Functionality in Metal-Organic Framework Minerals: Proton Conductivity, Stability and Potential for Polymorphism
Huskic, Igor; Novendra, Novendra; Lim, Dae-Woon; Topić, Filip; Titi, Hatem M.; Pekov, I. V.; Krivovichev, S.; Navrotsky, Alexandra; Kitagawa, Hiroshi; Friščić, Tomislav; Chemical Science  (2019) –; doi:10.1039/C8SC05088K

data_1550827
_publ_section_title
;
 Functionality in Metal-Organic Framework Minerals: Proton Conductivity,
 Stability and Potential for Polymorphism
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05088K
_journal_year                    2019
_chemical_compound_source        synthetic
_chemical_formula_moiety         'Na Fe C6 O12 2-, Mg O6 H12 2+, H6 O3'
_chemical_formula_sum            'C6 H18 Fe Mg Na O21'
_chemical_formula_weight         529.35
_chemical_name_common            Stepanovite
_chemical_name_systematic
'Sodium magnesium Iron(iii) oxalate nonahydrate'
_chemical_properties_physical
photo-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-09-19 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.8670(9)
_cell_length_b                   9.8670(9)
_cell_length_c                   36.735(3)
_cell_measurement_reflns_used    17286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.578
_cell_measurement_theta_min      5.258
_cell_volume                     3097.3(5)
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            15115
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_min         2.447
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       'rhombohedral block'
_exptl_crystal_F_000             1626
_exptl_crystal_recrystallization_method water
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 794 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1657
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.2611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                1629
_reflns_number_total             1657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05088k2.cif
_cod_data_source_block           StepI_100
_cod_original_cell_volume        3097.2(6)
_cod_database_code               1550827
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              79904