#------------------------------------------------------------------------------
#$Date: 2016-01-01 09:46:03 +0200 (Fri, 01 Jan 2016) $
#$Revision: 171842 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/81/7118178.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_7118178
loop_
_publ_author_name
'Pedrick, Elizabeth A.'
'Hrobárik, Peter'
'Seaman, Lani A.'
'Wu, Guang'
'Hayton, Trevor W.'
_publ_section_title
;
 Synthesis, structure and bonding of hexaphenyl thorium(iv): observation
 of a non-octahedral structure.
;
_journal_issue                   4
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              689
_journal_page_last               692
_journal_paper_doi               10.1039/c5cc08265j
_journal_volume                  52
_journal_year                    2015
_chemical_formula_sum            'C60 H90 Li2 O12 Th'
_chemical_formula_weight         1249.24
_chemical_name_systematic        '[Li(DME)3]2[Th(C6H5)6] '
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive, Oxygen-sensitive'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.8737(4)
_cell_length_b                   14.8737(4)
_cell_length_c                   24.3175(8)
_cell_measurement_temperature    100(2)
_cell_volume                     4658.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12517
_diffrn_reflns_theta_full        29.74
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.456
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.2453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1926
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0345P)²+1.0554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                2629
_reflns_number_total             2963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc08265j2.cif
_cod_data_source_block           complex_1
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7118178
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Th1 Th 0.6667 0.3333 0.3333 0.04075(9) Uani 1 6 d S
C1 C 0.7598(3) 0.4983(3) 0.39379(15) 0.0740(10) Uani 1 1 d .
C4 C 0.8503(3) 0.6758(2) 0.46168(13) 0.0637(9) Uani 1 1 d .
H4 H 0.8804 0.7356 0.4846 0.076 Uiso 1 1 calc R
C2 C 0.8449(3) 0.5236(3) 0.42723(16) 0.0693(9) Uani 1 1 d .
H2 H 0.8728 0.4784 0.4273 0.083 Uiso 1 1 calc R
C3 C 0.8912(2) 0.6106(3) 0.46032(14) 0.0641(8) Uani 1 1 d .
H3 H 0.9503 0.6254 0.4818 0.077 Uiso 1 1 calc R
C6 C 0.7230(2) 0.5675(3) 0.39673(13) 0.0629(8) Uani 1 1 d .
H6 H 0.6649 0.5541 0.3746 0.076 Uiso 1 1 calc R
C5 C 0.7651(3) 0.6536(2) 0.42945(14) 0.0619(8) Uani 1 1 d .
H5 H 0.7362 0.6979 0.4301 0.074 Uiso 1 1 calc R
O1 O 1.00288(13) 0.88178(13) 0.35456(7) 0.0426(4) Uani 1 1 d .
C8 C 0.9716(2) 0.7890(2) 0.32423(12) 0.0491(6) Uani 1 1 d .
H8A H 0.9490 0.7295 0.3496 0.059 Uiso 1 1 calc R
H8B H 1.0304 0.7955 0.3020 0.059 Uiso 1 1 calc R
O2 O 0.91402(14) 0.86434(13) 0.25793(7) 0.0471(4) Uani 1 1 d .
C7 C 1.0805(2) 0.8990(2) 0.39380(13) 0.0536(7) Uani 1 1 d .
H7A H 1.0543 0.8393 0.4187 0.080 Uiso 1 1 calc R
H7B H 1.0981 0.9618 0.4150 0.080 Uiso 1 1 calc R
H7C H 1.1425 0.9079 0.3748 0.080 Uiso 1 1 calc R
C9 C 0.8845(2) 0.7722(2) 0.28780(12) 0.0545(7) Uani 1 1 d .
H9A H 0.8679 0.7143 0.2621 0.065 Uiso 1 1 calc R
H9B H 0.8220 0.7539 0.3101 0.065 Uiso 1 1 calc R
C10 C 0.8418(3) 0.8489(3) 0.21553(13) 0.0655(8) Uani 1 1 d .
