#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:28:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179062 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302416.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4302416
loop_
_publ_author_name
'Duane C. Wilson'
'Shengming Liu'
'Xuenian Chen'
'Edward A. Meyers'
'Xiaoguang Bao'
'Andrey V. Prosvirin'
'Kim R. Dunbar'
'Christopher M. Hadad'
'Sheldon G. Shore'
_publ_section_title
;
Water-Free Rare Earth-Prussian Blue Type Analogues: Synthesis, Structure,
Computational Analysis, and Magnetic Data of {LnIII(DMF)6FeIII(CN)6}∞ (Ln
= Rare Earths Excluding Pm)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5725
_journal_page_last               5735
_journal_paper_doi               10.1021/ic8022369
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C24 H42 Fe N12 O6 Tb'
_chemical_formula_sum            'C24 H42 Fe N12 O6 Tb'
_chemical_formula_weight         809.47
_chemical_melting_point          ?
_chemical_name_common
; 
 Tb(DMF)6Fe(CN)6
;
_chemical_name_systematic
; 
 hexakis(N,N-dimethylformamide)Terbium(III) hexacyanoferrate(III) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.141(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6539(8)
_cell_length_b                   10.3270(3)
_cell_length_c                   18.1461(6)
_cell_measurement_reflns_used    6988
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      19.28
_cell_measurement_theta_min      2.52
_cell_volume                     3411.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49594
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26203
_diffrn_reflns_theta_full        19.32
_diffrn_reflns_theta_max         19.32
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rod
_exptl_crystal_F_000             1636
_refine_diff_density_max         0.778
_refine_diff_density_min         -2.517
_refine_diff_density_rms         0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         4187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0578P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                3764
_reflns_number_total             4187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8022369_si_002_03.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302416
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Tb1 Tb 0.0000 0.921740(17) 0.2500 0.00591(9) Uani 1 2 d S . .
Fe1 Fe -0.2500 0.7500 0.0000 0.00801(15) Uani 1 2 d S . .
C1 C -0.1630(2) 0.8071(3) 0.0863(2) 0.0099(6) Uani 1 1 d . . .
N1 N -0.11102(18) 0.8413(3) 0.13834(17) 0.0122(6) Uani 1 1 d . . .
C2 C -0.2639(2) 0.6177(3) 0.0697(2) 0.0111(6) Uani 1 1 d . . .
N2 N -0.2709(2) 0.5387(3) 0.1120(2) 0.0193(7) Uani 1 1 d . . .
C3 C -0.3078(2) 0.8744(3) 0.0332(2) 0.0131(7) Uani 1 1 d . . .
N3 N -0.3427(2) 0.9487(3) 0.0518(2) 0.0218(7) Uani 1 1 d . . .
O1 O -0.08717(16) 1.0920(2) 0.21030(16) 0.0136(5) Uani 1 1 d . . .
C11 C -0.1432(2) 1.1075(3) 0.2261(2) 0.0131(7) Uani 1 1 d . . .
H11 H -0.1430 1.0741 0.2737 0.016 Uiso 1 1 calc R . .
N11 N -0.20253(18) 1.1684(3) 0.17920(18) 0.0134(6) Uani 1 1 d . . .
C12 C -0.2087(2) 1.2156(4) 0.1012(2) 0.0184(8) Uani 1 1 d . . .
H12A H -0.1614 1.2120 0.0971 0.028 Uiso 1 1 calc R . .
H12B H -0.2259 1.3035 0.0945 0.028 Uiso 1 1 calc R . .
H12C H -0.2427 1.1624 0.0605 0.028 Uiso 1 1 calc R . .
C13 C -0.2662(2) 1.1836(4) 0.2009(2) 0.0233(8) Uani 1 1 d . . .
H13A H -0.3066 1.1350 0.1647 0.035 Uiso 1 1 calc R . .
H13B H -0.2793 1.2735 0.1981 0.035 Uiso 1 1 calc R . .
H13C H -0.2546 1.1524 0.2540 0.035 Uiso 1 1 calc R . .
