#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/04/1540492.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_1540492
loop_
_publ_author_name
'Sadakiyo, Masaaki'
'Yamada, Teppei'
'Kato, Kenichi'
'Takata, Masaki'
'Kitagawa, Hiroshi'
_publ_section_title
;
 A significant change in selective adsorption behaviour for ethanol by
 flexibility control through the type of central metals in a
 metal--organic framework
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1349
_journal_paper_doi               10.1039/C5SC03325J
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C10 H26 Fe2 N2 O18'
_chemical_formula_sum            'C10 H26 Fe2 N2 O18'
_chemical_formula_weight         574.03
_chemical_name_common            {H3N(CH2)4NH3}[Fe2(C2O4)3](H2O)6
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2015-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.1900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2586(9)
_cell_length_b                   15.8638(17)
_cell_length_c                   9.4209(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1134.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'yadokari-XG (K. Wakita, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker SMART APEX CCD-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode with a mirror focusing unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6475
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0303P)²+0.4219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                2592
_reflns_number_total             2699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc03325j2.cif
_cod_data_source_block           FeDAB-6H2O
_cod_depositor_comments
'Adding full bibliography for 1540492--1540493.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1540492
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Fe1 Fe 0.527480(18) 0.669966(9) 0.958035(17) 0.01163(6) Uani 1 1 d
O4 O 0.24755(10) 0.67737(5) 0.83600(9) 0.01611(16) Uani 1 1 d
O3 O 0.54540(10) 0.76675(5) 1.12135(9) 0.01503(16) Uani 1 1 d
O2 O 0.50434(9) 0.74902(5) 0.77290(9) 0.01422(15) Uani 1 1 d
O1 O 0.80398(10) 0.68853(5) 1.06562(9) 0.01491(15) Uani 1 1 d
O6 O 0.51242(11) 0.58416(5) 1.12307(9) 0.01597(16) Uani 1 1 d
O8 O 0.74618(12) 0.67726(5) 0.66391(11) 0.01918(18) Uani 1 1 d
O5 O 0.53490(10) 0.55290(5) 0.85179(9) 0.01613(16) Uani 1 1 d
O9 O 0.06139(12) 0.59842(6) 0.99772(10) 0.01854(17) Uani 1 1 d
O7 O 0.46081(15) 0.62104(9) 1.39727(14) 0.0428(3) Uani 1 1 d
N1 N 0.69365(13) 0.99763(7) 0.77191(12) 0.01644(19) Uani 1 1 d
C5 C 0.57830(15) 1.00985(7) 0.97885(13) 0.0165(2) Uani 1 1 d
C2 C 0.20015(13) 0.72080(6) 0.71591(12) 0.01247(19) Uani 1 1 d
C3 C 0.49370(13) 0.50878(7) 1.07898(12) 0.01290(19) Uani 1 1 d
C4 C 0.54523(15) 0.97819(8) 0.81860(13) 0.0178(2) Uani 1 1 d
C1 C 0.34949(13) 0.76423(6) 0.68109(12) 0.01197(19) Uani 1 1 d
H6 H 0.599(2) 1.0695(11) 0.9819(18) 0.029(4) Uiso 1 1 d
H4 H 0.445(2) 1.0038(9) 0.7443(17) 0.020(4) Uiso 1 1 d
H7 H 0.681(2) 0.9839(10) 1.0505(17) 0.024(4) Uiso 1 1 d
H5 H 0.533(2) 0.9220(11) 0.8152(19) 0.029(4) Uiso 1 1 d
H3 H 0.165(2) 0.5206(10) 1.175(2) 0.027(4) Uiso 1 1 d
H2 H 0.212(2) 0.4480(11) 1.2769(18) 0.024(4) Uiso 1 1 d
H1 H 0.283(2) 0.5268(10) 1.3318(19) 0.025(4) Uiso 1 1 d
H10 H 0.702(2) 0.7084(12) 0.7026(19) 0.032(5) Uiso 1 1 d
H11 H 0.830(3) 0.6976(12) 0.659(2) 0.034(5) Uiso 1 1 d
H13 H 0.107(2) 0.6247(11) 0.955(2) 0.032(4) Uiso 1 1 d
H12 H -0.010(2) 0.6293(12) 1.012(2) 0.035(5) Uiso 1 1 d
H9 H 0.495(2) 0.6170(12) 0.328(2) 0.042(5) Uiso 1 1 d
H8 H 0.548(3) 0.6345(14) 0.471(2) 0.049(6) Uiso 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'
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
O2 Fe1 O6 171.38(3) . .
O2 Fe1 O5 98.12(3) . .
O6 Fe1 O5 78.68(3) . .
O2 Fe1 O1 92.45(3) . .
O6 Fe1 O1 95.87(3) . .
O5 Fe1 O1 96.96(3) . .
O2 Fe1 O3 97.30(3) . .
O6 Fe1 O3 86.58(3) . .
O5 Fe1 O3 164.09(3) . .
O1 Fe1 O3 78.47(3) . .
O2 Fe1 O4 78.17(3) . .
O6 Fe1 O4 93.82(3) . .
O5 Fe1 O4 91.17(3) . .
O1 Fe1 O4 168.40(3) . .
O3 Fe1 O4 95.81(3) . .
C2 O4 Fe1 113.81(7) . .
C2 O3 Fe1 112.78(6) 4_676 .
C1 O2 Fe1 115.07(7) . .
C1 O1 Fe1 113.38(7) 4_676 .
C3 O6 Fe1 114.00(7) . .
C3 O5 Fe1 113.13(7) 3_667 .
C4 C5 C5 110.74(12) . 3_677
O4 C2 O3 126.82(10) . 4_575
O4 C2 C1 116.33(9) . .
O3 C2 C1 116.84(9) 4_575 .
O5 C3 O6 126.69(10) 3_667 .
O5 C3 C3 117.16(12) 3_667 3_667
O6 C3 C3 116.15(12) . 3_667
N1 C4 C5 112.38(9) . .
O1 C1 O2 126.24(9) 4_575 .
O1 C1 C2 117.19(9) 4_575 .
O2 C1 C2 116.56(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O2 2.0949(8) .
Fe1 O6 2.1067(8) .
Fe1 O5 2.1219(8) .
Fe1 O1 2.1227(8) .
Fe1 O3 2.1371(8) .
Fe1 O4 2.1417(8) .
O4 C2 1.2486(13) .
O3 C2 1.2527(13) 4_676
O2 C1 1.2532(13) .
O1 C1 1.2507(13) 4_676
O6 C3 1.2553(14) .
O5 C3 1.2490(13) 3_667
N1 C4 1.4884(14) .
C5 C4 1.5104(15) .
C5 C5 1.528(2) 3_677
C2 O3 1.2527(13) 4_575
C2 C1 1.5563(14) .
C3 O5 1.2490(13) 3_667
C3 C3 1.557(2) 3_667
C1 O1 1.2507(13) 4_575
