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_7129444
_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         'C90 H198 Ho6 O33 U3'
_chemical_formula_sum            'C90 H198 Ho6 O33 U3'
_chemical_formula_weight         3512.14
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-17 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7219(5)
_cell_length_b                   29.7219(5)
_cell_length_c                   29.7219(5)
_cell_measurement_reflns_used    9331
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.30
_cell_measurement_theta_min      2.37
_cell_volume                     26256.1(8)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_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  0.1000
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            134674
_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         25.347
_diffrn_reflns_theta_min         2.056
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.317
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1450 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.3962.
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    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             13440
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         8010
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0307
_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^)+175.3425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6821
_reflns_number_total             8010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05444a2.cif
_cod_data_source_block           mo_dg054_new2_0m_full
_cod_original_cell_volume        26256.1(13)
_cod_database_code               7129444
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.290
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C8(H8A,H8B,H8C), C26(H26A,
 H26B,H26C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C),
 C10(H10A,H10B,H10C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C3(H3A,H3B,H3C), C23(H23A,H23B,H23C),
  C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58142
_shelx_fab_checksum              54302
_olex2_submission_special_instructions 'No special instructions were received'