#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:56:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180364 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/33/7203366.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_7203366
loop_
_publ_author_name
'Zhang, Yuan-Zhu'
'Duan, Gong-Ping'
'Sato, Osamu'
'Gao, Song'
_publ_section_title
;
 Structures and magnetism of cyano-bridged grid-like two-dimensional
 4f?3d arrays
;
_journal_issue                   26
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2625
_journal_paper_doi               10.1039/b603050e
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C16 H18 Fe N8 O7 Sm'
_chemical_formula_weight         640.58
_chemical_name_common            2D-grid-FeSm
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 101.6915(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6684(4)
_cell_length_b                   7.4084(2)
_cell_length_c                   23.4344(8)
_cell_measurement_reflns_used    59801
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2323.76(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.1111
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25832
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         6.149
_refine_diff_density_min         -2.320
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.0739
_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)+(0.0697P)²+40.2354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                3137
_reflns_number_total             5269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603050e.txt
_cod_data_source_block           SmFe
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7203366
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Sm1 Sm 0.28413(4) 0.54393(9) 0.84963(3) 0.0183(2) Uani 1 1 d . . .
Fe1 Fe 0.0000 1.0328(4) 0.7500 0.0229(5) Uani 1 2 d S . .
Fe2 Fe 0.5000 0.0510(4) 0.7500 0.0226(5) Uani 1 2 d S . .
O1 O 0.1566(6) 0.5598(15) 0.9050(4) 0.038(2) Uani 1 1 d . . .
O2 O -0.5495(6) 0.5394(17) 0.9060(4) 0.046(3) Uani 1 1 d . . .
O3 O 0.3055(7) 0.2836(14) 0.9136(4) 0.038(2) Uani 1 1 d . . .
O4 O 0.3074(9) 0.8174(18) 0.9091(7) 0.093(6) Uani 1 1 d . . .
O5 O 0.1690(7) 0.0497(15) 0.9451(5) 0.049(3) Uani 1 1 d . . .
O6 O 0.1788(9) -0.0934(17) 1.0501(5) 0.062(3) Uani 1 1 d . . .
O7 O 0.4700(9) 0.0531(19) 0.9427(6) 0.074(4) Uani 1 1 d . . .
N1 N 0.1541(8) 0.7287(18) 0.7879(6) 0.044(3) Uani 1 1 d . . .
N2 N 0.0382(10) 1.042(2) 0.6250(6) 0.056(4) Uani 1 1 d . . .
N3 N 0.1609(8) 1.3231(14) 0.7923(5) 0.027(3) Uani 1 1 d . . .
N4 N 0.3719(10) 0.065(2) 0.6259(6) 0.058(4) Uani 1 1 d . . .
N6 N 0.3709(8) -0.2419(16) 0.7927(5) 0.035(3) Uani 1 1 d . . .
N7 N 0.0593(7) 0.5742(14) 0.9021(4) 0.026(2) Uani 1 1 d . . .
N8 N -0.4533(7) 0.5507(19) 0.9039(5) 0.038(3) Uani 1 1 d . . .
C1 C 0.0979(11) 0.8454(18) 0.7741(7) 0.036(4) Uani 1 1 d . . .
C2 C 0.0259(10) 1.036(2) 0.6712(6) 0.034(3) Uani 1 1 d . . .
C3 C 0.1011(9) 1.2130(18) 0.7742(6) 0.025(3) Uani 1 1 d . . .
C4 C 0.4177(11) 0.057(2) 0.6717(6) 0.035(3) Uani 1 1 d . . .
C6 C 0.4172(11) -0.1306(19) 0.7754(6) 0.032(3) Uani 1 1 d . . .
C7 C 0.0260(9) 0.648(2) 0.9470(6) 0.033(3) Uani 1 1 d . . .
H7 H 0.0714 0.6984 0.9780 0.040 Uiso 1 1 calc R . .
C8 C -0.0727(9) 0.651(2) 0.9477(6) 0.034(3) Uani 1 1 d . . .
H8 H -0.0936 0.7007 0.9797 0.041 Uiso 1 1 calc R . .
C9 C -0.1438(9) 0.5827(17) 0.9020(6) 0.026(3) Uani 1 1 d . . .
C10 C -0.1068(10) 0.521(2) 0.8539(6) 0.036(3) Uani 1 1 d . . .
H10 H -0.1510 0.4771 0.8214 0.043 Uiso 1 1 calc R . .
