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_1573427
_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
'C36 H51 N10 O14 S2 U3, 0.5(C12 H30 N2), 1[H2O]'
_chemical_formula_sum            'C42 H68 N11 O15 S2 U3'
_chemical_formula_weight         1745.28
_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   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.754(5)
_cell_length_b                   19.292(4)
_cell_length_c                   13.997(3)
_cell_measurement_reflns_used    5470
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      2.4
_cell_volume                     6414(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX-II CCD'
_computing_data_reduction        'Bruker SAINT'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44176
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.500
_diffrn_reflns_theta_min         2.485
_exptl_absorpt_coefficient_mu    7.683
_exptl_absorpt_correction_T_max  0.7632
_exptl_absorpt_correction_T_min  0.2362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       needle
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.975
_refine_diff_density_min         -2.724
_refine_diff_density_rms         0.247
_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     257
_refine_ls_number_reflns         5467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0455P)^2^+271.9907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4242
_reflns_number_total             5467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Uranium_SO.cif
_cod_data_source_block           trimer_hnet3_o_etoh_ua
_cod_database_code               1573427
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C21) = Uanis(N13) = Uanis(C18) = Uanis(C19) = Uanis(C25) =
Uanis(C24) = Uanis(N15) = Uanis(C26) = Uanis(C27)
Uanis(O11) = Uanis(O12) = Uanis(O1) = Uanis(O13)
Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(N40) = Uanis(C41) =
Uanis(C42)
Uanis(O2) = Uanis(C31) = Uanis(C32)
3. Others
 Fixed Sof: H31A(0.5) H31B(0.5) H32A(0.5) H32B(0.5) H32C(0.5) H40(0.5)
 C41(0.5) H41A(0.5) H41B(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C42(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C45(0.5) H45A(0.5) H45B(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5)
4.a Ternary CH refined with riding coordinates:
 N40(H40), C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C24(H24A,H24B), C18(H18A,H18B), C21(H21A,H21B), C31(H31A,
 H31B), C41(H41A,H41B), C45(H45A,H45B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14)
4.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C32(H32A,H32B,H32C), C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 48 electrons were 
found in a volume of 1160\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per formula unit 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38660
_shelx_hkl_checksum              5113
_shelx_fab_checksum              26462
_olex2_submission_special_instructions 'No special instructions were received'