A novel coordination geometry for the uranyl ion. Rhombohedral uranium environment in [UO2(OTf)2(bpy)2] and [UO2(phen)3][OTf]2
Jean-Claude Berthet; Michel Ephritikhine; Martine Nierlich; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b303255h

data_7103743
_publ_section_title
;
A novel coordination geometry for the uranyl ion. 
Rhombohedral uranium environment in [UO2(OTf)2(bpy)2] and [UO2(phen)3][OTf]2
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_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b303255h
_journal_year                    2003
_chemical_formula_sum            'C22 H16 F6 N4 O8 S2 U'
_chemical_formula_weight         880.54
_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                102.13(3)
_cell_angle_beta                 92.66(3)
_cell_angle_gamma                102.87(3)
_cell_formula_units_Z            1
_cell_length_a                   6.0290(12)
_cell_length_b                   10.031(2)
_cell_length_c                   11.462(2)
_cell_measurement_reflns_used    4085
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     657.5(2)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 2\%steps'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4085
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         3.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.429
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'MULABS in PLATON;Spek,1998'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.432
_refine_diff_density_min         -2.503
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                2015
_reflns_number_total             2016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303255h.txt
_cod_data_source_block           2jc
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7103743