Intrinsic and Extrinsic Proton Conductivity in Metal-Organic Frameworks
Tominaka, Satoshi; Cheetham, Tony; RSC Adv.  (2014) –; doi:10.1039/C4RA11473F

data_7218520
_publ_section_title
;
 Intrinsic and Extrinsic Proton Conductivity in Metal-Organic Frameworks
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA11473F
_journal_year                    2014
_chemical_formula_moiety         '2.94(C0.68 H1.36 Fe0.34 O2.04)'
_chemical_formula_sum            'C2 H4 Fe O6'
_chemical_formula_weight         179.90
_chemical_name_systematic        'Iron oxalate dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 128.20(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.209(4)
_cell_length_b                   5.5526(7)
_cell_length_c                   9.865(3)
_cell_measurement_reflns_used    872
_cell_measurement_temperature    297.20(14)
_cell_measurement_theta_max      26.7480
_cell_measurement_theta_min      4.1900
_cell_volume                     525.6(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      297.20(14)
_diffrn_detector_area_resol_mean 8.0591
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0115086000
_diffrn_orient_matrix_UB_12      0.1218706000
_diffrn_orient_matrix_UB_13      0.0272342000
_diffrn_orient_matrix_UB_21      -0.0718767000
_diffrn_orient_matrix_UB_22      0.0247105000
_diffrn_orient_matrix_UB_23      -0.0644341000
_diffrn_orient_matrix_UB_31      -0.0128803000
_diffrn_orient_matrix_UB_32      -0.0291664000
_diffrn_orient_matrix_UB_33      0.0590060000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2480
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.24
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.5126
_exptl_crystal_size_mid          0.0409
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         0.700
_refine_diff_density_min         -4.474
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         541
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.1090
_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/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2578
_refine_ls_wR_factor_ref         0.2684
_reflns_number_gt                479
_reflns_number_total             541
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra11473f3.cif
_cod_data_source_block           iron_oxalate_dihydrate_2_StackingFaults
_cod_original_cell_volume        525.6(3)
_cod_database_code               7218520
_chemical_oxdiff_formula         'Fe O6 C2 H4'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C1-O5
 1.25 with sigma of 0.02
 O2-C2
 1.25 with sigma of 0.02
 O3-C2 = C2-O2
 1.25 with sigma of 0.02
 O6-C1_$1 = C1_$1-O5_$1
 1.25 with sigma of 0.02
 O2_$1-C2_$1 = C2_$1-O3_$1
 1.25 with sigma of 0.02
 O6_$2-C1 = C1-O5
 1.25 with sigma of 0.02
 O3-O2
 2.237 with sigma of 0.04
 O6-O5_$1
 2.237 with sigma of 0.04
 O2_$1-O3_$1
 2.237 with sigma of 0.04
 O6_$2-O5
 2.237 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Fe1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.003
Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O5) \\sim
Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.003
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.003
4. Others
 Fixed Sof: C1(0.34) C2(0.66) O1(0.34) H1A(0.34) H1B(0.34) O2(0.66) O3(0.66)
 O4(0.66) H4A(0.66) H4B(0.66) O5(0.34) O6(0.34) Fe1(0.17) Fe2(0.33)
5.a Rotating group:
 O1(H1A,H1B), O4(H4A,H4B)
;