# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2000
# CCDC Number: 440/214


data_calcul2

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             Fe2[Mo(CN)8].8H20
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H16 Fe2 Mo N8 O8'
_chemical_formula_weight          559.93

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'
 'Mo'  'Mo'  -1.6832   0.6857
 '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'
 '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'

_symmetry_cell_setting            Tetragonal
_symmetry_space_group_name_H-M    I422

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

_cell_length_a                    11.809(2)
_cell_length_b                    11.809(2)
_cell_length_c                    13.108(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1828.1(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       2.44
_cell_measurement_theta_max       12.17

_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.034
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1112
_exptl_absorpt_coefficient_mu     2.297
_exptl_absorpt_correction_type    '\y scan'
_exptl_absorpt_correction_T_min   0.891085
_exptl_absorpt_correction_T_max   0.999508

_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   'Enraf nonius CAD4 diffractometer'
_diffrn_measurement_method        \q-2\q
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   60
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             1502
_diffrn_reflns_av_R_equivalents   0.0270
_diffrn_reflns_av_sigmaI/netI     0.0396
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.32
_diffrn_reflns_theta_max          29.88
_reflns_number_total              1337
_reflns_number_gt                 1094
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Enraf Nonius CAD4'
_computing_cell_refinement        MolEN
_computing_data_reduction         MolEN
_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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+54.9791P] 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_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.63(17)
_refine_ls_number_reflns          1337
_refine_ls_number_parameters      73
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0782
_refine_ls_R_factor_gt            0.0555
_refine_ls_wR_factor_ref          0.1482
_refine_ls_wR_factor_gt           0.1414
_refine_ls_goodness_of_fit_ref    1.288
_refine_ls_restrained_S_all       1.288
_refine_ls_shift/su_max           0.003
_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_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Mo1 Mo 0.0000 0.0000 0.5000 0.0062(5) Uani 1 d S . .
Fe1 Fe 0.19633(8) 0.30367(8) 0.2500 0.0161(3) Uani 1 d S . .
Mo2 Mo 0.0000 0.0000 0.0000 0.0119(6) Uani 1 d S . .
C1 C 0.0645(13) 0.1340(15) 0.4084(11) 0.032(4) Uani 1 d . . .
N1 N 0.0849(9) 0.2194(8) 0.3635(8) 0.025(2) Uani 1 d . . .
C2 C 0.0638(18) 0.1406(12) 0.0874(10) 0.040(5) Uani 1 d . . .
N2 N 0.1312(9) 0.1988(10) 0.1332(9) 0.030(2) Uani 1 d . . .
O1 O 0.2856(11) 0.1430(10) 0.2625(16) 0.025(4) Uani 0.50 d P . .
O2 O 0.1034(12) 0.4551(10) 0.2672(11) 0.027(4) Uani 0.50 d P . .
O3 O 0.1079(13) 0.3984(16) 0.5553(7) 0.097(5) Uani 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
Mo1 0.0041(7) 0.0041(7) 0.0102(12) 0.000 0.000 0.000
Fe1 0.0168(4) 0.0168(4) 0.0146(6) -0.0060(11) -0.0060(11) -0.0026(5)
Mo2 0.0135(9) 0.0135(9) 0.0087(13) 0.000 0.000 0.000
C1 0.032(7) 0.044(9) 0.019(7) 0.018(6) -0.014(5) -0.015(6)
N1 0.032(5) 0.023(5) 0.021(4) 0.008(4) 0.001(4) -0.013(4)
C2 0.090(13) 0.014(6) 0.016(7) 0.012(5) -0.023(7) -0.028(7)
N2 0.028(5) 0.029(5) 0.033(5) -0.006(4) -0.012(5) -0.006(4)
O1 0.034(6) 0.020(5) 0.019(10) -0.008(6) -0.001(7) -0.004(5)
O2 0.034(6) 0.022(5) 0.024(11) 0.005(5) -0.003(6) 0.010(5)
O3 0.074(11) 0.149(16) 0.066(6) -0.061(8) -0.047(7) 0.034(8)

_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
Mo1 C1 2.128(15) 5_556 ?
Mo1 C1 2.128(15) 2 ?
Mo1 C1 2.128(15) 7 ?
Mo1 C1 2.128(15) 3_556 ?
Mo1 C1 2.128(15) 4_556 ?
Mo1 C1 2.128(15) . ?
Mo1 C1 2.128(15) 6_556 ?
Mo1 C1 2.128(15) 8 ?
Fe1 O2 2.110(12) . ?
Fe1 O2 2.110(12) 14 ?
Fe1 N2 2.114(11) . ?
Fe1 N2 2.114(11) 14 ?
Fe1 O1 2.177(13) 14 ?
Fe1 O1 2.177(13) . ?
Fe1 N1 2.222(10) . ?
Fe1 N1 2.222(10) 14 ?
Mo2 C2 2.153(14) 6 ?
Mo2 C2 2.153(14) . ?
Mo2 C2 2.153(14) 8 ?
Mo2 C2 2.153(14) 4 ?
Mo2 C2 2.153(14) 2 ?
Mo2 C2 2.153(14) 5 ?
Mo2 C2 2.153(14) 3 ?
Mo2 C2 2.153(14) 7 ?
C1 N1 1.192(18) . ?
C2 N2 1.212(18) . ?
O1 O1 1.24(3) 14 ?
O2 O2 1.08(3) 14 ?

