{Mo<sub>4</sub>}-directed structural evolution of highly reduced molybdenum red clusters for efficient proton conduction.
Li, Bingbing; Lan, Yuxin; Su, Heyang; Xu, Jiaxin; Zhao, Qixin; Ma, Yubin; Zheng, Qi; Xuan, Weimin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6184–6189; doi:10.1039/d4dt00187g

data_7715463
_publ_section_title
;
 {Mo<sub>4</sub>}-directed structural evolution of highly reduced
 molybdenum red clusters for efficient proton conduction.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6184
_journal_page_last               6189
_journal_paper_doi               10.1039/d4dt00187g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'H68 Mo40 Na14 O148, 15(H4 O2), [+ solvents]3[H2O]'
_chemical_formula_sum            'H140 Mo40 Na14 O181'
_chemical_formula_weight         7196.52
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-07 deposited with the CCDC.	2024-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.538(3)
_cell_length_b                   20.538(3)
_cell_length_c                   41.601(8)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.331
_cell_measurement_theta_min      2.212
_cell_volume                     17548(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            86489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.386
_diffrn_reflns_theta_min         1.958
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1284 before and 0.0715 after correction.
The Ratio of minimum to maximum transmission is 0.7512.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.722
_exptl_crystal_description       prism
_exptl_crystal_F_000             13664
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.671
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4283
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+752.4692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3664
_reflns_number_total             4283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00187g2.cif
_cod_data_source_block           mo40
_cod_depositor_comments
'Adding full bibliography for 7715463--7715465.cif.'
_cod_original_cell_volume        17548(6)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               7715463
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O34-H34A = O34-H34B
 0.87 with sigma of 0.02
 O9-H9
 0.9 with sigma of 0.02
 O20-H20A = O20-H20B
 0.87 with sigma of 0.02
 O33-H33A = O33-H33B
 0.87 with sigma of 0.02
 H20A-H20B
 1.38 with sigma of 0.04
 H33A-H33B
 1.38 with sigma of 0.04
 H34A-H34B
 1.38 with sigma of 0.04
 Na3-H20A \\sim Na3-H20B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Na5(0.25) H20A(0.5) H20B(0.5) H23A(0.5) H23B(0.5) H28A(0.25)
 H28B(0.25) O33(0.5) H33A(0.5) H33B(0.5) O29(0.5) H29A(0.5) H29B(0.5) O27(0.25)
 H27A(0.25) H27B(0.25) O26(0.25) H26A(0.25) H26B(0.25) O31(0.5) H31A(0.5)
 H31B(0.5) O30(0.5) H30A(0.5) H30B(0.5) O34(0.5) H34A(0.5) H34B(0.5) O24(0.25)
 H24A(0.25) H24B(0.25) O35(0.5) H35A(0.5) H35B(0.5) O32(0.5) H32A(0.5)
 H32B(0.5) O25(0.25) H25A(0.25) H25B(0.25)
5.a Riding coordinates:
 O21(H21A,H21B), O20(H20A,H20B), O23(H23A,H23B), O28(H28A,H28B), O33(H33A,
 H33B), O29(H29A,H29B), O27(H27A,H27B), O26(H26A,H26B), O31(H31A,H31B),
 O30(H30A,H30B), O34(H34A,H34B), O24(H24A,H24B), O35(H35A,H35B), O32(H32A,H32B),
  O32(H9), O22(H22A,H22B), O25(H25A,H25B)
5.b Aromatic/amide H refined with riding coordinates:
 O13(H13)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 108 electrons were 
found in a volume of 1040\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
[+ solvents]3[H2O] per formula unit 
which account for 120 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96517
_shelx_fab_checksum              5325
_olex2_submission_special_instructions 'No special instructions were received'