#------------------------------------------------------------------------------
#$Date: 2019-11-28 20:57:21 +0100 (jue 28 de nov de 2019) $
#$Revision: 244737 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/95/7239506.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_7239506
loop_
_publ_author_name
'Horike, Satoshi'
'Sugimoto, Masayuki'
'Kongpatpanich, Kanokwan'
'Hijikata, Yuh'
'Inukai, Munehiro'
'Umeyama, Daiki'
'Kitao, Shinji'
'Seto, Makoto'
'Kitagawa, Susumu'
_publ_section_title
;
 Fe2+-based layered porous coordination polymers and soft encapsulation of
 guests via redox activity
;
_journal_issue                   11
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              3675
_journal_paper_doi               10.1039/c3ta01414b
_journal_volume                  1
_journal_year                    2013
_chemical_formula_sum            'C18 H12 Fe N2 O4'
_chemical_formula_weight         376.15
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 103.182(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.064(3)
_cell_length_b                   11.475(3)
_cell_length_c                   15.916(5)
_cell_measurement_temperature    223(2)
_cell_volume                     1789.6(9)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        yadokari
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13949
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.8459
_exptl_absorpt_correction_T_min  0.8459
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.659
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0987
_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)+(0.1497P)²+11.5383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2965
_refine_ls_wR_factor_ref         0.3074
_reflns_number_gt                3504
_reflns_number_total             4020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ta01414b.txt
_cod_data_source_block           FeCID-1_DMF
_cod_original_sg_symbol_H-M      P2/C
_cod_database_code               7239506
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
Fe1 Fe 0.12205(8) 0.26978(7) 0.66430(5) 0.0217(3) Uani 1 1 d .
O2 O -0.6612(4) 0.2781(4) 0.6727(3) 0.0287(10) Uani 1 1 d .
O3 O -0.0740(4) 0.2744(4) 0.5884(3) 0.0277(9) Uani 1 1 d .
C4 C -0.1720(6) 0.2774(5) 0.6253(4) 0.0212(11) Uani 1 1 d .
O5 O -0.1586(5) 0.2594(4) 0.7036(3) 0.0325(10) Uani 1 1 d .
O6 O -0.7949(5) 0.2871(5) 0.5437(3) 0.0379(12) Uani 1 1 d .
C28 C -0.4257(6) 0.2884(5) 0.6065(4) 0.0227(11) Uani 1 1 d .
H1 H -0.4148 0.2668 0.6647 0.027 Uiso 1 1 calc R
C8 C -0.3121(6) 0.3015(5) 0.5713(4) 0.0221(11) Uani 1 1 d .
N8 N 0.1246(5) 0.0796(5) 0.6615(3) 0.0298(11) Uani 1 1 d .
C10 C 0.0242(7) 0.5232(6) 0.6185(4) 0.0315(14) Uani 1 1 d .
H2 H -0.0451 0.4827 0.5800 0.038 Uiso 1 1 calc R
C11 C -0.5554(6) 0.3073(6) 0.5552(4) 0.0260(12) Uani 1 1 d .
C12 C 0.1254(6) -0.1656(6) 0.6682(4) 0.0282(13) Uani 1 1 d .
C13 C 0.0226(7) 0.6427(6) 0.6162(4) 0.0323(14) Uani 1 1 d .
H3 H -0.0468 0.6819 0.5768 0.039 Uiso 1 1 calc R
C14 C -0.3279(6) 0.3393(7) 0.4862(4) 0.0330(14) Uani 1 1 d .
H4 H -0.2511 0.3495 0.4627 0.040 Uiso 1 1 calc R
C15 C 0.2229(8) 0.6437(6) 0.7285(5) 0.0382(16) Uani 1 1 d .
H5 H 0.2941 0.6824 0.7669 0.046 Uiso 1 1 calc R
C16 C 0.2150(8) 0.5212(6) 0.7271(5) 0.0391(16) Uani 1 1 d .
