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_7717551
_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         'C41 H63 Mo3 O S4 U'
_chemical_formula_sum            'C41 H63 Mo3 O S4 U'
_chemical_formula_weight         1226.00
_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             2024-09-24
_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                 99.7002(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.17593(8)
_cell_length_b                   19.26021(16)
_cell_length_c                   20.25129(16)
_cell_measurement_reflns_used    33658
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.6750
_cell_measurement_theta_min      3.1680
_cell_volume                     4296.78(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.118a (Rigaku OD, 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 0.997
_diffrn_measured_fraction_theta_max 0.976
_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    -82.00   3.00   0.50    1.18    --  -47.03 105.00 143.00  170
  2  \w     18.00  83.00   0.50    1.18    --   47.03-105.00  43.00  130
  3  \w    -81.00 -21.00   0.50    4.73    --  -91.75 105.00 143.00  120
  4  \w   -162.00 -83.00   0.50    4.73    --  -91.75-105.00  43.00  158
  5  \w    105.00 178.00   0.50    4.73    --  113.25 105.00 143.00  146
  6  \w     43.00 107.00   0.50    4.73    --  113.25-105.00  43.00  128
  7  \w   -119.00 -24.00   0.50    1.18    --  -47.03 -77.00  60.00  190
  8  \w    -14.00  28.00   0.50    1.18    --  -47.03  19.00  30.00   84
  9  \w    -14.00  28.00   0.50    1.18    --  -47.03  19.00 150.00   84
 10  \w    -14.00  28.00   0.50    1.18    --  -47.03  19.00-150.00   84
 11  \w     34.00  93.00   0.50    1.18    --   47.03-125.00 -60.00  118
 12  \w   -163.00 -83.00   0.50    4.73    --  -91.75 -94.00-180.00  160
 13  \w     91.00 178.00   0.50    4.73    --  113.25  77.00 120.00  174
 14  \w     42.00 106.00   0.50    4.73    --  113.25 -94.00 120.00  128
 15  \w     44.00 111.00   0.50    4.73    --  113.25-125.00 -30.00  134
 16  \w     42.00 106.00   0.50    4.73    --  113.25 -94.00  90.00  128
 17  \w    101.00 178.00   0.50    4.73    --  113.25  30.00-120.00  154
 18  \w    101.00 178.00   0.50    4.73    --  113.25  30.00-120.00  154
 19  \w     44.00 111.00   0.50    4.73    --  113.25-125.00 120.00  134
 20  \w     42.00  84.00   0.50    4.73    --  113.25 -61.00 120.00   84
 21  \w    101.00 178.00   0.50    4.73    --  113.25  30.00 -30.00  154
 22  \w     42.00  84.00   0.50    4.73    --  113.25 -61.00 150.00   84
 23  \w     42.00  84.00   0.50    4.73    --  113.25 -61.00-180.00   84
 24  \w     42.00 106.00   0.50    4.73    --  113.25 -94.00 -30.00  128
 25  \w     42.00  84.00   0.50    4.73    --  113.25 -61.00-120.00   84
 26  \w     91.00 178.00   0.50    4.73    --  113.25  77.00 120.00  174
 27  \w    101.00 178.00   0.50    4.73    --  113.25  30.00 -30.00  154
 28  \w     91.00 178.00   0.50    4.73    --  113.25  77.00  30.00  174
 29  \w     42.00  84.00   0.50    4.73    --  113.25 -61.00 -60.00   84
 30  \w     42.00 106.00   0.50    4.73    --  113.25 -94.00-120.00  128
 31  \w     42.00 106.00   0.50    4.73    --  113.25 -94.00  60.00  128
 32  \w     42.00  84.00   0.50    4.73    --  113.25 -61.00-150.00   84
 33  \w   -119.00 -24.00   0.50    1.18    --  -47.03 -77.00 150.00  190
 34  \w     24.00 119.00   0.50    1.18    --   47.03  77.00  90.00  190
 35  \w     32.00 119.00   0.50    1.18    --   47.03  57.00   0.00  174
 36  \w     32.00 119.00   0.50    1.18    --   47.03  57.00-120.00  174
 37  \w     24.00 119.00   0.50    1.18    --   47.03  77.00 -90.00  190
 38  \w     24.00 119.00   0.50    1.18    --   47.03  77.00-180.00  190
;
_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      -0.0047500000
_diffrn_orient_matrix_UB_12      0.0052174000
_diffrn_orient_matrix_UB_13      0.0754143000
_diffrn_orient_matrix_UB_21      0.0357715000
_diffrn_orient_matrix_UB_22      -0.0771217000
_diffrn_orient_matrix_UB_23      0.0088095000
_diffrn_orient_matrix_UB_31      0.1351460000
_diffrn_orient_matrix_UB_32      0.0205865000
_diffrn_orient_matrix_UB_33      0.0137784000
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62579
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.106
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41623
_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    1.895
_exptl_crystal_description       block
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.027
_refine_diff_density_max         3.004
_refine_diff_density_min         -3.149
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0419P)^2^+66.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8248
_reflns_number_total             9171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02803a2.cif
_cod_data_source_block           matkp27
_cod_depositor_comments
'Adding full bibliography for 7717551--7717554.cif.'
_cod_database_code               7717551
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.621
_shelx_estimated_absorpt_t_min   0.238
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.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), 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), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              31592
_shelx_hkl_checksum              63380
_olex2_submission_original_sample_id matkp27
_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 1.974
_oxdiff_exptl_absorpt_empirical_full_min 0.564