Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_rf 
_database_code_CSD                  184701

_journal_coden_Cambridge      186

loop_
_publ_author_name   
_publ_author_address
'Martin, S.'
;
Departamento de Quimica Inorganica
Facultad de Farmacia
Universidad del Pais Vasco
Apdo. 450
01080 Vitoria
Spain
;
'Barandika, M. G.' 
;
Departamento de Quimica Inorganica
Facultad de Farmacia
Universidad del Pais Vasco
Apdo. 450
01080 Vitoria
Spain
;
'Cortes, R.'
;
Departamento de Quimica Inorganica
Facultad de Farmacia
Universidad del Pais Vasco
Apdo. 450
01080 Vitoria
Spain
;
'Larramendi, J. I. R.'
;
Departamento de Quimica Inorganica
Facultad de Farmacia
Universidad del Pais Vasco
Apdo. 450
01080 Vitoria
Spain
;
'Ezpeleta, J. M.'
;
Departamento de Fisica Aplicada II
Facultad de Farmacia
Universidad del Pais Vasco
Apdo. 450
01080 Vitoria
Spain
;
'Lezama, L.'
;
Departamento de Quimica Inorganica
Facultad de Ciencias
Universidad del Pais Vasco
Apdo. 644
48080 Bilbao
Spain
;
'Rojo, T.'
;
Departamento de Quimica Inorganica
Facultad de Ciencias
Universidad del Pais Vasco
Apdo. 644
48080 Bilbao
Spain
;

_publ_contact_author_name         'Martin, S.'
_publ_contact_author_address
;
Departamento de Quimica Inorganica
Facultad de Farmacia
Universidad del Pais Vasco
Apdo. 450
01080 Vitoria
Spain
;
_publ_contact_author_email        'qibmahes@vc.ehu.es'
_publ_requested_journal           'J.Chem.Soc.,Dalton Trans.'

_publ_section_title		
;
Structural Analysis and Magnetic Properties of the 1D Compound
[Fe(dca)2bipy(H2O)]·1/2H2O and the 3D Compound [Ni(dca)2bipy]
(dca==dicyanamide; bipy==4,4'-bipyridine)
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C14 H11 Fe N8 O1.50' 
_chemical_formula_weight          371.16 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'Fe'  'Fe'   0.3463   0.8444 
'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' 
'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' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            tetragonal
_symmetry_space_group_name_H-M    'I 41 c d'

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x, -y, z' 
'-x, y, z+1/2' 
'x, -y, z+1/2' 
'y, -x+1/2, z+1/4' 
'-y, x+1/2, z+1/4' 
'y+1/2, x, z+1/4' 
'-y+1/2, -x, z+1/4' 
'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' 
'x+1/2, -y+1/2, z+1' 
'y+1/2, -x+1, z+3/4' 
'-y+1/2, x+1, z+3/4' 
'y+1, x+1/2, z+3/4' 
'-y+1, -x+1/2, z+3/4' 

_cell_length_a                    22.366(5) 
_cell_length_b                    22.366(5) 
_cell_length_c                    13.311(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      6658(2) 
_cell_formula_units_Z             16 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     .
_cell_measurement_theta_min       . 
_cell_measurement_theta_max       . 

_exptl_crystal_description        'prismatic'
_exptl_crystal_colour             'dark red'
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.09
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.481 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3024 
_exptl_absorpt_coefficient_mu     0.928 
_exptl_absorpt_correction_type    'numerical'
_exptl_absorpt_correction_T_min   0.9060
_exptl_absorpt_correction_T_max   0.9388

