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_1573428
_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         'C35 H49 N10 O14 S2 U3, C20 H20 P'
_chemical_formula_sum            'C55 H69 N10 O14 P S2 U3'
_chemical_formula_weight         1903.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 103.020(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7520(10)
_cell_length_b                   18.3410(10)
_cell_length_c                   28.125(2)
_cell_measurement_reflns_used    25756
_cell_measurement_temperature    203.15
_cell_measurement_theta_max      28.97
_cell_measurement_theta_min      4.60
_cell_volume                     6408.9(8)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0741
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46613
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         4.599
_exptl_absorpt_coefficient_mu    7.721
_exptl_absorpt_correction_T_max  0.8485
_exptl_absorpt_correction_T_min  0.3154
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       needle
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         10577
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0257P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7167
_reflns_number_total             10577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Uranium_SO.cif
_cod_data_source_block           trimer_etpph3_o_meoh_ua
_cod_database_code               1573428
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N35, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N15, C26, C27, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C46(H46A,H46B), C38(H38A,H38B), C40(H40A,H40B), C24(H24A,
 H24B), C18(H18A,H18B), C20(H20A,H20B), C81(H81A,H81B), C26(H26A,H26B)
3.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C27(H27A,H27B,H27C)
3.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C12(H12), C13(H13), C14(H14), C76(H76),
 C75(H75), C74(H74), C73(H73), C72(H72), C56(H56), C55(H55), C54(H54), C53(H53),
  C52(H52), C66(H66), C65(H65), C64(H64), C63(H63), C62(H62)
3.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C25(H25A,H25B,H25C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C82(H82A,
 H82B,H82C)
;
_shelx_res_checksum              87385
_shelx_hkl_checksum              44231
_olex2_submission_special_instructions 'No special instructions were received'