Convenient access to the anhydrous thorium tetrachloride complexes ThCl(4)(DME)(2), ThCl(4)(1,4-dioxane)(2) and ThCl(4)(THF)(3.5) using commercially available and inexpensive starting materials.
Cantat, Thibault; Scott, Brian L.; Kiplinger, Jaqueline L.; Chemical communications (Cambridge, England) 46 (2010) 919–921; doi:10.1039/b923558b

data_7105213
_publ_section_title
;
 Convenient access to the anhydrous thorium tetrachloride complexes
 ThCl(4)(DME)(2), ThCl(4)(1,4-dioxane)(2) and ThCl(4)(THF)(3.5) using
 commercially available and inexpensive starting materials.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              919
_journal_page_last               921
_journal_paper_doi               10.1039/b923558b
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C20 H48 Cl4 O9 Th'
_chemical_formula_weight         806.42
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.515(5)
_cell_angle_beta                 107.115(5)
_cell_angle_gamma                92.690(5)
_cell_formula_units_Z            2
_cell_length_a                   10.744(5)
_cell_length_b                   10.896(5)
_cell_length_c                   13.900(6)
_cell_measurement_reflns_used    1639
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      36.5
_cell_measurement_theta_min      5.2
_cell_volume                     1525.9(11)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_sigmaI/netI    0.1126
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14789
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.278
_exptl_absorpt_correction_T_max  0.7425
_exptl_absorpt_correction_T_min  0.4501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.079
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.661
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         5562
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.660
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                3912
_reflns_number_total             5562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b923558b.txt
_cod_data_source_block           apx876s
_cod_depositor_comments
;
 Changing atom type of atom 'O8'' from 'C' to 'O'.

 Antanas Vaitkus,
 2016-12-20

 Moving all atoms from disorder site B/2 (assembly/group) to the previously
 unused disorder site A/2 since atoms in disorder sites A/1 and B/2 seem to
 be simultaneously occupying the same site.

 Antanas Vaitkus,
 2016-12-20

 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-20
;
_cod_database_code               7105213