Synthesis, Electrochemistry, and Reactivity of the Actinide Trisulfides [K(18-crown-6)][An(η(3)-S3)(NR2)3] (An = U, Th; R = SiMe3).
Smiles, Danil E.; Wu, Guang; Hayton, Trevor W.; Inorganic chemistry 55 (2016) 9150–9153; doi:10.1021/acs.inorgchem.6b01618

data_4348784
_publ_section_title
;
 Synthesis, Electrochemistry, and Reactivity of the Actinide Trisulfides
 [K(18-crown-6)][An(\h(3)-S3)(NR2)3] (An = U, Th; R = SiMe3).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9150
_journal_page_last               9153
_journal_paper_doi               10.1021/acs.inorgchem.6b01618
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C36 H88 F6 K N3 O13 S2 Si6 U'
_chemical_formula_weight         1394.88
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 105.370(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.095(3)
_cell_length_b                   23.499(4)
_cell_length_c                   19.344(4)
_cell_measurement_reflns_used    19633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.00
_cell_measurement_theta_min      12.62
_cell_volume                     6178(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40590
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         8.790
_refine_diff_density_min         -2.385
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       0.00029(3)
_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   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         13643
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0920
_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^)+(0.0101P)^2^+198.2388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                10335
_reflns_number_total             13643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01618_si_001.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4348784