Fingerprinting the oxidation state of U(iv) by emission spectroscopy.
Hashem, Emtithal; Lorusso, Giulia; Evangelisti, Marco; McCabe, Thomas; Schulzke, Carola; Platts, James A.; Baker, Robert J.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14677–14680; doi:10.1039/c3dt52151f

data_7021987
_publ_section_title
;
 Fingerprinting the oxidation state of U(iv) by emission spectroscopy.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14677
_journal_page_last               14680
_journal_paper_doi               10.1039/c3dt52151f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C33 H36 N10 S5 U'
_chemical_formula_weight         971.05
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.810(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2687(6)
_cell_length_b                   18.5947(9)
_cell_length_c                   15.3116(7)
_cell_measurement_temperature    100(2)
_cell_volume                     3945.1(3)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_molecular_graphics    'Bruker Apex2'
_computing_publication_material  'Bruker Apex2 and Mercury'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20737
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         66.942
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.354
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.3656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'bruker Apex2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.267
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.266
_refine_ls_extinction_coef       0.00060(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0658P)^2^+5.7258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6507
_reflns_number_total             6619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52151f.txt
_cod_data_source_block           shelx
_cod_database_code               7021987
_shelxl_version_number           2013-3