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_7129438
_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         'C36 H81 Ho2 Li O11 U'
_chemical_formula_sum            'C36 H81 Ho2 Li O11 U'
_chemical_formula_weight         1264.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-24 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                85.160(2)
_cell_angle_beta                 88.706(2)
_cell_angle_gamma                79.534(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5390(6)
_cell_length_b                   10.9635(6)
_cell_length_c                   21.2841(13)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.19
_cell_volume                     2409.7(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0840
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            122129
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.181
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.650
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1306 before and 0.0735 after correction.
The Ratio of minimum to maximum transmission is 0.4742.
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    1.743
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.351
_exptl_crystal_size_min          0.282
_refine_diff_density_max         1.591
_refine_diff_density_min         -3.356
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     476
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0323
_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^)+13.7030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9869
_reflns_number_total             11046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05444a2.cif
_cod_data_source_block           mo_dg122_full
_cod_database_code               7129438
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.256
_shelx_estimated_absorpt_t_min   0.153
_olex2_refinement_description
;
1. Fixed Uiso
 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 Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C)
;
_shelx_res_checksum              24445
_olex2_submission_special_instructions 'No special instructions were received'