#------------------------------------------------------------------------------
#$Date: 2019-11-23 16:11:56 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/61/7236139.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_7236139
loop_
_publ_author_name
'Tu, Thach N.'
'Phan, Nghi Q.'
'Vu, Thanh T.'
'Nguyen, Ha L.'
'Cordova, Kyle E.'
'Furukawa, Hiroyasu'
_publ_section_title
;
 High proton conductivity at low relative humidity in an anionic Fe-based
 metal--organic framework
;
_journal_issue                   10
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              3638
_journal_paper_doi               10.1039/C5TA10467J
_journal_volume                  4
_journal_year                    2016
_chemical_formula_sum            'C18 H21 Fe2 N2 O14 S2'
_chemical_formula_weight         665.19
_chemical_name_systematic        VNU-15
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-20 deposited with the CCDC.
2016-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.7581(7)
_cell_length_b                   18.8268(9)
_cell_length_c                   38.9998(18)
_cell_measurement_reflns_used    300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.9142\%
_cell_measurement_theta_min      3.6931\%
_cell_volume                     12304.5(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  BrukerD8Venturediffractometer
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1476
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            18293
_diffrn_reflns_theta_full        63.66
_diffrn_reflns_theta_max         63.66
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    9.385
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Octahedral
_exptl_crystal_F_000             5424
_exptl_crystal_preparation       'proton conductivity'
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
;
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0547
_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)+(0.0633P)²+31.0633P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                1984
_reflns_number_total             2535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ta10467j2.cif
_cod_data_source_block           VNU-15
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7236139
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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
C1 C 0.6153(14) 0.1109(12) 0.1893(2) 0.026(5) Uani 0.50 1 d P A -1
C2 C 0.6194(5) 0.0401(6) 0.1747(2) 0.020(2) Uani 0.50 1 d P A -1
H2 H 0.6249 -0.0001 0.1893 0.024 Uiso 0.50 1 calc PR A -1
C3 C 0.6153(5) 0.0313(4) 0.1400(2) 0.0188(18) Uani 0.50 1 d P A -1
C4 C 0.6132(5) 0.1595(4) 0.13171(19) 0.019(2) Uiso 0.50 1 d P A -1
C5 C 0.6129(6) 0.1674(6) 0.1687(3) 0.023(2) Uani 0.50 1 d P A -1
H5 H 0.6109 0.2136 0.1784 0.027 Uiso 0.50 1 calc PR A -1
Fe2 Fe 0.3750 0.3750 0.20508(2) 0.0213(3) Uani 1 2 d S . .
N1 N 0.4743(3) 0.5501(3) 0.24571(13) 0.0544(13) Uani 1 1 d . . .
HN1A H 0.4221 0.5616 0.2505 0.065 Uiso 0.50 1 calc PR . .
HN1B H 0.4750 0.5050 0.2367 0.065 Uiso 0.50 1 calc PR . .
C8 C 0.4235(3) 0.1067(2) 0.15932(11) 0.0309(11) Uani 1 1 d . . .
H8 H 0.4246 0.0939 0.1829 0.037 Uiso 1 1 calc R . .
Fe1 Fe 0.5000 0.2500 0.2500 0.0217(3) Uani 1 2 d S . .
C9 C 0.6250 0.1250 0.22704(15) 0.0257(15) Uani 1 2 d S . .
S1 S 0.56956(8) 0.39589(7) 0.20846(4) 0.0474(4) Uani 1 1 d . . .
O5 O 0.60037(17) 0.17851(15) 0.24403(7) 0.0256(7) Uani 1 1 d . . .
O6 O 0.48723(18) 0.42304(16) 0.20864(8) 0.0356(8) Uani 1 1 d . . .
H1 H 0.6250 -0.015(4) 0.1250 0.05(2) Uiso 1 2 d S . .
O7 O 0.40760(19) 0.29728(16) 0.16945(7) 0.0338(8) Uani 1 1 d . . .
O8 O 0.4441(2) 0.21393(16) 0.20721(8) 0.0355(8) Uani 1 1 d . . .
O9 O 0.57243(19) 0.32575(18) 0.22430(10) 0.0481(10) Uani 1 1 d . . .
C11 C 0.4256(3) 0.2345(2) 0.17740(11) 0.0265(10) Uani 1 1 d . . .
O10 O 0.5946(3) 0.3878(3) 0.17277(13) 0.101(2) Uani 1 1 d . . .
C12 C 0.4232(3) 0.1785(2) 0.15001(11) 0.0284(11) Uani 1 1 d . . .
C13 C 0.4223(3) 0.1957(2) 0.11555(11) 0.0325(11) Uani 1 1 d . . .
H13 H 0.4208 0.2442 0.1088 0.039 Uiso 1 1 calc R . .
O11 O 0.6220(3) 0.4437(3) 0.2255(2) 0.128(3) Uani 1 1 d . . .
C14 C 0.5054(4) 0.6001(4) 0.2201(2) 0.083(2) Uani 1 1 d . . .
H14A H 0.4724 0.5979 0.1994 0.125 Uiso 1 1 calc R . .
H14B H 0.5605 0.5873 0.2144 0.125 Uiso 1 1 calc R . .
H14C H 0.5041 0.6484 0.2295 0.125 Uiso 1 1 calc R . .
