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_1570168
_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         'C31 H46 O U'
_chemical_formula_sum            'C31 H46 O U'
_chemical_formula_weight         672.71
_chemical_properties_physical    Air-sensitive,Heat-sensitive,Radioactive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-09
_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                108.404(4)
_cell_angle_beta                 95.865(4)
_cell_angle_gamma                90.279(4)
_cell_formula_units_Z            4
_cell_length_a                   8.9923(12)
_cell_length_b                   17.002(2)
_cell_length_c                   19.547(3)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.21
_cell_volume                     2818.6(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.1204
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.104
_diffrn_reflns_theta_min         1.924
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.779
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method 'From reaction mixture in pentane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.148
_refine_diff_density_min         -3.104
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0629
_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^)+67.1595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8251
_reflns_number_total             12370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04857h5.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 1570163--1570169.cif.'
_cod_original_cell_volume        2818.5(6)
_cod_database_code               1570168
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.520
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: U1(0.97) U1'(0.03) U2(0.97) U2'(0.03)
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C61(H61A,H61B)
3.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C54(H54), C56(H56)
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), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              80726
_olex2_submission_special_instructions 'No special instructions were received'