Stable Uranium(VI) Methyl and Acetylide Complexes and the Elucidation of an Inverse Trans Influence Ligand Series
Andrew J. Lewis; Patrick J. Carroll; Eric J. Schelter; Journal of the American Chemical Society 135 (2013) 13185–13192; doi:10.1021/ja406610r

data_4120739
_publ_section_title
;
 Stable Uranium(VI) Methyl and Acetylide Complexes and the Elucidation of
 an Inverse Trans Influence Ligand Series
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13185
_journal_page_last               13192
_journal_paper_doi               10.1021/ja406610r
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C19 H57 N3 O Si6 U'
_chemical_formula_weight         750.25
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8834(13)
_cell_length_b                   12.5642(13)
_cell_length_c                   22.928(2)
_cell_measurement_temperature    143(1)
_cell_volume                     3423.3(6)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67249
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.967
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.505(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         7880
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0156
_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^)+(0.0182P)^2^+1.3376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0366
_reflns_number_gt                7563
_reflns_number_total             7880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406610r_si_002_1.cif
_cod_data_source_block           4389
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4120739