#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:21:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179661 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/14/4511493.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_4511493
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)(H2O)3Fe(CN)6.H2O
_chemical_formula_sum            'C9 H15 Fe N7 O5 Sm'
_chemical_formula_weight         507.48
_chemical_melting_point          ?
_chemical_name_common            Sm(DMF)(H2O)3Fe(CN)6.H2O
_chemical_name_systematic        Sm(DMF)(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                78.771(11)
_cell_angle_beta                 85.126(11)
_cell_angle_gamma                79.362(11)
_cell_formula_units_Z            2
_cell_length_a                   7.555(3)
_cell_length_b                   9.136(4)
_cell_length_c                   13.022(6)
_cell_measurement_temperature    293(2)
_cell_volume                     865.3(7)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5429
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    4.230
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0436
_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)+(0.0238P)²+2.1671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                2557
_reflns_number_total             3021
_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_cell_volume        865.3(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4511493
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 0.32475(4) 0.76410(3) 0.30384(2) 0.01737(8) Uani 1 1 d .
Fe1 Fe 0.72709(10) 0.22240(8) 0.27813(6) 0.01589(19) Uani 1 1 d .
C1 C 0.7294(8) 0.2632(6) 0.1263(5) 0.0274(16) Uani 1 1 d .
C2 C 0.7259(8) 0.1798(6) 0.4297(5) 0.0222(14) Uani 1 1 d .
C3 C 0.5705(9) 0.0752(6) 0.2830(5) 0.0251(15) Uani 1 1 d .
C4 C 0.8720(8) 0.3771(6) 0.2773(5) 0.0271(15) Uani 1 1 d .
C5 C 0.9405(8) 0.0698(6) 0.2755(5) 0.0242(15) Uani 1 1 d .
C6 C 0.5225(8) 0.3816(6) 0.2878(5) 0.0238(15) Uani 1 1 d .
N1 N 0.7400(8) 0.2856(6) 0.0379(4) 0.0410(16) Uani 1 1 d .
N2 N 0.7243(7) 0.1575(6) 0.5189(4) 0.0304(13) Uani 1 1 d .
N3 N 0.4757(7) -0.0095(5) 0.2883(4) 0.0347(14) Uani 1 1 d .
N4 N 0.9503(8) 0.4704(6) 0.2814(5) 0.0502(17) Uani 1 1 d .
N5 N 1.0713(7) -0.0193(5) 0.2765(4) 0.0309(14) Uani 1 1 d .
N6 N 0.4118(7) 0.4829(5) 0.2983(4) 0.0322(14) Uani 1 1 d .
O11 O 0.5242(6) 0.7643(5) 0.1572(3) 0.0348(12) Uani 1 1 d .
N11 N 0.7076(7) 0.7570(6) 0.0136(4) 0.0315(14) Uani 1 1 d .
C11 C 0.5987(8) 0.6996(7) 0.0869(5) 0.0302(16) Uani 1 1 d .
H11A H 0.5760 0.6033 0.0859 0.036 Uiso 1 1 calc R
C12 C 0.7829(10) 0.6775(8) -0.0724(6) 0.053(2) Uani 1 1 d .
H12A H 0.7440 0.5812 -0.0618 0.079 Uiso 1 1 calc R
H12B H 0.9122 0.6623 -0.0739 0.079 Uiso 1 1 calc R
H12C H 0.7417 0.7372 -0.1379 0.079 Uiso 1 1 calc R
C13 C 0.7526(10) 0.9074(7) 0.0127(6) 0.051(2) Uani 1 1 d .
H13A H 0.6961 0.9456 0.0733 0.076 Uiso 1 1 calc R
H13B H 0.7100 0.9755 -0.0496 0.076 Uiso 1 1 calc R
H13C H 0.8810 0.8993 0.0137 0.076 Uiso 1 1 calc R
O1W O 0.5984(6) 0.6573(5) 0.4014(4) 0.0493(14) Uani 1 1 d .
H1WA H 0.6239 0.7210 0.4315 0.074 Uiso 1 1 calc R
O2W O 0.1469(6) 0.7109(4) 0.1712(3) 0.0328(11) Uani 1 1 d .
H2WA H 0.0819 0.7892 0.1452 0.049 Uiso 1 1 calc R
O3W O 0.0917(6) 0.6390(5) 0.4070(3) 0.0366(12) Uani 1 1 d .
H3WA H 0.0211 0.7007 0.4351 0.055 Uiso 1 1 calc R
O4W O 0.7961(7) 0.7798(5) 0.5276(4) 0.0467(14) Uani 1 1 d D
H4WA H 0.775(9) 0.8613(15) 0.547(2) 0.05(2) 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
O11 Sm1 O3W 144.99(15) . .