C11 C -0.0097(8) 0.5258(17) 0.8539(5) 0.021(3) Uiso 1 1 d . . .
H11 H 0.0120 0.4949 0.8200 0.025 Uiso 1 1 calc R . .
C12 C -0.2514(9) 0.5734(18) 0.9026(5) 0.028(3) Uani 1 1 d . . .
C13 C -0.2851(10) 0.562(3) 0.9545(6) 0.053(5) Uani 1 1 d . . .
H13 H -0.2394 0.5614 0.9898 0.064 Uiso 1 1 calc R . .
C14 C -0.3845(10) 0.552(3) 0.9542(6) 0.061(5) Uani 1 1 d . . .
H14 H -0.4057 0.5449 0.9894 0.073 Uiso 1 1 calc R . .
C15 C -0.4189(7) 0.5593(14) 0.8522(4) 0.010(2) Uiso 1 1 d . . .
H15 H -0.4645 0.5543 0.8168 0.012 Uiso 1 1 calc R . .
C16 C -0.3238(10) 0.5743(18) 0.8522(5) 0.030(3) Uani 1 1 d . . .
H16 H -0.3040 0.5861 0.8167 0.036 Uiso 1 1 calc R . .
N5 N 0.3710(9) 0.3471(17) 0.7897(5) 0.039(3) Uani 1 1 d . . .
C5 C 0.4172(9) 0.2363(18) 0.7743(6) 0.024(3) Uani 1 1 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
_geom_angle_publ_flag
O1 Sm1 O2 114.8(3) . 1_655 ?
O1 Sm1 O3 73.2(3) . . ?
O2 Sm1 O3 70.4(3) 1_655 . ?
O1 Sm1 O4 70.9(4) . . ?
O2 Sm1 O4 72.3(4) 1_655 . ?
O3 Sm1 O4 108.8(5) . . ?
O1 Sm1 N1 76.8(4) . . ?
O2 Sm1 N1 145.6(4) 1_655 . ?
O3 Sm1 N1 141.9(4) . . ?
O4 Sm1 N1 82.5(5) . . ?
O1 Sm1 N5 145.5(4) . . ?
O2 Sm1 N5 78.1(4) 1_655 . ?
O3 Sm1 N5 82.6(4) . . ?
O4 Sm1 N5 141.9(4) . . ?
N1 Sm1 N5 111.3(4) . . ?
O1 Sm1 N6 137.2(4) . 1_565 ?
O2 Sm1 N6 78.7(4) 1_655 1_565 ?
O3 Sm1 N6 144.9(3) . 1_565 ?
O4 Sm1 N6 76.0(5) . 1_565 ?
N1 Sm1 N6 72.6(4) . 1_565 ?
N5 Sm1 N6 75.0(4) . 1_565 ?
O1 Sm1 N3 80.7(3) . 1_545 ?
O2 Sm1 N3 137.9(4) 1_655 1_545 ?
O3 Sm1 N3 78.3(4) . 1_545 ?
O4 Sm1 N3 146.6(4) . 1_545 ?
N1 Sm1 N3 74.0(4) . 1_545 ?
N5 Sm1 N3 70.4(4) . 1_545 ?
N6 Sm1 N3 117.4(4) 1_565 1_545 ?
C3 Fe1 C3 92.1(8) . 2_556 ?
C3 Fe1 C1 178.0(6) . 2_556 ?
C3 Fe1 C1 89.9(5) 2_556 2_556 ?
C3 Fe1 C1 89.9(5) . . ?
C3 Fe1 C1 178.0(6) 2_556 . ?
C1 Fe1 C1 88.1(8) 2_556 . ?
C3 Fe1 C2 90.7(6) . . ?
C3 Fe1 C2 88.3(6) 2_556 . ?
C1 Fe1 C2 88.9(6) 2_556 . ?
C1 Fe1 C2 92.2(6) . . ?
C3 Fe1 C2 88.3(6) . 2_556 ?
C3 Fe1 C2 90.7(6) 2_556 2_556 ?
C1 Fe1 C2 92.2(6) 2_556 2_556 ?
C1 Fe1 C2 88.9(6) . 2_556 ?
C2 Fe1 C2 178.6(9) . 2_556 ?
C6 Fe2 C6 91.5(8) 2_656 . ?
C6 Fe2 C5 89.4(5) 2_656 2_656 ?
C6 Fe2 C5 178.9(6) . 2_656 ?
C6 Fe2 C5 178.9(6) 2_656 . ?
