New uranium(VI) and isothiouronium complexes: synthesis, crystal structure, spectroscopic characterization and a DFT study
Grabias, Ewelina; Tarasiuk, Bogdan; Dołęga, Anna; Majdan, Marek; CrystEngComm  (2020) –; doi:10.1039/D0CE00746C

data_7240928
_publ_section_title
;
 New uranium(VI) and isothiouronium complexes: synthesis, crystal
 structure, spectroscopic characterization and a DFT study
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00746C
_journal_year                    2020
_chemical_formula_moiety         'C12 H20 N4 S2, 2(C2 H3 O2)'
_chemical_formula_sum            'C16 H26 N4 O4 S2'
_chemical_formula_weight         402.53
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-06-18T11:42:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-06-29 deposited with the CCDC.	2020-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.793(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2940(2)
_cell_length_b                   13.8446(4)
_cell_length_c                   16.1184(4)
_cell_measurement_reflns_used    15768
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.93
_cell_volume                     2069.44(9)
_computing_cell_refinement
;
        X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
        X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
        X-Area Integrate 1.72.0.0 (STOE, 2018)
        X-Area X-Red32 1.63.4.0 (STOE, 2017)
;
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
        for outlier rejection, version 1.81, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14953
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9391
_exptl_absorpt_correction_T_min  0.8384
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
        Structure Analysis", published in
        F. R. Ahmed (Editor), "Crystallographic Computing",
        Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+1.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0
_reflns_number_gt                3488
_reflns_number_total             4057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00746c2.cif
_cod_data_source_block           ad_15
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7240928
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              73001