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_1570169
_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         'C33 H50 O2 U'
_chemical_formula_sum            'C33 H50 O2 U'
_chemical_formula_weight         716.76
_chemical_properties_physical    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             2022-10-13
_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                91.227(3)
_cell_angle_beta                 106.016(3)
_cell_angle_gamma                95.893(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0523(8)
_cell_length_b                   11.2703(9)
_cell_length_c                   14.4867(11)
_cell_measurement_reflns_used    9327
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      28.79
_cell_measurement_theta_min      2.22
_cell_volume                     1567.1(2)
_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      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Photon II CMOS area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46028
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.581
_diffrn_reflns_theta_min         2.215
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.204
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5973
_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    1.519
_exptl_crystal_description       fragment
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.953
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         8737
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+8.3634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7529
_reflns_number_total             8737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04857h5.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1570163--1570169.cif.'
_cod_database_code               1570169
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C30, C30', C31, C31'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C30(0.75) H30A(0.75) H30B(0.75) C30'(0.25) H30C(0.25) H30D(0.25)
 C31(0.75) H31A(0.75) H31B(0.75) C31'(0.25) H31C(0.25) H31D(0.25) H32C(0.25)
 H32D(0.25) H32A(0.75) H32B(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C30'(H30C,H30D), C31(H31A,H31B), C31'(H31C,H31D), C32(H32C,
 H32D), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25)
4.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), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              9714
_olex2_submission_special_instructions 'No special instructions were received'