(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4095
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_ref         0.1570
_refine_ls_wR_factor_gt          0.1471
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.95211(8) 0.2500 0.0403(3) Uani 1 2 d S . .
Co2 Co -0.35101(4) 0.89900(5) -0.45207(6) 0.0402(2) Uani 1 1 d . . .
Cr1 Cr -0.17429(4) 0.75002(6) -0.07574(7) 0.0419(3) Uani 1 1 d . . .
O8 O -0.04764(19) 0.9388(3) 0.0806(3) 0.0440(9) Uani 1 1 d . . .
O2 O -0.3171(2) 0.9013(3) -0.2850(3) 0.0453(10) Uani 1 1 d . . .
O9 O -0.10801(17) 0.6606(3) -0.0329(3) 0.0438(9) Uani 1 1 d . . .
O1 O -0.28356(19) 0.7974(3) -0.3914(3) 0.0442(9) Uani 1 1 d . . .
O13 O -0.3754(2) 0.8908(3) -0.6071(3) 0.0540(11) Uani 1 1 d . . .
O12 O -0.4199(2) 0.8139(3) -0.4839(3) 0.0557(11) Uani 1 1 d . . .
O4 O -0.20709(18) 0.7399(3) -0.2305(3) 0.0445(9) Uani 1 1 d . . .
O7 O -0.1176(2) 0.8496(3) -0.0521(3) 0.0459(10) Uani 1 1 d . . .
O10 O -0.22430(17) 0.6456(3) -0.0891(3) 0.0429(9) Uani 1 1 d . . .
O15 O -0.0611(2) 1.0458(3) 0.2338(4) 0.0542(11) Uani 1 1 d . . .
O11 O -0.13987(18) 0.7703(3) 0.0792(3) 0.0436(9) Uani 1 1 d . . .
O3 O -0.24455(19) 0.8344(3) -0.1305(3) 0.0434(9) Uani 1 1 d . . .
C5 C -0.0862(3) 0.8774(4) 0.0440(4) 0.0389(12) Uani 1 1 d . . .
C2 C -0.2736(3) 0.8469(4) -0.2307(4) 0.0398(13) Uani 1 1 d . . .
C1 C -0.2540(3) 0.7907(4) -0.2913(4) 0.0416(13) Uani 1 1 d . . .
C7 C -0.0491(5) 1.1045(5) 0.3180(7) 0.083(3) Uani 1 1 d . . .
H7A H -0.0845 1.1432 0.2928 0.124 Uiso 1 1 calc R . .
H7B H -0.0127 1.1401 0.3398 0.124 Uiso 1 1 calc R . .
H7C H -0.0418 1.0702 0.3788 0.124 Uiso 1 1 calc R . .
C8 C -0.4852(3) 0.8335(6) -0.5521(7) 0.086(3) Uani 1 1 d . . .
H8A H -0.5089 0.7826 -0.5544 0.129 Uiso 1 1 calc R . .
H8B H -0.4961 0.8466 -0.6241 0.129 Uiso 1 1 calc R . .
H8C H -0.4946 0.8846 -0.5239 0.129 Uiso 1 1 calc R . .
O16 O -0.1775(3) 1.0173(5) 0.0809(5) 0.098(2) Uani 1 1 d . . .
O17 O -0.3788(3) 1.0385(5) -0.6958(5) 0.102(2) Uani 1 1 d . . .
C9 C -0.3679(4) 0.8143(6) -0.6531(6) 0.086(3) Uani 1 1 d . . .
H9A H -0.3824 0.8265 -0.7272 0.130 Uiso 1 1 calc R . .
H9B H -0.3917 0.7657 -0.6508 0.130 Uiso 1 1 calc R . .
H9C H -0.3243 0.7981 -0.6130 0.130 Uiso 1 1 calc R . .
C80 C 0.1223(8) 0.8922(7) 0.1426(12) 0.128(5) Uani 1 1 d . . .
C70 C -0.2070(5) 1.0638(11) -0.0176(10) 0.140(5) Uani 1 1 d . . .
C90 C -0.4364(5) 1.0797(9) -0.7689(10) 0.127(5) Uani 1 1 d . . .
O19 O 0.1118(4) 0.8071(4) 0.1599(5) 0.101(2) Uani 1 1 d . . .
O5 O -0.09442(18) 0.5142(3) -0.0140(3) 0.0438(9) Uani 1 1 d . . .
O6 O -0.21675(18) 0.4976(3) -0.0841(3) 0.0441(9) Uani 1 1 d . . .
C4 C -0.1945(3) 0.5742(4) -0.0724(4) 0.0422(13) Uani 1 1 d . . .
C3 C -0.1269(3) 0.5821(4) -0.0366(4) 0.0404(13) Uani 1 1 d . . .
O14 O -0.06523(19) 0.8503(3) 0.2182(3) 0.0455(10) Uani 1 1 d . . .
