p<i>K</i><sub>a</sub> of alcohols dictates their reactivity with reduced uranium-substituted thiomolybdate clusters.
Patra, Kamaless; Brennessel, William W.; Matson, Ellen M.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 966–976; doi:10.1039/d4dt02803a

data_7717553
_publ_section_title
;
 p<i>K</i><sub>a</sub> of alcohols dictates their reactivity with reduced
 uranium-substituted thiomolybdate clusters.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              966
_journal_page_last               976
_journal_paper_doi               10.1039/d4dt02803a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C42 H72 Mo3 O3 S4 U'
_chemical_formula_sum            'C42 H72 Mo3 O3 S4 U'
_chemical_formula_weight         1279.08
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-27
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_audit_update_record
;
2024-10-04 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2794(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.97728(7)
_cell_length_b                   17.85746(11)
_cell_length_c                   24.61165(16)
_cell_measurement_reflns_used    46310
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.4510
_cell_measurement_theta_min      3.0080
_cell_volume                     4795.59(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00  27.00   0.50    0.33    --  -47.28  34.00-157.00  106
  2  \w   -121.00 -34.00   0.50    0.33    --  -47.28 -34.00  45.00  174
  3  \w     34.00 121.00   0.50    0.33    --   47.28  34.00-157.00  174
  4  \w    -26.00  52.00   0.50    0.33    --   47.28 -34.00  45.00  156
  5  \w   -165.00 -79.00   0.50    1.32    --  -91.75 -34.00  45.00  172
  6  \w    100.00 178.00   0.50    1.32    --  113.25  34.00-157.00  156
  7  \w    -14.00  28.00   0.50    0.33    --  -47.28  19.00   0.00   84
  8  \w    -14.00  28.00   0.50    0.33    --  -47.28  19.00 -30.00   84
  9  \w    -86.00 -13.00   0.50    0.33    --  -47.28 125.00 -30.00  146
 10  \w    -58.00 -19.00   0.50    1.32    --  -91.75  61.00  60.00   78
 11  \w    -58.00 -19.00   0.50    1.32    --  -91.75  61.00   0.00   78
 12  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00 -90.00   84
 13  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00 120.00   84
 14  \w     42.00 106.00   0.50    1.32    --  113.25 -94.00 150.00  128
 15  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00-120.00   84
 16  \w     42.00 106.00   0.50    1.32    --  113.25 -94.00 -90.00  128
 17  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00  90.00   84
 18  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00  60.00   84
 19  \w    100.00 178.00   0.50    1.32    --  113.25  15.00 -30.00  156
 20  \w     44.00 111.00   0.50    1.32    --  113.25-125.00 -60.00  134
 21  \w    101.00 178.00   0.50    1.32    --  113.25  30.00-120.00  154
 22  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00  30.00   84
 23  \w     44.00 111.00   0.50    1.32    --  113.25-125.00 -60.00  134
 24  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00 150.00   84
 25  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00-180.00   84
 26  \w     42.00 106.00   0.50    1.32    --  113.25 -94.00 120.00  128
 27  \w    101.00 178.00   0.50    1.32    --  113.25  30.00  90.00  154
 28  \w    101.00 178.00   0.50    1.32    --  113.25  30.00  90.00  154
 29  \w     42.00  84.00   0.50    1.32    --  113.25 -61.00 -60.00   84
 30  \w     42.00 106.00   0.50    1.32    --  113.25 -94.00-180.00  128
 31  \w     42.00 106.00   0.50    1.32    --  113.25 -94.00  30.00  128
 32  \w     25.00 119.00   0.50    0.33    --   47.28  77.00   0.00  188
 33  \w     25.00 119.00   0.50    0.33    --   47.28  77.00  90.00  188
 34  \w     25.00 119.00   0.50    0.33    --   47.28  77.00 -90.00  188
 35  \w     34.00  93.00   0.50    0.33    --   47.28-125.00-120.00  118
 36  \w     25.00 119.00   0.50    0.33    --   47.28  77.00 -30.00  188
 37  \w     25.00 119.00   0.50    0.33    --   47.28  77.00-150.00  188
 38  \w    101.00 178.00   0.50    1.32    --  113.25  30.00 150.00  154
 39  \w    101.00 139.00   0.50    1.32    --  113.25  30.00 -90.00   76
 40  \w    100.00 178.00   0.50    1.32    --  113.25  15.00  30.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1366723000
_diffrn_orient_matrix_UB_12      -0.0212383000
_diffrn_orient_matrix_UB_13      0.0037097000
_diffrn_orient_matrix_UB_21      0.0194900000
_diffrn_orient_matrix_UB_22      0.0315655000
_diffrn_orient_matrix_UB_23      0.0585381000
_diffrn_orient_matrix_UB_31      -0.0295073000
_diffrn_orient_matrix_UB_32      -0.0774498000
_diffrn_orient_matrix_UB_33      0.0228936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            80766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.182
_diffrn_reflns_theta_min         3.064
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.118a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         10319
_refine_ls_number_restraints     634
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+10.2427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9238
_reflns_number_total             10319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02803a2.cif
_cod_data_source_block           matkp25
_cod_depositor_comments
'Adding full bibliography for 7717551--7717554.cif.'
