#------------------------------------------------------------------------------
#$Date: 2016-12-20 13:24:18 +0200 (Tue, 20 Dec 2016) $
#$Revision: 189272 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/52/7105214.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7105214
loop_
_publ_author_name
'Cantat, Thibault'
'Scott, Brian L.'
'Kiplinger, Jaqueline L.'
_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            'C12 H32 Cl4 O10 Th'
_chemical_formula_weight         710.22
_chemical_name_systematic        ?
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2963(13)
_cell_length_b                   12.3952(15)
_cell_length_c                   18.491(2)
_cell_measurement_reflns_used    6195
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      54.8
_cell_measurement_theta_min      4.4
_cell_volume                     2359.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.813
_exptl_absorpt_correction_T_max  0.7723
_exptl_absorpt_correction_T_min  0.3156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.923
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                2107
_reflns_number_total             2861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b923558b.txt
_cod_data_source_block           apx912a
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-20
;
_cod_original_sg_symbol_H-M      'P bna'
_cod_database_code               7105214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z'
'x-1/2, y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Th1 Th 0.912706(18) 0.7500 0.5000 0.01192(8) Uani 1 2 d S . . 0
Cl1 Cl 1.11225(10) 0.64303(9) 0.56998(6) 0.0209(2) Uani 1 1 d . . . 0
Cl2 Cl 0.72581(10) 0.74340(8) 0.39523(6) 0.0196(2) Uani 1 1 d . . . 0
O1 O 0.9949(3) 0.8743(2) 0.59373(14) 0.0156(6) Uani 1 1 d . . . 2
O2 O 0.8250(3) 0.9333(2) 0.48104(16) 0.0188(7) Uani 1 1 d . . . 2
O3 O 0.0944(3) 0.4269(2) 0.72472(16) 0.0226(7) Uani 1 1 d . . . 0
O4 O 0.2774(3) 0.3992(2) 0.83623(16) 0.0243(7) Uani 1 1 d . . . 0
O5 O 0.5834(3) -0.0065(3) 0.44013(17) 0.0230(7) Uani 1 1 d . . . 0
C1 C 0.1505(4) 0.5179(4) 0.7610(2) 0.0264(11) Uani 1 1 d . . . 0
H1A H 0.0949 0.5393 0.8009 0.032 Uiso 1 1 calc R . . 0
H1B H 0.1565 0.5781 0.7277 0.032 Uiso 1 1 calc R . . 0
C2 C 0.2821(4) 0.4911(4) 0.7890(3) 0.0274(11) Uani 1 1 d . . . 0
H2A H 0.3396 0.4759 0.7487 0.033 Uiso 1 1 calc R . . 0
H2B H 0.3168 0.5526 0.8151 0.033 Uiso 1 1 calc R . . 0
C3 C 0.2226(5) 0.3089(4) 0.7989(2) 0.0266(11) Uani 1 1 d . . . 0
H3A H 0.2171 0.2477 0.8315 0.032 Uiso 1 1 calc R . . 0
H3B H 0.2782 0.2890 0.7587 0.032 Uiso 1 1 calc R . . 0
C4 C 0.0893(4) 0.3363(4) 0.7712(3) 0.0282(11) Uani 1 1 d . . . 0
H4A H 0.0539 0.2751 0.7453 0.034 Uiso 1 1 calc R . . 0
H4B H 0.0323 0.3519 0.8117 0.034 Uiso 1 1 calc R . . 0
C5 C 0.5639(4) 0.0935(4) 0.4772(3) 0.0241(10) Uani 1 1 d . . . 0
H5A H 0.4941 0.1334 0.4542 0.029 Uiso 1 1 calc R . . 0
H5B H 0.6423 0.1367 0.4744 0.029 Uiso 1 1 calc R . . 0
C6 C 0.4697(4) -0.0729(4) 0.4446(3) 0.0265(11) Uani 1 1 d . . . 0
H6A H 0.4854 -0.1409 0.4202 0.032 Uiso 1 1 calc R . . 0
H6B H 0.3976 -0.0372 0.4207 0.032 Uiso 1 1 calc R . . 0
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Th1 O2 137.10(14) . 3_566 ?
O2 Th1 O1 69.56(9) . . ?
O2 Th1 O1 126.87(9) 3_566 . ?
O2 Th1 O1 126.87(9) . 3_566 ?
O2 Th1 O1 69.56(9) 3_566 3_566 ?
O1 Th1 O1 139.90(13) . 3_566 ?
O2 Th1 Cl2 79.37(7) . 3_566 ?
O2 Th1 Cl2 70.69(7) 3_566 3_566 ?
O1 Th1 Cl2 74.04(7) . 3_566 ?
O1 Th1 Cl2 139.29(7) 3_566 3_566 ?
O2 Th1 Cl2 70.69(7) . . ?
O2 Th1 Cl2 79.37(7) 3_566 . ?
O1 Th1 Cl2 139.29(7) . . ?
O1 Th1 Cl2 74.04(7) 3_566 . ?
Cl2 Th1 Cl2 90.43(5) 3_566 . ?
O2 Th1 Cl1 76.37(7) . 3_566 ?
O2 Th1 Cl1 141.15(7) 3_566 3_566 ?
O1 Th1 Cl1 76.97(7) . 3_566 ?
O1 Th1 Cl1 73.51(7) 3_566 3_566 ?
Cl2 Th1 Cl1 147.19(3) 3_566 3_566 ?
Cl2 Th1 Cl1 101.88(3) . 3_566 ?
O2 Th1 Cl1 141.15(7) . . ?
O2 Th1 Cl1 76.37(7) 3_566 . ?
O1 Th1 Cl1 73.51(7) . . ?
O1 Th1 Cl1 76.97(7) 3_566 . ?
Cl2 Th1 Cl1 101.88(3) 3_566 . ?
Cl2 Th1 Cl1 147.19(3) . . ?
Cl1 Th1 Cl1 84.09(5) 3_566 . ?
C4 O3 C1 110.8(3) . . ?
C3 O4 C2 109.9(3) . . ?
C5 O5 C6 110.8(3) . . ?
O3 C1 C2 110.7(4) . . ?
O3 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
O4 C2 C1 111.0(4) . . ?
O4 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
O4 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O4 C3 C4 110.3(4) . . ?
O4 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
O4 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 C3 110.6(4) . . ?
O3 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
O3 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O5 C5 C6 110.2(4) . 5_656 ?
O5 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 5_656 . ?
O5 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 5_656 . ?
H5A C5 H5B 108.1 . . ?
O5 C6 C5 109.9(4) . 5_656 ?
O5 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 5_656 . ?
O5 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 5_656 . ?
H6A C6 H6B 108.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O2 2.470(3) . ?
Th1 O2 2.470(3) 3_566 ?
Th1 O1 2.469(3) . ?
Th1 O1 2.469(3) 3_566 ?
Th1 Cl2 2.7318(11) 3_566 ?
Th1 Cl2 2.7318(11) . ?
Th1 Cl1 2.7665(11) 3_566 ?
Th1 Cl1 2.7665(11) . ?
O3 C4 1.416(6) . ?
O3 C1 1.433(5) . ?
O4 C3 1.431(5) . ?
O4 C2 1.437(5) . ?
O5 C5 1.430(6) . ?
O5 C6 1.433(5) . ?
C1 C2 1.488(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.504(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.509(7) 5_656 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C5 1.509(7) 5_656 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
