# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Zhang, Bin'
_publ_contact_author_email       zhangbin@iccas.ac.cn

_publ_section_title              
;
Mn(C2O4)(H2O)0.25: An Antiferromagnetic Oxalate-based Cage Compound
;
loop_
_publ_author_name
'Bin Zhang'
'Yan Zhang'
'Jinbiao Zhang'
'Xiang Hao'
'Daoben Zhu'

# Attachment '- CCDC801821.cif'

data_CCDC801821
_database_code_depnum_ccdc_archive 'CCDC 801821'
#TrackingRef '- CCDC801821.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H0.50 Mn1 O4.25'
_chemical_formula_weight         147.46

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P bcn'

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

_cell_length_a                   9.010(3)
_cell_length_b                   7.117(2)
_cell_length_c                   11.755(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     753.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2418
_cell_measurement_theta_min      1.7325
_cell_measurement_theta_max      27.4745

_exptl_crystal_description       block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_absorpt_coefficient_mu    3.377
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_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            5938
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.65
_diffrn_reflns_theta_max         27.48
_reflns_number_total             861
_reflns_number_gt                848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0328P)^2^+0.8972P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         861
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_restrained_S_all      1.314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.81867(4) -0.00357(4) 0.45343(3) 0.01098(19) Uani 1 1 d . . .
O1 O 0.6143(2) -0.1851(3) 0.46186(15) 0.0163(4) Uani 1 1 d . . .
O2 O 0.37586(19) -0.1839(2) 0.51720(17) 0.0180(4) Uani 1 1 d . . .
O3 O 0.9416(2) 0.0122(2) 0.60996(16) 0.0147(4) Uani 1 1 d . . .
O4 O 0.8075(2) 0.0088(2) 0.7700(2) 0.0177(5) Uani 1 1 d . . .
O5 O 0.5000 0.0867(10) 0.2500 0.049(2) Uani 0.50 2 d SP . .
H1 H 0.584(10) -0.018(9) 0.260(9) 0.04(2) Uiso 0.50 1 d P . .
C1 C 0.4972(3) -0.1078(4) 0.49371(19) 0.0133(5) Uani 1 1 d . . .
C2 C 0.9258(3) 0.0117(3) 0.7163(2) 0.0130(5) 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
Mn1 0.0091(3) 0.0123(3) 0.0115(3) -0.00018(12) 0.00062(12) 0.00011(13)
O1 0.0103(8) 0.0136(8) 0.0250(9) -0.0003(7) 0.0040(7) 0.0001(7)
O2 0.0096(9) 0.0129(8) 0.0315(10) 0.0001(8) 0.0056(7) -0.0017(7)
O3 0.0142(9) 0.0198(10) 0.0102(8) -0.0005(6) -0.0007(7) -0.0005(7)
O4 0.0137(10) 0.0264(12) 0.0131(9) 0.0007(7) 0.0010(7) 0.0001(7)
O5 0.034(4) 0.031(4) 0.082(6) 0.000 -0.019(4) 0.000
C1 0.0111(12) 0.0126(13) 0.0163(12) 0.0000(8) 0.0007(9) 0.0011(8)
C2 0.0144(13) 0.0114(12) 0.0133(12) 0.0004(8) -0.0004(10) 0.0000(9)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 2.150(2) . ?
Mn1 O4 2.158(2) 7 ?
Mn1 O2 2.2297(19) 5_656 ?
Mn1 O1 2.2517(19) . ?
Mn1 O3 2.286(2) 5_756 ?
Mn1 O2 2.3089(19) 4_546 ?
Mn1 O1 2.348(2) 8_765 ?
O1 C1 1.247(3) . ?
O1 Mn1 2.348(2) 8_755 ?
O2 C1 1.251(3) . ?
O2 Mn1 2.2297(19) 5_656 ?
O2 Mn1 2.3089(19) 4_446 ?
O3 C2 1.258(3) . ?
O3 Mn1 2.286(2) 5_756 ?
O4 C2 1.239(3) . ?
O4 Mn1 2.158(2) 7_556 ?
O5 H1 1.07(8) . ?
C1 C1 1.543(5) 5_656 ?
C2 C2 1.555(5) 3_756 ?

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 Mn1 O4 151.58(8) . 7 ?
O3 Mn1 O2 103.96(7) . 5_656 ?
O4 Mn1 O2 97.37(7) 7 5_656 ?
O3 Mn1 O1 114.42(7) . . ?
O4 Mn1 O1 89.77(7) 7 . ?
O2 Mn1 O1 72.16(8) 5_656 . ?
O3 Mn1 O3 78.09(8) . 5_756 ?
O4 Mn1 O3 73.63(7) 7 5_756 ?
O2 Mn1 O3 144.03(6) 5_656 5_756 ?
O1 Mn1 O3 140.53(6) . 5_756 ?
O3 Mn1 O2 78.89(7) . 4_546 ?
O4 Mn1 O2 98.23(7) 7 4_546 ?
O2 Mn1 O2 136.78(6) 5_656 4_546 ?
O1 Mn1 O2 67.87(7) . 4_546 ?
O3 Mn1 O2 79.17(6) 5_756 4_546 ?
O3 Mn1 O1 77.36(6) . 8_765 ?
O4 Mn1 O1 94.06(6) 7 8_765 ?
O2 Mn1 O1 67.54(7) 5_656 8_765 ?
O1 Mn1 O1 139.68(6) . 8_765 ?
O3 Mn1 O1 78.25(6) 5_756 8_765 ?
O2 Mn1 O1 150.02(7) 4_546 8_765 ?
C1 O1 Mn1 116.88(16) . . ?
C1 O1 Mn1 130.99(16) . 8_755 ?
Mn1 O1 Mn1 109.97(7) . 8_755 ?
C1 O2 Mn1 117.53(16) . 5_656 ?
C1 O2 Mn1 130.16(16) . 4_446 ?
Mn1 O2 Mn1 112.20(7) 5_656 4_446 ?
C2 O3 Mn1 142.33(19) . . ?
C2 O3 Mn1 115.53(18) . 5_756 ?
Mn1 O3 Mn1 101.91(8) . 5_756 ?
C2 O4 Mn1 118.00(18) . 7_556 ?
O1 C1 O2 127.9(2) . . ?
O1 C1 C1 116.1(3) . 5_656 ?
O2 C1 C1 116.0(3) . 5_656 ?
O4 C2 O3 127.2(3) . . ?
O4 C2 C2 118.7(3) . 3_756 ?
O3 C2 C2 114.1(3) . 3_756 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.107