H6 H 0.2812 0.4792 0.7669 0.047 Uiso 1 1 calc R
C17 C -0.6785(6) 0.2898(5) 0.5925(4) 0.0257(12) Uani 1 1 d .
C18 C 0.1230(6) 0.7057(5) 0.6718(4) 0.0244(12) Uani 1 1 d .
C19 C -0.5709(7) 0.3443(7) 0.4699(4) 0.0381(16) Uani 1 1 d .
H7 H -0.6588 0.3572 0.4354 0.046 Uiso 1 1 calc R
N9 N 0.1194(5) 0.4617(5) 0.6727(3) 0.0261(11) Uani 1 1 d .
C29 C -0.4590(7) 0.3619(8) 0.4362(5) 0.046(2) Uani 1 1 d .
H8 H -0.4701 0.3893 0.3793 0.055 Uiso 1 1 calc R
C23 C 0.0365(14) 0.0189(12) 0.6031(9) 0.031(3) Uiso 0.50 1 d P
H9 H -0.0263 0.0589 0.5600 0.037 Uiso 0.50 1 calc PR
C25 C 0.0346(15) -0.1056(12) 0.6041(10) 0.034(3) Uiso 0.50 1 d P
H10 H -0.0279 -0.1466 0.5614 0.041 Uiso 0.50 1 calc PR
C26 C 0.2202(14) -0.0963(12) 0.7262(10) 0.031(3) Uiso 0.50 1 d P
H11 H 0.2877 -0.1326 0.7688 0.037 Uiso 0.50 1 calc PR
C27 C 0.2157(15) 0.0232(12) 0.7215(10) 0.032(3) Uiso 0.50 1 d P
H12 H 0.2790 0.0667 0.7620 0.038 Uiso 0.50 1 calc PR
C30 C 0.0034(17) -0.1070(14) 0.6398(11) 0.042(3) Uiso 0.50 1 d P
H13 H -0.0790 -0.1483 0.6229 0.051 Uiso 0.50 1 calc PR
C31 C 0.0047(18) 0.0143(15) 0.6368(11) 0.045(4) Uiso 0.50 1 d P
H14 H -0.0784 0.0539 0.6173 0.054 Uiso 0.50 1 calc PR
C32 C 0.2339(15) 0.0210(12) 0.6899(10) 0.033(3) Uiso 0.50 1 d P
H15 H 0.3154 0.0628 0.7096 0.040 Uiso 0.50 1 calc PR
C33 C 0.2409(17) -0.1023(14) 0.6939(11) 0.039(3) Uiso 0.50 1 d P
H16 H 0.3251 -0.1398 0.7142 0.047 Uiso 0.50 1 calc PR
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
O5 Fe1 O3 121.64(18) 2_556 .
O5 Fe1 O2 89.79(18) 2_556 1_655
O3 Fe1 O2 148.50(18) . 1_655
O5 Fe1 N8 87.9(2) 2_556 .
O3 Fe1 N8 91.60(19) . .
O2 Fe1 N8 91.66(19) 1_655 .
O5 Fe1 N9 89.88(19) 2_556 .
O3 Fe1 N9 89.23(18) . .
O2 Fe1 N9 88.75(18) 1_655 .
N8 Fe1 N9 177.69(19) . .
O5 Fe1 O6 148.90(18) 2_556 1_655
O3 Fe1 O6 89.41(17) . 1_655
O2 Fe1 O6 59.12(16) 1_655 1_655
N8 Fe1 O6 93.5(2) . 1_655
N9 Fe1 O6 88.6(2) . 1_655
C17 O2 Fe1 92.1(4) . 1_455
C4 O3 Fe1 118.2(4) . .
O5 C4 O3 123.2(6) . .
O5 C4 C8 118.6(5) . .
O3 C4 C8 118.2(5) . .
C4 O5 Fe1 166.5(5) . 2_556
C17 O6 Fe1 87.1(4) . 1_455
C11 C28 C8 119.6(5) . .
C11 C28 H1 120.2 . .
