#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:26:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178812 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/66/4106631.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_4106631
loop_
_publ_author_name
'Wenshan Ren'
'Guofu Zi'
'De-Cai Fang'
'Marc D. Walter'
_publ_section_title
;
 Thorium Oxo and Sulfido Metallocenes: Synthesis, Structure, Reactivity,
 and Computational Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13183
_journal_page_last               13196
_journal_paper_doi               10.1021/ja205280k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C47 H68 O2 Th'
_chemical_formula_sum            'C47 H68 O2 Th'
_chemical_formula_weight         897.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.0548(14)
_cell_length_b                   17.0548(14)
_cell_length_c                   12.2849(12)
_cell_measurement_reflns_used    2786
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.36
_cell_measurement_theta_min      2.39
_cell_volume                     3094.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18640
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    3.650
_exptl_absorpt_correction_T_max  0.5595
_exptl_absorpt_correction_T_min  0.5289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       Block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.561
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0323
_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/[σ²(Fo²)+(0.0044P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                4533
_reflns_number_total             4748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205280k_si_002_02.cif
_cod_data_source_block           compound7
_cod_database_code               4106631
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -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
C1 C 0.5647(3) 0.8732(3) 0.3502(3) 0.0161(9) Uani 1 1 d .
C2 C 0.5011(2) 0.9029(3) 0.3258(3) 0.0174(9) Uani 1 1 d .
C3 C 0.4696(3) 0.8724(3) 0.2180(3) 0.0177(9) Uani 1 1 d .
H3 H 0.4288 0.8836 0.1806 0.021 Uiso 1 1 calc R
C4 C 0.5086(3) 0.8232(3) 0.1761(3) 0.0172(9) Uani 1 1 d .
C5 C 0.5683(3) 0.8265(2) 0.2565(3) 0.0169(9) Uani 1 1 d .
H5 H 0.6055 0.8014 0.2494 0.020 Uiso 1 1 calc R
C6 C 0.6131(3) 0.8723(2) 0.4558(3) 0.0211(9) Uani 1 1 d .
C7 C 0.6666(3) 0.8233(3) 0.4380(4) 0.0295(11) Uani 1 1 d .
H7A H 0.6259 0.7617 0.4172 0.044 Uiso 1 1 calc R
H7B H 0.6969 0.8242 0.5043 0.044 Uiso 1 1 calc R
H7C H 0.7105 0.8532 0.3815 0.044 Uiso 1 1 calc R
C8 C 0.6814(3) 0.9666(3) 0.4987(3) 0.0266(9) Uani 1 1 d .
H8A H 0.7281 0.9979 0.4456 0.040 Uiso 1 1 calc R
H8B H 0.7077 0.9608 0.5651 0.040 Uiso 1 1 calc R
H8C H 0.6510 1.0002 0.5124 0.040 Uiso 1 1 calc R
C9 C 0.5434(3) 0.8185(3) 0.5452(3) 0.0286(11) Uani 1 1 d .
H9A H 0.5104 0.8486 0.5637 0.043 Uiso 1 1 calc R
H9B H 0.5742 0.8146 0.6086 0.043 Uiso 1 1 calc R
H9C H 0.5021 0.7586 0.5192 0.043 Uiso 1 1 calc R
C10 C 0.4465(3) 0.9336(3) 0.3971(3) 0.0195(10) Uani 1 1 d .
C11 C 0.4934(3) 0.9908(3) 0.4984(4) 0.0297(12) Uani 1 1 d .
H11A H 0.5445 1.0472 0.4765 0.045 Uiso 1 1 calc R
H11B H 0.5133 0.9586 0.5442 0.045 Uiso 1 1 calc R
H11C H 0.4515 1.0022 0.5378 0.045 Uiso 1 1 calc R
C12 C 0.3608(2) 0.8466(3) 0.4337(3) 0.0245(10) Uani 1 1 d .
H12A H 0.3778 0.8109 0.4777 0.037 Uiso 1 1 calc R
H12B H 0.3282 0.8123 0.3709 0.037 Uiso 1 1 calc R
H12C H 0.3230 0.8623 0.4754 0.037 Uiso 1 1 calc R
C13 C 0.4147(3) 0.9881(3) 0.3298(4) 0.0300(12) Uani 1 1 d .
H13A H 0.3812 1.0066 0.3755 0.045 Uiso 1 1 calc R
H13B H 0.3767 0.9513 0.2715 0.045 Uiso 1 1 calc R
H13C H 0.4664 1.0407 0.3003 0.045 Uiso 1 1 calc R
C14 C 0.4886(3) 0.7738(3) 0.0668(3) 0.0211(10) Uani 1 1 d .
C15 C 0.3910(3) 0.7410(3) 0.0325(4) 0.0341(13) Uani 1 1 d .
