#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:21:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179661 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/14/4511491.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_4511491
loop_
_publ_author_name
'Chen, Wen-Tong'
'Wang, Ming-Sheng'
'Cai, Li-Zhen'
'Xu, Gang'
'Akitsu, Takashiro'
'Akita-Tanaka, Motoko'
Guo,
'Huang, Jin-Shun'
_publ_section_title
;
 An Effective Approach to Layered Structures of Hybrid Prussian Blue
 Complexes:  Monolayered
 [Sm(DMF)2(H2O)3(μ-CN)3M(CN)3]n·nH2O and Bilayered
 [Sm(DMF)(H2O)3(μ-CN)4M(CN)2]n·nH2O (M = Fe, Co)
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1738
_journal_paper_doi               10.1021/cg060199c
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety         Sm(DMF)2(H2O)3Fe(CN)6.H2O
_chemical_formula_sum            'C12 H22 Fe N8 O6 Sm'
_chemical_formula_weight         580.58
_chemical_melting_point          ?
_chemical_name_common            Sm(DMF)2(H2O)3Fe(CN)6.H2O
_chemical_name_systematic        Sm(DMF)2(H2O)3Fe(CN)6.H2O
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.147(5)
_cell_angle_beta                 100.299(9)
_cell_angle_gamma                100.984(7)
_cell_formula_units_Z            2
_cell_length_a                   7.6462(14)
_cell_length_b                   9.2014(14)
_cell_length_c                   16.206(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1094.6(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_publication_material  'Siemens SHELXTLTM 5'
_computing_structure_refinement  'Siemens SHELXTLTM 5'
_computing_structure_solution    'Siemens SHELXTLTM 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7011
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    3.361
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0221
_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)+(0.0323P)²+0.7321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                3566
_reflns_number_total             3786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060199csi20060406_060643.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4511491
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Sm1 Sm 0.04001(2) 0.295384(15) 0.257455(8) 0.01594(7) Uani 1 1 d .
Fe1 Fe -0.34863(6) 0.74888(4) 0.27120(2) 0.01561(10) Uani 1 1 d .
C1 C -0.2913(5) 0.7694(3) 0.3937(2) 0.0258(7) Uani 1 1 d .
N1 N -0.2617(5) 0.7823(4) 0.46567(19) 0.0439(8) Uani 1 1 d .
C2 C -0.4080(5) 0.7226(4) 0.1484(2) 0.0310(8) Uani 1 1 d .
N2 N -0.4430(6) 0.7012(4) 0.0763(2) 0.0564(10) Uani 1 1 d .
C3 C -0.5607(5) 0.5946(3) 0.27123(19) 0.0229(7) Uani 1 1 d .
N3 N -0.6906(4) 0.5055(3) 0.26864(19) 0.0321(7) Uani 1 1 d .
C4 C -0.1502(4) 0.9123(3) 0.26761(19) 0.0210(7) Uani 1 1 d .
N4 N -0.0471(4) 1.0186(3) 0.26417(19) 0.0301(6) Uani 1 1 d .
C5 C -0.4900(4) 0.9020(4) 0.2761(2) 0.0246(7) Uani 1 1 d .
N5 N -0.5615(5) 1.0003(4) 0.2788(2) 0.0441(8) Uani 1 1 d .
C6 C -0.1928(4) 0.6058(3) 0.26766(19) 0.0226(7) Uani 1 1 d .
N6 N -0.0962(4) 0.5235(3) 0.26531(18) 0.0311(7) Uani 1 1 d .
O21 O -0.0821(4) 0.2878(3) 0.37977(15) 0.0370(6) Uani 1 1 d .
C21 C -0.1305(5) 0.2121(4) 0.4354(2) 0.0307(8) Uani 1 1 d .
H21A H -0.1079 0.1162 0.4354 0.037 Uiso 1 1 calc R
N21 N -0.2103(4) 0.2580(3) 0.49362(18) 0.0328(7) Uani 1 1 d .
C22 C -0.2560(7) 0.4038(5) 0.4962(3) 0.0587(13) Uani 1 1 d .
