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_1568509
_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         'C72 H80 O6 U2, 2(C7 H8)'
_chemical_formula_sum            'C86 H96 O6 U2'
_chemical_formula_weight         1701.68
_chemical_properties_physical    Air-sensitive
_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             2021-07-15
_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                 101.1333(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9293(18)
_cell_length_b                   10.2778(10)
_cell_length_c                   19.647(2)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.30
_cell_volume                     3552.3(6)
_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)'
_diffrn_ambient_temperature      220.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0958
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.425
_diffrn_reflns_theta_min         1.408
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.608
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       rod
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5911
_reflns_number_total             8020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06375a3.cif
_cod_data_source_block           7
_cod_database_code               1568509
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.418
_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:
 C30(H30), C36(H36), C32(H32), C26(H26), C35(H35), C34(H34), C33(H33),
 C28(H28), C29(H29), C27(H27), C2S(H2S), C3S(H3S), C6S(H6S), C5S(H5S), C4S(H4S)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C7(H7A,H7B,
 H7C), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C9(H9A,H9B,
 H9C), C19(H19A,H19B,H19C), C8(H8A,H8B,H8C), C7S(H7SA,H7SB,H7SC)
;
_shelx_res_checksum              38657
_shelx_hkl_checksum              53836
_olex2_submission_special_instructions 'No special instructions were received'