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_1568513
_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         'C62 H82 O7 U2, 1.5(C5 H12)'
_chemical_formula_sum            'C69.5 H90 O7 U2'
_chemical_formula_weight         1513.47
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-15
_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                 100.911(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.0997(15)
_cell_length_b                   14.4756(6)
_cell_length_c                   20.4007(7)
_cell_measurement_reflns_used    9141
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.87
_cell_measurement_theta_min      3.80
_cell_volume                     12497.8(8)
_computing_cell_refinement       'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_computing_data_collection       'Bruker Apex3 V.2018.1-0'
_computing_data_reduction        'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_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      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            134606
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.587
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'Incoatec IMuS microfocus Cu tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.878
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4050
_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    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             5976
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.477
_refine_diff_density_min         -7.130
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         12727
_refine_ls_number_restraints     1041
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.1225
_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^)+(0.0001P)^2^+2003.6687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2819
_refine_ls_wR_factor_ref         0.2921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10034
_reflns_number_total             12727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06375a3.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C69.50 H90 O7 U2'
_cod_database_code               1568513
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.146
_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. Restrained distances
 C40'-C44' \\sim C40-C44 \\sim C43'-C44' \\sim C42'-C43' \\sim C43-C44 \\sim
C42'-C41' \\sim C43-C42 ~
 C42-C41 \\sim C40'-C41' \\sim C40-C41
 with sigma of 0.02
 C47'-C42' \\sim C46'-C41' \\sim C40'-C45' \\sim C49'-C44' \\sim C43'-C48'
\\sim C43-C48 \\sim C42-C47
 \\sim C46-C41 \\sim C49-C44 \\sim C45-C40 \\sim C49'-C44'
 with sigma of 0.02
 C46-C47 \\sim C48-C49 \\sim C46'-C47' \\sim C48'-C49' \\sim C49'-C45' \\sim
C48'-C47'
 with sigma of 0.02
 C21-C22 \\sim C26-C21 \\sim C51-C50 \\sim C55-C50
 with sigma of 0.02
 C23-C22 \\sim C26-C25 \\sim C51-C52 \\sim C55-C54
 with sigma of 0.02
 C52-C53 \\sim C53-C54 \\sim C25-C24 \\sim C23-C24
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C41(0.6) C42(0.6) C43(0.6) C44(0.6) C40(0.6) C46(0.6) H46A(0.6)
 H46B(0.6) H46C(0.6) C47(0.6) H47A(0.6) H47B(0.6) H47C(0.6) C48(0.6) H48A(0.6)
 H48B(0.6) H48C(0.6) C48'(0.4) H48D(0.4) H48E(0.4) H48F(0.4) C44'(0.4)
 C43'(0.4) C41'(0.4) C40'(0.4) C42'(0.4) C49(0.6) H49A(0.6) H49B(0.6) H49C(0.6)
 C49'(0.4) H49D(0.4) H49E(0.4) H49F(0.4) C47'(0.4) H47D(0.4) H47E(0.4)
 H47F(0.4) C45'(0.4) H45A(0.4) H45B(0.4) H45C(0.4) C46'(0.4) H46D(0.4)
 H46E(0.4) H46F(0.4) C45(0.6) H45D(0.6) H45E(0.6) H45F(0.6)
5.a Free rotating group:
 C41(C42,C43,C44,C40,C46,C47,C48), C33(C31,C30,C34,C36,C35,C39), C3(C4,C5,C1,
 C2,C8,C9,C10,C6,C7)
5.b Me refined with riding coordinates:
 C48'(H48D,H48E,H48F), C49'(H49D,H49E,H49F), C47'(H47D,H47E,H47F), C45'(H45A,
 H45B,H45C), C46'(H46D,H46E,H46F)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C54(H54), C52(H52)
5.d Idealised Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C36(H36A,
 H36B,H36C), C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C49(H49A,H49B,H49C), C45(H45D,H45E,H45F),
 C58(H58A,H58B,H58C)
5.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C39(H39A,H39B,
 H39C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              54632
_shelx_hkl_checksum              51840
_shelx_fab_checksum              62891
_olex2_submission_special_instructions 'No special instructions were received'