Expanding the Chemistry of Actinide Metallocene Bromides. Synthesis, Properties and Molecular Structures of the Tetravalent and Trivalent Uranium Bromide Complexes: (C5Me4R)2UBr2, (C5Me4R)2U(O-2,6-iPr2C6H3)(Br), and [K(THF)][(C5Me4R)2UBr2] (R = Me, Et)
Lichtscheidl, Alejandro; Pagano, Justin; Scott, Brian; Nelson, Andrew; Kiplinger, Jaqueline; Inorganics 4 (2016) 1–; doi:10.3390/inorganics4010001

data_1542399
_publ_section_title
;
 Expanding the Chemistry of Actinide Metallocene Bromides. Synthesis,
 Properties and Molecular Structures of the Tetravalent and Trivalent
 Uranium Bromide Complexes: (C5Me4R)2UBr2, (C5Me4R)2U(O-2,6-iPr2C6H3)(Br),
 and [K(THF)][(C5Me4R)2UBr2] (R = Me, Et)
;
_journal_issue                   1
_journal_name_full               Inorganics
_journal_page_first              1
_journal_paper_doi               10.3390/inorganics4010001
_journal_volume                  4
_journal_year                    2016
_chemical_formula_sum            'C20 H30 Br2 U'
_chemical_formula_weight         668.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           42
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2'
_symmetry_space_group_name_H-M   'F m m 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9546(12)
_cell_length_b                   17.323(2)
_cell_length_c                   8.1940(7)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      34.99
_cell_measurement_theta_min      2.35
_cell_volume                     2122.7(3)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker D8 with CMOS detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12057
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.35
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.410
_exptl_absorpt_correction_T_max  0.5476
_exptl_absorpt_correction_T_min  0.2087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.310
_refine_diff_density_min         -2.841
_refine_diff_density_rms         0.677
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.051(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         2388
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                2385
_reflns_number_total             2388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            dq0052a.cif
_cod_data_source_block           dq0052a
_cod_original_cell_volume        2122.7(4)
_cod_original_sg_symbol_H-M      'F mm2'
_cod_database_code               1542399