C6 C -0.0975(3) 0.8292(4) 0.1204(4) 0.0403(13) 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 0.0403(6) 0.0400(6) 0.0415(6) 0.000 0.0233(5) 0.000
Co2 0.0408(4) 0.0394(4) 0.0418(4) 0.0004(3) 0.0238(4) 0.0004(3)
Cr1 0.0420(5) 0.0393(5) 0.0422(5) -0.0005(4) 0.0221(4) -0.0006(4)
O8 0.048(2) 0.046(2) 0.042(2) 0.0041(18) 0.0266(19) -0.0043(19)
O2 0.053(3) 0.042(2) 0.046(2) -0.0006(18) 0.031(2) 0.0095(19)
O9 0.031(2) 0.042(2) 0.053(2) 0.0024(18) 0.0195(18) -0.0029(16)
O1 0.050(2) 0.045(2) 0.041(2) -0.0023(17) 0.0281(19) 0.0069(19)
O13 0.068(3) 0.056(3) 0.042(2) -0.0013(19) 0.033(2) -0.004(2)
O12 0.048(3) 0.062(3) 0.061(3) 0.005(2) 0.033(2) -0.012(2)
O4 0.046(2) 0.044(2) 0.043(2) -0.0027(18) 0.0244(18) 0.0068(19)
O7 0.054(3) 0.044(2) 0.039(2) 0.0000(17) 0.0250(19) -0.0072(19)
O10 0.033(2) 0.041(2) 0.050(2) 0.0007(17) 0.0199(18) 0.0025(17)
O15 0.052(3) 0.052(3) 0.065(3) -0.005(2) 0.036(2) 0.005(2)
O11 0.048(2) 0.045(2) 0.039(2) 0.0026(17) 0.0254(18) -0.0054(19)
O3 0.051(2) 0.043(2) 0.039(2) -0.0011(17) 0.0269(19) 0.0058(18)
C5 0.042(3) 0.036(3) 0.043(3) 0.003(2) 0.026(3) 0.002(3)
C2 0.041(3) 0.037(3) 0.048(3) -0.004(2) 0.029(3) -0.002(2)
C1 0.040(3) 0.037(3) 0.047(3) -0.003(2) 0.023(3) 0.000(2)
C7 0.104(7) 0.060(5) 0.092(6) -0.001(4) 0.060(5) 0.025(5)
C8 0.048(4) 0.086(6) 0.110(7) -0.022(5) 0.035(4) -0.021(4)
O16 0.047(3) 0.143(6) 0.104(4) 0.024(4) 0.041(3) -0.005(3)
O17 0.090(5) 0.117(5) 0.108(5) 0.050(4) 0.061(4) -0.002(4)
C9 0.091(6) 0.100(7) 0.056(4) -0.018(4) 0.034(4) 0.019(5)
C80 0.232(15) 0.071(6) 0.181(11) -0.009(7) 0.177(12) -0.013(8)
C70 0.087(8) 0.209(15) 0.123(9) 0.067(9) 0.059(7) 0.004(9)
C90 0.066(6) 0.184(13) 0.140(9) 0.072(9) 0.063(7) 0.022(7)
O19 0.165(7) 0.078(4) 0.111(5) -0.022(4) 0.109(5) -0.002(4)
O5 0.035(2) 0.042(2) 0.052(2) 0.0001(18) 0.0234(18) -0.0019(18)
O6 0.036(2) 0.039(2) 0.055(2) -0.0021(17) 0.0239(19) -0.0014(17)
C4 0.045(3) 0.043(3) 0.040(3) -0.001(2) 0.024(3) -0.003(3)
C3 0.037(3) 0.045(3) 0.036(3) 0.001(2) 0.018(2) 0.004(3)
O14 0.046(2) 0.050(2) 0.038(2) 0.0021(17) 0.0223(18) -0.0071(19)
C6 0.043(3) 0.040(3) 0.038(3) 0.001(2) 0.023(3) 0.000(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O15 2.012(4) 2 ?
Co1 O15 2.012(4) . ?
Co1 O8 2.104(4) . ?
Co1 O8 2.104(4) 2 ?
Co1 O14 2.108(4) . ?
Co1 O14 2.108(4) 2 ?
Co2 O12 2.007(4) . ?
Co2 O13 2.021(4) . ?
Co2 O1 2.089(4) . ?
Co2 O5 2.091(4) 4_454 ?
Co2 O6 2.105(4) 4_454 ?
Co2 O2 2.120(4) . ?
Cr1 O10 1.955(4) . ?
Cr1 O4 1.961(4) . ?
Cr1 O3 1.965(4) . ?
Cr1 O7 1.967(4) . ?
Cr1 O9 1.967(4) . ?
Cr1 O11 1.972(4) . ?
O8 C5 1.230(7) . ?
O2 C2 1.246(7) . ?
O9 C3 1.255(7) . ?
O1 C1 1.240(7) . ?
O13 C9 1.396(9) . ?
O12 C8 1.424(9) . ?
O4 C1 1.276(7) . ?