H22A H -0.2226 0.4521 0.4491 0.088 Uiso 1 1 calc R
H22B H -0.1912 0.4626 0.5478 0.088 Uiso 1 1 calc R
H22C H -0.3843 0.3932 0.4934 0.088 Uiso 1 1 calc R
C23 C -0.2504(7) 0.1661(5) 0.5611(3) 0.0590(13) Uani 1 1 d .
H23A H -0.2139 0.0730 0.5521 0.088 Uiso 1 1 calc R
H23B H -0.3784 0.1480 0.5607 0.088 Uiso 1 1 calc R
H23C H -0.1849 0.2175 0.6147 0.088 Uiso 1 1 calc R
O11 O -0.0138(4) 0.3379(3) 0.11388(14) 0.0392(6) Uani 1 1 d .
C11 C 0.0064(5) 0.3294(4) 0.0397(2) 0.0372(9) Uani 1 1 d .
H11A H 0.0931 0.4034 0.0252 0.045 Uiso 1 1 calc R
N11 N -0.0841(5) 0.2250(4) -0.01996(19) 0.0465(9) Uani 1 1 d .
C12 C -0.0619(9) 0.2323(8) -0.1076(3) 0.087(2) Uani 1 1 d .
H12A H 0.0286 0.3186 -0.1108 0.130 Uiso 1 1 calc R
H12B H -0.1754 0.2386 -0.1423 0.130 Uiso 1 1 calc R
H12C H -0.0243 0.1444 -0.1272 0.130 Uiso 1 1 calc R
C13 C -0.2156(7) 0.1004(6) -0.0031(3) 0.0690(15) Uani 1 1 d .
H13A H -0.2175 0.1073 0.0561 0.104 Uiso 1 1 calc R
H13B H -0.1825 0.0087 -0.0198 0.104 Uiso 1 1 calc R
H13C H -0.3340 0.1027 -0.0344 0.104 Uiso 1 1 calc R
O1W O -0.2870(3) 0.2071(3) 0.20085(16) 0.0375(6) Uani 1 1 d .
H1WA H -0.3251 0.2687 0.1723 0.056 Uiso 1 1 calc R
O2W O 0.2783(3) 0.2390(3) 0.36645(15) 0.0358(6) Uani 1 1 d .
H2WA H 0.3032 0.1596 0.3515 0.054 Uiso 1 1 calc R
O3W O 0.2366(3) 0.1779(3) 0.18262(15) 0.0310(5) Uani 1 1 d .
H3WA H 0.2996 0.2412 0.1612 0.047 Uiso 1 1 calc R
O4W O -0.4781(4) 0.6545(3) -0.09817(15) 0.0379(6) Uani 1 1 d D
H4WA H -0.503(7) 0.5643(12) -0.106(3) 0.058(15) Uiso 1 1 d D
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'
Sm Sm -0.1638 3.4418 '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
O21 Sm1 O11 144.58(10) . .
O21 Sm1 O3W 141.78(8) . .
O11 Sm1 O3W 70.04(9) . .
O21 Sm1 O1W 77.54(9) . .
O11 Sm1 O1W 72.50(9) . .
O3W Sm1 O1W 114.45(9) . .
O21 Sm1 O2W 74.87(9) . .
O11 Sm1 O2W 140.52(9) . .
O3W Sm1 O2W 73.63(8) . .
O1W Sm1 O2W 138.93(8) . .
O21 Sm1 N3 113.10(10) . 1_655
O11 Sm1 N3 83.46(10) . 1_655
O3W Sm1 N3 78.36(9) . 1_655
O1W Sm1 N3 145.44(9) . 1_655
O2W Sm1 N3 74.49(9) . 1_655
O21 Sm1 N6 74.96(9) . .
O11 Sm1 N6 79.15(9) . .
O3W Sm1 N6 142.22(8) . .
O1W Sm1 N6 74.52(9) . .
O2W Sm1 N6 125.17(9) . .
N3 Sm1 N6 76.88(10) 1_655 .