_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   'STOE IPDS'
_diffrn_measurement_method
; 
image plate with oscillating crystal geometry
;
_diffrn_detector_area_resol_mean  6.7   
_diffrn_standards_number          .
_diffrn_standards_interval_count  .
_diffrn_standards_interval_time   .
_diffrn_standards_decay_%         .
_diffrn_reflns_number             20690 
_diffrn_reflns_av_R_equivalents   0.1280 
_diffrn_reflns_av_sigmaI/netI     0.1350 
_diffrn_reflns_limit_h_min        -27 
_diffrn_reflns_limit_h_max        27 
_diffrn_reflns_limit_k_min        -27 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.55 
_diffrn_reflns_theta_max          25.93 
_reflns_number_total              3143 
_reflns_number_gt                 1770 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'STOE IPDS software (STOE, 1998)'
_computing_cell_refinement        'STOE IPDS software (STOE, 1998)'
_computing_data_reduction         'JANA98 (Petricek & Dusek, 1998)'
_computing_structure_solution
;
SIR97 (Altomare, Cascaramo, Giacovazzo, Guagliardi, Molitemi, Burla,
Polidori, Camalli & Spagna, 1997)
;
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP (Johnson, 1965)'
_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. 
H atoms belonging to water molecules could not be determined.
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme
'calc'
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00132(16) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.01(4) 
_refine_ls_number_reflns          3143 
_refine_ls_number_parameters      244 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0954 
_refine_ls_R_factor_gt            0.0458 
_refine_ls_wR_factor_ref          0.1284 
_refine_ls_wR_factor_gt           0.1086 
_refine_ls_goodness_of_fit_ref    0.648 
_refine_ls_restrained_S_all       0.648 
_refine_ls_shift/su_max           0.011 
_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 
Fe Fe 0.60971(3) 0.40465(3) 0.3527(2) 0.0306(2) Uani 1 d . . . 
O11 O 0.5574(6) 0.4842(7) 0.3889(18) 0.041(4) Uani 0.50 d P . . 
O12 O 0.5589(7) 0.4891(9) 0.3184(15) 0.036(4) Uani 0.50 d P . . 
O2 O 0.5310(3) 0.4985(6) 0.105(3) 0.045(2) Uani 0.50 d P . . 
N1 N 0.67320(18) 0.33009(16) 0.3497(7) 0.0257(9) Uani 1 d . . . 
N2 N 0.6618(3) 0.4457(3) 0.2356(6) 0.0479(19) Uani 1 d . . . 
N3 N 0.6652(3) 0.4435(3) 0.4688(6) 0.053(2) Uani 1 d . . . 
N4 N 0.5567(3) 0.3631(3) 0.4677(8) 0.057(2) Uani 1 d . . . 
N5 N 0.5548(3) 0.3638(3) 0.2405(7) 0.059(2) Uani 1 d . . . 
N61 N 0.515(2) 0.3163(13) 0.627(3) 0.077(10) Uani 0.50 d P . . 
N62 N 0.4966(14) 0.3202(12) 0.584(3) 0.064(15) Uani 0.50 d P . . 
N7 N 0.7131(3) 0.4969(5) 0.6066(19) 0.086(3) Uani 1 d . . . 
N8 N 0.8786(2) 0.0878(2) 0.352(2) 0.0532(14) Uani 1 d . . . 
C1 C 0.6839(4) 0.4730(4) 0.1713(8) 0.049(2) Uani 1 d . . . 
C2 C 0.6846(4) 0.4698(4) 0.5348(8) 0.048(2) Uani 1 d . . . 
C3 C 0.5310(4) 0.3446(4) 0.5362(10) 0.056(3) Uani 1 d . . . 
C4 C 0.5270(5) 0.3459(4) 0.1763(11) 0.063(3) Uani 1 d . . . 
C5 C 0.7320(2) 0.3397(2) 0.3495(8) 0.0303(13) Uani 1 d . . . 
H5 H 0.7457 0.3790 0.3507 0.036 Uiso 1 calc R . . 
C6 C 0.7733(2) 0.2946(2) 0.3476(7) 0.0278(12) Uani 1 d . . . 
H6 H 0.8139 0.3035 0.3459 0.033 Uiso 1 calc R . . 
C7 C 0.7546(2) 0.23542(19) 0.3483(9) 0.0246(11) Uani 1 d . . . 
C8 C 0.6938(2) 0.2256(2) 0.3482(7) 0.0276(12) Uani 1 d . . . 
H8 H 0.6790 0.1867 0.3467 0.033 Uiso 1 calc R . . 
C9 C 0.6548(2) 0.2735(2) 0.3502(8) 0.0302(12) Uani 1 d . . . 
H9 H 0.6139 0.2659 0.3521 0.036 Uiso 1 calc R . . 
C10 C 0.7980(2) 0.1847(2) 0.3488(9) 0.0294(13) Uani 1 d . . . 
C11 C 0.8588(2) 0.1934(3) 0.3510(10) 0.0462(16) Uani 1 d . . . 
H11 H 0.8742 0.2320 0.3507 0.055 Uiso 1 calc R . . 
C12 C 0.8971(3) 0.1449(3) 0.3538(10) 0.0558(18) Uani 1 d . . . 
H12 H 0.9380 0.1523 0.3573 0.067 Uiso 1 calc R . . 
C13 C 0.8194(3) 0.0805(2) 0.3493(10) 0.0551(18) Uani 1 d . . . 
H13 H 0.8048 0.0415 0.3494 0.066 Uiso 1 calc R . . 
C14 C 0.7784(3) 0.1263(2) 0.3467(10) 0.0461(17) Uani 1 d . . . 
H14 H 0.7377 0.1179 0.3437 0.055 Uiso 1 calc R . . 