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
C1 Mo1 C1 148.3(9) 5_556 2 ?
C1 Mo1 C1 138.0(8) 5_556 7 ?
C1 Mo1 C1 71.4(4) 2 7 ?
C1 Mo1 C1 71.4(4) 5_556 3_556 ?
C1 Mo1 C1 138.0(8) 2 3_556 ?
C1 Mo1 C1 77.6(7) 7 3_556 ?
C1 Mo1 C1 71.4(4) 5_556 4_556 ?
C1 Mo1 C1 83.9(10) 2 4_556 ?
C1 Mo1 C1 148.3(10) 7 4_556 ?
C1 Mo1 C1 111.3(8) 3_556 4_556 ?
C1 Mo1 C1 77.6(7) 5_556 . ?
C1 Mo1 C1 111.3(8) 2 . ?
C1 Mo1 C1 71.4(4) 7 . ?
C1 Mo1 C1 83.9(10) 3_556 . ?
C1 Mo1 C1 138.0(8) 4_556 . ?
C1 Mo1 C1 111.3(8) 5_556 6_556 ?
C1 Mo1 C1 77.6(7) 2 6_556 ?
C1 Mo1 C1 83.9(10) 7 6_556 ?
C1 Mo1 C1 71.4(4) 3_556 6_556 ?
C1 Mo1 C1 71.4(4) 4_556 6_556 ?
C1 Mo1 C1 148.3(9) . 6_556 ?
C1 Mo1 C1 83.9(10) 5_556 8 ?
C1 Mo1 C1 71.4(4) 2 8 ?
C1 Mo1 C1 111.3(8) 7 8 ?
C1 Mo1 C1 148.3(10) 3_556 8 ?
C1 Mo1 C1 77.6(7) 4_556 8 ?
C1 Mo1 C1 71.4(4) . 8 ?
C1 Mo1 C1 138.0(8) 6_556 8 ?
O2 Fe1 O2 29.5(8) . 14 ?
O2 Fe1 N2 112.6(5) . . ?
O2 Fe1 N2 85.4(5) 14 . ?
O2 Fe1 N2 85.4(5) . 14 ?
O2 Fe1 N2 112.6(5) 14 14 ?
N2 Fe1 N2 161.9(6) . 14 ?
O2 Fe1 O1 150.7(5) . 14 ?
O2 Fe1 O1 169.3(6) 14 14 ?
N2 Fe1 O1 88.8(5) . 14 ?
N2 Fe1 O1 73.7(6) 14 14 ?
O2 Fe1 O1 169.3(6) . . ?
O2 Fe1 O1 150.7(5) 14 . ?
N2 Fe1 O1 73.7(6) . . ?
N2 Fe1 O1 88.8(5) 14 . ?
O1 Fe1 O1 33.0(7) 14 . ?
O2 Fe1 N1 90.0(5) . . ?
O2 Fe1 N1 78.6(5) 14 . ?
N2 Fe1 N1 90.4(3) . . ?
N2 Fe1 N1 91.4(3) 14 . ?
O1 Fe1 N1 110.5(5) 14 . ?
O1 Fe1 N1 81.2(5) . . ?
O2 Fe1 N1 78.6(5) . 14 ?
O2 Fe1 N1 90.0(5) 14 14 ?
N2 Fe1 N1 91.4(3) . 14 ?
N2 Fe1 N1 90.4(3) 14 14 ?
O1 Fe1 N1 81.2(5) 14 14 ?
O1 Fe1 N1 110.5(5) . 14 ?
N1 Fe1 N1 168.2(5) . 14 ?
C2 Mo2 C2 145.3(11) 6 . ?
C2 Mo2 C2 139.0(12) 6 8 ?
C2 Mo2 C2 73.6(3) . 8 ?
C2 Mo2 C2 73.6(3) 6 4 ?
C2 Mo2 C2 139.0(12) . 4 ?
C2 Mo2 C2 75.1(10) 8 4 ?
C2 Mo2 C2 75.1(10) 6 2 ?
C2 Mo2 C2 115.7(7) . 2 ?
C2 Mo2 C2 73.6(3) 8 2 ?
C2 Mo2 C2 79.1(8) 4 2 ?
C2 Mo2 C2 115.7(7) 6 5 ?
C2 Mo2 C2 75.1(10) . 5 ?
C2 Mo2 C2 79.1(8) 8 5 ?
C2 Mo2 C2 73.6(3) 4 5 ?
C2 Mo2 C2 145.3(11) 2 5 ?
C2 Mo2 C2 73.6(3) 6 3 ?
C2 Mo2 C2 79.1(8) . 3 ?
C2 Mo2 C2 145.3(11) 8 3 ?
C2 Mo2 C2 115.7(7) 4 3 ?
C2 Mo2 C2 139.0(12) 2 3 ?
C2 Mo2 C2 73.6(3) 5 3 ?
C2 Mo2 C2 79.1(8) 6 7 ?
C2 Mo2 C2 73.6(3) . 7 ?
C2 Mo2 C2 115.7(7) 8 7 ?
C2 Mo2 C2 145.3(11) 4 7 ?
C2 Mo2 C2 73.6(3) 2 7 ?
C2 Mo2 C2 139.0(12) 5 7 ?
C2 Mo2 C2 75.1(10) 3 7 ?
N1 C1 Mo1 168.5(14) . . ?
C1 N1 Fe1 146.0(12) . . ?
N2 C2 Mo2 158.7(16) . . ?
C2 N2 Fe1 158.5(13) . . ?
O1 O1 Fe1 73.5(4) 14 . ?
O2 O2 Fe1 75.2(4) 14 . ?

_diffrn_measured_fraction_theta_max    0.500
_diffrn_reflns_theta_full              29.88
_diffrn_measured_fraction_theta_full   0.500
_refine_diff_density_max    1.250
_refine_diff_density_min   -0.883
_refine_diff_density_rms    0.223