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_1570165
_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         'C30 H44 O U'
_chemical_formula_sum            'C30 H44 O U'
_chemical_formula_weight         658.68
_chemical_properties_physical    Air-sensitive,Heat-sensitive,Radioactive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-25
_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                 111.688(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7245(7)
_cell_length_b                   33.797(3)
_cell_length_c                   10.1074(8)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      30.23
_cell_measurement_theta_min      2.25
_cell_volume                     2769.3(4)
_computing_cell_refinement       'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_data_collection       'Bruker Apex4 V.2022.1-1'
_computing_data_reduction        'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon II CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            73191
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.879
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4614
_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    1.580
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.048
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+4.1992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6422
_reflns_number_total             7364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04857h5.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 1570163--1570169.cif.'
_cod_database_code               1570165
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.372
_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. Others
 Fixed Sof: C11(0.6) C11'(0.4) C12(0.6) C12'(0.4) C13(0.6) C13'(0.4) C14(0.6)
 C14'(0.4) C15(0.6) C15'(0.4) C16(0.6) H16A(0.6) H16B(0.6) H16C(0.6) C16'(0.4)
 H16D(0.4) H16E(0.4) H16F(0.4) C17(0.6) H17A(0.6) H17B(0.6) H17C(0.6) C17'(0.4)
 H17D(0.4) H17E(0.4) H17F(0.4) C18(0.6) H18A(0.6) H18B(0.6) H18C(0.6) C18'(0.4)
 H18D(0.4) H18E(0.4) H18F(0.4) C19(0.6) H19A(0.6) H19B(0.6) H19C(0.6) C19'(0.4)
 H19D(0.4) H19E(0.4) H19F(0.4) C20(0.6) H20A(0.6) H20B(0.6) H20C(0.6) C20'(0.4)
 H20D(0.4) H20E(0.4) H20F(0.4)
3.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25)
3.b Idealised Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C16'(H16D,H16E,H16F), C17(H17A,H17B,H17C), C17'(H17D,
 H17E,H17F), C18(H18A,H18B,H18C), C18'(H18D,H18E,H18F), C19(H19A,H19B,H19C),
 C19'(H19D,H19E,H19F), C20(H20A,H20B,H20C), C20'(H20D,H20E,H20F)
3.c 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), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              64687
_olex2_submission_special_instructions 'No special instructions were received'