_cod_database_code               7717553
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
All non-hydrogen atoms have similar U: within 0.4A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 0.4A
Uanis(C5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C5, C4, C3, C2, C1} sigma for 1-2: 0.02, 1-3: 0.04
{C2, C3, C4, C5, C1} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C1, C2, C3, C4, C5}
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A}
{C7, C8, C9, C10, C6} sigma for 1-2: 0.02, 1-3: 0.04
{C10, C9, C8, C7, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C6, C7, C8, C9, C10}
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B}
5. Others
 1*[Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(C6)+Sof(H6A)+Sof(H6B)+Sof(H6C)+
 Sof(C7)+Sof(H7A)+Sof(H7B)+Sof(H7C)+Sof(C8)+Sof(H8A)+Sof(H8B)+Sof(H8C)+Sof(C9)+
 Sof(H9A)+Sof(H9B)+Sof(H9C)+Sof(C10)+Sof(H10A)+Sof(H10B)+Sof(H10C)]+1*[Sof(C1A)+
 Sof(C2A)+Sof(C3A)+Sof(C4A)+Sof(C5A)+Sof(C6A)+Sof(H6D)+Sof(H6E)+Sof(H6F)+
 Sof(C7A)+Sof(H7D)+Sof(H7E)+Sof(H7F)+Sof(C8A)+Sof(H8D)+Sof(H8E)+Sof(H8F)+
 Sof(C9A)+Sof(H9D)+Sof(H9E)+Sof(H9F)+Sof(C10A)+Sof(H10D)+Sof(H10E)+Sof(H10F)]+1*
 [Sof(C1B)+Sof(C2B)+Sof(C3B)+Sof(C4B)+Sof(C5B)+Sof(C6B)+Sof(H6G)+Sof(H6H)+
 Sof(H6I)+Sof(C7B)+Sof(H7G)+Sof(H7H)+Sof(H7I)+Sof(C8B)+Sof(H8G)+Sof(H8H)+
 Sof(H8I)+Sof(C9B)+Sof(H9G)+Sof(H9H)+Sof(H9I)+Sof(C10B)+Sof(H10G)+Sof(H10H)+
 Sof(H10I)]=1 with esd of 0.0001
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6D)=Sof(H6E)=
 Sof(H6F)=Sof(C7A)=Sof(H7D)=Sof(H7E)=Sof(H7F)=Sof(C8A)=Sof(H8D)=Sof(H8E)=
 Sof(H8F)=Sof(C9A)=Sof(H9D)=Sof(H9E)=Sof(H9F)=Sof(C10A)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=FVAR(2)
 Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6G)=Sof(H6H)=
 Sof(H6I)=Sof(C7B)=Sof(H7G)=Sof(H7H)=Sof(H7I)=Sof(C8B)=Sof(H8G)=Sof(H8H)=
 Sof(H8I)=Sof(C9B)=Sof(H9G)=Sof(H9H)=Sof(H9I)=Sof(C10B)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=FVAR(3)
6.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C6A(H6D,H6E,H6F), C7A(H7D,H7E,H7F), C8A(H8D,H8E,H8F), C9A(H9D,H9E,
 H9F), C10A(H10D,H10E,H10F), C6B(H6G,H6H,H6I), C7B(H7G,H7H,H7I), C8B(H8G,H8H,
 H8I), C9B(H9G,H9H,H9I), C10B(H10G,H10H,H10I), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              13529
_shelx_hkl_checksum              66109
_olex2_submission_original_sample_id matkp25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.741