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_4088230
_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            'C39.5 H70 Cl2 N2 O3 U'
_chemical_formula_weight         929.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.9253(5)
_cell_angle_beta                 88.4904(5)
_cell_angle_gamma                65.5842(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2214(5)
_cell_length_b                   11.7908(5)
_cell_length_c                   17.7903(8)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.25
_cell_volume                     2091.12(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24838
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.722
_diffrn_reflns_theta_min         1.943
_exptl_absorpt_coefficient_mu    4.045
_exptl_absorpt_correction_T_max  0.8126
_exptl_absorpt_correction_T_min  0.4514
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.8060P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9183
_reflns_number_total             9915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00942_si_003.cif
_cod_data_source_block           clw8
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C39.50 H70 Cl2 N2 O3 U'
_cod_database_code               4088230
_shelx_estimated_absorpt_t_min   0.367
_shelx_estimated_absorpt_t_max   0.754
_shelxl_version_number           2013-2
_shelx_res_checksum              66157
_shelx_hkl_checksum              28939