Thiocyanate complexes of uranium in multiple oxidation States: a combined structural, magnetic, spectroscopic, spectroelectrochemical, and theoretical study.
Hashem, Emtithal; Platts, James A.; Hartl, František; Lorusso, Giulia; Evangelisti, Marco; Schulzke, Carola; Baker, Robert J.; Inorganic chemistry 53 (2014) 8624–8637; doi:10.1021/ic501236j

data_4340567
_publ_section_title
;
 Thiocyanate complexes of uranium in multiple oxidation States: a combined
 structural, magnetic, spectroscopic, spectroelectrochemical, and
 theoretical study.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8624
_journal_page_last               8637
_journal_paper_doi               10.1021/ic501236j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C76 H150 N14 S8 U'
_chemical_formula_weight         1754.61
_chemical_name_systematic
;
 tetrabutylammonium octakis(thiocyanato-N)uranate(IV)
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.3721(9)
_cell_length_b                   17.9946(6)
_cell_length_c                   19.9695(7)
_cell_measurement_reflns_used    37016
_cell_measurement_temperature    175(2)
_cell_volume                     9476.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.975
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35881
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         66.96
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    6.800
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker 2012/1)'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.399
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         14001
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.1875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                12953
_reflns_number_total             14001
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501236j_si_002.cif
_cod_data_source_block           cu_ehabu4n_0ma
_cod_depositor_comments
'Adding full bibliography for 4340567--4340568.cif.'
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4340567