# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1939
  
data_[Cd(tren)]2[Fe(CN)6](H2O)3
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 catena-bis(tris(2-Amineoethyl)amine-cadmium(ii)) hexacyano-iron(ii) trihydrate
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C99 Cd11 Fe10.50 N77 O33' 
_chemical_formula_weight          4618.58 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Cd'  'Cd'  -0.8075   1.2024 
 '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' 
 'C'  'C'   0.0033   0.0016 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    7.5219(19) 
_cell_length_b                    28.593(7) 
_cell_length_c                    7.7246(19) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.345(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      1594.2(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        plate
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     9.621 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              4396 
_exptl_absorpt_coefficient_mu     12.212 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   0.1938
_exptl_absorpt_correction_T_max   0.5803
_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   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             9264 
_diffrn_reflns_av_R_equivalents   0.0217 
_diffrn_reflns_av_sigmaI/netI     0.0176 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -36 
_diffrn_reflns_limit_k_max        34 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          2.84 
_diffrn_reflns_theta_max          27.04 
_reflns_number_total              3464 
_reflns_number_gt                 3338 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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^)+(0.0403P)^2^+6.2060P] 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          3464 
_refine_ls_number_parameters      187 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0441 
_refine_ls_R_factor_gt            0.0425 
_refine_ls_wR_factor_ref          0.1093 
_refine_ls_wR_factor_gt           0.1085 
_refine_ls_goodness_of_fit_ref    1.180 
_refine_ls_restrained_S_all       1.180 
_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 
Cd1 Cd 0.37693(4) 0.051384(11) 0.59443(4) 0.02827(12) Uani 1 1 d . . . 
Fe1 Fe 1.0000 0.0000 1.0000 0.01941(17) Uani 1 2 d S . . 
N1 N 0.0651(7) 0.0741(2) 0.5108(8) 0.0586(14) Uani 1 1 d . . . 
N2 N 0.3593(6) 0.14401(14) 0.6030(6) 0.0380(9) Uani 1 1 d . . . 
N3 N 0.5032(9) 0.0777(2) 0.8884(7) 0.0669(17) Uani 1 1 d . . . 
N4 N 0.4710(7) 0.08408(18) 0.3574(6) 0.0481(11) Uani 1 1 d . . . 
N5 N 0.6894(6) 0.01243(16) 0.6505(5) 0.0374(9) Uani 1 1 d . . . 
N6 N 1.0690(7) 0.10626(17) 1.0167(7) 0.0492(11) Uani 1 1 d . . . 
N7 N 0.7307(6) 0.00951(16) 1.2340(6) 0.0395(10) Uani 1 1 d . . . 
C1 C 0.0327(10) 0.1222(3) 0.5119(16) 0.094(3) Uani 1 1 d . . . 
C2 C 0.1674(13) 0.1559(3) 0.5538(19) 0.123(5) Uani 1 1 d . . . 
C3 C 0.4474(12) 0.1592(2) 0.7890(9) 0.069(2) Uani 1 1 d . . . 
C4 C 0.5585(14) 0.1239(3) 0.9069(10) 0.087(3) Uani 1 1 d . . . 
C5 C 0.456(2) 0.1612(3) 0.4842(17) 0.143(6) Uani 1 1 d . . . 
C6 C 0.5052(13) 0.1335(3) 0.3626(14) 0.084(3) Uani 1 1 d . . . 
C7 C 0.8064(6) 0.00810(15) 0.7831(5) 0.0243(8) Uani 1 1 d . . . 
C8 C 1.0413(6) 0.06660(16) 1.0103(6) 0.0270(8) Uani 1 1 d . . . 
C9 C 0.8303(6) 0.00629(15) 1.1421(6) 0.0264(8) Uani 1 1 d . . . 
O1 O 0.0068(7) 0.20410(14) -0.0011(7) 0.0582(11) Uani 1 1 d . . . 
O2 O 0.8708(7) 0.24789(19) 0.6229(7) 0.0718(14) Uani 1 1 d . . . 
