# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Lahcene Ouahab'
_publ_contact_author_email       LAHCENE.OUAHAB@UNIV-RENNES1.FR

_publ_section_title              
;
Porous 2D coordination polymeric formate
built up by Mn(II) linking of Fe3O units: influence
of guest molecules on magnetic properties
;
loop_
_publ_author_name
'Lahcene Ouahab'
'Olivier Cador'
'Konstantin S. Gavrilenko'
'Stephane Golhen'
'Sergey V. Kolotilov'
;
A.S.Lytvynenko
;
'Vitaly V. Pavlishchuk'

# Attachment 'Fe3O_form_9Mn_aq_3-disord_form1.cif'

data_1tiers
_database_code_depnum_ccdc_archive 'CCDC 684199'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Mn(H2O)3 Fe3O(CO2H)9], 3.5 CO2H2'
_chemical_formula_sum            'C12.50 H22 Fe3 Mn O29'
_chemical_formula_weight         858.79

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63'

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

_cell_length_a                   12.369(5)
_cell_length_b                   12.369(5)
_cell_length_c                   12.992(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1721.4(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12857
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    1.695
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'Kappa CCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6483
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         30.02
_reflns_number_total             3273
_reflns_number_gt                2699
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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^)+(0.0983P)^2^+0.0000P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         3273
_refine_ls_number_parameters     151
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1508
_refine_ls_wR_factor_gt          0.1358
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_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 0.0736(4) 0.2394(4) 0.8032(4) 0.0488(9) Uani 1 1 d . . .
H1 H 0.0909 0.2940 0.7483 0.059 Uiso 1 1 calc R . .
C2 C 0.0731(4) 0.2360(5) 1.0931(4) 0.0521(10) Uani 1 1 d . . .
H2 H 0.0891 0.2889 1.1490 0.062 Uiso 1 1 calc R . .
C3 C -0.3163(4) 0.1158(4) 1.0111(3) 0.0446(8) Uani 1 1 d . . .
H3 H -0.3304 0.0654 1.0684 0.054 Uiso 1 1 calc R . .
C4 C -0.0652(7) 0.4103(6) 1.2322(5) 0.0820(18) Uani 1 1 d . . .
H4 H -0.0455 0.3774 1.2889 0.098 Uiso 1 1 calc R . .
O1 O 0.0000 0.0000 0.9467(4) 0.0351(7) Uani 1 3 d S . .
O2 O -0.0372(3) 0.1841(3) 0.8367(3) 0.0554(8) Uani 1 1 d . . .
O3 O 0.1607(3) 0.2282(3) 0.8359(3) 0.0563(8) Uani 1 1 d . . .
O4 O -0.0355(4) 0.1814(3) 1.0604(3) 0.0603(9) Uani 1 1 d . . .
O5 O -0.2282(3) -0.0653(3) 1.0597(3) 0.0579(9) Uani 1 1 d . . .
O6 O -0.2459(3) 0.1156(2) 0.9415(3) 0.0485(6) Uani 1 1 d . . .
O7 O -0.3682(3) 0.1801(3) 1.0074(3) 0.0481(6) Uani 1 1 d . . .
O8 O -0.2121(3) 0.2975(3) 0.8030(3) 0.0590(8) Uani 1 1 d . . .
O9 O -0.1594(5) 0.3349(4) 1.1759(4) 0.0860(13) Uani 1 1 d . . .
H9 H -0.2115 0.3574 1.1758 0.129 Uiso 1 1 calc R . .
O10 O 0.0023(6) 0.4810(5) 0.7160(5) 0.106(2) Uani 1 1 d . . .
Mn1 Mn -0.3333 0.3333 0.89979(8) 0.0411(2) Uani 1 3 d S . .
Fe1 Fe -0.12126(4) 0.05277(4) 0.94743(6) 0.03880(16) Uani 1 1 d . . .
O1S O 0.226(2) 0.672(3) 0.989(2) 0.152(10) Uani 0.33 1 d P A 1
C2S C 0.349(3) 0.776(2) 0.995(4) 0.078(10) Uani 0.17 1 d P . 1

