Heterobimetallic uranyl(vi) alkoxides of lanthanoids: formation through simple ligand exchange
Grödler, Dennis; Weidemann, Martin L.; Lichtenberg, Andreas; Greven, Tobias; Nickstadt, Robin; Haydo, Malek; Wickleder, Mathias; Klein, Axel; Johrendt, Dirk; Mathur, Sanjay; Zegke, Markus; Raauf, Aida; Chemical Communications  (2022) –; doi:10.1039/D1CC05444A

data_7129443
_publ_section_title
;
 Heterobimetallic uranyl(vi) alkoxides of lanthanoids: formation through
 simple ligand exchange
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05444A
_journal_year                    2022
_chemical_formula_moiety         'C60 H130 Dy4 O22 U2, 2(C6 H6)'
_chemical_formula_sum            'C72 H142 Dy4 O22 U2'
_chemical_formula_weight         2485.91
_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
_audit_creation_date             2021-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-11-17 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.612(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5252(13)
_cell_length_b                   17.6822(13)
_cell_length_c                   32.478(3)
_cell_measurement_reflns_used    300
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      0.7444
_cell_measurement_theta_min      0.4695
_cell_volume                     9356.9(13)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1387
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            189088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.027
_diffrn_reflns_theta_min         2.760
_exptl_absorpt_coefficient_mu    26.849
_exptl_absorpt_correction_T_max  0.1713
_exptl_absorpt_correction_T_min  0.0462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1452 before and 0.0970 after correction. The Ratio of minimum to maximum transmission is 0.2697. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             4792
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.555
_refine_diff_density_min         -1.918
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         18536
_refine_ls_number_restraints     892
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+208.6859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13412
_reflns_number_total             18536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05444a2.cif
_cod_data_source_block           db053_0m_a
_cod_database_code               7129443
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. 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
3.a Aromatic/amide H refined with riding coordinates:
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
 C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
3.b X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C43(H43A,H43B)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C)
;
_shelx_res_checksum              13525
_olex2_submission_special_instructions 'No special instructions were received'