C8 C28 H1 120.2 . .
C28 C8 C14 120.1(5) . .
C28 C8 C4 120.1(5) . .
C14 C8 C4 119.8(5) . .
C32 N8 C23 110.8(10) . .
C32 N8 C27 25.3(7) . .
C23 N8 C27 119.3(10) . .
C32 N8 C31 115.8(11) . .
C23 N8 C31 29.0(7) . .
C27 N8 C31 110.5(10) . .
C32 N8 Fe1 122.0(7) . .
C23 N8 Fe1 122.0(7) . .
C27 N8 Fe1 118.7(7) . .
C31 N8 Fe1 121.9(8) . .
N9 C10 C13 123.2(6) . .
N9 C10 H2 118.4 . .
C13 C10 H2 118.4 . .
C28 C11 C19 120.1(6) . .
C28 C11 C17 119.6(5) . .
C19 C11 C17 120.3(6) . .
C33 C12 C30 118.4(11) . .
C33 C12 C25 109.4(10) . .
C30 C12 C25 29.7(7) . .
C33 C12 C26 25.0(7) . .
C30 C12 C26 110.9(10) . .
C25 C12 C26 115.7(10) . .
C33 C12 C18 123.0(8) . 1_545
C30 C12 C18 118.6(9) . 1_545
C25 C12 C18 120.8(8) . 1_545
C26 C12 C18 123.5(7) . 1_545
C10 C13 C18 120.1(6) . .
C10 C13 H3 119.9 . .
C18 C13 H3 119.9 . .
C8 C14 C29 119.5(6) . .
C8 C14 H4 120.2 . .
C29 C14 H4 120.2 . .
C18 C15 C16 118.2(6) . .
C18 C15 H5 120.9 . .
C16 C15 H5 120.9 . .
N9 C16 C15 123.6(6) . .
N9 C16 H6 118.2 . .
C15 C16 H6 118.2 . .
O6 C17 O2 121.5(6) . .
O6 C17 C11 119.8(6) . .
O2 C17 C11 118.7(5) . .
C15 C18 C13 117.7(6) . .
C15 C18 C12 121.5(6) . 1_565
C13 C18 C12 120.8(5) . 1_565
C29 C19 C11 120.4(6) . .
C29 C19 H7 119.8 . .
C11 C19 H7 119.8 . .
C16 N9 C10 117.1(6) . .
C16 N9 Fe1 122.4(4) . .
C10 N9 Fe1 120.3(4) . .
C19 C29 C14 120.1(6) . .
C19 C29 H8 119.9 . .
C14 C29 H8 119.9 . .
N8 C23 C25 121.7(12) . .
N8 C23 H9 119.1 . .
C25 C23 H9 119.1 . .
C12 C25 C23 119.8(12) . .
C12 C25 H10 120.1 . .
C23 C25 H10 120.1 . .
C27 C26 C12 121.1(12) . .
C27 C26 H11 119.4 . .
C12 C26 H11 119.4 . .
N8 C27 C26 122.3(13) . .
N8 C27 H12 118.9 . .
C26 C27 H12 118.9 . .
C12 C30 C31 118.9(15) . .
C12 C30 H13 120.6 . .
C31 C30 H13 120.6 . .
C30 C31 N8 122.7(15) . .
C30 C31 H14 118.7 . .
N8 C31 H14 118.7 . .
N8 C32 C33 124.7(13) . .
N8 C32 H15 117.7 . .
C33 C32 H15 117.7 . .
C12 C33 C32 119.5(13) . .
C12 C33 H16 120.3 . .
C32 C33 H16 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O5 2.054(5) 2_556
Fe1 O3 2.066(4) .
Fe1 O2 2.157(4) 1_655
Fe1 N8 2.184(6) .
Fe1 N9 2.207(5) .
Fe1 O6 2.270(5) 1_655
O2 C17 1.256(8) .
O2 Fe1 2.157(4) 1_455
O3 C4 1.258(7) .