C6 Fe2 C5 89.4(5) . . ?
C5 Fe2 C5 89.7(7) 2_656 . ?
C6 Fe2 C4 89.3(6) 2_656 . ?
C6 Fe2 C4 92.4(6) . . ?
C5 Fe2 C4 88.2(6) 2_656 . ?
C5 Fe2 C4 90.1(6) . . ?
C6 Fe2 C4 92.4(6) 2_656 2_656 ?
C6 Fe2 C4 89.3(6) . 2_656 ?
C5 Fe2 C4 90.1(6) 2_656 2_656 ?
C5 Fe2 C4 88.2(6) . 2_656 ?
C4 Fe2 C4 177.6(9) . 2_656 ?
N7 O1 Sm1 144.9(7) . . ?
N8 O2 Sm1 144.8(8) . 1_455 ?
C1 N1 Sm1 159.4(13) . . ?
C3 N3 Sm1 169.5(10) . 1_565 ?
C6 N6 Sm1 168.7(12) . 1_545 ?
O1 N7 C7 119.3(10) . . ?
O1 N7 C11 122.6(10) . . ?
C7 N7 C11 117.9(10) . . ?
O2 N8 C14 119.1(11) . . ?
O2 N8 C15 123.2(10) . . ?
C14 N8 C15 117.6(10) . . ?
N1 C1 Fe1 177.6(13) . . ?
N2 C2 Fe1 177.5(14) . . ?
N3 C3 Fe1 175.6(12) . . ?
N4 C4 Fe2 177.6(15) . . ?
N6 C6 Fe2 176.9(13) . . ?
N7 C7 C8 120.8(12) . . ?
C7 C8 C9 121.9(13) . . ?
C8 C9 C10 115.4(12) . . ?
C8 C9 C12 123.5(12) . . ?
C10 C9 C12 121.0(11) . . ?
C11 C10 C9 121.1(12) . . ?
C10 C11 N7 121.9(11) . . ?
C16 C12 C13 116.2(12) . . ?
C16 C12 C9 122.4(11) . . ?
C13 C12 C9 121.3(12) . . ?
C14 C13 C12 120.5(13) . . ?
N8 C14 C13 121.6(13) . . ?
C16 C15 N8 121.1(10) . . ?
C15 C16 C12 123.0(11) . . ?
C5 N5 Sm1 164.0(12) . . ?
N5 C5 Fe2 177.9(13) . . ?
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
Sm1 O1 2.377(8) . ?
Sm1 O2 2.388(8) 1_655 ?
Sm1 O3 2.423(9) . ?
Sm1 O4 2.443(11) . ?
Sm1 N1 2.467(12) . ?
Sm1 N5 2.487(12) . ?
Sm1 N6 2.520(11) 1_565 ?
Sm1 N3 2.530(11) 1_545 ?
Fe1 C3 1.922(13) . ?
Fe1 C3 1.922(13) 2_556 ?
Fe1 C1 1.932(15) 2_556 ?
Fe1 C1 1.932(14) . ?
Fe1 C2 1.950(16) . ?
Fe1 C2 1.950(16) 2_556 ?
Fe2 C6 1.928(14) 2_656 ?
Fe2 C6 1.928(15) . ?
Fe2 C5 1.937(13) 2_656 ?
Fe2 C5 1.937(13) . ?
Fe2 C4 1.948(15) . ?
Fe2 C4 1.948(15) 2_656 ?
O1 N7 1.322(12) . ?
O2 N8 1.329(12) . ?
O2 Sm1 2.388(8) 1_455 ?
N1 C1 1.158(17) . ?
N2 C2 1.129(18) . ?
N3 C3 1.172(15) . ?
N3 Sm1 2.530(11) 1_565 ?
N4 C4 1.130(18) . ?
N6 C6 1.161(17) . ?
N6 Sm1 2.520(11) 1_545 ?
N7 C7 1.346(16) . ?
N7 C11 1.366(15) . ?
N8 C14 1.350(17) . ?
N8 C15 1.388(14) . ?
C7 C8 1.353(17) . ?
C8 C9 1.389(17) . ?
C9 C10 1.401(18) . ?
C9 C12 1.475(17) . ?
C10 C11 1.328(17) . ?
C12 C16 1.378(18) . ?
C12 C13 1.389(18) . ?
C13 C14 1.360(18) . ?
C15 C16 1.304(16) . ?
N5 C5 1.138(16) . ?
