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_7129435
_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         'C58 H120 Ho4 O24 U2'
_chemical_formula_sum            'C58 H120 Ho4 O24 U2'
_chemical_formula_weight         2337.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2021-09-14
_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                 124.648(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.351(2)
_cell_length_b                   17.629(2)
_cell_length_c                   16.5056(19)
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.709
_cell_measurement_theta_min      2.559
_cell_volume                     4632.2(9)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.995
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            124112
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.311
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.914
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1595 before and 0.0856 after correction. The Ratio of minimum to maximum transmission is 0.6399. 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    1.676
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.148
_refine_diff_density_max         2.195
_refine_diff_density_min         -2.609
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5680
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+255.9823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5107
_reflns_number_total             5680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05444a2.cif
_cod_data_source_block           dg054plate_tw_monoc
_cod_original_cell_volume        4632.1(9)
_cod_database_code               7129435
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.428
_shelx_estimated_absorpt_t_min   0.299
_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 0.005 and sigma for terminal atoms of 0.01
Uanis(C19A) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C12) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(O8)=1-FVAR(1)
 Sof(O8A)=FVAR(1)
 Fixed Sof: Ho2(0.5) Ho1(0.5) O4(0.5) O6(0.5) O3(0.5) O5(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C13(0.5) C14(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) C20(0.66667) H20A(0.66667) H20B(0.66667) H20C(0.66667)
 C17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C5(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) H6C(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C19(0.5) C21(0.66667) H21A(0.66667) H21B(0.66667) H21C(0.66667)
 C22(0.66667) H22A(0.66667) H22B(0.66667) H22C(0.66667) C2(0.5) H2A(0.5)
 H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) C9(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C17A(0.5) C18A(0.5)
 H18D(0.5) H18E(0.5) H18F(0.5) C19A(0.5) C20A(0.33333) H20D(0.33333)
 H20E(0.33333) H20F(0.33333) C21A(0.33333) H21D(0.33333) H21E(0.33333)
 H21F(0.33333) C22A(0.33333) H22D(0.33333) H22E(0.33333) H22F(0.33333)
4.a Me refined with riding coordinates:
 C16(H16A,H16B,H16C)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C7(H7A,H7B,
 H7C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C2(H2A,H2B,
 H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C18A(H18D,H18E,
 H18F), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              27285
_olex2_submission_special_instructions 'No special instructions were received'