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 0.050(2) 0.051(2) 0.044(2) 0.0122(18) 0.0081(17) 0.0244(17)
C2 0.053(2) 0.056(3) 0.048(2) -0.0143(19) -0.0006(18) 0.0270(18)
C3 0.0467(18) 0.0467(18) 0.0469(19) 0.0060(14) 0.0067(14) 0.0282(15)
C4 0.106(5) 0.064(3) 0.080(4) 0.000(3) -0.033(4) 0.045(3)
O1 0.0333(10) 0.0333(10) 0.0388(17) 0.000 0.000 0.0166(5)
O2 0.0504(16) 0.0598(17) 0.0591(19) 0.0211(16) 0.0131(15) 0.0300(15)
O3 0.0457(16) 0.0537(16) 0.062(2) 0.0169(16) 0.0056(15) 0.0192(13)
O4 0.0567(18) 0.068(2) 0.064(2) -0.0220(17) -0.0063(16) 0.0372(17)
O5 0.062(2) 0.0636(19) 0.058(2) 0.0222(16) 0.0207(16) 0.0384(18)
O6 0.0506(13) 0.0550(14) 0.0516(13) 0.0065(15) 0.0110(15) 0.0351(12)
O7 0.0502(14) 0.0465(13) 0.0578(18) 0.0098(13) 0.0125(12) 0.0317(12)
O8 0.0657(19) 0.0643(18) 0.0590(19) 0.0170(15) 0.0183(15) 0.0415(16)
O9 0.104(3) 0.058(2) 0.084(3) -0.0008(19) -0.031(3) 0.032(2)
O10 0.097(3) 0.083(3) 0.116(4) 0.000(3) 0.058(3) 0.027(3)
Mn1 0.0413(3) 0.0413(3) 0.0407(4) 0.000 0.000 0.02067(14)
Fe1 0.0389(2) 0.0415(2) 0.0395(3) 0.0034(2) 0.0033(2) 0.02273(19)
O1S 0.153(18) 0.21(2) 0.17(2) 0.004(19) 0.037(17) 0.15(2)
C2S 0.08(2) 0.011(8) 0.13(3) -0.007(11) 0.00(2) 0.015(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
C1 O3 1.230(5) . ?
C1 O2 1.265(5) . ?
C2 O4 1.238(6) . ?
C2 O5 1.240(6) 4 ?
C3 O7 1.248(4) . ?
C3 O6 1.256(5) . ?
C4 O10 1.188(8) 2_565 ?
C4 O9 1.295(8) . ?
O1 Fe1 1.9117(9) 4 ?
O1 Fe1 1.9117(9) . ?
O1 Fe1 1.9117(9) 3 ?
O2 Fe1 2.025(3) . ?
O3 Fe1 2.023(3) 4 ?
O4 Fe1 2.030(3) . ?
O5 C2 1.240(6) 3 ?
O5 Fe1 2.020(3) . ?
O6 Fe1 2.047(3) . ?
O7 Mn1 2.217(3) . ?
O8 Mn1 2.166(3) . ?
O10 C4 1.188(8) 2_564 ?
Mn1 O8 2.166(3) 4_455 ?
Mn1 O8 2.166(3) 3_565 ?
Mn1 O7 2.217(3) 3_565 ?
Mn1 O7 2.217(3) 4_455 ?
Fe1 O3 2.023(3) 3 ?
O1S C2S 1.21(4) 3_665 ?
O1S C2S 1.42(4) . ?
C2S O1S 1.21(4) 4_565 ?

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 C1 O2 126.4(4) . . ?
O4 C2 O5 127.3(4) . 4 ?
O7 C3 O6 123.4(4) . . ?
O10 C4 O9 124.0(5) 2_565 . ?
Fe1 O1 Fe1 119.997(3) 4 . ?
Fe1 O1 Fe1 119.997(3) 4 3 ?
Fe1 O1 Fe1 119.997(3) . 3 ?
C1 O2 Fe1 131.4(3) . . ?
C1 O3 Fe1 133.2(3) . 4 ?
C2 O4 Fe1 132.5(3) . . ?
C2 O5 Fe1 131.4(3) 3 . ?
C3 O6 Fe1 128.9(3) . . ?
C3 O7 Mn1 128.8(3) . . ?
O8 Mn1 O8 89.68(14) . 4_455 ?
O8 Mn1 O8 89.68(14) . 3_565 ?
O8 Mn1 O8 89.68(14) 4_455 3_565 ?
O8 Mn1 O7 92.85(11) . . ?
O8 Mn1 O7 92.90(14) 4_455 . ?
O8 Mn1 O7 176.40(14) 3_565 . ?
O8 Mn1 O7 92.90(14) . 3_565 ?
O8 Mn1 O7 176.40(14) 4_455 3_565 ?
O8 Mn1 O7 92.85(11) 3_565 3_565 ?
O7 Mn1 O7 84.47(14) . 3_565 ?
O8 Mn1 O7 176.40(14) . 4_455 ?
O8 Mn1 O7 92.85(11) 4_455 4_455 ?
O8 Mn1 O7 92.90(14) 3_565 4_455 ?
O7 Mn1 O7 84.47(14) . 4_455 ?
O7 Mn1 O7 84.47(14) 3_565 4_455 ?
O1 Fe1 O5 95.66(14) . . ?
O1 Fe1 O3 94.67(13) . 3 ?
O5 Fe1 O3 91.99(14) . 3 ?
O1 Fe1 O2 95.44(14) . . ?
O5 Fe1 O2 168.85(13) . . ?
O3 Fe1 O2 88.04(17) 3 . ?
O1 Fe1 O4 94.56(15) . . ?
O5 Fe1 O4 86.64(17) . . ?
O3 Fe1 O4 170.77(13) 3 . ?
O2 Fe1 O4 91.54(14) . . ?
O1 Fe1 O6 176.82(15) . . ?
O5 Fe1 O6 87.50(13) . . ?
O3 Fe1 O6 84.99(14) 3 . ?
O2 Fe1 O6 81.39(13) . . ?
O4 Fe1 O6 85.83(14) . . ?
C2S O1S C2S 112(2) 3_665 . ?
O1S C2S O1S 127(2) 4_565 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.309