C4 O5 1.240(7) .
C4 C8 1.500(8) .
O5 Fe1 2.054(5) 2_556
O6 C17 1.250(8) .
O6 Fe1 2.270(5) 1_455
C28 C11 1.390(9) .
C28 C8 1.390(8) .
C28 H1 0.9400 .
C8 C14 1.397(8) .
N8 C32 1.280(15) .
N8 C23 1.326(15) .
N8 C27 1.330(15) .
N8 C31 1.398(18) .
C10 N9 1.336(8) .
C10 C13 1.371(9) .
C10 H2 0.9400 .
C11 C19 1.396(9) .
C11 C17 1.505(8) .
C12 C33 1.353(17) .
C12 C30 1.382(17) .
C12 C25 1.388(15) .
C12 C26 1.413(15) .
C12 C18 1.478(9) 1_545
C13 C18 1.386(9) .
C13 H3 0.9400 .
C14 C29 1.401(9) .
C14 H4 0.9400 .
C15 C18 1.385(9) .
C15 C16 1.408(10) .
C15 H5 0.9400 .
C16 N9 1.328(9) .
C16 H6 0.9400 .
C18 C12 1.478(9) 1_565
C19 C29 1.369(9) .
C19 H7 0.9400 .
C29 H8 0.9400 .
C23 C25 1.429(19) .
C23 H9 0.9400 .
C25 H10 0.9400 .
C26 C27 1.37(2) .
C26 H11 0.9400 .
C27 H12 0.9400 .
C30 C31 1.39(2) .
C30 H13 0.9400 .
C31 H14 0.9400 .
C32 C33 1.42(2) .
C32 H15 0.9400 .
C33 H16 0.9400 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O5 Fe1 O3 C4 4.0(5) 2_556 .
O2 Fe1 O3 C4 -171.7(4) 1_655 .
N8 Fe1 O3 C4 92.5(4) . .
N9 Fe1 O3 C4 -85.4(4) . .
O6 Fe1 O3 C4 -174.0(4) 1_655 .
Fe1 O3 C4 O5 -11.8(8) . .
Fe1 O3 C4 C8 169.6(4) . .
O3 C4 O5 Fe1 81(2) . 2_556
C8 C4 O5 Fe1 -99.9(18) . 2_556
C11 C28 C8 C14 3.3(9) . .
C11 C28 C8 C4 -178.0(5) . .
O5 C4 C8 C28 -8.4(8) . .
O3 C4 C8 C28 170.3(5) . .
O5 C4 C8 C14 170.4(6) . .
O3 C4 C8 C14 -10.9(9) . .
O5 Fe1 N8 C32 -68.4(10) 2_556 .
O3 Fe1 N8 C32 170.0(10) . .
O2 Fe1 N8 C32 21.3(10) 1_655 .
N9 Fe1 N8 C32 -79(5) . .
O6 Fe1 N8 C32 80.5(10) 1_655 .
O5 Fe1 N8 C23 139.2(9) 2_556 .
O3 Fe1 N8 C23 17.6(9) . .
O2 Fe1 N8 C23 -131.0(8) 1_655 .
N9 Fe1 N8 C23 129(5) . .
O6 Fe1 N8 C23 -71.9(8) 1_655 .
O5 Fe1 N8 C27 -39.3(9) 2_556 .
O3 Fe1 N8 C27 -160.9(9) . .
O2 Fe1 N8 C27 50.4(9) 1_655 .
N9 Fe1 N8 C27 -50(5) . .
O6 Fe1 N8 C27 109.6(9) 1_655 .
O5 Fe1 N8 C31 104.9(10) 2_556 .
O3 Fe1 N8 C31 -16.7(10) . .
O2 Fe1 N8 C31 -165.4(10) 1_655 .
N9 Fe1 N8 C31 94(5) . .
O6 Fe1 N8 C31 -106.2(10) 1_655 .
C8 C28 C11 C19 -2.8(10) . .
C8 C28 C11 C17 178.3(5) . .
