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_7117746
_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 H43 B2 F2 N12 U1'
_chemical_formula_sum            'C30 H43 B2 F2 N12 U'
_chemical_formula_weight         869.41
_chemical_name_systematic        Tp*2UF2
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-06-15 deposited with the CCDC.
2015-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.165(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7840(6)
_cell_length_b                   22.3831(10)
_cell_length_c                   17.0603(7)
_cell_measurement_reflns_used    35248
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.641
_cell_measurement_theta_min      4.447
_cell_volume                     4493.0(4)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_unetI/netI     0.1356
_diffrn_reflns_laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35248
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.641
_diffrn_reflns_theta_min         4.447
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    10.495
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_T_min  0.030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1708
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.653
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1023P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                4733
_reflns_number_total             7912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05049a2.cif
_cod_data_source_block           CLC4
_cod_database_code               7117746
_shelx_estimated_absorpt_t_min   0.228
_shelx_estimated_absorpt_t_max   0.420
_shelxl_version_number           2014/6
_shelx_res_checksum              93344
_shelx_hkl_checksum              80379
_shelx_fab_checksum              56