Different Protonic Species Affecting Proton Conductivity in Hollow Spherelike Polyoxometalates.
Liu, Wen-Jing; Dong, Long-Zhang; Li, Run-Han; Chen, Yong-Jun; Sun, Sheng-Nan; Li, Shun-Li; Lan, Ya-Qian; ACS applied materials & interfaces 11 (2019) 7030–7036; doi:10.1021/acsami.8b20509

data_4514540
_publ_section_title
;
 Different Protonic Species Affecting Proton Conductivity in Hollow
 Spherelike Polyoxometalates.
;
_journal_issue                   7
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              7030
_journal_page_last               7036
_journal_paper_doi               10.1021/acsami.8b20509
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'Mo12 O40 P, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Mo12 N6 O40 P'
_chemical_formula_weight         2029.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.881(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9687(14)
_cell_length_b                   13.8385(17)
_cell_length_c                   12.4508(15)
_cell_measurement_reflns_used    7722
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.66
_cell_volume                     2042.7(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11690
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.658
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.715
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0480 before and 0.0324 after correction. The Ratio of minimum to maximum transmission is 0.8831. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.300
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.41
_refine_diff_density_max         1.585
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3931
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0980
_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^)+121.6833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3746
_reflns_number_total             3931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b20509_si_003.cif
_cod_data_source_block           mo_17092023_0m
_cod_database_code               4514540
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.311
_shelx_estimated_absorpt_t_min   0.280
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
N4 \\sim C6 \\sim C4 \\sim C5 \\sim N0AA: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N3 \\sim C1 \\sim C2 \\sim N1 \\sim C0AA: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O16)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O22) \\sim Ueq,
Uanis(O9) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
3. Others
 Fixed Sof: O4(0.5) O1(0.5) O3(0.5) O2(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5)
 N3(0.5) H3(0.5) C0AA(0.5) H0Ab(0.5) N1(0.5) H1a(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N0AA(H0AA), C5(H5), C6(H6), C4(H4a), C1(H1), C2(H2), N3(H3),
 C0AA(H0Ab), N1(H1a)
4.b Fitted pentagon refined as free rotating group:
 C1(C2,N3,C0AA,N1)
;
_olex2_submission_special_instructions 'No special instructions were received'