Synthesis of terminal monochalcogenide and dichalcogenide complexes of uranium using polychalcogenides, [en](2-) (e = te, N = 2; e = se, N = 4), as chalcogen atom transfer reagents.
Smiles, Danil E.; Wu, Guang; Hayton, Trevor W.; Inorganic chemistry 53 (2014) 10240–10247; doi:10.1021/ic501267f

data_4341490
_publ_section_title
;
 Synthesis of terminal monochalcogenide and dichalcogenide complexes of
 uranium using polychalcogenides, [en](2-) (e = te, N = 2; e = se, N = 4),
 as chalcogen atom transfer reagents.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10240
_journal_page_last               10247
_journal_paper_doi               10.1021/ic501267f
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C32 H83 K N3 O6.5 Si6 Te2 U'
_chemical_formula_weight         1314.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                88.872(2)
_cell_angle_beta                 88.828(2)
_cell_angle_gamma                69.715(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1133(12)
_cell_length_b                   14.6606(17)
_cell_length_c                   17.909(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2736.1(5)
_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_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38729
_diffrn_reflns_theta_full        30.67
_diffrn_reflns_theta_max         30.67
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    4.256
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         16824
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0255P)^2^+1.3600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                14452
_reflns_number_total             16824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501267f_si_002.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32 H83 K N3 O6.50 Si6 Te2 U'
_cod_database_code               4341490