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_4320779
_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{(u-H)PhB(MeC3H2N2S)2}2(THF)3][BPh4]'
_chemical_formula_sum            'C64 H76 B3 N8 O3 S4 U'
_chemical_formula_weight         1404.03
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
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_cell_angle_beta                 100.09(1)
_cell_angle_gamma                90.00
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_cell_length_a                   15.792(2)
_cell_length_b                   18.071(3)
_cell_length_c                   22.989(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.8
_cell_measurement_theta_min      7.6
_cell_volume                     6459.1(18)
_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\qscan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_standards_decay_%        33.2
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_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.8058
_exptl_absorpt_correction_type   'empirical via\y-scan North et al(1968)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
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_refine_ls_R_factor_all          0.1847
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+53.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1938
_refine_ls_wR_factor_obs         0.1050
_reflns_number_observed          7241
_reflns_number_total             14068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0106827_1.cif
_cod_data_source_block           uphtim
_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^)+(0.0000P)^2^+53.0759P] 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^)+(0.0000P)^2^+53.0759P] 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        6459.0(18)
_cod_database_code               4320779