[(C5Me5)2U(Me)(OTf)]2: A New Reagent for Uranium Metallocene Chemistry. Preparation of the First Actinide Hydrazonato Complexes
Kiplinger, Jaqueline L.; John, Kevin D.; Morris, David E.; Scott, Brian L.; Burns, Carol J.; Organometallics 21 (2002) 4306–; doi:10.1021/om0205804

data_4077093
_publ_section_title
;
 [(C5Me5)2U(Me)(OTf)]2:&#x00A0; A New Reagent for Uranium Metallocene
 Chemistry. Preparation of the First Actinide Hydrazonato Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4306
_journal_paper_doi               10.1021/om0205804
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C48 H75.33 F6 O6 S2 U2'
_chemical_formula_weight         1402.60
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 105.133(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   27.1938(13)
_cell_length_b                   12.3954(6)
_cell_length_c                   24.2842(11)
_cell_measurement_temperature    203(2)
_cell_volume                     7901.8(6)
_computing_cell_refinement       'Bruker SAINT 4.05'
_computing_data_collection       'Bruker SMART 4.210"'
_computing_data_reduction        'Bruker SAINT 4.05'
_computing_molecular_graphics    'SHELXTL/NT 5.10'
_computing_publication_material  'SHELXTL/NT 5.10'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker P4/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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14258
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         0.78
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    6.285
_exptl_absorpt_correction_T_max  0.4329
_exptl_absorpt_correction_T_min  0.3139
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         14258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                10914
_reflns_number_total             14258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205804.cif
_cod_data_source_block           ccd387
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4077093