Reductive Silylation of the Uranyl Ion with Ph3SiOTf
Pedrick, Elizabeth A.; Wu, Guang; Hayton, Trevor W.; Inorganic Chemistry  (2014) 141111154001001–; doi:10.1021/ic502267t

data_4341675
_publ_section_title
;
 Reductive Silylation of the Uranyl Ion with Ph3SiOTf
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              141111154001001
_journal_paper_doi               10.1021/ic502267t
_journal_year                    2014
_chemical_formula_sum            'C99 H102 F3 N2 O8 S Si2 U'
_chemical_formula_weight         1831.10
_chemical_name_systematic
; 
 ? 
;
_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                63.9150(10)
_cell_angle_beta                 73.8000(10)
_cell_angle_gamma                69.2320(10)
_cell_formula_units_Z            1
_cell_length_a                   13.2871(2)
_cell_length_b                   14.1711(3)
_cell_length_c                   15.2003(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2377.60(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker kappa apex'
_diffrn_measurement_method       'omega scan'
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18712
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_correction_T_min  0.7726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             937
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.665
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         10088
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0566P)^2^+2.4611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                10005
_reflns_number_total             10088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502267t_si_002.cif
_cod_data_source_block           complex_2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341675