#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:28:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179062 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302420.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_4302420
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 Yb'
_chemical_formula_sum            'C24 H42 Fe N12 O6 Yb'
_chemical_formula_weight         823.59
_chemical_melting_point          ?
_chemical_name_common
; 
 Yb(DMF)6Fe(CN)6
;
_chemical_name_systematic
; 
 hexakis(N,N-dimethylformamide)Ytterbium(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                 113.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.768(4)
_cell_length_b                   10.326(2)
_cell_length_c                   18.258(4)
_cell_measurement_reflns_used    8906
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      33.57
_cell_measurement_theta_min      2.45
_cell_volume                     3429.6(14)
_computing_cell_refinement       'Bruker SAINT v7.23A'
_computing_data_collection       'Bruker APEX2 v2.0-2'
_computing_data_reduction        'Bruker SAINT v7.23A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 0.7
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Platinum 200 CCD detector (Fairchild)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'Channel-cut Si(111)'
_diffrn_radiation_source         'Beamline 11.3.1 ALS at LBL'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.77507
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24444
_diffrn_reflns_theta_full        33.65
_diffrn_reflns_theta_max         33.65
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS v2.10; Sheldrick, 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Cylindrical
_exptl_crystal_F_000             1655
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.788
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         5220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0349
_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)+(0.0141P)²+0.5765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                4710
_reflns_number_total             5220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8022369_si_002_07.cif
_cod_data_source_block           9
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_database_code               4302420
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
Yb1 Yb 0.0000 0.579510(14) 0.2500 0.01561(6) Uani 1 2 d S . .
Fe1 Fe 0.2500 0.7500 0.5000 0.01848(12) Uani 1 2 d S . .
C1 C 0.16174(17) 0.6924(3) 0.41313(18) 0.0213(5) Uani 1 1 d . . .
N1 N 0.10915(15) 0.6587(2) 0.36046(15) 0.0245(5) Uani 1 1 d . . .
C2 C 0.26311(18) 0.8833(3) 0.43071(19) 0.0241(6) Uani 1 1 d . . .
N2 N 0.26950(19) 0.9627(3) 0.3889(2) 0.0362(7) Uani 1 1 d . . .
C3 C 0.30766(19) 0.6269(3) 0.4664(2) 0.0274(6) Uani 1 1 d . . .
N3 N 0.3418(2) 0.5526(3) 0.4474(2) 0.0421(8) Uani 1 1 d . . .
O1 O 0.08593(14) 0.41375(19) 0.28950(16) 0.0269(5) Uani 1 1 d . . .
N11 N 0.20057(15) 0.3338(3) 0.32010(17) 0.0276(5) Uani 1 1 d . . .
C11 C 0.14149(19) 0.3970(3) 0.2741(2) 0.0248(6) Uani 1 1 d . . .
H11 H 0.1411 0.4324 0.2258 0.030 Uiso 1 1 calc R . .
C12 C 0.2078(2) 0.2858(4) 0.3980(2) 0.0356(8) Uani 1 1 d . . .
H12A H 0.2401 0.3435 0.4396 0.053 Uiso 1 1 calc R . .
H12B H 0.2288 0.1985 0.4061 0.053 Uiso 1 1 calc R . .
H12C H 0.1592 0.2833 0.4007 0.053 Uiso 1 1 calc R . .
C13 C 0.2644(2) 0.3162(4) 0.2992(2) 0.0407(9) Uani 1 1 d . . .
H13A H 0.2532 0.3502 0.2456 0.061 Uiso 1 1 calc R . .
H13B H 0.2761 0.2238 0.3006 0.061 Uiso 1 1 calc R . .
H13C H 0.3067 0.3628 0.3375 0.061 Uiso 1 1 calc R . .
O2 O 0.01201(12) 0.4943(2) 0.13677(12) 0.0227(4) Uani 1 1 d . . .
N21 N -0.02564(14) 0.3574(2) 0.03009(15) 0.0224(5) Uani 1 1 d . . .
C21 C -0.03751(18) 0.4431(3) 0.07821(18) 0.0208(5) Uani 1 1 d . . .
H21 H -0.0869 0.4670 0.0673 0.025 Uiso 1 1 calc R . .
C22 C -0.08709(19) 0.3015(3) -0.03612(19) 0.0298(7) Uani 1 1 d . . .
H22A H -0.1322 0.3493 -0.0435 0.045 Uiso 1 1 calc R . .
H22B H -0.0930 0.2105 -0.0246 0.045 Uiso 1 1 calc R . .
H22C H -0.0774 0.3072 -0.0847 0.045 Uiso 1 1 calc R . .
C23 C 0.04815(19) 0.3138(3) 0.0426(2) 0.0293(6) Uani 1 1 d . . .
H23A H 0.0844 0.3696 0.0820 0.044 Uiso 1 1 calc R . .
H23B H 0.0548 0.3181 -0.0078 0.044 Uiso 1 1 calc R . .
H23C H 0.0548 0.2243 0.0620 0.044 Uiso 1 1 calc R . .
O3 O 0.04447(14) 0.7493(2) 0.20047(13) 0.0281(5) Uani 1 1 d . . .
N31 N 0.05986(17) 0.9645(3) 0.19252(17) 0.0297(6) Uani 1 1 d . . .
C31 C 0.07787(19) 0.8519(3) 0.22887(19) 0.0256(6) Uani 1 1 d . . .
H31 H 0.1181 0.8486 0.2790 0.031 Uiso 1 1 calc R . .
C32 C 0.1046(3) 1.0799(3) 0.2267(3) 0.0453(11) Uani 1 1 d . . .
H32A H 0.1459 1.0562 0.2760 0.068 Uiso 1 1 calc R . .
