Emission spectroscopy of uranium(iv) compounds: a combined synthetic, spectroscopic and computational study
Hashem, Emtithal; Swinburne, Adam N.; Schulzke, Carola; Evans, Rachel C.; Platts, James A.; Kerridge, Andrew; Natrajan, Louise S.; Baker, Robert J.; RSC Advances 3 (2013) 4350–; doi:10.1039/c3ra22712j

data_7238898
_publ_section_title
;
 Emission spectroscopy of uranium(iv) compounds: a combined synthetic,
 spectroscopic and computational study
;
_journal_issue                   13
_journal_name_full               'RSC Advances'
_journal_page_first              4350
_journal_paper_doi               10.1039/c3ra22712j
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'Cl4 O2 U, 2(C5 H5 N), 2(C5H6 N)'
_chemical_formula_sum            'C20 H22 Cl4 N4 O2 U'
_chemical_formula_weight         730.25
_chemical_name_common
'bis pyridinium tetrachlorodioxouranate pyridine solvate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.85(3)
_cell_angle_beta                 91.90(3)
_cell_angle_gamma                115.10(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4466(17)
_cell_length_b                   9.1058(18)
_cell_length_c                   9.865(2)
_cell_measurement_reflns_used    2317
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      31.1529
_cell_measurement_theta_min      2.2839
_cell_volume                     621.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_details
;
scan:
Number of images: 300
Slice: -110.0000 - 40.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 0.0000
XTD: 44.7245
2theta: -19.7193
scan:
Number of images: 244
Slice: -55.0000 - 67.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 0.0000
XTD: 44.7245
2theta: -19.7193
scan:
Number of images: 170
Slice: -55.0000 - 30.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 90.0000
XTD: 44.7245
2theta: -19.7193
scan:
Number of images: 60
Slice: -50.0000 - -20.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 90.0000
XTD: 44.7245
2theta: -19.7193
;
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6237
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.36
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    6.988
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4796
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.432
_refine_diff_density_min         -4.142
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0117(16)
_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   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.8684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                3298
_reflns_number_total             3306
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ra22712j.txt
_cod_data_source_block           eh1011
_cod_original_cell_volume        621.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238898