#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:28:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179062 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302415.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_4302415
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 Gd N12 O6'
_chemical_formula_sum            'C24 H42 Fe Gd N12 O6'
_chemical_formula_weight         807.80
_chemical_melting_point          ?
_chemical_name_common
; 
 Gd(DMF)6Fe(CN)6 
;
_chemical_name_systematic
; 
 hexakis(N,N-dimethylformamide)Gadolinium(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                 112.13(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.732(4)
_cell_length_b                   10.343(2)
_cell_length_c                   18.202(4)
_cell_measurement_reflns_used    26753
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.26
_cell_volume                     3441.1(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18374
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    2.386
_exptl_absorpt_correction_T_max  0.9106
_exptl_absorpt_correction_T_min  0.8321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'R.H.Blessing (1997) J. Appl. Cryst. 421-426'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Chunck
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0121P)²+4.8694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                2621
_reflns_number_total             3038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8022369_si_002_02.cif
_cod_data_source_block           3
_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_cell_volume        3441.2(12)
_cod_database_code               4302415
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
Gd1 Gd 0.0000 0.07836(2) 0.2500 0.01270(7) Uani 1 2 d S . .
Fe1 Fe -0.2500 0.2500 0.0000 0.01570(15) Uani 1 2 d S . .
O13 O -0.08815(10) -0.09040(19) 0.21017(11) 0.0208(5) Uani 1 1 d . . .
O12 O 0.01250(10) -0.00813(19) 0.13370(11) 0.0185(5) Uani 1 1 d . . .
N12 N -0.02624(12) -0.1451(2) 0.02808(13) 0.0159(5) Uani 1 1 d . . .
N3 N -0.11076(13) 0.1600(2) 0.13802(14) 0.0193(6) Uani 1 1 d . . .
C12 C -0.03665(15) -0.0592(3) 0.07600(17) 0.0167(7) Uani 1 1 d . . .
H12 H -0.0856 -0.0339 0.0658 0.020 Uiso 1 1 calc . . .
N11 N 0.06034(13) 0.4689(2) 0.19328(14) 0.0222(6) Uani 1 1 d . . .
C3 C -0.16281(16) 0.1930(3) 0.08628(18) 0.0176(7) Uani 1 1 d . . .
N13 N -0.20290(12) -0.1683(2) 0.17927(14) 0.0194(6) Uani 1 1 d . . .
N2 N -0.34231(15) 0.0520(3) 0.05194(17) 0.0329(7) Uani 1 1 d . . .
O11 O 0.04609(11) 0.25310(19) 0.20048(11) 0.0218(5) Uani 1 1 d . . .
C11 C 0.07815(16) 0.3564(3) 0.22798(17) 0.0196(7) Uani 1 1 d . . .
H11 H 0.1182 0.3532 0.2775 0.023 Uiso 1 1 calc . . .
N1 N -0.27093(14) 0.4608(3) 0.11133(16) 0.0275(7) Uani 1 1 d . . .
C2 C -0.30793(16) 0.1259(3) 0.03311(18) 0.0217(7) Uani 1 1 d . . .
C1 C -0.26391(16) 0.3832(3) 0.06977(18) 0.0206(7) Uani 1 1 d . . .
C13 C -0.14395(16) -0.1072(3) 0.22566(17) 0.0208(7) Uani 1 1 d . . .
H13 H -0.1438 -0.0735 0.2743 0.025 Uiso 1 1 calc . . .
C13B C -0.20898(17) -0.2148(3) 0.10148(18) 0.0279(8) Uani 1 1 d . . .
H13A H -0.2288 -0.3029 0.0935 0.042 Uiso 1 1 calc R . .
H13B H -0.1605 -0.2149 0.0983 0.042 Uiso 1 1 calc R . .
H13C H -0.2418 -0.1579 0.0603 0.042 Uiso 1 1 calc R . .
C11B C 0.10371(19) 0.5844(3) 0.2261(2) 0.0368(9) Uani 1 1 d . . .
H11A H 0.0718 0.6526 0.2323 0.055 Uiso 1 1 calc R . .
H11B H 0.1269 0.6142 0.1901 0.055 Uiso 1 1 calc R . .
H11C H 0.1415 0.5639 0.2779 0.055 Uiso 1 1 calc R . .
C12B C -0.08774(16) -0.2008(3) -0.03702(17) 0.0236(7) Uani 1 1 d . . .
H12A H -0.0795 -0.1913 -0.0866 0.035 Uiso 1 1 calc R . .
H12B H -0.1329 -0.1558 -0.0417 0.035 Uiso 1 1 calc R . .
H12C H -0.0921 -0.2927 -0.0266 0.035 Uiso 1 1 calc R . .
C13A C -0.26642(16) -0.1845(3) 0.20084(19) 0.0320(8) Uani 1 1 d . . .
H13D H -0.2789 -0.2765 0.1991 0.048 Uiso 1 1 calc R . .
H13E H -0.3080 -0.1367 0.1634 0.048 Uiso 1 1 calc R . .
H13F H -0.2551 -0.1513 0.2546 0.048 Uiso 1 1 calc R . .
C12A C 0.04686(15) -0.1907(3) 0.03853(18) 0.0231(7) Uani 1 1 d . . .
H12D H 0.0525 -0.1898 -0.0127 0.035 Uiso 1 1 calc R . .
H12E H 0.0536 -0.2790 0.0596 0.035 Uiso 1 1 calc R . .
