# 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

_publ_contact_author_name        'Robert Podgajny'
_publ_contact_author_email       PODGAJNY@CHEMIA.UJ.EDU.PL

_publ_section_title              
;
Iron(II)-octacyanoniobate(IV) ferromagnet with TC 43 K
;
_publ_requested_category         FM
loop_
_publ_author_name
'Robert Podgajny'
'Maria Balanda'
'Mariusz Czapla'
'Czeslaw Kapusta'
'Magdalena Makarewicz'
'Wojciech Nitek'
;
R.Peka
;
'Robert Peka'
'Dawid Pinkowicz'
'Barbara Sieklucka'
'Dariusz Zajac'
'Jan Zukrowski'

# Attachment 'archive_FeNb.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-09-21 at 16:36:56
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\program files\wingx\files\archive.dat
# CIF files read : dp009 import struct

data_dp009
_database_code_depnum_ccdc_archive 'CCDC 717898'

_audit_creation_date             2008-09-21T16:36:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            dpx
_chemical_formula_moiety         'C8 Fe2 N8 Nb1'
_chemical_formula_sum            'C32 H64 Fe8 N32 Nb4 O32'
_chemical_formula_weight         2227.08
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4/m
_symmetry_space_group_name_Hall  -I4
_symmetry_Int_Tables_number      87
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   11.989(5)
_cell_length_b                   11.989(5)
_cell_length_c                   13.237(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1902.6(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3577
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.15
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.0028683
_diffrn_orient_matrix_ub_12      0.0833123
_diffrn_orient_matrix_ub_13      -0.0029744
_diffrn_orient_matrix_ub_21      0.0320625
_diffrn_orient_matrix_ub_22      -0.0038492
_diffrn_orient_matrix_ub_23      -0.0768989
_diffrn_orient_matrix_ub_31      -0.0696902
_diffrn_orient_matrix_ub_32      0.0013595
_diffrn_orient_matrix_ub_33      -0.0291249
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_number            6916
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             1140
_reflns_number_gt                1025
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.0230P)^2^+4.2132P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_number_reflns         1140
_refine_ls_number_parameters     76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0618
_refine_ls_wR_factor_gt          0.0599
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.42
_refine_diff_density_rms         0.089

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.073 0.622 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Nb1 Nb 0 0 0.24964(3) 0.01371(15) Uani 1 4 d S . .
Fe2 Fe 0.30913(4) 0.19885(4) 0 0.02010(16) Uani 1 2 d S . .
O1 O 0.2161(2) 0.3502(2) 0 0.0384(7) Uani 1 2 d S . .
H1B H 0.1872 0.3531 0.0561 0.058 Uiso 1 1 d R . .
O2 O 0.3941(3) 0.0458(3) 0 0.0491(8) Uani 1 2 d S . .
H2A H 0.3896 0.0093 0.0592 0.074 Uiso 1 1 d R . .
N1 N 0.20183(18) 0.13010(19) 0.11359(18) 0.0306(5) Uani 1 1 d . . .
N3 N 0.41779(18) 0.27614(19) -0.11136(17) 0.0291(5) Uani 1 1 d . . .
C1 C 0.1359(2) 0.0833(2) 0.15971(19) 0.0226(5) Uani 1 1 d . . .
C3 C 0.45091(19) 0.3491(2) -0.15868(19) 0.0220(5) Uani 1 1 d . . .
O3 O 0.0880(3) 0.3814(3) 0.1876(3) 0.0759(10) Uani 1 1 d . . .
H3A H 0.097(6) 0.458(7) 0.228(5) 0.15(3) Uiso 1 1 d . . .
H3B H 0.112(7) 0.335(7) 0.219(6) 0.15(3) Uiso 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
Nb1 0.01354(17) 0.01354(17) 0.0140(2) 0 0 0
Fe2 0.0201(3) 0.0215(3) 0.0186(3) 0 0 -0.00657(18)
O1 0.0349(16) 0.0373(16) 0.0429(17) 0 0 0.0043(13)
O2 0.0434(18) 0.0371(17) 0.067(2) 0 0 0.0085(14)
N1 0.0273(12) 0.0354(13) 0.0291(13) 0.0034(10) 0.0044(9) -0.0074(9)
N3 0.0302(12) 0.0307(12) 0.0265(12) 0.0064(9) 0.0019(9) -0.0074(9)
C1 0.0232(12) 0.0213(12) 0.0233(13) 0.0020(10) 0.0011(10) 0.0004(9)
C3 0.0193(12) 0.0234(12) 0.0232(12) 0.0019(10) 0.0011(9) 0.0000(9)
O3 0.105(3) 0.0544(19) 0.068(2) 0.0041(17) 0.0091(18) -0.0067(18)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
Nb1 C1 2.251(3) 3 ?
Nb1 C1 2.251(3) 2 ?
Nb1 C1 2.251(3) . ?
Nb1 C1 2.251(3) 4 ?
Nb1 C3 2.257(3) 7 ?
Nb1 C3 2.257(3) 6_545 ?
Nb1 C3 2.257(3) 5_445 ?
Nb1 C3 2.257(3) 8_455 ?
Fe2 O2 2.099(3) . ?
Fe2 O1 2.130(3) . ?
Fe2 N1 2.144(2) 11 ?
Fe2 N1 2.144(2) . ?
Fe2 N3 2.175(2) 11 ?
Fe2 N3 2.175(2) . ?
O1 H1B 0.82 . ?
O2 H2A 0.8991 . ?
N1 C1 1.145(3) . ?
N3 C3 1.146(3) . ?
C3 Nb1 2.257(3) 5_554 ?
O3 H3A 1.07(9) . ?
O3 H3B 0.75(8) . ?

