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_4127768
_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            'C84 H142 K O10 Th'
_chemical_formula_weight         1583.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6539(18)
_cell_length_b                   31.523(2)
_cell_length_c                   9.6026(6)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.22
_cell_volume                     8370.9(9)
_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 0.985
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            78825
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.292
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3340
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.965
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.495(6)
_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     846
_refine_ls_number_reflns         20184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0265P)^2^+10.6787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                17359
_reflns_number_total             20184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04399_si_001.cif
_cod_data_source_block           dnh67
_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_cell_volume        8371.0(9)
_cod_database_code               4127768
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.662
_shelx_estimated_absorpt_t_max   0.831
_exptl_absorpt_special_details
; 
 Reflections not merged 
   78889 Corrected reflections written to file dnh67s.hkl 
 Estimated minimum and maximum transmission:  0.6292  0.7457 
 The ratio of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.2000 
 Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              5091
_shelx_hkl_checksum              54716