[(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_4077095
_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            'C35 H43 F3 N2 O3 S U'
_chemical_formula_weight         866.80
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_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            2
_cell_length_a                   13.1069(10)
_cell_length_b                   11.9922(8)
_cell_length_c                   10.9540(8)
_cell_measurement_temperature    203(2)
_cell_volume                     1721.8(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8083
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    4.827
_exptl_absorpt_correction_T_max  0.5951
_exptl_absorpt_correction_T_min  0.2754
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.439
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3238
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.426
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                2802
_reflns_number_total             3238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205804.cif
_cod_data_source_block           ccd396b
_cod_original_sg_symbol_H-M      'P mn21'
_cod_database_code               4077095