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 
Fe 0.0259(4) 0.0257(4) 0.0403(5) -0.0027(8) -0.0006(8) 0.0012(3) 
O11 0.021(7) 0.013(5) 0.089(16) 0.014(8) 0.006(8) -0.008(5) 
O12 0.041(9) 0.040(7) 0.028(9) 0.005(7) 0.008(7) 0.014(6) 
O2 0.030(3) 0.078(5) 0.028(6) 0.030(5) -0.007 -0.009(5) 
N1 0.029(2) 0.023(2) 0.025(3) 0.001(3) 0.001(4) -0.0017(16) 
N2 0.064(4) 0.035(3) 0.045(5) 0.014(3) -0.005(4) -0.005(3) 
N3 0.053(4) 0.060(4) 0.046(6) -0.027(4) 0.009(4) -0.009(3) 
N4 0.054(4) 0.047(4) 0.071(6) -0.009(4) 0.029(4) -0.009(3) 
N5 0.052(4) 0.048(4) 0.077(7) 0.008(4) -0.037(4) -0.008(3) 
N61 0.114(19) 0.059(14) 0.06(2) 0.028(13) 0.078(17) 0.055(12) 
N62 0.13(3) 0.029(10) 0.04(3) -0.005(10) 0.048(19) -0.016(12) 
N7 0.070(4) 0.116(5) 0.070(6) -0.065(6) -0.029(10) 0.016(6) 
N8 0.051(3) 0.038(3) 0.071(4) 0.002(7) -0.004(9) 0.014(2) 
C1 0.051(5) 0.041(5) 0.056(8) 0.015(5) -0.009(5) 0.006(4) 
C2 0.052(5) 0.049(5) 0.043(7) -0.021(4) 0.010(4) -0.011(4) 
C3 0.054(7) 0.033(5) 0.082(9) -0.008(5) 0.035(6) 0.006(4) 
C4 0.061(7) 0.028(5) 0.100(10) 0.019(5) -0.040(7) -0.004(4) 
C5 0.037(3) 0.020(2) 0.034(4) 0.005(4) 0.005(4) 0.003(2) 
C6 0.026(3) 0.031(3) 0.027(4) -0.003(4) -0.001(4) -0.001(2) 
C7 0.037(3) 0.025(3) 0.012(3) 0.000(5) 0.002(4) 0.001(2) 
C8 0.032(3) 0.023(3) 0.028(4) -0.002(4) 0.001(4) -0.0067(19) 
C9 0.031(3) 0.029(3) 0.031(4) -0.002(4) 0.000(4) 0.001(2) 
C10 0.037(3) 0.032(3) 0.020(3) 0.003(4) 0.005(5) 0.007(2) 
C11 0.038(3) 0.030(3) 0.071(5) 0.007(6) -0.004(6) 0.001(2) 
C12 0.034(3) 0.045(3) 0.088(6) 0.003(6) 0.004(5) 0.010(3) 
C13 0.054(4) 0.027(3) 0.084(6) -0.001(6) 0.003(6) 0.007(2) 
C14 0.034(3) 0.028(3) 0.077(5) -0.006(5) -0.003(5) 0.006(2) 