O21 Sm1 N4 78.52(9) . 1_545
O11 Sm1 N4 107.84(9) . 1_545
O3W Sm1 N4 72.81(9) . 1_545
O1W Sm1 N4 70.27(9) . 1_545
O2W Sm1 N4 74.83(9) . 1_545
N3 Sm1 N4 142.56(10) 1_655 1_545
N6 Sm1 N4 139.54(10) . 1_545
C4 Fe1 C5 84.78(13) . .
C4 Fe1 C6 91.52(13) . .
C5 Fe1 C6 176.22(13) . .
C4 Fe1 C3 175.51(13) . .
C5 Fe1 C3 91.12(14) . .
C6 Fe1 C3 92.60(13) . .
C4 Fe1 C1 91.45(13) . .
C5 Fe1 C1 89.32(14) . .
C6 Fe1 C1 90.04(13) . .
C3 Fe1 C1 90.33(14) . .
C4 Fe1 C2 89.78(14) . .
C5 Fe1 C2 91.64(15) . .
C6 Fe1 C2 89.07(14) . .
C3 Fe1 C2 88.50(14) . .
C1 Fe1 C2 178.50(14) . .
N1 C1 Fe1 178.4(3) . .
N2 C2 N2 0.0(7) 1 .
N2 C2 Fe1 177.2(3) 1 .
N2 C2 Fe1 177.2(3) . .
N2 N2 C2 0(10) 1 .
N3 C3 Fe1 177.2(3) . .
C3 N3 Sm1 175.0(3) . 1_455
N4 C4 Fe1 172.3(3) . .
C4 N4 Sm1 152.2(3) . 1_565
N5 C5 Fe1 174.7(3) . .
N6 C6 Fe1 178.2(3) . .
C6 N6 Sm1 165.3(3) . .
C21 O21 Sm1 147.0(2) . .
O21 C21 N21 124.3(3) . .
O21 C21 H21A 117.8 . .
N21 C21 H21A 117.8 . .
C21 N21 C22 121.2(3) . .
C21 N21 C23 121.0(3) . .
C22 N21 C23 117.8(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 . .
C11 O11 Sm1 156.4(3) . .
O11 C11 N11 125.4(4) . .
O11 C11 H11A 117.3 . .
N11 C11 H11A 117.3 . .
C11 N11 C13 121.7(3) . .
C11 N11 C12 121.2(4) . .
C13 N11 C12 117.1(4) . .
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 . .
Sm1 O1W H1WA 109.5 . .
Sm1 O2W H2WA 109.5 . .
Sm1 O3W H3WA 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 O21 2.337(2) .
Sm1 O11 2.364(2) .
Sm1 O3W 2.446(2) .
Sm1 O1W 2.460(2) .
Sm1 O2W 2.460(2) .
Sm1 N3 2.513(3) 1_655
Sm1 N6 2.520(3) .
Sm1 N4 2.522(3) 1_545
Fe1 C4 1.934(3) .
Fe1 C5 1.938(3) .
Fe1 C6 1.941(3) .
Fe1 C3 1.941(3) .
Fe1 C1 1.942(3) .
Fe1 C2 1.947(3) .
C1 N1 1.141(4) .
C2 N2 1.145(5) 1
C2 N2 1.145(5) .
N2 N2 0.000(10) 1
C3 N3 1.153(4) .
N3 Sm1 2.513(3) 1_455
C4 N4 1.145(4) .
N4 Sm1 2.522(3) 1_565
C5 N5 1.145(4) .
C6 N6 1.157(4) .
O21 C21 1.244(4) .
C21 N21 1.299(4) .
C21 H21A 0.9300 .
N21 C22 1.448(5) .
N21 C23 1.470(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 .
O11 C11 1.238(4) .
C11 N11 1.307(5) .
C11 H11A 0.9300 .
N11 C13 1.451(6) .
N11 C12 1.466(5) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
O1W H1WA 0.8200 .
O2W H2WA 0.8200 .
O3W H3WA 0.8200 .
O4W H4WA 0.810(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O4W 0.82 2.02 2.779(4) 153.3 2_465
O2W H2WA N4 0.82 2.81 3.028(4) 97.2 1_545
O3W H3WA O4W 0.82 1.99 2.790(4) 163.9 2_565