O3 O 0.7646(8) 0.22050(19) 0.2308(8) 0.0754(14) 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 
Cd1 0.02836(19) 0.03003(19) 0.02662(18) 0.00132(12) 0.00806(13) 0.00288(12) 
Fe1 0.0163(4) 0.0252(4) 0.0158(4) 0.0019(3) 0.0030(3) 0.0004(3) 
N1 0.030(2) 0.060(3) 0.077(4) -0.007(3) 0.001(2) 0.002(2) 
N2 0.051(3) 0.030(2) 0.031(2) -0.0006(16) 0.0070(18) 0.0033(17) 
N3 0.092(4) 0.057(3) 0.032(2) -0.003(2) -0.013(3) 0.021(3) 
N4 0.058(3) 0.052(3) 0.041(2) 0.006(2) 0.026(2) 0.007(2) 
N5 0.029(2) 0.050(3) 0.028(2) 0.0035(17) -0.0020(17) 0.0001(17) 
N6 0.051(3) 0.039(3) 0.056(3) 0.002(2) 0.013(2) -0.006(2) 
N7 0.038(2) 0.051(3) 0.036(2) 0.0038(19) 0.0228(19) 0.0074(19) 
C1 0.044(4) 0.071(5) 0.173(10) 0.033(6) 0.040(5) 0.027(4) 
C2 0.066(5) 0.049(4) 0.204(12) -0.016(6) -0.044(7) 0.026(4) 
C3 0.093(5) 0.041(3) 0.054(4) -0.021(3) -0.009(4) 0.005(3) 
C4 0.120(7) 0.068(5) 0.043(4) -0.003(3) -0.025(4) -0.019(5) 
C5 0.318(19) 0.036(4) 0.144(9) -0.009(5) 0.178(12) -0.033(7) 
C6 0.103(6) 0.054(4) 0.126(7) -0.006(4) 0.083(6) -0.024(4) 
C7 0.0206(19) 0.030(2) 0.0224(19) 0.0018(15) 0.0055(16) 0.0002(15) 
C8 0.0223(19) 0.032(2) 0.025(2) -0.0007(17) 0.0044(16) 0.0007(16) 
C9 0.0239(19) 0.031(2) 0.025(2) 0.0056(16) 0.0074(16) 0.0035(16) 
O1 0.071(3) 0.037(2) 0.070(3) 0.004(2) 0.025(2) 0.0026(19) 
O2 0.069(3) 0.069(3) 0.077(3) -0.005(3) 0.020(3) 0.009(3) 
O3 0.079(4) 0.066(3) 0.087(4) -0.004(3) 0.032(3) -0.006(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 
Cd1 N3 2.326(5) . ? 
Cd1 N4 2.336(5) . ? 
Cd1 N1 2.343(5) . ? 
Cd1 N7 2.459(4) 3_657 ? 
Cd1 N5 2.526(4) . ? 
Cd1 N5 2.575(4) 3_656 ? 
Cd1 N2 2.653(4) . ? 
Fe1 C7 1.899(4) 3_757 ? 
Fe1 C7 1.899(4) . ? 
Fe1 C9 1.912(4) . ? 
Fe1 C9 1.912(4) 3_757 ? 
Fe1 C8 1.927(5) . ? 
Fe1 C8 1.927(5) 3_757 ? 
N1 C1 1.398(10) . ? 
N2 C5 1.411(9) . ? 
N2 C2 1.426(10) . ? 
N2 C3 1.468(7) . ? 
N3 C4 1.379(10) . ? 
N4 C6 1.434(9) . ? 
N5 C7 1.154(6) . ? 
N5 Cd1 2.575(4) 3_656 ? 
N6 C8 1.151(6) . ? 
N7 C9 1.172(6) . ? 
N7 Cd1 2.459(4) 3_657 ? 
C1 C2 1.369(13) . ? 
C3 C4 1.456(11) . ? 
C5 C6 1.358(11) . ? 
  
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 
N3 Cd1 N4 120.3(2) . . ? 
N3 Cd1 N1 106.4(2) . . ? 
N4 Cd1 N1 100.0(2) . . ? 
N3 Cd1 N7 79.0(2) . 3_657 ? 
N4 Cd1 N7 157.54(16) . 3_657 ? 
N1 Cd1 N7 83.61(18) . 3_657 ? 
N3 Cd1 N5 82.57(18) . . ? 
N4 Cd1 N5 80.71(16) . . ? 
N1 Cd1 N5 168.71(17) . . ? 
N7 Cd1 N5 91.54(14) 3_657 . ? 
N3 Cd1 N5 152.66(16) . 3_656 ? 
N4 Cd1 N5 75.30(16) . 3_656 ? 
N1 Cd1 N5 91.24(17) . 3_656 ? 
N7 Cd1 N5 82.49(14) 3_657 3_656 ? 
