{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_7715464
_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         'H75.2 K6 Mo28 Na8 O122.1, 13.9(H2 O)'
_chemical_formula_sum            'H105 K6 Mo28 Na8 O136'
_chemical_formula_weight         5386.66
_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             2024-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-07 deposited with the CCDC.	2024-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                103.8710(10)
_cell_angle_beta                 93.2930(10)
_cell_angle_gamma                102.0700(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4876(3)
_cell_length_b                   17.1451(6)
_cell_length_c                   32.3504(11)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.322
_cell_measurement_theta_min      2.361
_cell_volume                     6010.1(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            134317
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_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    3.185
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1375 before and 0.0954 after correction.
The Ratio of minimum to maximum transmission is 0.9042.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.975
_exptl_crystal_description       refine
_exptl_crystal_F_000             5138
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.175
_refine_diff_density_min         -1.805
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1559
_refine_ls_number_reflns         21788
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+52.8829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17602
_reflns_number_total             21788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00187g2.cif
_cod_data_source_block           mo28
_cod_depositor_comments
'Adding full bibliography for 7715463--7715465.cif.'
_cod_database_code               7715464
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.630
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H11Q_$2-H13J
 2.1 with sigma of 0.02
 K6-H11K \\sim K6-H11L
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O122) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O112(0.8) H11I(0.8) H11J(0.8) O122(0.8) H12K(0.8) H12L(0.8)
 O132(0.6) H13K(0.6) H13L(0.6) O127(0.6) H12M(0.6) H12N(0.6) O136(0.4)
 H13A(0.4) H13B(0.4) O139(0.5) H13C(0.5) H13D(0.5) O137(0.8) H13O(0.8)
 H13P(0.8) O141(0.5) H14A(0.5) H14B(0.5) O128(0.6) H12S(0.6) H12T(0.6)
 O138(0.4) H13S(0.4) H13T(0.4)
5.a Riding coordinates:
 O93(H93A,H93B), O94(H94A,H94B), O118(H11A,H11B), O96(H96A,H96B), O108(H10A,
 H10B), O92(H92A,H92B), O102(H10C,H10D), O103(H10E,H10F), O119(H11C,H11D),
 O107(H107), O106(H10G,H10H), O110(H11E,H11F), O104(H10I,H10J), O89(H89A,H89B),
 O117(H11G,H11H), O105(H10K,H10L), O90(H90A,H90B), O125(H12A,H12B), O87(H87A,
 H87B), O88(H88A,H88B), O95(H95A,H95B), O97(H97A,H97B), O91(H91A,H91B),
 O100(H10M,H10N), O85(H85A,H85B), O133(H13E,H13F), O98(H98A,H98B), O121(H12C,
 H12D), O135(H13G,H13H), O123(H12E,H12F), O124(H12G,H12H), O101(H10O,H10P),
 O116(H11M,H11N), O86(H86A,H86B), O99(H99A,H99B), O134(H13I,H13J), O120(H12I,
 H12J), O114(H11O,H11P), O109(H10Q,H10R), O112(H11I,H11J), O122(H12K,H12L),
 O129(H12O,H12P), O115(H11Q,H11R), O132(H13K,H13L), O130(H13M,H13N), O126(H12Q,
 H12R), O127(H12M,H12N), O136(H13A,H13B), O139(H13C,H13D), O111(H11S,H11T),
 O113(H11K,H11L), O137(H13O,H13P), O141(H14A,H14B), O131(H13Q,H13R), O128(H12S,
 H12T), O138(H13S,H13T)
;
_shelx_res_checksum              71529
_olex2_submission_special_instructions 'No special instructions were received'