N9 C10 C13 C18 0.1(11) . .
C28 C8 C14 C29 -1.1(11) . .
C4 C8 C14 C29 -179.8(7) . .
C18 C15 C16 N9 2.0(12) . .
Fe1 O6 C17 O2 3.0(6) 1_455 .
Fe1 O6 C17 C11 -177.1(5) 1_455 .
Fe1 O2 C17 O6 -3.2(7) 1_455 .
Fe1 O2 C17 C11 176.9(5) 1_455 .
C28 C11 C17 O6 -167.8(6) . .
C19 C11 C17 O6 13.3(10) . .
C28 C11 C17 O2 12.1(9) . .
C19 C11 C17 O2 -166.8(7) . .
C16 C15 C18 C13 -1.0(10) . .
C16 C15 C18 C12 -178.9(6) . 1_565
C10 C13 C18 C15 0.0(10) . .
C10 C13 C18 C12 178.0(6) . 1_565
C28 C11 C19 C29 0.1(12) . .
C17 C11 C19 C29 179.0(7) . .
C15 C16 N9 C10 -1.9(11) . .
C15 C16 N9 Fe1 174.0(6) . .
C13 C10 N9 C16 0.9(10) . .
C13 C10 N9 Fe1 -175.2(5) . .
O5 Fe1 N9 C16 47.5(6) 2_556 .
O3 Fe1 N9 C16 169.1(6) . .
O2 Fe1 N9 C16 -42.3(6) 1_655 .
N8 Fe1 N9 C16 58(5) . .
O6 Fe1 N9 C16 -101.5(6) 1_655 .
O5 Fe1 N9 C10 -136.7(5) 2_556 .
O3 Fe1 N9 C10 -15.1(5) . .
O2 Fe1 N9 C10 133.5(5) 1_655 .
N8 Fe1 N9 C10 -126(5) . .
O6 Fe1 N9 C10 74.4(5) 1_655 .
C11 C19 C29 C14 2.1(14) . .
C8 C14 C29 C19 -1.6(13) . .
C32 N8 C23 C25 27.9(18) . .
C27 N8 C23 C25 1.5(19) . .
C31 N8 C23 C25 -78(2) . .
Fe1 N8 C23 C25 -177.0(10) . .
C33 C12 C25 C23 -29.7(17) . .
C30 C12 C25 C23 84(2) . .
C26 C12 C25 C23 -3.5(17) . .
C18 C12 C25 C23 178.5(10) 1_545 .
N8 C23 C25 C12 1(2) . .
C33 C12 C26 C27 84(3) . .
C30 C12 C26 C27 -28.2(18) . .
C25 C12 C26 C27 3.8(18) . .
C18 C12 C26 C27 -178.2(11) 1_545 .
C32 N8 C27 C26 -78(3) . .
C23 N8 C27 C26 -1(2) . .
C31 N8 C27 C26 29.3(19) . .
Fe1 N8 C27 C26 177.3(11) . .
C12 C26 C27 N8 -1(2) . .
C33 C12 C30 C31 2(2) . .
C25 C12 C30 C31 -78(2) . .
C26 C12 C30 C31 28.0(19) . .
C18 C12 C30 C31 179.6(12) 1_545 .
C12 C30 C31 N8 0(2) . .
C32 N8 C31 C30 -2(2) . .
C23 N8 C31 C30 85(2) . .
C27 N8 C31 C30 -29(2) . .
Fe1 N8 C31 C30 -175.8(13) . .
C23 N8 C32 C33 -28(2) . .
C27 N8 C32 C33 87(3) . .
C31 N8 C32 C33 3(2) . .
Fe1 N8 C32 C33 176.7(12) . .
C30 C12 C33 C32 -1(2) . .
C25 C12 C33 C32 30.2(18) . .
C26 C12 C33 C32 -79(3) . .
C18 C12 C33 C32 -178.7(11) 1_545 .
N8 C32 C33 C12 -2(3) . .