N5 Cd1 N5 78.00(14) . 3_656 ? 
N3 Cd1 N2 70.25(17) . . ? 
N4 Cd1 N2 69.41(16) . . ? 
N1 Cd1 N2 71.19(17) . . ? 
N7 Cd1 N2 131.83(14) 3_657 . ? 
N5 Cd1 N2 119.11(14) . . ? 
N5 Cd1 N2 136.47(13) 3_656 . ? 
C7 Fe1 C7 180.0 3_757 . ? 
C7 Fe1 C9 88.57(18) 3_757 . ? 
C7 Fe1 C9 91.43(18) . . ? 
C7 Fe1 C9 91.43(18) 3_757 3_757 ? 
C7 Fe1 C9 88.57(18) . 3_757 ? 
C9 Fe1 C9 180.000(1) . 3_757 ? 
C7 Fe1 C8 90.54(18) 3_757 . ? 
C7 Fe1 C8 89.46(18) . . ? 
C9 Fe1 C8 90.52(18) . . ? 
C9 Fe1 C8 89.48(18) 3_757 . ? 
C7 Fe1 C8 89.46(18) 3_757 3_757 ? 
C7 Fe1 C8 90.54(18) . 3_757 ? 
C9 Fe1 C8 89.48(18) . 3_757 ? 
C9 Fe1 C8 90.52(18) 3_757 3_757 ? 
C8 Fe1 C8 180.0 . 3_757 ? 
C1 N1 Cd1 115.7(4) . . ? 
C5 N2 C2 114.4(10) . . ? 
C5 N2 C3 111.1(8) . . ? 
C2 N2 C3 109.6(7) . . ? 
C5 N2 Cd1 107.1(4) . . ? 
C2 N2 Cd1 106.5(4) . . ? 
C3 N2 Cd1 107.9(3) . . ? 
C4 N3 Cd1 116.1(4) . . ? 
C6 N4 Cd1 117.6(4) . . ? 
C7 N5 Cd1 129.8(4) . . ? 
C7 N5 Cd1 121.2(4) . 3_656 ? 
Cd1 N5 Cd1 102.00(14) . 3_656 ? 
C9 N7 Cd1 129.4(4) . 3_657 ? 
C2 C1 N1 125.1(6) . . ? 
C1 C2 N2 121.5(6) . . ? 
C4 C3 N2 115.4(5) . . ? 
N3 C4 C3 119.7(6) . . ? 
C6 C5 N2 122.4(7) . . ? 
C5 C6 N4 120.9(6) . . ? 
N5 C7 Fe1 179.1(4) . . ? 
N6 C8 Fe1 178.9(4) . . ? 
N7 C9 Fe1 177.8(4) . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
N3 Cd1 N1 C1 60.7(7) . . . . ? 
N4 Cd1 N1 C1 -65.2(7) . . . . ? 
N7 Cd1 N1 C1 137.3(7) 3_657 . . . ? 
N5 Cd1 N1 C1 -157.8(9) . . . . ? 
N5 Cd1 N1 C1 -140.4(6) 3_656 . . . ? 
N2 Cd1 N1 C1 -1.1(6) . . . . ? 
N3 Cd1 N2 C5 122.0(8) . . . . ? 
N4 Cd1 N2 C5 -13.0(8) . . . . ? 
N1 Cd1 N2 C5 -121.9(8) . . . . ? 
N7 Cd1 N2 C5 175.6(8) 3_657 . . . ? 
N5 Cd1 N2 C5 53.0(8) . . . . ? 
N5 Cd1 N2 C5 -50.9(8) 3_656 . . . ? 
N3 Cd1 N2 C2 -115.2(7) . . . . ? 
N4 Cd1 N2 C2 109.7(7) . . . . ? 
N1 Cd1 N2 C2 0.8(7) . . . . ? 
N7 Cd1 N2 C2 -61.6(7) 3_657 . . . ? 
N5 Cd1 N2 C2 175.7(7) . . . . ? 
N5 Cd1 N2 C2 71.8(7) 3_656 . . . ? 
N3 Cd1 N2 C3 2.4(5) . . . . ? 
N4 Cd1 N2 C3 -132.7(5) . . . . ? 
N1 Cd1 N2 C3 118.4(5) . . . . ? 
N7 Cd1 N2 C3 56.0(5) 3_657 . . . ? 
N5 Cd1 N2 C3 -66.7(5) . . . . ? 