H12F H 0.0836 -0.1338 0.0758 0.035 Uiso 1 1 calc R . .
C11A C -0.00112(18) 0.4821(3) 0.11759(19) 0.0361(9) Uani 1 1 d . . .
H11D H -0.0317 0.5551 0.1203 0.054 Uiso 1 1 calc R . .
H11E H -0.0303 0.4025 0.1063 0.054 Uiso 1 1 calc R . .
H11F H 0.0174 0.4974 0.0753 0.054 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 0.0033 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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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
O11 Gd1 O11 79.47(10) . 2 ?
O11 Gd1 O13 142.41(7) . . ?
O11 Gd1 O13 109.71(7) 2 . ?
O11 Gd1 O13 109.71(7) . 2 ?
O11 Gd1 O13 142.41(7) 2 2 ?
O13 Gd1 O13 85.47(9) . 2 ?
O11 Gd1 O12 76.39(7) . . ?
O11 Gd1 O12 144.08(7) 2 . ?
O13 Gd1 O12 76.31(6) . . ?
O13 Gd1 O12 71.82(6) 2 . ?
O11 Gd1 O12 144.08(7) . 2 ?
O11 Gd1 O12 76.39(7) 2 2 ?
O13 Gd1 O12 71.82(6) . 2 ?
O13 Gd1 O12 76.31(6) 2 2 ?
O12 Gd1 O12 136.13(9) . 2 ?
O11 Gd1 N3 73.02(7) . 2 ?
O11 Gd1 N3 76.94(7) 2 2 ?
O13 Gd1 N3 143.99(7) . 2 ?
O13 Gd1 N3 71.69(7) 2 2 ?
O12 Gd1 N3 119.72(7) . 2 ?
O12 Gd1 N3 75.87(7) 2 2 ?
O11 Gd1 N3 76.94(7) . . ?
O11 Gd1 N3 73.02(7) 2 . ?
O13 Gd1 N3 71.69(7) . . ?
O13 Gd1 N3 143.99(7) 2 . ?
O12 Gd1 N3 75.87(7) . . ?
O12 Gd1 N3 119.72(7) 2 . ?
N3 Gd1 N3 140.64(11) 2 . ?
C3 Fe1 C3 180.0(3) . 7_455 ?
C3 Fe1 C2 90.33(12) . 7_455 ?
C3 Fe1 C2 89.67(12) 7_455 7_455 ?
C3 Fe1 C2 89.67(12) . . ?
C3 Fe1 C2 90.33(12) 7_455 . ?
C2 Fe1 C2 180.0(2) 7_455 . ?
C3 Fe1 C1 89.25(12) . . ?
C3 Fe1 C1 90.75(12) 7_455 . ?
C2 Fe1 C1 88.82(12) 7_455 . ?
C2 Fe1 C1 91.18(12) . . ?
C3 Fe1 C1 90.75(12) . 7_455 ?
C3 Fe1 C1 89.25(12) 7_455 7_455 ?
C2 Fe1 C1 91.18(12) 7_455 7_455 ?
C2 Fe1 C1 88.82(12) . 7_455 ?
C1 Fe1 C1 180.0(2) . 7_455 ?
C13 O13 Gd1 129.82(18) . . ?
C12 O12 Gd1 126.60(18) . . ?
C12 N12 C12B 121.1(2) . . ?
C12 N12 C12A 121.7(2) . . ?
C12B N12 C12A 117.2(2) . . ?
C3 N3 Gd1 177.5(2) . . ?
O12 C12 N12 125.4(3) . . ?
C11 N11 C11A 121.0(3) . . ?
C11 N11 C11B 121.4(3) . . ?
C11A N11 C11B 117.5(3) . . ?
N3 C3 Fe1 179.5(3) . . ?
C13 N13 C13B 120.8(2) . . ?
C13 N13 C13A 121.7(2) . . ?
C13B N13 C13A 117.4(2) . . ?
C11 O11 Gd1 135.76(18) . . ?
O11 C11 N11 124.5(3) . . ?
N2 C2 Fe1 179.3(3) . . ?
N1 C1 Fe1 178.9(3) . . ?
O13 C13 N13 124.4(3) . . ?
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
Gd1 O11 2.3502(19) . ?
Gd1 O11 2.3502(19) 2 ?
Gd1 O13 2.3766(19) . ?
Gd1 O13 2.3766(19) 2 ?
Gd1 O12 2.3949(19) . ?
Gd1 O12 2.3949(19) 2 ?
Gd1 N3 2.508(2) 2 ?
Gd1 N3 2.508(2) . ?
Fe1 C3 1.933(3) . ?
Fe1 C3 1.933(3) 7_455 ?
Fe1 C2 1.958(3) 7_455 ?
Fe1 C2 1.958(3) . ?
Fe1 C1 1.962(3) . ?
Fe1 C1 1.962(3) 7_455 ?
O13 C13 1.247(3) . ?
O12 C12 1.247(3) . ?
N12 C12 1.314(4) . ?
N12 C12B 1.458(3) . ?
N12 C12A 1.460(3) . ?
N3 C3 1.153(4) . ?
N11 C11 1.307(4) . ?
N11 C11A 1.459(4) . ?
N11 C11B 1.460(4) . ?
N13 C13 1.314(4) . ?
N13 C13B 1.457(4) . ?
N13 C13A 1.457(4) . ?
N2 C2 1.157(4) . ?
O11 C11 1.247(3) . ?
N1 C1 1.147(4) . ?
