Isolation of a Square-Planar Th(III) Complex: Synthesis and Structure of [Th(OC<sub>6</sub>H<sub>2</sub><sup>t</sup>Bu<sub>2</sub>-2,6-Me-4)<sub>4</sub>]<sup>1</sup>.
Huh, Daniel N.; Roy, Saswata; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Journal of the American Chemical Society 141 (2019) 12458–12463; doi:10.1021/jacs.9b04399

data_4127769
_publ_section_title
;
 Isolation of a Square-Planar Th(III) Complex: Synthesis and Structure of
 [Th(OC<sub>6</sub>H<sub>2</sub><sup>t</sup>Bu<sub>2</sub>-2,6-Me-4)<sub>4</sub>]<sup>1</sup>.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12458
_journal_page_last               12463
_journal_paper_doi               10.1021/jacs.9b04399
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C78.5 H128.5 Li O8.5 Th'
_chemical_formula_weight         1447.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.3671(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.987(3)
_cell_length_b                   19.879(3)
_cell_length_c                   39.091(6)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.58
_cell_volume                     16237(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 0.946
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            97331
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.731
_diffrn_reflns_theta_min         1.414
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             6084
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   0.4315
_exptl_transmission_factor_min   0.3792
_refine_diff_density_max         1.471
_refine_diff_density_min         -3.513
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         19934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+86.8133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16597
_reflns_number_total             19934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04399_si_002.cif
_cod_data_source_block           dnh72_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C78.50 H128.50 Li O8.50 Th'
_cod_database_code               4127769
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.792
_exptl_absorpt_special_details
; 
 Reflections not merged 
   98849 Corrected reflections written to file dnh72s.hkl 
 Estimated minimum and maximum transmission:  0.3792  0.4315 
 The ratio of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.6000 
 Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              35463
_shelx_hkl_checksum              94810
_shelx_fab_checksum              99920