{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_7715465
_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         'H50 Mo30 Na8 O110, 23(H2 O), 2[H2O]'
_chemical_formula_sum            'H106 Mo30 Na8 O135'
_chemical_formula_weight         5328.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_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                117.502(3)
_cell_angle_beta                 92.025(3)
_cell_angle_gamma                90.738(3)
_cell_formula_units_Z            2
_cell_length_a                   17.5249(13)
_cell_length_b                   19.2536(17)
_cell_length_c                   20.5386(19)
_cell_measurement_reflns_used    9080
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.392
_cell_measurement_theta_min      2.386
_cell_volume                     6139.8(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruke D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            145349
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.426
_diffrn_reflns_theta_min         1.978
_diffrn_source_current           1.41
_diffrn_source_power             0.0705
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.107
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1560 before and 0.0777 after correction.
The Ratio of minimum to maximum transmission is 0.7292.
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    2.879
_exptl_crystal_description       needle
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.123
_refine_diff_density_min         -2.170
_refine_diff_density_rms         0.368
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1475
_refine_ls_number_reflns         22517
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0921
_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^)+(0.0174P)^2^+510.5080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.1962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19021
_reflns_number_total             22517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00187g2.cif
_cod_data_source_block           mo30
_cod_depositor_comments
'Adding full bibliography for 7715463--7715465.cif.'
_cod_database_code               7715465
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.562
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H12J-H11F
 2.1 with sigma of 0.02
 H11D-H12T
 2.1 with sigma of 0.02
 H11T-H97A
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O106) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O113) \\sim Ueq, Uanis(O122) \\sim Ueq, Uanis(O133) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O58) \\sim Ueq, Uanis(O98) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O85) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O55) \\sim Ueq, Uanis(O73) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
Uanis(O36) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O111) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O71) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O68) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(O70) \\sim Ueq, Uanis(O59) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Na8(0.5) O105(0.5) H10I(0.5) H10J(0.5) Na10(0.5) O116(0.5)
 H11G(0.5) H11H(0.5) O113(0.5) H11A(0.5) H11B(0.5) O110(0.5) H11O(0.5)
 H11P(0.5) O120(0.5) H12C(0.5) H12D(0.5) O121(0.5) H12E(0.5) H12F(0.5)
 O126(0.6) H12G(0.6) H12H(0.6) O127(0.5) H12K(0.5) H12L(0.5) O125(0.5)
 H12M(0.5) H12N(0.5) O131(0.5) H13E(0.5) H13F(0.5) O130(0.5) H13G(0.5)
 H13H(0.5) O135(0.5) H13K(0.5) H13L(0.5) O136(0.5) H13M(0.5) H13N(0.5)
 O137(0.5) H13O(0.5) H13P(0.5) O139(0.4) H13Q(0.4) H13R(0.4) O140(0.5)
 H14A(0.5) H14B(0.5) O141(0.5) H14C(0.5) H14D(0.5) O142(0.5) H14E(0.5) H14F(0.5)
5.a Riding coordinates:
 O15(H51,H15), O17(H17), O6(H60,H6), O53(H53), O4(H4,H8), O58(H58,H75),
 O91(H91A,H91B), O92(H92A,H92B), O93(H93A,H93B), O94(H94A,H94B), O97(H97A,H97B),
  O100(H10Q,H10R), O98(H98A,H98B), O99(H99A,H99B), O95(H95A,H95B), O96(H96A,
 H96B), O101(H10A,H10B), O102(H10C,H10D), O103(H10E,H10F), O104(H10G,H10H),
 O105(H10I,H10J), O108(H10K,H10L), O107(H10M,H10N), O106(H10O,H10P), O111(H11C,
 H11D), O109(H10S,H10T), O112(H11E,H11F), O116(H11G,H11H), O118(H11I,H11J),
 O114(H11K,H11L), O115(H11M,H11N), O113(H11A,H11B), O110(H11O,H11P), O119(H11Q,
 H11R), O120(H12C,H12D), O121(H12E,H12F), O126(H12G,H12H), O123(H12I,H12J),
 O127(H12K,H12L), O125(H12M,H12N), O122(H12A,H12B), O129(H12O,H12P), O128(H12Q,
 H12R), O132(H13C,H13D), O133(H13A,H13B), O131(H13E,H13F), O130(H13G,H13H),
 O134(H13I,H13J), O135(H13K,H13L), O136(H13M,H13N), O137(H13O,H13P), O139(H13Q,
 H13R), O140(H14A,H14B), O141(H14C,H14D), O142(H14E,H14F), O143(H14G,H14H),
 O117(H11S,H11T), O124(H12S,H12T)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 40 electrons were 
found in a volume of 367\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[H2O] per formula unit 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26334
_shelx_fab_checksum              92591
_olex2_submission_special_instructions 'No special instructions were received'