_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 
Fe N5 2.139(9) . ? 
Fe N4 2.148(9) . ? 
Fe N2 2.152(9) . ? 
Fe N3 2.164(8) . ? 
Fe O11 2.183(17) . ? 
Fe N1 2.191(4) . ? 
Fe O12 2.25(2) . ? 
O11 O12 0.944(10) . ? 
O2 O2 1.387(12) 2_665 ? 
N1 C9 1.331(6) . ? 
N1 C5 1.333(6) . ? 
N2 C1 1.162(12) . ? 
N3 C2 1.142(11) . ? 
N4 C3 1.154(13) . ? 
N5 C4 1.130(13) . ? 
N61 N62 0.71(5) . ? 
N61 C4 1.32(3) 3_655 ? 
N61 C3 1.41(4) . ? 
N62 C3 1.14(3) . ? 
N62 C4 1.46(4) 3_655 ? 
N7 C1 1.27(2) 4_565 ? 
N7 C2 1.299(19) . ? 
N8 C13 1.334(8) . ? 
N8 C12 1.343(7) . ? 
C1 N7 1.27(2) 4_564 ? 
C4 N61 1.32(3) 3_654 ? 
C4 N62 1.46(4) 3_654 ? 
C5 C6 1.369(6) . ? 
C6 C7 1.387(7) . ? 
C7 C8 1.379(7) . ? 
C7 C10 1.492(6) . ? 
C8 C9 1.382(7) . ? 
C10 C11 1.374(7) . ? 
C10 C14 1.378(7) . ? 
C11 C12 1.382(8) . ? 
C13 C14 1.376(7) . ? 

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 
N5 Fe N4 89.8(2) . . ? 
N5 Fe N2 89.2(4) . . ? 
N4 Fe N2 179.0(4) . . ? 
N5 Fe N3 178.3(3) . . ? 
N4 Fe N3 89.0(4) . . ? 
N2 Fe N3 92.02(19) . . ? 
N5 Fe O11 101.2(6) . . ? 
N4 Fe O11 84.3(5) . . ? 
N2 Fe O11 95.8(5) . . ? 
N3 Fe O11 79.8(6) . . ? 
N5 Fe N1 91.9(3) . . ? 
N4 Fe N1 92.4(3) . . ? 
N2 Fe N1 87.7(3) . . ? 
N3 Fe N1 86.9(3) . . ? 
O11 Fe N1 166.4(7) . . ? 
N5 Fe O12 85.8(5) . . ? 
N4 Fe O12 103.2(6) . . ? 
N2 Fe O12 76.6(6) . . ? 
N3 Fe O12 95.6(5) . . ? 
O11 Fe O12 24.5(3) . . ? 
N1 Fe O12 164.2(6) . . ? 
O12 O11 Fe 82(2) . . ? 
O11 O12 Fe 74(2) . . ? 
C9 N1 C5 117.3(4) . . ? 
C9 N1 Fe 121.5(3) . . ? 
C5 N1 Fe 121.1(3) . . ? 
C1 N2 Fe 171.3(7) . . ? 
C2 N3 Fe 166.6(7) . . ? 
C3 N4 Fe 173.1(9) . . ? 
C4 N5 Fe 174.5(8) . . ? 
N62 N61 C4 86(5) . 3_655 ? 
N62 N61 C3 53(4) . . ? 
C4 N61 C3 113(2) 3_655 . ? 
N61 N62 C3 97(6) . . ? 
N61 N62 C4 65(4) . 3_655 ? 
C3 N62 C4 122(2) . 3_655 ? 
C1 N7 C2 119.5(6) 4_565 . ? 
C13 N8 C12 115.1(5) . . ? 
N2 C1 N7 174.0(11) . 4_564 ? 
N3 C2 N7 172.7(9) . . ? 
N62 C3 N4 162(2) . . ? 
N62 C3 N61 30(3) . . ? 
N4 C3 N61 165(2) . . ? 
N5 C4 N61 161(2) . 3_654 ? 
N5 C4 N62 168(2) . 3_654 ? 
N61 C4 N62 29(2) 3_654 3_654 ? 
N1 C5 C6 123.1(5) . . ? 
C5 C6 C7 120.1(5) . . ? 
C8 C7 C6 116.7(4) . . ? 
C8 C7 C10 121.3(5) . . ? 
C6 C7 C10 122.0(5) . . ? 
C7 C8 C9 119.9(4) . . ? 
N1 C9 C8 122.8(5) . . ? 
C11 C10 C14 116.7(5) . . ? 
C11 C10 C7 122.4(5) . . ? 
C14 C10 C7 120.9(5) . . ? 
C10 C11 C12 120.3(5) . . ? 
N8 C12 C11 123.6(5) . . ? 
N8 C13 C14 124.8(5) . . ? 
C13 C14 C10 119.5(5) . . ? 

_diffrn_measured_fraction_theta_max    0.494 
_diffrn_reflns_theta_full              25.93 
_diffrn_measured_fraction_theta_full   0.494 
_refine_diff_density_max    0.905 
_refine_diff_density_min   -0.325 
_refine_diff_density_rms    0.085