Cooperative dihydrogen activation with unsupported uranium-metal bonds and characterization of a terminal U(iv) hydride.
Ward, Robert J.; Rungthanaphatsophon, Pokpong; Huang, Patrick; Kelley, Steven P.; Walensky, Justin R.; Chemical science 14 (2023) 12255–12263; doi:10.1039/d3sc04857h

data_1570163
_publ_section_title
;
 Cooperative dihydrogen activation with unsupported uranium-metal bonds
 and characterization of a terminal U(iv) hydride.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              12255
_journal_page_last               12263
_journal_paper_doi               10.1039/d3sc04857h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '3(C39 H56 Al O U), C7 H8'
_chemical_formula_sum            'C124 H176 Al3 O3 U3'
_chemical_formula_weight         2509.67
_chemical_properties_physical    Air-sensitive,Heat-sensitive,Radioactive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-19 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.0880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7527(3)
_cell_length_b                   28.5642(6)
_cell_length_c                   17.9883(4)
_cell_measurement_reflns_used    9270
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      74.22
_cell_measurement_theta_min      5.46
_cell_volume                     5802.3(2)
_computing_cell_refinement       'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_computing_data_collection       'Bruker Apex3 V.2018.1-0'
_computing_data_reduction        'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            146525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.239
_diffrn_reflns_theta_min         2.988
_diffrn_source                   'Incoatec IMuS microfocus Cu tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.231
_exptl_absorpt_correction_T_max  0.0780
_exptl_absorpt_correction_T_min  0.0087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             2518
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexamethyldisiloxane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         4.650
_refine_diff_density_min         -4.355
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         12021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0951P)^2^+21.7070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11988
_reflns_number_total             12021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04857h5.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1570163--1570169.cif.'
_cod_database_code               1570163
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.230
_shelx_estimated_absorpt_t_min   0.084
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Others
 Fixed Sof: H64A(0.5) H64B(0.5) H64C(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5)
3.a Riding coordinates:
 C56(H56A,H56B), C57(H57A,H57), C58(H58A,H58B)
3.b Me refined with riding coordinates:
 C64(H64A,H64B,H64C), C5S(H5SA,H5SB,H5SC)
3.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C23(H23), C52(H52), C54(H54), C3S(H3S), C2S(H2S), C4S(H4S)
3.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C17(H17A,H17B,
 H17C), C27(H27A,H27B,H27C), C38(H38A,H38B,H38C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C46(H46A,H46B,H46C), C29(H29A,H29B,H29C), C45(H45A,H45B,H45C),
 C7(H7A,H7B,H7C), C49(H49A,H49B,H49C), C39(H39A,H39B,H39C), C10(H10A,H10B,H10C),
  C63(H63A,H63B,H63C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C8(H8A,H8B,H8C),
 C35(H35A,H35B,H35C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C47(H47A,H47B,
 H47C), C62(H62A,H62B,H62C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              75896
_olex2_submission_special_instructions 'No special instructions were received'