C15 C 0.5200(5) 0.5509(5) 0.2772(2) 0.096(3) Uani 1 1 d . . .
H15D H 0.5735 0.5319 0.2728 0.144 Uiso 1 1 calc R . .
H15E H 0.4931 0.5215 0.2944 0.144 Uiso 1 1 calc R . .
H15G H 0.5242 0.5998 0.2856 0.144 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
C5 C1 C2 119.9(10) . .
C5 C1 C9 116.9(15) . .
C2 C1 C9 122.6(14) . .
C3 C2 C1 119.7(10) . .
C1 C5 C4 121.2(12) . .
O7 Fe2 O7 96.69(17) . 2
O7 Fe2 O6 88.66(12) . 2
O7 Fe2 O6 96.42(13) 2 2
O7 Fe2 O6 96.42(13) . .
O7 Fe2 O6 88.65(12) 2 .
O6 Fe2 O6 172.37(18) 2 .
O7 Fe2 O5 160.37(11) . 26_565
O7 Fe2 O5 102.92(11) 2 26_565
O6 Fe2 O5 88.29(12) 2 26_565
O6 Fe2 O5 85.02(12) . 26_565
O7 Fe2 O5 102.92(11) . 21_655
O7 Fe2 O5 160.37(11) 2 21_655
O6 Fe2 O5 85.02(12) 2 21_655
O6 Fe2 O5 88.29(12) . 21_655
O5 Fe2 O5 57.49(14) 26_565 21_655
C15 N1 C14 112.5(6) . .
C13 C8 C12 120.5(4) 8_544 .
O8 Fe1 O8 180.00(16) 21_655 .
O8 Fe1 O9 95.76(14) 21_655 21_655
O8 Fe1 O9 84.24(14) . 21_655
O8 Fe1 O9 84.24(14) 21_655 .
O8 Fe1 O9 95.76(14) . .
O9 Fe1 O9 179.998(1) 21_655 .
O8 Fe1 O5 93.55(12) 21_655 21_655
O8 Fe1 O5 86.45(12) . 21_655
O9 Fe1 O5 85.57(12) 21_655 21_655
O9 Fe1 O5 94.43(12) . 21_655
O8 Fe1 O5 86.45(12) 21_655 .
O8 Fe1 O5 93.54(12) . .
O9 Fe1 O5 94.43(12) 21_655 .
O9 Fe1 O5 85.57(12) . .
O5 Fe1 O5 180.00(12) 21_655 .
O5 C9 O5 117.4(5) . 14_545
O5 C9 C1 127.8(12) . .
O5 C9 C1 113.9(11) 14_545 .
O5 C9 C1 113.9(11) . 14_545
O5 C9 C1 127.8(12) 14_545 14_545
C1 C9 C1 23.8(10) . 14_545
O11 S1 O9 110.8(3) . .
O11 S1 O10 109.4(4) . .
O9 S1 O10 107.4(3) . .
O11 S1 O6 110.9(3) . .
O9 S1 O6 110.09(19) . .
O10 S1 O6 108.1(2) . .
C9 O5 Fe1 143.0(2) . .
C9 O5 Fe2 92.6(3) . 21_655
Fe1 O5 Fe2 108.88(11) . 21_655
S1 O6 Fe2 133.8(2) . .
C11 O7 Fe2 123.8(3) . .
C11 O8 Fe1 140.0(3) . .
S1 O9 Fe1 142.1(2) . .
O7 C11 O8 125.0(4) . .
O7 C11 C12 118.6(4) . .
O8 C11 C12 116.4(4) . .
C13 C12 C8 118.6(4) . .
C13 C12 C11 121.8(4) . .
C8 C12 C11 119.6(4) . .
C12 C13 C8 120.9(4) . 8_544
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C5 1.33(2) .
C1 C2 1.45(2) .
C1 C9 1.504(11) .
C2 C3 1.366(12) .
C4 C5 1.449(13) .
Fe2 O7 2.091(3) .
Fe2 O7 2.091(3) 2
Fe2 O6 2.091(3) 2
Fe2 O6 2.091(3) .
Fe2 O5 2.264(3) 26_565
Fe2 O5 2.264(3) 21_655
N1 C15 1.446(9) .
N1 C14 1.466(8) .
C8 C13 1.384(6) 8_544
C8 C12 1.398(6) .
Fe1 O8 2.030(3) 21_655
Fe1 O8 2.030(3) .
Fe1 O9 2.124(3) 21_655
Fe1 O9 2.124(3) .
Fe1 O5 2.167(3) 21_655
Fe1 O5 2.167(3) .
C9 O5 1.274(4) .
C9 O5 1.274(4) 14_545
C9 C1 1.505(11) 14_545
S1 O11 1.422(5) .
S1 O9 1.459(3) .
S1 O10 1.462(5) .
S1 O6 1.471(3) .
O5 Fe2 2.264(3) 21_655
O7 C11 1.259(5) .
O8 C11 1.264(5) .
C11 C12 1.502(6) .
C12 C13 1.383(6) .
C13 C8 1.384(6) 8_544
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 -0.010 0.125 754 233 ' '
2 -0.005 0.252 0.375 754 233 ' '
3 -0.013 0.486 0.625 754 233 ' '
4 -0.005 0.752 0.875 754 233 ' '
