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_7717554
_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         'C46 H63 Cl2 Mo3 O S4 U, 1.5(C7 H8)'
_chemical_formula_sum            'C56.5 H75 Cl2 Mo3 O S4 U'
_chemical_formula_weight         1495.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-08
_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                 97.3244(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.11244(9)
_cell_length_b                   20.41551(16)
_cell_length_c                   24.6678(2)
_cell_measurement_reflns_used    59473
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9930
_cell_measurement_theta_min      2.7800
_cell_volume                     5550.62(8)
_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    -63.00  25.00   0.50    0.47    --  -47.28  64.00 -37.00  176
  2  \w   -119.00 -30.00   0.50    0.47    --  -47.28 -64.00-174.00  178
  3  \w     30.00 119.00   0.50    0.47    --   47.28  64.00 -37.00  178
  4  \w    -24.00  65.00   0.50    0.47    --   47.28 -64.00-174.00  178
  5  \w   -163.00 -74.00   0.50    1.90    --  -91.75 -64.00-174.00  178
  6  \w    -63.00 -19.00   0.50    1.90    --  -91.75  64.00 -37.00   88
  7  \w     96.00 178.00   0.50    1.90    --  113.25  64.00 -37.00  164
  8  \w     42.00  89.00   0.50    1.90    --  113.25 -64.00-174.00   94
  9  \w    -86.00 -13.00   0.50    0.47    --  -47.28 125.00  60.00  146
 10  \w    -86.00 -13.00   0.50    0.47    --  -47.28 125.00  60.00  146
 11  \w    -58.00 -19.00   0.50    1.90    --  -91.75  61.00 150.00   78
 12  \w    -58.00 -19.00   0.50    1.90    --  -91.75  61.00  90.00   78
 13  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00 120.00   84
 14  \w     97.00 178.00   0.50    1.90    --  113.25  61.00  60.00  162
 15  \w     97.00 178.00   0.50    1.90    --  113.25  61.00-120.00  162
 16  \w     42.00 118.00   0.50    1.90    --  113.25 -77.00 120.00  152
 17  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00-120.00   84
 18  \w     42.00 118.00   0.50    1.90    --  113.25 -77.00 -60.00  152
 19  \w     42.00 118.00   0.50    1.90    --  113.25 -77.00 -60.00  152
 20  \w    101.00 178.00   0.50    1.90    --  113.25  30.00   0.00  154
 21  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00  60.00   84
 22  \w     95.00 178.00   0.50    1.90    --  113.25 125.00   0.00  166
 23  \w     42.00 106.00   0.50    1.90    --  113.25 -94.00 -60.00  128
 24  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00 -60.00   84
 25  \w     42.00 106.00   0.50    1.90    --  113.25 -94.00 120.00  128
 26  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00  30.00   84
 27  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00 150.00   84
 28  \w     42.00 118.00   0.50    1.90    --  113.25 -77.00 -30.00  152
 29  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00-150.00   84
 30  \w     42.00  84.00   0.50    1.90    --  113.25 -61.00 -30.00   84
 31  \w   -119.00 -32.00   0.50    0.47    --  -47.28 -57.00  90.00  174
 32  \w   -119.00 -25.00   0.50    0.47    --  -47.28 -77.00  30.00  188
 33  \w     25.00 119.00   0.50    0.47    --   47.28  77.00  30.00  188
 34  \w     32.00 119.00   0.50    0.47    --   47.28  57.00 150.00  174
 35  \w     32.00 119.00   0.50    0.47    --   47.28  57.00 -60.00  174
 36  \w     25.00 119.00   0.50    0.47    --   47.28  77.00-150.00  188
 37  \w    101.00 178.00   0.50    1.90    --  113.25  30.00-150.00  154
;
_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      -0.1333378000
_diffrn_orient_matrix_UB_12      0.0153808000
_diffrn_orient_matrix_UB_13      -0.0211751000
_diffrn_orient_matrix_UB_21      -0.0008655000
_diffrn_orient_matrix_UB_22      0.0538873000
_diffrn_orient_matrix_UB_23      0.0436145000
_diffrn_orient_matrix_UB_31      0.0414988000
_diffrn_orient_matrix_UB_32      0.0505089000
_diffrn_orient_matrix_UB_33      -0.0401269000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0271
_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       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            92991
_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         80.174
_diffrn_reflns_theta_min         2.819
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32215
_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    1.789
_exptl_crystal_description       needle
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.019
_refine_diff_density_max         4.102
_refine_diff_density_min         -2.074
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         11963
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+21.9364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11246
_reflns_number_total             11963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02803a2.cif
_cod_data_source_block           matkp26
_cod_depositor_comments
'Adding full bibliography for 7717551--7717554.cif.'
_cod_original_cell_volume        5550.63(8)
_cod_original_formula_sum        'C56.50 H75 Cl2 Mo3 O S4 U'
_cod_database_code               7717554
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.172
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C54, C56, C58, C60, C55, C57, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C54, C55, C60, C59, C58, C57, C56} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C54, C55, C56, C57, C58, C59, C60}
5. Others
 Fixed Sof: C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5) C56(0.5) H56(0.5)
 C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C45(H45), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
6.b 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), 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), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              74492
_shelx_hkl_checksum              3403
_olex2_submission_original_sample_id matkp26
_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 2.923
_oxdiff_exptl_absorpt_empirical_full_min 0.774