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

data_7218522
_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         'C2 H4 Fe O6'
_chemical_formula_sum            'C2 H4 Fe O6'
_chemical_formula_weight         179.90
_chemical_name_systematic        'Iron(II) 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             2014-05-28
_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                 128.03(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.065(12)
_cell_length_b                   5.559(2)
_cell_length_c                   9.817(9)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1220
_cell_measurement_theta_min      4.1990
_cell_volume                     518.6(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0591
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0059923000
_diffrn_orient_matrix_UB_12      0.1267128000
_diffrn_orient_matrix_UB_13      0.0037463000
_diffrn_orient_matrix_UB_21      0.0475059000
_diffrn_orient_matrix_UB_22      0.0177649000
_diffrn_orient_matrix_UB_23      -0.0189690000
_diffrn_orient_matrix_UB_31      -0.0576264000
_diffrn_orient_matrix_UB_32      0.0012956000
_diffrn_orient_matrix_UB_33      -0.0892374000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1413
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            1742
_diffrn_reflns_theta_full        14.05
_diffrn_reflns_theta_max         26.20
_diffrn_reflns_theta_min         4.25
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.0591
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.307
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0879
_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^)+(0.1236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2406
_reflns_number_gt                354
_reflns_number_total             466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra11473f2.cif
_cod_data_source_block           Iron_oxalate_dihydrate_1_pure
_cod_original_cell_volume        518.6(7)
_cod_database_code               7218522
_chemical_oxdiff_formula         'Fe C2 O6 H4'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O5(H5A,H5B)
;