H32B H 0.0743 1.1454 0.2383 0.068 Uiso 1 1 calc R . .
H32C H 0.1236 1.1151 0.1886 0.068 Uiso 1 1 calc R . .
C33 C -0.0024(2) 0.9776(4) 0.1162(3) 0.0438(9) Uani 1 1 d . . .
H33A H 0.0158 0.9951 0.0743 0.066 Uiso 1 1 calc R . .
H33B H -0.0337 1.0493 0.1190 0.066 Uiso 1 1 calc R . .
H33C H -0.0309 0.8971 0.1040 0.066 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 0.0040 0.0020 '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 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3580 0.9920 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.4960 6.4160 '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 Yb1 O3 80.64(12) 2 . ?
O3 Yb1 O1 109.80(9) 2 2 ?
O3 Yb1 O1 141.89(9) . 2 ?
O3 Yb1 O1 141.89(9) 2 . ?
O3 Yb1 O1 109.80(9) . . ?
O1 Yb1 O1 84.84(13) 2 . ?
O3 Yb1 O2 145.07(8) 2 . ?
O3 Yb1 O2 75.69(7) . . ?
O1 Yb1 O2 76.30(8) 2 . ?
O1 Yb1 O2 71.48(9) . . ?
O3 Yb1 O2 75.69(7) 2 2 ?
O3 Yb1 O2 145.07(8) . 2 ?
O1 Yb1 O2 71.48(9) 2 2 ?
O1 Yb1 O2 76.30(8) . 2 ?
O2 Yb1 O2 135.89(10) . 2 ?
O3 Yb1 N1 76.74(9) 2 . ?
O3 Yb1 N1 73.73(8) . . ?
O1 Yb1 N1 143.65(9) 2 . ?
O1 Yb1 N1 71.81(9) . . ?
O2 Yb1 N1 119.45(8) . . ?
O2 Yb1 N1 76.07(8) 2 . ?
O3 Yb1 N1 73.73(8) 2 2 ?
O3 Yb1 N1 76.74(9) . 2 ?
O1 Yb1 N1 71.81(9) 2 2 ?
O1 Yb1 N1 143.65(9) . 2 ?
O2 Yb1 N1 76.07(8) . 2 ?
O2 Yb1 N1 119.45(8) 2 2 ?
N1 Yb1 N1 140.96(12) . 2 ?
C1 Fe1 C1 180.000(1) . 7_566 ?
C1 Fe1 C2 90.50(13) . 7_566 ?
C1 Fe1 C2 89.50(12) 7_566 7_566 ?
C1 Fe1 C2 89.50(12) . . ?
C1 Fe1 C2 90.50(13) 7_566 . ?
C2 Fe1 C2 180.0 7_566 . ?
C1 Fe1 C3 90.44(13) . 7_566 ?
C1 Fe1 C3 89.56(13) 7_566 7_566 ?
C2 Fe1 C3 90.75(14) 7_566 7_566 ?
C2 Fe1 C3 89.25(14) . 7_566 ?
C1 Fe1 C3 89.56(13) . . ?
C1 Fe1 C3 90.44(13) 7_566 . ?
C2 Fe1 C3 89.25(14) 7_566 . ?
C2 Fe1 C3 90.75(14) . . ?
C3 Fe1 C3 180.00(18) 7_566 . ?
N1 C1 Fe1 179.2(3) . . ?
C1 N1 Yb1 177.9(2) . . ?
N2 C2 Fe1 178.7(3) . . ?
N3 C3 Fe1 178.9(3) . . ?
C11 O1 Yb1 129.4(2) . . ?
C11 N11 C12 121.0(3) . . ?
C11 N11 C13 122.4(3) . . ?
C12 N11 C13 116.5(3) . . ?
O1 C11 N11 124.4(3) . . ?
O1 C11 H11 117.8 . . ?
N11 C11 H11 117.8 . . ?
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 Yb1 126.72(19) . . ?
C21 N21 C22 120.4(3) . . ?
C21 N21 C23 121.8(3) . . ?
C22 N21 C23 117.8(3) . . ?
O2 C21 N21 124.4(3) . . ?
O2 C21 H21 117.8 . . ?
N21 C21 H21 117.8 . . ?
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 Yb1 134.8(2) . . ?
C31 N31 C33 121.6(3) . . ?
C31 N31 C32 120.2(3) . . ?
C33 N31 C32 118.2(3) . . ?
O3 C31 N31 123.0(3) . . ?
O3 C31 H31 118.5 . . ?
N31 C31 H31 118.5 . . ?
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
Yb1 O3 2.299(2) 2 ?
Yb1 O3 2.299(2) . ?
Yb1 O1 2.319(2) 2 ?
Yb1 O1 2.319(2) . ?
Yb1 O2 2.343(2) . ?
Yb1 O2 2.343(2) 2 ?
Yb1 N1 2.446(3) . ?
Yb1 N1 2.446(3) 2 ?
Fe1 C1 1.936(3) . ?
Fe1 C1 1.936(3) 7_566 ?
Fe1 C2 1.954(3) 7_566 ?
Fe1 C2 1.954(3) . ?
Fe1 C3 1.959(3) 7_566 ?
Fe1 C3 1.959(3) . ?
C1 N1 1.159(4) . ?
C2 N2 1.160(5) . ?
C3 N3 1.161(5) . ?
O1 C11 1.248(4) . ?
N11 C11 1.315(4) . ?
N11 C12 1.460(4) . ?
N11 C13 1.466(4) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O2 C21 1.250(4) . ?
N21 C21 1.331(4) . ?
N21 C22 1.456(4) . ?
N21 C23 1.457(4) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O3 C31 1.249(4) . ?
N31 C31 1.317(4) . ?
N31 C33 1.460(5) . ?
N31 C32 1.470(5) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