O11 Sm1 O2W 76.67(15) . .
O3W Sm1 O2W 76.39(15) . .
O11 Sm1 O1W 83.94(16) . .
O3W Sm1 O1W 103.76(16) . .
O2W Sm1 O1W 141.01(14) . .
O11 Sm1 N5 111.55(16) . 1_465
O3W Sm1 N5 82.16(16) . 1_465
O2W Sm1 N5 74.74(16) . 1_465
O1W Sm1 N5 144.25(16) . 1_465
O11 Sm1 N3 73.05(16) . 1_565
O3W Sm1 N3 141.81(15) . 1_565
O2W Sm1 N3 126.21(16) . 1_565
O1W Sm1 N3 77.81(17) . 1_565
N5 Sm1 N3 76.58(17) 1_465 1_565
O11 Sm1 N2 142.62(17) . 2_666
O3W Sm1 N2 70.41(16) . 2_666
O2W Sm1 N2 138.80(16) . 2_666
O1W Sm1 N2 72.09(16) . 2_666
N5 Sm1 N2 77.17(17) 1_465 2_666
N3 Sm1 N2 74.12(17) 1_565 2_666
O11 Sm1 N6 77.84(16) . .
O3W Sm1 N6 73.09(15) . .
O2W Sm1 N6 72.71(16) . .
O1W Sm1 N6 70.30(16) . .
N5 Sm1 N6 142.76(18) 1_465 .
N3 Sm1 N6 138.57(17) 1_565 .
N2 Sm1 N6 118.04(17) 2_666 .
C5 Fe1 C6 175.7(3) . .
C5 Fe1 C2 88.7(2) . .
C6 Fe1 C2 88.6(2) . .
C5 Fe1 C1 90.8(2) . .
C6 Fe1 C1 91.9(3) . .
C2 Fe1 C1 179.5(2) . .
C5 Fe1 C3 91.9(3) . .
C6 Fe1 C3 91.4(2) . .
C2 Fe1 C3 89.6(2) . .
C1 Fe1 C3 90.2(3) . .
C5 Fe1 C4 91.2(3) . .
C6 Fe1 C4 85.5(2) . .
C2 Fe1 C4 89.0(3) . .
C1 Fe1 C4 91.2(3) . .
C3 Fe1 C4 176.6(2) . .
N1 C1 Fe1 176.5(6) . .
N2 C2 Fe1 178.7(5) . .
N3 C3 Fe1 178.0(5) . .
N4 C4 Fe1 176.0(6) . .
N5 C5 Fe1 177.4(6) . .
N6 C6 Fe1 173.2(6) . .
C2 N2 Sm1 153.9(5) . 2_666
C3 N3 Sm1 168.2(5) . 1_545
C5 N5 Sm1 170.2(5) . 1_645
C6 N6 Sm1 148.7(5) . .
C11 O11 Sm1 148.7(4) . .
C11 N11 C12 121.5(6) . .
C11 N11 C13 120.3(5) . .
C12 N11 C13 118.2(5) . .
O11 C11 N11 124.3(6) . .
O11 C11 H11A 117.9 . .
N11 C11 H11A 117.9 . .
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 . .
O4W O4W H4WA 0(10) 1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 O11 2.330(4) .
Sm1 O3W 2.440(4) .
Sm1 O2W 2.446(4) .
Sm1 O1W 2.462(5) .
Sm1 N5 2.480(5) 1_465
Sm1 N3 2.507(5) 1_565
Sm1 N2 2.526(5) 2_666
Sm1 N6 2.545(5) .
Fe1 C5 1.930(6) .
Fe1 C6 1.931(6) .
Fe1 C2 1.935(6) .
Fe1 C1 1.939(6) .
Fe1 C3 1.938(7) .
Fe1 C4 1.939(6) .
C1 N1 1.127(8) .
C2 N2 1.139(7) .
C3 N3 1.137(8) .
C4 N4 1.135(8) .
C5 N5 1.158(7) .
C6 N6 1.149(7) .
N2 Sm1 2.526(5) 2_666
N3 Sm1 2.507(5) 1_545
N5 Sm1 2.480(5) 1_645
O11 C11 1.227(7) .
N11 C11 1.301(7) .
N11 C12 1.471(8) .
N11 C13 1.473(8) .
C11 H11A 0.9300 .
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 O4W 0.000(14) 1
O4W H4WA 0.817(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 N2 0.82 2.74 2.936(7) 95.9 2_666
O1W H1WA O4W 0.82 2.08 2.816(7) 148.6 1
O2W H2WA N5 0.82 2.66 2.990(6) 105.8 1_465
O3W H3WA O4W 0.82 2.10 2.870(6) 157.0 1_455
