Electrochemical Studies of Tris(cyclopentadienyl) Thorium and Uranium Complexes in the +2, +3, and +4 Oxidation States
Wedal, Justin C.; Barlow, Jeffrey M.; Ziller, Joseph W.; Yang, Jenny Y.; Evans, William J.; Chemical Science  (2021) –; doi:10.1039/D1SC01906F

data_1562427
_publ_section_title
;
 Electrochemical Studies of Tris(cyclopentadienyl) Thorium and Uranium
 Complexes in the +2, +3, and +4 Oxidation States
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01906F
_journal_year                    2021
_chemical_formula_sum            'C51 H99 Cs N2 O6 Si6 Th'
_chemical_formula_weight         1369.81
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-03-07 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.6711(10)
_cell_angle_beta                 104.3758(9)
_cell_angle_gamma                95.7421(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1953(8)
_cell_length_b                   12.7501(8)
_cell_length_c                   22.2212(14)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.22
_cell_volume                     3250.2(4)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 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  0.0464
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.322
_diffrn_reflns_theta_min         1.645
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_T_max  0.6471
_exptl_absorpt_correction_T_min  0.5186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.613
_refine_diff_density_min         -2.543
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         16125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+8.7843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13147
_reflns_number_total             16125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01906f2.cif
_cod_data_source_block           jcw48
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1562427
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.791
_exptl_absorpt_special_details
; 
Reflections not merged 
43962 Corrected reflections written to file jcw48s.hkl 
Estimated minimum and maximum transmission:  0.5186  0.6471 
The ratio (0.8014) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.3000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              37014
_shelx_hkl_checksum              31107