#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:28:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179062 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302419.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_4302419
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 Tm'
_chemical_formula_sum            'C24 H42 Fe N12 O6 Tm'
_chemical_formula_weight         819.48
_chemical_melting_point          ?
_chemical_name_common
; 
 Tm(DMF)6Fe(CN)6
;
_chemical_name_systematic
; 
 hexakis(N,N-dimethylformamide)Thulium(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                 113.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.834(4)
_cell_length_b                   10.357(2)
_cell_length_c                   18.326(4)
_cell_measurement_reflns_used    3183
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.26
_cell_volume                     3460.1(15)
_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-97
_computing_publication_material  SHELXTL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5486
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    3.020
_exptl_absorpt_correction_T_max  0.8887
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0318
_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)+(0.0674P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                2352
_reflns_number_total             3017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8022369_si_002_06.cif
_cod_data_source_block           8
_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               4302419
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
Tm1 Tm 0.5000 0.42045(5) 0.2500 0.0214(2) Uani 1 2 d S . .
Fe1 Fe 0.2500 0.2500 0.0000 0.0249(4) Uani 1 2 d S . .
C1 C 0.3379(4) 0.3069(7) 0.0862(4) 0.0262(18) Uani 1 1 d . . .
N1 N 0.3909(3) 0.3406(6) 0.1388(4) 0.0306(16) Uani 1 1 d . . .
C2 C 0.1926(5) 0.3734(9) 0.0332(5) 0.037(2) Uani 1 1 d . . .
N2 N 0.1583(5) 0.4453(8) 0.0520(6) 0.062(3) Uani 1 1 d . . .
C3 C 0.2370(4) 0.1159(9) 0.0693(5) 0.035(2) Uani 1 1 d . . .
N3 N 0.2304(5) 0.0374(8) 0.1101(5) 0.053(2) Uani 1 1 d . . .
O1 O 0.4131(3) 0.5857(5) 0.2096(3) 0.0371(14) Uani 1 1 d . . .
C11 C 0.3583(5) 0.6037(8) 0.2253(5) 0.035(2) Uani 1 1 d . . .
H11 H 0.3591 0.5700 0.2726 0.042 Uiso 1 1 calc R . .
N11 N 0.2996(4) 0.6669(7) 0.1797(4) 0.0368(17) Uani 1 1 d . . .
C12 C 0.2371(5) 0.6836(11) 0.2015(6) 0.060(3) Uani 1 1 d . . .
H12A H 0.1967 0.6331 0.1668 0.089 Uiso 1 1 calc R . .
H12B H 0.2234 0.7731 0.1969 0.089 Uiso 1 1 calc R . .
H12C H 0.2501 0.6557 0.2553 0.089 Uiso 1 1 calc R . .
C13 C 0.2925(5) 0.7139(10) 0.1021(5) 0.051(3) Uani 1 1 d . . .
H13A H 0.3399 0.7148 0.0994 0.077 Uiso 1 1 calc R . .
H13B H 0.2728 0.7998 0.0942 0.077 Uiso 1 1 calc R . .
H13C H 0.2603 0.6581 0.0615 0.077 Uiso 1 1 calc R . .
O2 O 0.5447(3) 0.2511(5) 0.2011(3) 0.0373(14) Uani 1 1 d . . .
C21 C 0.5774(4) 0.1473(9) 0.2278(5) 0.034(2) Uani 1 1 d . . .
H21 H 0.6173 0.1499 0.2763 0.041 Uiso 1 1 calc R . .
N21 N 0.5595(4) 0.0367(7) 0.1928(4) 0.0403(19) Uani 1 1 d . . .
C22 C 0.6031(7) -0.0785(9) 0.2259(7) 0.070(3) Uani 1 1 d . . .
H22A H 0.6424 -0.0572 0.2753 0.105 Uiso 1 1 calc R . .
H22B H 0.6229 -0.1108 0.1894 0.105 Uiso 1 1 calc R . .
H22C H 0.5725 -0.1433 0.2348 0.105 Uiso 1 1 calc R . .
C23 C 0.4975(6) 0.0241(10) 0.1168(6) 0.063(3) Uani 1 1 d . . .
H23A H 0.4700 0.1031 0.1047 0.094 Uiso 1 1 calc R . .
H23B H 0.4666 -0.0454 0.1196 0.094 Uiso 1 1 calc R . .
H23C H 0.5151 0.0061 0.0760 0.094 Uiso 1 1 calc R . .
O3 O 0.5112(3) 0.5061(5) 0.1364(3) 0.0302(13) Uani 1 1 d . . .
C31 C 0.4631(4) 0.5586(8) 0.0775(5) 0.031(2) Uani 1 1 d . . .
H31 H 0.4146 0.5359 0.0663 0.037 Uiso 1 1 calc R . .
N31 N 0.4742(3) 0.6415(7) 0.0306(4) 0.0290(15) Uani 1 1 d . . .
C32 C 0.4134(4) 0.6972(8) -0.0359(5) 0.040(2) Uani 1 1 d . . .
H32A H 0.3689 0.6523 -0.0428 0.061 Uiso 1 1 calc R . .
H32B H 0.4226 0.6892 -0.0834 0.061 Uiso 1 1 calc R . .
H32C H 0.4084 0.7868 -0.0256 0.061 Uiso 1 1 calc R . .
C33 C 0.5480(4) 0.6852(9) 0.0439(5) 0.043(2) Uani 1 1 d . . .
H33A H 0.5545 0.7724 0.0632 0.064 Uiso 1 1 calc R . .
