Unique Uranium(III) Cations Anchored by Polydentate Sulfur-Based Ligands: Synthesis and Structure of [U{H(R)B(timMe)2}2(THF)3][BPh4] (R = H, Ph)
Leonor Maria; Ângela Domingos; Isabel Santos; Inorganic Chemistry 40 (2001) 6863–6864; doi:10.1021/ic0106827

data_4320780
_publ_section_title
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 Unique Uranium(III) Cations Anchored by Polydentate Sulfur-Based Ligands:
 Synthesis and Structure of [U{H(R)B(timMe)2}2(THF)3][BPh4] (R = H, Ph)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6863
_journal_page_last               6864
_journal_paper_doi               10.1021/ic0106827
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     '[U{H(u-H)B(MeC3H2N2S)2}2(THF)3][BPh4].OC4H8'
_chemical_formula_sum            'C56 H76 B3 N8 O4 S4 U'
_chemical_formula_weight         1323.95
_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
_cell_angle_alpha                113.09(3)
_cell_angle_beta                 106.39(3)
_cell_angle_gamma                97.91(2)
_cell_formula_units_Z            2
_cell_length_a                   12.818(4)
_cell_length_b                   16.290(3)
_cell_length_c                   18.355(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.1
_cell_measurement_theta_min      7.7
_cell_volume                     3246(2)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MOLEN(Fair,1990)
_computing_molecular_graphics    ORTEP(Johnson,1976)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4-Enraf-Nonius
_diffrn_measurement_method       \w/2\qscans
_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  0.0789
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9727
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        13.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.676
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.8086
_exptl_absorpt_correction_type   'empirical via\y-scan North et al(1968)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.221
_refine_diff_density_min         -3.609
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.101
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         7951
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.330
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_obs          0.1092
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1668P)^2^+2.4067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3690
_refine_ls_wR_factor_obs         0.2489
_reflns_number_observed          5431
_reflns_number_total             9297
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0106827_2.cif
_cod_data_source_block           uh2btim
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1668P)^2^+2.4067P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1668P)^2^+2.4067P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3245.7(21)
_cod_database_code               4320780