N5 Cd1 N2 C3 -170.6(4) 3_656 . . . ? 
N4 Cd1 N3 C4 29.8(7) . . . . ? 
N1 Cd1 N3 C4 -82.6(7) . . . . ? 
N7 Cd1 N3 C4 -162.5(7) 3_657 . . . ? 
N5 Cd1 N3 C4 104.4(7) . . . . ? 
N5 Cd1 N3 C4 149.3(6) 3_656 . . . ? 
N2 Cd1 N3 C4 -20.2(6) . . . . ? 
N3 Cd1 N4 C6 -38.2(6) . . . . ? 
N1 Cd1 N4 C6 77.6(6) . . . . ? 
N7 Cd1 N4 C6 175.1(6) 3_657 . . . ? 
N5 Cd1 N4 C6 -113.8(6) . . . . ? 
N5 Cd1 N4 C6 166.3(6) 3_656 . . . ? 
N2 Cd1 N4 C6 12.2(6) . . . . ? 
N3 Cd1 N5 C7 10.6(5) . . . . ? 
N4 Cd1 N5 C7 133.1(5) . . . . ? 
N1 Cd1 N5 C7 -132.3(9) . . . . ? 
N7 Cd1 N5 C7 -68.1(5) 3_657 . . . ? 
N5 Cd1 N5 C7 -150.0(6) 3_656 . . . ? 
N2 Cd1 N5 C7 73.1(5) . . . . ? 
N3 Cd1 N5 Cd1 160.7(2) . . . 3_656 ? 
N4 Cd1 N5 Cd1 -76.82(18) . . . 3_656 ? 
N1 Cd1 N5 Cd1 17.7(10) . . . 3_656 ? 
N7 Cd1 N5 Cd1 81.99(16) 3_657 . . 3_656 ? 
N5 Cd1 N5 Cd1 0.0 3_656 . . 3_656 ? 
N2 Cd1 N5 Cd1 -136.89(14) . . . 3_656 ? 
Cd1 N1 C1 C2 1.4(15) . . . . ? 
N1 C1 C2 N2 0(2) . . . . ? 
C5 N2 C2 C1 117.6(13) . . . . ? 
C3 N2 C2 C1 -117.0(13) . . . . ? 
Cd1 N2 C2 C1 -0.5(15) . . . . ? 
C5 N2 C3 C4 -102.6(10) . . . . ? 
C2 N2 C3 C4 130.0(9) . . . . ? 
Cd1 N2 C3 C4 14.5(9) . . . . ? 
Cd1 N3 C4 C3 38.7(12) . . . . ? 
N2 C3 C4 N3 -35.7(13) . . . . ? 
C2 N2 C5 C6 -103.9(15) . . . . ? 
C3 N2 C5 C6 131.4(14) . . . . ? 
Cd1 N2 C5 C6 13.8(17) . . . . ? 
N2 C5 C6 N4 -4(2) . . . . ? 
Cd1 N4 C6 C5 -10.5(14) . . . . ? 
Cd1 N5 C7 Fe1 145(29) . . . . ? 
Cd1 N5 C7 Fe1 0(30) 3_656 . . . ? 
C7 Fe1 C7 N5 -66(100) 3_757 . . . ? 
C9 Fe1 C7 N5 -122(30) . . . . ? 
C9 Fe1 C7 N5 58(30) 3_757 . . . ? 
C8 Fe1 C7 N5 148(30) . . . . ? 
C8 Fe1 C7 N5 -32(30) 3_757 . . . ? 
C7 Fe1 C8 N6 53(22) 3_757 . . . ? 
C7 Fe1 C8 N6 -127(22) . . . . ? 
C9 Fe1 C8 N6 141(22) . . . . ? 
C9 Fe1 C8 N6 -39(22) 3_757 . . . ? 
C8 Fe1 C8 N6 -73(100) 3_757 . . . ? 
Cd1 N7 C9 Fe1 -56(12) 3_657 . . . ? 
C7 Fe1 C9 N7 -16(12) 3_757 . . . ? 
C7 Fe1 C9 N7 164(12) . . . . ? 
C9 Fe1 C9 N7 -146(100) 3_757 . . . ? 
C8 Fe1 C9 N7 -107(12) . . . . ? 
C8 Fe1 C9 N7 73(12) 3_757 . . . ? 
  
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              27.04 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    1.118 
_refine_diff_density_min   -0.654 
_refine_diff_density_rms    0.115