O2 O 0.01285(15) 1.0076(2) 0.13389(14) 0.0114(5) Uani 1 1 d . . .
C21 C -0.0375(2) 1.0585(3) 0.0760(2) 0.0098(6) Uani 1 1 d . . .
H21 H -0.0856 1.0340 0.0665 0.012 Uiso 1 1 calc R . .
N21 N -0.02642(17) 1.1446(2) 0.02787(17) 0.0099(6) Uani 1 1 d . . .
C22 C -0.0880(2) 1.2007(3) -0.0369(2) 0.0151(7) Uani 1 1 d . . .
H22A H -0.1325 1.1575 -0.0409 0.023 Uiso 1 1 calc R . .
H22B H -0.0804 1.1907 -0.0858 0.023 Uiso 1 1 calc R . .
H22C H -0.0917 1.2911 -0.0267 0.023 Uiso 1 1 calc R . .
C23 C 0.0470(2) 1.1906(3) 0.0385(2) 0.0152(7) Uani 1 1 d . . .
H23A H 0.0530 1.2779 0.0580 0.023 Uiso 1 1 calc R . .
H23B H 0.0530 1.1879 -0.0116 0.023 Uiso 1 1 calc R . .
H23C H 0.0831 1.1360 0.0761 0.023 Uiso 1 1 calc R . .
O3 O 0.04521(16) 0.7465(2) 0.19979(15) 0.0147(5) Uani 1 1 d . . .
C31 C 0.0787(2) 0.6433(3) 0.2290(2) 0.0129(7) Uani 1 1 d . . .
H31 H 0.1180 0.6468 0.2777 0.015 Uiso 1 1 calc R . .
N31 N 0.06001(19) 0.5308(3) 0.19292(18) 0.0147(6) Uani 1 1 d . . .
C32 C 0.1044(3) 0.4155(3) 0.2261(3) 0.0241(9) Uani 1 1 d . . .
H32A H 0.1422 0.4367 0.2763 0.036 Uiso 1 1 calc R . .
H32B H 0.1264 0.3856 0.1901 0.036 Uiso 1 1 calc R . .
H32C H 0.0737 0.3487 0.2335 0.036 Uiso 1 1 calc R . .
C33 C -0.0016(3) 0.5172(4) 0.1169(3) 0.0259(9) Uani 1 1 d . . .
H33A H -0.0337 0.5903 0.1087 0.039 Uiso 1 1 calc R . .
H33B H -0.0281 0.4393 0.1173 0.039 Uiso 1 1 calc R . .
H33C H 0.0166 0.5129 0.0747 0.039 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.3496 2.7654 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Tb1 O3 79.07(12) . 2 ?
O3 Tb1 O1 110.73(9) . 2 ?
O3 Tb1 O1 142.22(9) 2 2 ?
O3 Tb1 O1 142.22(9) . . ?
O3 Tb1 O1 110.73(9) 2 . ?
O1 Tb1 O1 84.20(13) 2 . ?
O3 Tb1 O2 76.23(8) . . ?
O3 Tb1 O2 144.24(8) 2 . ?
O1 Tb1 O2 71.80(9) 2 . ?
O1 Tb1 O2 76.15(8) . . ?
O3 Tb1 O2 144.24(8) . 2 ?
O3 Tb1 O2 76.23(8) 2 2 ?
O1 Tb1 O2 76.15(8) 2 2 ?
O1 Tb1 O2 71.80(9) . 2 ?
O2 Tb1 O2 136.35(11) . 2 ?
O3 Tb1 N1 76.76(10) . . ?
O3 Tb1 N1 73.45(9) 2 . ?
O1 Tb1 N1 143.60(9) 2 . ?
O1 Tb1 N1 71.91(9) . . ?
O2 Tb1 N1 75.99(9) . . ?
O2 Tb1 N1 119.33(9) 2 . ?
O3 Tb1 N1 73.45(9) . 2 ?
O3 Tb1 N1 76.76(10) 2 2 ?
O1 Tb1 N1 71.91(9) 2 2 ?
