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_1568511
_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         'C61 H82 O5 U2, C5 H12'
_chemical_formula_sum            'C66 H94 O5 U2'
_chemical_formula_weight         1443.47
_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             2021-07-28
_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                 90.283(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5339(9)
_cell_length_b                   26.165(2)
_cell_length_c                   21.8935(18)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.28
_cell_volume                     6034.2(9)
_computing_cell_refinement       'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_data_collection       'Bruker Apex3 V.2016.9-0'
_computing_data_reduction        'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_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      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            87013
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.913
_diffrn_reflns_theta_min         1.557
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.408
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       prism
_exptl_crystal_F_000             2856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.369
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         12939
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0318P)^2^+26.3389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9246
_reflns_number_total             12939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06375a3.cif
_cod_data_source_block           5
_cod_database_code               1568511
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.253
_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. Restrained distances
 C4S-C5S = C4S-C3S = C2S-C3S
 1.54 with sigma of 0.02
 C4S'-C5S' = C4S'-C3S' = C4S-C5S = C4S-C3S = C2S-C3S = C1S-C2S
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: O3(0.75) O2(0.75) C32(0.75) C31(0.75) O2'(0.25) O3'(0.25)
 C7AA(0.25) C5S(0.6) C3S(0.6) C4S(0.6) H2SA(0.6) H2SB(0.6) H2SC(0.4) H2SD(0.4)
 C5S'(0.4) C3S'(0.4) C4S'(0.4) C1S(0.6) C1S'(0.4) C1AA(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C4S(H4SA,H4SB), C2S(H2SA,H2SB), C2S(H2SC,H2SD)
4.b Me refined with riding coordinates:
 C5S(H5SA,H5SB,H5SC), C1S(H1SA,H1SB,H1SC)
4.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C57(H57), C25(H25), C23(H23)
4.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C7(H7A,H7B,H7C), C16(H16A,H16B,
 H16C), C40(H40A,H40B,H40C), C60(H60A,H60B,H60C), C6(H6A,H6B,H6C), C8(H8A,H8B,
 H8C), C61(H61A,H61B,H61C), C39(H39A,H39B,H39C), C52(H52A,H52B,H52C), C59(H59A,
 H59B,H59C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C10(H10A,H10B,H10C),
 C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
  C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              50661
_shelx_hkl_checksum              52916
_olex2_submission_special_instructions 'No special instructions were received'