Effect of the ammonium ion on proton conduction in porous ionic crystals based on Keggin-type silicododecatungstate
Miyazawa, Satoru; Hosono, Reina; Osuga, Ryota; Kondo, Junko Nomura; Uchida, Sayaka; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618008227

data_2021255
_publ_section_title
;
 Effect of the ammonium ion on proton conduction in porous ionic crystals
 based on Keggin-type silicododecatungstate
;
_journal_coeditor_code           JR3010
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618008227
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'(N H4)2 [Cr3 (C H O2)6 O (C7 H9 N)3]2 [Si W12 O40], 8H2 O'
_chemical_formula_moiety
'2(H4 N1 +), C54 H56 Cr6 N6 O21 2+, Si W12 O40 4-, 8(H2 O)'
_chemical_formula_sum            'C54 H80 Cr6 N8 O69 Si W12'
_chemical_formula_weight         4491.50
_chemical_name_systematic
;
Diammonium tris(4-ethylpyridine)hexaformatooxidotrichromium
\a-silicododecatungstate
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'by CrystalStructure 4.2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.885(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   32.303(4)
_cell_length_b                   25.546(3)
_cell_length_c                   13.561(2)
_cell_measurement_reflns_used    15010
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      1.04
_cell_volume                     10455(2)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2007)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2007)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2007)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2015)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXL97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35536
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         1.044
_exptl_absorpt_coefficient_mu    13.867
_exptl_absorpt_correction_T_max  0.062
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8232.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.11
_refine_diff_density_min         -3.90
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0924P)^2^+183.1520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1750
_reflns_number_gt                7855
_reflns_number_total             9475
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jr3010sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        10456(2)
_cod_database_code               2021255
_shelx_hkl_checksum              30300
_shelx_res_checksum              14034
_cod_database_fobs_code 2021255