Bonding in Uranium(V) Hexafluoride Based on the Experimental Electron Density Distribution Measured at 20 K.
Gianopoulos, Christopher G.; Zhurov, Vladimir V.; Minasian, Stefan G.; Batista, Enrique R.; Jelsch, Christian; Pinkerton, A. Alan; Inorganic chemistry 56 (2017) 1775–1778; doi:10.1021/acs.inorgchem.6b02971

data_4345174
_publ_contact_author
;
A. Alan Pinkerton
;
_publ_section_title
;
 Bonding in Uranium(V) Hexafluoride Based on the Experimental Electron
 Density Distribution Measured at 20 K.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1775
_journal_page_last               1778
_journal_paper_doi               10.1021/acs.inorgchem.6b02971
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C24 H20 F6 P U'
_chemical_formula_sum            'C24 H20 F6 P U'
_chemical_formula_weight         691.40
_chemical_name_common
'tetraphenyl phosphonium uranium hexafluoride'
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_type_scat_source           'Volkov et al, (2006)'
_audit_creation_method           'MoPro v15.10   rev. 1113 '
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.25180(10)
_cell_length_b                   12.25180(10)
_cell_length_c                   7.2893(2)
_cell_measurement_reflns_used    216113
_cell_measurement_temperature    20.0(1)
_cell_measurement_theta_max      70.888
_cell_measurement_theta_min      2.351
_cell_volume                     1094.17(3)
_computing_cell_refinement       'Otwinowski & Minor (1997)'
_computing_data_collection       CrystalClear,(2005)
_computing_data_reduction
;
Zhurova et al,(1999), Zhurov et al,(2008), Blessing, (1995,1997)
;
_computing_molecular_graphics    'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_computing_publication_material  'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_computing_structure_refinement  'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_computing_structure_solution    'Sheldrick (1997)'
_diffrn_ambient_temperature      20.0(1)
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Rigaku R-axis Rapid'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.00859
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            74795
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_max         67.51
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    7.551
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Zhurov, V. V.; Tanaka, K. General absorption correction for arbitrary shaped crystal with automatic
measurements of crystal shapes. Proc. of the 28th Japan Workshop of Frontiers of X-Ray Diffraction
Technologies in Russia/CIS, Nagoya, Japan, Dec.4 2003, P.169-178.
;
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       prism
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Rogers (1981),  4355 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.0082(8)
_refine_ls_abs_structure_Rogers  1.
_refine_ls_extinction_coef       0.07481
_refine_ls_extinction_expression
;
Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      2.554
_refine_ls_R_factor_all          0.0066
_refine_ls_R_factor_gt           0.0066
_refine_ls_shift/su_max          -0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'calc w =1/[\s^2^(Fo^2^)+(0.002P)^2^+0.002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0096
_refine_ls_wR_factor_ref         0.0096
_reflns_Friedel_fraction_max     0.902
_reflns_number_gt                9388
_reflns_number_total             9388
_reflns_threshold_expression
;
I>3\s, non-overlapped & non-partial reflections
;
_cod_data_source_file            ic6b02971_si_001.cif
_cod_data_source_block           PPh4UF6
_cod_depositor_comments          'Adding full bibliography for 4345174.cif.'
_cod_database_code               4345174
_shelx_hkl_checksum              20140