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 Nb1 C1 73.77(6) 3 2 ?
C1 Nb1 C1 116.16(13) 3 . ?
C1 Nb1 C1 73.77(6) 2 . ?
C1 Nb1 C1 73.77(6) 3 4 ?
C1 Nb1 C1 116.16(13) 2 4 ?
C1 Nb1 C1 73.77(6) . 4 ?
C1 Nb1 C3 145.96(9) 3 7 ?
C1 Nb1 C3 79.62(9) 2 7 ?
C1 Nb1 C3 74.93(9) . 7 ?
C1 Nb1 C3 138.49(9) 4 7 ?
C1 Nb1 C3 138.49(9) 3 6_545 ?
C1 Nb1 C3 145.96(9) 2 6_545 ?
C1 Nb1 C3 79.62(9) . 6_545 ?
C1 Nb1 C3 74.93(9) 4 6_545 ?
C3 Nb1 C3 73.19(6) 7 6_545 ?
C1 Nb1 C3 74.93(9) 3 5_445 ?
C1 Nb1 C3 138.49(9) 2 5_445 ?
C1 Nb1 C3 145.96(9) . 5_445 ?
C1 Nb1 C3 79.62(9) 4 5_445 ?
C3 Nb1 C3 114.94(13) 7 5_445 ?
C3 Nb1 C3 73.19(6) 6_545 5_445 ?
C1 Nb1 C3 79.62(9) 3 8_455 ?
C1 Nb1 C3 74.93(9) 2 8_455 ?
C1 Nb1 C3 138.49(9) . 8_455 ?
C1 Nb1 C3 145.96(9) 4 8_455 ?
C3 Nb1 C3 73.19(6) 7 8_455 ?
C3 Nb1 C3 114.94(13) 6_545 8_455 ?
C3 Nb1 C3 73.19(6) 5_445 8_455 ?
O2 Fe2 O1 177.46(12) . . ?
O2 Fe2 N1 87.44(9) . 11 ?
O1 Fe2 N1 90.75(8) . 11 ?
O2 Fe2 N1 87.44(9) . . ?
O1 Fe2 N1 90.75(8) . . ?
N1 Fe2 N1 89.08(13) 11 . ?
O2 Fe2 N3 94.68(9) . 11 ?
O1 Fe2 N3 87.19(9) . 11 ?
N1 Fe2 N3 177.26(9) 11 11 ?
N1 Fe2 N3 92.74(9) . 11 ?
O2 Fe2 N3 94.68(9) . . ?
O1 Fe2 N3 87.19(9) . . ?
N1 Fe2 N3 92.74(9) 11 . ?
N1 Fe2 N3 177.26(9) . . ?
N3 Fe2 N3 85.36(12) 11 . ?
Fe2 O1 H1B 104.9 . . ?
Fe2 O2 H2A 113.3 . . ?
C1 N1 Fe2 167.5(2) . . ?
C3 N3 Fe2 154.5(2) . . ?
N1 C1 Nb1 176.7(2) . . ?
N3 C3 Nb1 174.6(2) . 5_554 ?
H3A O3 H3B 109(7) . . ?