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_4311750
_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         'C42 H54 B2 N13 U, C7 H8'
_chemical_formula_sum            'C49 H62 B2 N13 U'
_chemical_formula_weight         1092.77
_chemical_name_systematic
;
bis(hydrotris(3,5-dimethylpyrazolyl)borato)(diphenylamido)
uranium(III)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.632(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.760(3)
_cell_length_b                   16.996(2)
_cell_length_c                   17.581(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.9
_cell_measurement_theta_min      7.0
_cell_volume                     4951.3(12)
_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-3 (Farrugia,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4496
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        18.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.326
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.9107
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                3307
_reflns_number_total             4338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049204xsi20040724_020648.cif
_cod_data_source_block           utpmenph
_cod_original_cell_volume        4951.1(13)
_cod_database_code               4311750