H33B H 0.5548 0.6817 -0.0052 0.064 Uiso 1 1 calc R . .
H33C H 0.5834 0.6303 0.0823 0.064 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'
Tm Tm -0.3139 5.2483 '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
O2 Tm1 O2 80.7(3) 2_655 . ?
O2 Tm1 O1 141.78(19) 2_655 2_655 ?
O2 Tm1 O1 109.4(2) . 2_655 ?
O2 Tm1 O1 109.4(2) 2_655 . ?
O2 Tm1 O1 141.78(19) . . ?
O1 Tm1 O1 85.6(3) 2_655 . ?
O2 Tm1 O3 75.97(19) 2_655 2_655 ?
O2 Tm1 O3 144.84(19) . 2_655 ?
O1 Tm1 O3 75.97(19) 2_655 2_655 ?
O1 Tm1 O3 71.87(19) . 2_655 ?
O2 Tm1 O3 144.84(19) 2_655 . ?
O2 Tm1 O3 75.97(19) . . ?
O1 Tm1 O3 71.87(19) 2_655 . ?
O1 Tm1 O3 75.97(19) . . ?
O3 Tm1 O3 135.7(3) 2_655 . ?
O2 Tm1 N1 73.6(2) 2_655 . ?
O2 Tm1 N1 76.7(2) . . ?
O1 Tm1 N1 144.0(2) 2_655 . ?
O1 Tm1 N1 71.6(2) . . ?
O3 Tm1 N1 120.1(2) 2_655 . ?
O3 Tm1 N1 75.68(19) . . ?
O2 Tm1 N1 76.7(2) 2_655 2_655 ?
O2 Tm1 N1 73.6(2) . 2_655 ?
O1 Tm1 N1 71.6(2) 2_655 2_655 ?
O1 Tm1 N1 144.0(2) . 2_655 ?
O3 Tm1 N1 75.68(19) 2_655 2_655 ?
O3 Tm1 N1 120.1(2) . 2_655 ?
N1 Tm1 N1 140.7(3) . 2_655 ?
C1 Fe1 C1 180.0(4) 7 . ?
C1 Fe1 C2 90.3(3) 7 . ?
C1 Fe1 C2 89.7(3) . . ?
C1 Fe1 C2 89.7(3) 7 7 ?
C1 Fe1 C2 90.3(3) . 7 ?
C2 Fe1 C2 180.0(5) . 7 ?
C1 Fe1 C3 90.4(3) 7 . ?
C1 Fe1 C3 89.6(3) . . ?
C2 Fe1 C3 91.2(4) . . ?
C2 Fe1 C3 88.8(4) 7 . ?
C1 Fe1 C3 89.6(3) 7 7 ?
C1 Fe1 C3 90.4(3) . 7 ?
C2 Fe1 C3 88.8(4) . 7 ?
C2 Fe1 C3 91.2(4) 7 7 ?
C3 Fe1 C3 180.0(6) . 7 ?
N1 C1 Fe1 179.4(7) . . ?
C1 N1 Tm1 177.5(6) . . ?
N2 C2 Fe1 179.3(9) . . ?
N3 C3 Fe1 179.2(8) . . ?
C11 O1 Tm1 129.9(5) . . ?
O1 C11 N11 124.6(8) . . ?
O1 C11 H11 117.7 . . ?
N11 C11 H11 117.7 . . ?
C11 N11 C12 121.6(8) . . ?
C11 N11 C13 120.6(7) . . ?
C12 N11 C13 117.6(7) . . ?
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 Tm1 136.3(5) . . ?
O2 C21 N21 124.8(7) . . ?
O2 C21 H21 117.6 . . ?
N21 C21 H21 117.6 . . ?
C21 N21 C23 121.2(8) . . ?
C21 N21 C22 121.2(8) . . ?
C23 N21 C22 117.6(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 Tm1 128.5(5) . . ?
O3 C31 N31 126.2(7) . . ?
O3 C31 H31 116.9 . . ?
N31 C31 H31 116.9 . . ?
C31 N31 C32 121.1(7) . . ?
C31 N31 C33 121.2(7) . . ?
C32 N31 C33 117.6(7) . . ?
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
Tm1 O2 2.300(5) 2_655 ?
Tm1 O2 2.300(5) . ?
Tm1 O1 2.332(5) 2_655 ?
Tm1 O1 2.332(5) . ?
Tm1 O3 2.353(5) 2_655 ?
Tm1 O3 2.353(5) . ?
Tm1 N1 2.458(6) . ?
Tm1 N1 2.458(6) 2_655 ?
Fe1 C1 1.927(7) 7 ?
Fe1 C1 1.927(7) . ?
Fe1 C2 1.961(10) . ?
Fe1 C2 1.961(10) 7 ?
Fe1 C3 1.966(10) . ?
Fe1 C3 1.966(10) 7 ?
C1 N1 1.165(9) . ?
C2 N2 1.150(11) . ?
C3 N3 1.148(11) . ?
O1 C11 1.244(10) . ?
C11 N11 1.310(10) . ?
C11 H11 0.9300 . ?
N11 C12 1.454(10) . ?
N11 C13 1.457(11) . ?
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 1.251(10) . ?
C21 N21 1.292(11) . ?
C21 H21 0.9300 . ?
N21 C23 1.456(12) . ?
N21 C22 1.457(11) . ?
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 1.248(9) . ?
C31 N31 1.295(10) . ?
C31 H31 0.9300 . ?
N31 C32 1.455(9) . ?
N31 C33 1.458(10) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
