Synthesis and Characterization of a Novel Tetranuclear 5f Compound: A New Synthon for Exploring U(IV) Chemistry
Brian S. Newell; Trevor C. Schwaab; Matthew P. Shores; Inorganic Chemistry 50 (2011) 12108–12115; doi:10.1021/ic201670z

data_4327017
_publ_contact_author_address
;Department of Chemistry
Colorado State University
Fort Collins, CO 80521
;
_publ_contact_author_email       shores@lamar.colostate.edu
_publ_contact_author_fax         011(970)4911801
_publ_contact_author_name        'Matthew P. Shores'
_publ_contact_author_phone       011(970)4916033
_publ_section_title
;
 Synthesis and Characterization of a Novel Tetranuclear 5f Compound: A New
 Synthon for Exploring U(IV) Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12108
_journal_page_last               12115
_journal_paper_doi               10.1021/ic201670z
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C24 H64 Cl16 P8 U4, 2(C H2 Cl2)'
_chemical_formula_sum            'C26 H68 Cl20 P8 U4'
_chemical_formula_weight         2289.68
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.3334(7)
_cell_length_b                   37.3334(7)
_cell_length_c                   12.9469(3)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.52
_cell_volume                     18045.2(6)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2009)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            200336
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    7.908
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4240
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       rod
_exptl_crystal_F_000             8416
_exptl_crystal_size_max          0.715
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         2.501
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         11243
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1156P)^2^+300.9731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                8988
_reflns_number_total             11243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201670z_si_002_4.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4327017