Tetrahalide Complexes of the [U(NR)2]2+ Ion: Synthesis, Theory, and Chlorine K-Edge X-ray Absorption Spectroscopy
Liam P. Spencer; Ping Yang; Stefan G. Minasian; Robert E. Jilek; Enrique R. Batista; Kevin S. Boland; James M. Boncella; Steven D. Conradson; David L. Clark; Trevor W. Hayton; Stosh A. Kozimor; Richard L. Martin; Molly M. MacInnes; Angela C. Olson; Brian L. Scott; David K. Shuh; Marianne P. Wilkerson; Journal of the American Chemical Society 135 (2013) 2279–2290; doi:10.1021/ja310575j

data_4119318
_publ_section_title
;
 Tetrahalide Complexes of the [U(NR)2]2+ Ion: Synthesis, Theory, and
 Chlorine K-Edge X-ray Absorption Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2279
_journal_page_last               2290
_journal_paper_doi               10.1021/ja310575j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C60 H66 Cl12 N2 O0 P2 U'
_chemical_formula_weight         1540.52
_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-97
_cell_angle_alpha                89.350(4)
_cell_angle_beta                 78.614(4)
_cell_angle_gamma                89.676(4)
_cell_formula_units_Z            2
_cell_length_a                   12.202(4)
_cell_length_b                   14.586(5)
_cell_length_c                   18.386(6)
_cell_measurement_temperature    120(1)
_cell_volume                     3207.7(18)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0984
_diffrn_reflns_av_sigmaI/netI    0.1349
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29745
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.119
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       orange
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.885
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0877P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                6608
_reflns_number_total             11049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310575j_si_002_1.cif
_cod_data_source_block           apx570
_cod_original_cell_volume        3207.8(17)
_cod_database_code               4119318