Synthetic Utility of Tetrabutylammonium Salts in Uranium Metallocene Chemistry
Webster, Christopher L.; Langeslay, Ryan R.; Ziller, Joseph W.; Evans, William J.; Organometallics 35 (2016) 520–; doi:10.1021/acs.organomet.5b00942

data_4088225
_publ_section_title
;
 Synthetic Utility of Tetrabutylammonium Salts in Uranium Metallocene
 Chemistry
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              520
_journal_paper_doi               10.1021/acs.organomet.5b00942
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C29 H42 Cl N O2 U'
_chemical_formula_weight         710.11
_space_group_crystal_system      triclinic
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_space_group_name_H-M_alt        'P -1'
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_cell_length_b                   10.3929(16)
_cell_length_c                   17.363(3)
_cell_measurement_temperature    88(2)
_cell_volume                     1401.0(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.946
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
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_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16363
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.284
_diffrn_reflns_theta_min         2.118
_exptl_absorpt_coefficient_mu    5.913
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.6093
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.047
_refine_diff_density_max         3.148
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0544P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0836
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_reflns_number_gt                5844
_reflns_number_total             6574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00942_si_005.cif
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_cod_database_code               4088225
_shelx_estimated_absorpt_t_min   0.387
_shelx_estimated_absorpt_t_max   0.769
_shelxl_version_number           2013-2
_shelx_res_checksum              19023
_shelx_hkl_checksum              78276