Synthesis of low-valent uranium fluorides by C-F bond activation
Christopher L. Clark; Jill J. Lockhart; Phillip E. Fanwick; Suzanne C. Bart; Chem.Commun. 51 (2015) 14084–; doi:10.1039/C5cc05049A

data_7117745
_publ_section_title
;
 Synthesis of low-valent uranium fluorides by C-F bond activation
;
_journal_name_full               Chem.Commun.
_journal_page_first              14084
_journal_paper_doi               10.1039/C5cc05049A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C30 H37 B2 F1 N12 U1,C4 H8 O1'
_chemical_formula_sum            'C34 H45 B2 F N12 O U'
_chemical_formula_weight         916.47
_chemical_name_systematic        Tp*2UF
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-15 deposited with the CCDC.
2015-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                102.1530(10)
_cell_angle_beta                 98.0670(10)
_cell_angle_gamma                96.7400(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4532(3)
_cell_length_b                   11.0258(3)
_cell_length_c                   18.1147(7)
_cell_measurement_reflns_used    26856
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.864
_cell_measurement_theta_min      1.991
_cell_volume                     1997.41(11)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Burla, et. al., 2005)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26856
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.864
_diffrn_reflns_theta_min         1.991
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    4.110
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Pentane/Benzene'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.000
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                7259
_reflns_number_total             9438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05049a2.cif
_cod_data_source_block           CLC1
_cod_database_code               7117745
_shelx_estimated_absorpt_t_min   0.426
_shelx_estimated_absorpt_t_max   0.638
_shelxl_version_number           2013-4
_shelx_res_checksum              8367
_shelx_hkl_checksum              3242