Systematic Studies of Early Actinide Complexes: Uranium(IV) Fluoroketimides
Schelter, Eric J.; Yang, Ping; Scott, Brian L.; Thompson, J. D.; Martin, Richard L.; Hay, P. Jeffrey; Morris, David E.; Kiplinger, Jaqueline L.; Inorganic Chemistry 46 (2007) 7477–7488; doi:10.1021/ic700455b

data_4333265
_publ_section_title
;
 Systematic Studies of Early Actinide Complexes:&#x00A0; Uranium(IV)
 Fluoroketimides
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7477
_journal_page_last               7488
_journal_paper_doi               10.1021/ic700455b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C36 H42 F4 N2 U'
_chemical_formula_weight         816.75
_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                108.7930(10)
_cell_angle_beta                 90.4760(10)
_cell_angle_gamma                102.7000(10)
_cell_formula_units_Z            4
_cell_length_a                   10.6877(6)
_cell_length_b                   17.5713(9)
_cell_length_c                   19.3511(10)
_cell_measurement_temperature    141(2)
_cell_volume                     3343.8(3)
_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      141(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.885
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32786
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.903
_exptl_absorpt_correction_T_max  0.6951
_exptl_absorpt_correction_T_min  0.3406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.163
_refine_diff_density_min         -1.852
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         15664
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                12729
_reflns_number_total             15664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700455bsup1.cif
_cod_data_source_block           apx053
_cod_database_code               4333265