H10A H 0.8400 0.7988 0.1888 0.098 Uiso 1 1 calc R
H10B H 0.8630 0.9151 0.1970 0.098 Uiso 1 1 calc R
H10C H 0.7726 0.8223 0.2315 0.098 Uiso 1 1 calc R
Li1 Li 1.0000 1.0000 0.3043(3) 0.0390(15) Uani 1 3 d S
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'
Li Li -0.0003 0.0001 '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'
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
C1 Th1 C1 179.998(1) 18_545 3_665
C1 Th1 C1 89.07(12) 18_545 2_655
C1 Th1 C1 90.94(12) 3_665 2_655
C1 Th1 C1 89.07(12) 18_545 .
C1 Th1 C1 90.93(12) 3_665 .
C1 Th1 C1 90.93(12) 2_655 .
C1 Th1 C1 90.93(12) 18_545 16_655
C1 Th1 C1 89.06(12) 3_665 16_655
C1 Th1 C1 89.07(12) 2_655 16_655
C1 Th1 C1 179.999(1) . 16_655
C1 Th1 C1 90.93(12) 18_545 17
C1 Th1 C1 89.06(12) 3_665 17
C1 Th1 C1 180.0 2_655 17
C1 Th1 C1 89.07(12) . 17
C1 Th1 C1 90.93(12) 16_655 17
C2 C1 C6 114.4(3) . .
C2 C1 Th1 124.9(3) . .
C6 C1 Th1 120.6(3) . .
C3 C4 C5 119.5(3) . .
C3 C2 C1 123.7(3) . .
C4 C3 C2 119.0(3) . .
C5 C6 C1 124.0(3) . .
C6 C5 C4 119.5(3) . .
C7 O1 C8 111.5(2) . .
C7 O1 Li1 125.39(18) . .
C8 O1 Li1 111.5(2) . .
O1 C8 C9 107.9(2) . .
C9 O2 C10 111.9(2) . .
C9 O2 Li1 113.7(2) . .
C10 O2 Li1 126.3(2) . .
O2 C9 C8 108.7(2) . .
O2 Li1 O2 93.8(2) 3_675 2_765
O2 Li1 O2 93.8(2) 3_675 .
O2 Li1 O2 93.8(2) 2_765 .
O2 Li1 O1 163.21(8) 3_675 .
O2 Li1 O1 100.60(7) 2_765 .
O2 Li1 O1 76.80(7) . .
O2 Li1 O1 100.60(7) 3_675 2_765
O2 Li1 O1 76.80(7) 2_765 2_765
O2 Li1 O1 163.21(8) . 2_765
O1 Li1 O1 91.1(2) . 2_765
O2 Li1 O1 76.80(7) 3_675 3_675
O2 Li1 O1 163.21(8) 2_765 3_675
O2 Li1 O1 100.60(7) . 3_675
O1 Li1 O1 91.1(2) . 3_675
O1 Li1 O1 91.1(2) 2_765 3_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 C1 2.589(3) 18_545
Th1 C1 2.589(3) 3_665
Th1 C1 2.589(3) 2_655
Th1 C1 2.589(3) .
Th1 C1 2.589(3) 16_655
Th1 C1 2.589(3) 17
C1 C2 1.388(5) .
C1 C6 1.389(5) .
C4 C3 1.379(5) .
C4 C5 1.381(5) .
C2 C3 1.381(5) .
C6 C5 1.365(5) .
O1 C7 1.418(3) .
O1 C8 1.422(3) .
O1 Li1 2.160(4) .
C8 C9 1.484(4) .
O2 C9 1.413(3) .
O2 C10 1.423(3) .
O2 Li1 2.097(4) .
Li1 O2 2.097(4) 3_675
Li1 O2 2.097(4) 2_765
Li1 O1 2.160(4) 2_765
Li1 O1 2.160(4) 3_675