O1 Tb1 N1 143.60(9) . 2 ?
O2 Tb1 N1 119.33(9) . 2 ?
O2 Tb1 N1 75.99(9) 2 2 ?
N1 Tb1 N1 141.08(12) . 2 ?
C1 Fe1 C1 180.00(19) 7_465 . ?
C1 Fe1 C2 89.19(14) 7_465 7_465 ?
C1 Fe1 C2 90.81(14) . 7_465 ?
C1 Fe1 C2 90.81(14) 7_465 . ?
C1 Fe1 C2 89.19(14) . . ?
C2 Fe1 C2 180.00(15) 7_465 . ?
C1 Fe1 C3 90.66(14) 7_465 . ?
C1 Fe1 C3 89.34(14) . . ?
C2 Fe1 C3 88.84(14) 7_465 . ?
C2 Fe1 C3 91.16(14) . . ?
C1 Fe1 C3 89.34(14) 7_465 7_465 ?
C1 Fe1 C3 90.66(14) . 7_465 ?
C2 Fe1 C3 91.16(14) 7_465 7_465 ?
C2 Fe1 C3 88.84(14) . 7_465 ?
C3 Fe1 C3 180.00(19) . 7_465 ?
N1 C1 Fe1 179.6(3) . . ?
C1 N1 Tb1 178.3(3) . . ?
N2 C2 Fe1 178.8(4) . . ?
N3 C3 Fe1 178.9(4) . . ?
C11 O1 Tb1 128.7(2) . . ?
O1 C11 N11 123.8(3) . . ?
O1 C11 H11 118.1 . . ?
N11 C11 H11 118.1 . . ?
C11 N11 C13 121.3(3) . . ?
C11 N11 C12 121.1(3) . . ?
C13 N11 C12 117.5(3) . . ?
N11 C12 H12A 109.5 . . ?
N11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C21 O2 Tb1 125.6(2) . . ?
O2 C21 N21 124.1(3) . . ?
O2 C21 H21 117.9 . . ?
N21 C21 H21 117.9 . . ?
C21 N21 C22 120.6(3) . . ?
C21 N21 C23 122.1(3) . . ?
C22 N21 C23 117.2(3) . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N21 C23 H23A 109.5 . . ?
N21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C31 O3 Tb1 134.7(2) . . ?
O3 C31 N31 122.3(4) . . ?
O3 C31 H31 118.9 . . ?
N31 C31 H31 118.9 . . ?
C31 N31 C33 122.1(3) . . ?
C31 N31 C32 120.1(3) . . ?
C33 N31 C32 117.6(3) . . ?
N31 C32 H32A 109.5 . . ?
N31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N31 C33 H33A 109.5 . . ?
N31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
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
Tb1 O3 2.346(2) . ?
Tb1 O3 2.346(2) 2 ?
Tb1 O1 2.369(2) 2 ?
Tb1 O1 2.369(2) . ?
Tb1 O2 2.385(2) . ?
Tb1 O2 2.385(2) 2 ?
Tb1 N1 2.495(3) . ?
Tb1 N1 2.495(3) 2 ?
Fe1 C1 1.924(4) 7_465 ?
Fe1 C1 1.924(4) . ?
Fe1 C2 1.950(3) 7_465 ?
Fe1 C2 1.950(3) . ?
Fe1 C3 1.955(3) . ?
Fe1 C3 1.955(3) 7_465 ?
C1 N1 1.155(5) . ?
C2 N2 1.162(5) . ?
C3 N3 1.161(5) . ?
O1 C11 1.249(5) . ?
C11 N11 1.315(5) . ?
C11 H11 0.9300 . ?
N11 C13 1.454(5) . ?
N11 C12 1.459(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O2 C21 1.254(4) . ?
C21 N21 1.321(4) . ?
C21 H21 0.9300 . ?
N21 C22 1.452(5) . ?
N21 C23 1.460(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
O3 C31 1.260(4) . ?
C31 N31 1.317(5) . ?
C31 H31 0.9300 . ?
N31 C33 1.459(5) . ?
N31 C32 1.464(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
