Uranium-Mediated Thiourea/Urea Conversion on Chelating Ligands
Noufele, Christelle Njiki; Roca Jungfer, Maximilian; Hagenbach, Adelheid; Nguyen, Hung Huy; Abram, Ulrich; Inorganics 12 (2024) 295–; doi:10.3390/inorganics12110295

data_1573426
_publ_section_title
;
 Uranium-Mediated Thiourea/Urea Conversion on Chelating Ligands
;
_journal_issue                   11
_journal_name_full               Inorganics
_journal_page_first              295
_journal_paper_doi               10.3390/inorganics12110295
_journal_volume                  12
_journal_year                    2024
_chemical_formula_moiety         'C34 H47 N10 O14 S2 U3, C6 H16 N, H2 O'
_chemical_formula_sum            'C40 H65 N11 O15 S2 U3'
_chemical_formula_weight         1718.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.67(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.356(2)
_cell_length_b                   9.5250(10)
_cell_length_c                   34.782(2)
_cell_measurement_reflns_used    22715
_cell_measurement_temperature    203.15
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      4.63
_cell_volume                     11889(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      203.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS T2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            41286
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.500
_diffrn_reflns_theta_min         4.589
_exptl_absorpt_coefficient_mu    8.288
_exptl_absorpt_correction_T_max  0.7866
_exptl_absorpt_correction_T_min  0.4448
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Shape'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       needle
_exptl_crystal_F_000             6480
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9805
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6080
_reflns_number_total             9805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Uranium_SO.cif
_cod_data_source_block           trimer_o_hnet3_oh_ua
_cod_database_code               1573426
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C26) = Uanis(C27) = Uanis(C25) = Uanis(C18) = Uanis(C20) =
Uanis(C21) = Uanis(C19) = Uanis(C40) = Uanis(C41) = Uanis(C38) = Uanis(C39) =
Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(N15) = Uanis(N35)
3. Rigid body (RIGU) restrains
 C23, N14, C22, N15, C43, N34, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 N60(H60)
4.b Free rotating group:
 O50(H2,H50A,H50B)
4.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C20(H20A,H20B), C18(H18A,H18B), C46(H46A,
 H46B), C44(H44A,H44B), C38(H38A,H38B), C40(H40A,H40B), C61(H61A,H61B),
 C63(H63A,H63B), C65(H65A,H65B)
4.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C32(H32), C33(H33), C34(H34)
4.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C19(H19A,H19B,
 H19C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              95217
_shelx_hkl_checksum              74560
_olex2_submission_special_instructions 'No special instructions were received'