O7 C5 1.253(7) . ?
O10 C4 1.251(7) . ?
O15 C7 1.410(9) . ?
O11 C6 1.260(7) . ?
O3 C2 1.251(6) . ?
C5 C6 1.499(8) . ?
C2 C1 1.504(8) . ?
O16 C70 1.398(12) . ?
O17 C90 1.398(12) . ?
C80 O19 1.350(11) . ?
O5 C3 1.233(7) . ?
O5 Co2 2.091(4) 4_444 ?
O6 C4 1.244(7) . ?
O6 Co2 2.105(4) 4_444 ?
C4 C3 1.509(8) . ?
O14 C6 1.245(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
O15 Co1 O15 92.1(3) 2 . ?
O15 Co1 O8 96.03(17) 2 . ?
O15 Co1 O8 91.50(17) . . ?
O15 Co1 O8 91.50(17) 2 2 ?
O15 Co1 O8 96.03(17) . 2 ?
O8 Co1 O8 169.1(2) . 2 ?
O15 Co1 O14 174.23(16) 2 . ?
O15 Co1 O14 90.20(17) . . ?
O8 Co1 O14 78.63(15) . . ?
O8 Co1 O14 93.51(16) 2 . ?
O15 Co1 O14 90.20(17) 2 2 ?
O15 Co1 O14 174.23(16) . 2 ?
O8 Co1 O14 93.51(16) . 2 ?
O8 Co1 O14 78.63(15) 2 2 ?
O14 Co1 O14 88.0(2) . 2 ?
O12 Co2 O13 91.09(18) . . ?
O12 Co2 O1 93.12(18) . . ?
O13 Co2 O1 96.00(17) . . ?
O12 Co2 O5 94.41(18) . 4_454 ?
O13 Co2 O5 91.90(18) . 4_454 ?
O1 Co2 O5 168.97(15) . 4_454 ?
O12 Co2 O6 174.56(18) . 4_454 ?
O13 Co2 O6 91.25(18) . 4_454 ?
O1 Co2 O6 91.52(16) . 4_454 ?
O5 Co2 O6 80.60(15) 4_454 4_454 ?
O12 Co2 O2 91.14(17) . . ?
O13 Co2 O2 174.44(18) . . ?
O1 Co2 O2 78.79(15) . . ?
O5 Co2 O2 93.00(16) 4_454 . ?
O6 Co2 O2 86.98(16) 4_454 . ?
O10 Cr1 O4 89.43(17) . . ?
O10 Cr1 O3 93.87(17) . . ?
O4 Cr1 O3 82.40(16) . . ?
O10 Cr1 O7 175.05(17) . . ?
O4 Cr1 O7 93.47(17) . . ?
O3 Cr1 O7 90.49(18) . . ?
O10 Cr1 O9 83.96(17) . . ?
O4 Cr1 O9 93.29(17) . . ?
O3 Cr1 O9 175.21(16) . . ?
O7 Cr1 O9 91.87(17) . . ?
O10 Cr1 O11 94.77(16) . . ?
O4 Cr1 O11 175.46(17) . . ?
O3 Cr1 O11 95.56(16) . . ?
O7 Cr1 O11 82.46(16) . . ?
O9 Cr1 O11 88.88(17) . . ?
C5 O8 Co1 112.8(3) . . ?
C2 O2 Co2 112.5(3) . . ?
C3 O9 Cr1 111.9(4) . . ?
C1 O1 Co2 112.5(4) . . ?
C9 O13 Co2 124.4(4) . . ?
C8 O12 Co2 124.8(5) . . ?
C1 O4 Cr1 113.8(3) . . ?
C5 O7 Cr1 113.4(4) . . ?
C4 O10 Cr1 111.2(4) . . ?
C7 O15 Co1 123.5(5) . . ?
C6 O11 Cr1 112.2(3) . . ?
C2 O3 Cr1 112.9(4) . . ?
O8 C5 O7 126.8(5) . . ?
O8 C5 C6 117.9(5) . . ?
O7 C5 C6 115.3(5) . . ?
O2 C2 O3 126.4(5) . . ?
O2 C2 C1 116.9(5) . . ?
O3 C2 C1 116.7(5) . . ?
O1 C1 O4 127.0(5) . . ?
O1 C1 C2 119.1(5) . . ?
O4 C1 C2 114.0(5) . . ?
C3 O5 Co2 110.3(4) . 4_444 ?
C4 O6 Co2 110.7(4) . 4_444 ?
O6 C4 O10 124.6(5) . . ?
O6 C4 C3 118.0(5) . . ?
O10 C4 C3 117.4(5) . . ?
O5 C3 O9 124.5(5) . . ?
O5 C3 C4 120.2(5) . . ?
O9 C3 C4 115.4(5) . . ?
C6 O14 Co1 111.9(4) . . ?
O14 C6 O11 125.1(5) . . ?
O14 C6 C5 118.5(5) . . ?
O11 C6 C5 116.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.148