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_7129441
_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         'C40 H92 Cl Ho3 O13 U'
_chemical_formula_sum            'C40 H92 Cl Ho3 O13 U'
_chemical_formula_weight         1549.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1829(11)
_cell_length_b                   21.6096(13)
_cell_length_c                   17.8158(15)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.485
_cell_measurement_theta_min      2.287
_cell_volume                     5460.3(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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  0.1623
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            256608
_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         25.362
_diffrn_reflns_theta_min         2.063
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.356
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1591 before and 0.0959 after correction. The Ratio of minimum to maximum transmission is 0.5885. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_description       needles
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5141
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0501P)^2^+40.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4128
_reflns_number_total             5141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05444a2.cif
_cod_data_source_block           mo_dg107_pnmaa
_cod_database_code               7129441
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.262
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(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. Others
 Fixed Sof: H9a(0.5) H9b(0.5) H21a(0.5) H21b(0.5) H21c(0.5) C8(0.5) H8a(0.5)
 H8b(0.5) H8c(0.5) C10(0.5) H10a(0.5) H10b(0.5) H10c(0.5) C11(0.5) H11a(0.5)
 H11b(0.5) H11c(0.5) C6(0.5) H6a(0.5) H6b(0.5) H6c(0.5) C9(0.5) H9c(0.5)
 H9d(0.5) H9e(0.5) C7(0.5) H7a(0.5) H7b(0.5) H7c(0.5) H24a(0.5) H24b(0.5)
 H24c(0.5) C25(0.5) H25a(0.5) H25b(0.5) H25c(0.5) C26(0.5) H26a(0.5) H26b(0.5)
 H26c(0.5)
4.a Rotating group:
 O9(H9a,H9b)
4.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C18(H18a,H18b,H18c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C19(H19a,H19b,H19c), C15(H15a,H15b,H15c), C3(H3a,H3b,H3c), C4(H4a,H4b,
 H4c), C14(H14a,H14b,H14c), C17(H17a,H17b,H17c), C2(H2a,H2b,H2c), C8(H8a,H8b,
 H8c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C6(H6a,H6b,H6c), C9(H9c,H9d,
 H9e), C7(H7a,H7b,H7c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C26(H26a,H26b,
 H26c)
;
_olex2_submission_special_instructions 'No special instructions were received'