Isolation of C1 through C4 derivatives from CO using heteroleptic uranium(iii) metallocene aryloxide complexes
Ward, Robert J.; Rosal, Iker del; Kelley, Steven P.; Maron, Laurent; Walensky, Justin R.; Chemical Science 14 (2023) 2024–2032; doi:10.1039/D2SC06375A

data_1568510
_publ_section_title
;
 Isolation of C1 through C4 derivatives from CO using heteroleptic
 uranium(iii) metallocene aryloxide complexes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2024
_journal_page_last               2032
_journal_paper_doi               10.1039/D2SC06375A
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C38 H52 O2 U'
_chemical_formula_sum            'C38 H52 O2 U'
_chemical_formula_weight         778.82
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-16 deposited with the CCDC.	2023-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.637(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.266(4)
_cell_length_b                   16.193(5)
_cell_length_c                   15.544(5)
_cell_measurement_reflns_used    9346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.28
_cell_volume                     3309.5(18)
_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      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66665
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         1.549
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.935
_exptl_absorpt_correction_T_max  0.4302
_exptl_absorpt_correction_T_min  0.2393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+12.7568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5563
_reflns_number_total             7042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06375a3.cif
_cod_data_source_block           8
_cod_database_code               1568510
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.243
_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.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C34(H34), C23(H23), C25(H25)
2.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C27(H27A,H27B,H27C), C9(H9A,H9B,
 H9C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C37(H37A,H37B,
 H37C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              54161
_shelx_hkl_checksum              55751
_olex2_submission_special_instructions 'No special instructions were received'