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_1550830
_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 (H2O)6 2+'
_chemical_formula_sum            'C6 H12 Fe Mg Na O18'
_chemical_formula_weight         475.31
_chemical_name_systematic
'Sodium magnesium iron(III) oxalate hexahydrate'
_chemical_properties_physical
'moisture-sensitive, photo-sensitive,Moisture-sensitive,Deliquescent,Light-sensitive'
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :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                   9.77454(19)
_cell_length_b                   9.77454(19)
_cell_length_c                   29.7940(11)
_cell_measurement_reflns_used    23935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.781
_cell_measurement_theta_min      5.566
_cell_volume                     2465.20(11)
_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_pressure         101325
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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  0.1089
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            58144
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         39.297
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker D8'
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_crystal_colour            'dull green'
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1446
_exptl_crystal_recrystallization_method 'dehydrated from nonahydrate'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.617
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0830P)^2^+6.4457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                5643
_reflns_number_total             6325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05088k2.cif
_cod_data_source_block           StepI_dehydr
_cod_original_cell_volume        2465.20(13)
_cod_database_code               1550830
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.813
_shelx_res_checksum              23559