Uranium (III) Scorpionates: Synthesis and Structure of [(TpMe2)2U{N(C6H5)2}] and [(TpMe2)2U{N(SiMe3)2}]
Maria Augusta Antunes; Gregory M. Ferrence; Ângela Domingos; Robert McDonald; Carol J. Burns; Josef Takats; Noémia Marques; Inorganic Chemistry 43 (2004) 6640–6643; doi:10.1021/ic049204x

data_4311751
_publ_contact_author             'Ferrence, Gregory M.'
_publ_contact_author_email       ferrence@ilstu.edu
_publ_section_title
;
 Uranium (III) Scorpionates: Synthesis and Structure of
 [(TpMe2)2U{N(C6H5)2}] and [(TpMe2)2U{N(SiMe3)2}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6640
_journal_page_last               6643
_journal_paper_doi               10.1021/ic049204x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C36 H62 B2 N13 Si2 U, 2.5(C4 H8 O)'
_chemical_formula_sum            'C46 H82 B2 N13 O2.5 Si2 U'
_chemical_formula_weight         1173.08
_chemical_name_systematic
;
bis(hydrotris(3,5-dimethylpyrazolyl)borato)(bis(trimethylsilyl)amido)
uranium(III)
;
_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                82.681(4)
_cell_angle_beta                 79.948(4)
_cell_angle_gamma                71.766(4)
_cell_formula_units_Z            2
_cell_length_a                   10.779(2)
_cell_length_b                   16.163(3)
_cell_length_c                   16.736(3)
_cell_measurement_reflns_used    4023
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.10
_cell_measurement_theta_min      2.21
_cell_volume                     2718.6(9)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Bruker P4/RA diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\f and\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13687
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.079
_exptl_absorpt_correction_T_max  0.7089
_exptl_absorpt_correction_T_min  0.5016
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.328
_refine_diff_density_min         -1.891
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11084
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0526P)^2^+4.7998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                8612
_reflns_number_total             11084
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic049204xsi20040724_020717.cif
_cod_data_source_block           tak9918
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2718.5(9)
_cod_database_code               4311751