H15A H 0.3505 0.7007 0.0869 0.051 Uiso 1 1 calc R
H15B H 0.3791 0.7097 -0.0357 0.051 Uiso 1 1 calc R
H15C H 0.3821 0.7921 0.0249 0.051 Uiso 1 1 calc R
C16 C 0.5511(3) 0.8384(3) -0.0206(3) 0.0281(12) Uani 1 1 d .
H16A H 0.5437 0.8906 -0.0242 0.042 Uiso 1 1 calc R
H16B H 0.5361 0.8082 -0.0898 0.042 Uiso 1 1 calc R
H16C H 0.6128 0.8570 -0.0028 0.042 Uiso 1 1 calc R
C17 C 0.5031(3) 0.6938(3) 0.0759(3) 0.0350(13) Uani 1 1 d .
H17A H 0.5647 0.7144 0.0963 0.052 Uiso 1 1 calc R
H17B H 0.4907 0.6633 0.0069 0.052 Uiso 1 1 calc R
H17C H 0.4631 0.6528 0.1301 0.052 Uiso 1 1 calc R
C18 C 0.8141(4) 1.0000 0.1667 0.0253(15) Uani 1 2 d S
C19 C 0.9059(3) 1.0798(3) 0.1340(4) 0.0299(12) Uani 1 1 d .
C20 C 0.9484(4) 1.0739(4) 0.0399(4) 0.0456(15) Uani 1 1 d .
H20 H 0.9211 1.0214 -0.0019 0.055 Uiso 1 1 calc R
C21 C 1.0312(4) 1.1461(4) 0.0085(5) 0.0545(18) Uani 1 1 d .
H21 H 1.0592 1.1422 -0.0545 0.065 Uiso 1 1 calc R
C22 C 1.0717(3) 1.2234(5) 0.0705(5) 0.061(2) Uani 1 1 d .
H22 H 1.1268 1.2721 0.0487 0.073 Uiso 1 1 calc R
C23 C 1.0316(4) 1.2289(4) 0.1634(5) 0.0589(18) Uani 1 1 d .
H23 H 1.0605 1.2805 0.2065 0.071 Uiso 1 1 calc R
C24 C 0.9473(3) 1.1573(4) 0.1943(4) 0.0423(14) Uani 1 1 d .
H24 H 0.9191 1.1624 0.2566 0.051 Uiso 1 1 calc R
O1 O 0.77631(18) 1.0251(2) 0.2545(2) 0.0249(7) Uani 1 1 d .
Th1 Th 0.653343(10) 1.0000 0.1667 0.01686(6) Uani 1 2 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'
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
C5 C1 C2 106.3(3) . .
C5 C1 C6 120.2(4) . .
C2 C1 C6 132.8(4) . .
C5 C1 Th1 69.1(2) . .
C2 C1 Th1 77.5(2) . .
C6 C1 Th1 124.6(2) . .
C3 C2 C1 106.1(3) . .
C3 C2 C10 117.9(3) . .
C1 C2 C10 133.5(3) . .
C3 C2 Th1 70.1(2) . .
C1 C2 Th1 74.5(2) . .
C10 C2 Th1 133.0(3) . .
C4 C3 C2 110.8(4) . .
C4 C3 Th1 73.0(2) . .
C2 C3 Th1 81.8(2) . .
C4 C3 H3 124.6 . .
C2 C3 H3 124.6 . .
Th1 C3 H3 112.5 . .
C5 C4 C3 105.7(3) . .
C5 C4 C14 126.7(4) . .
C3 C4 C14 127.6(4) . .
C5 C4 Th1 75.7(2) . .
C3 C4 Th1 78.3(2) . .
C14 C4 Th1 113.1(3) . .
C4 C5 C1 111.1(4) . .
C4 C5 Th1 75.2(2) . .
C1 C5 Th1 82.6(2) . .
C4 C5 H5 124.5 . .
C1 C5 H5 124.5 . .
Th1 C5 H5 109.8 . .
C7 C6 C8 106.0(4) . .
C7 C6 C9 105.6(3) . .
C8 C6 C9 109.6(3) . .
C7 C6 C1 110.7(3) . .
C8 C6 C1 114.1(3) . .
C9 C6 C1 110.4(4) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C13 C10 C11 106.4(4) . .
C13 C10 C12 106.8(4) . .
C11 C10 C12 108.4(3) . .
C13 C10 C2 110.9(3) . .
C11 C10 C2 117.6(4) . .
C12 C10 C2 106.3(3) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C17 C14 C16 109.5(4) . .
C17 C14 C15 109.3(4) . .
C16 C14 C15 108.1(4) . .
C17 C14 C4 110.0(3) . .
C16 C14 C4 109.7(3) . .
C15 C14 C4 110.2(4) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C14 C17 H17A 109.5 . .
C14 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C14 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
O1 C18 O1 106.1(5) . 5_675
O1 C18 C19 110.5(2) . 5_675
O1 C18 C19 110.3(2) 5_675 5_675
O1 C18 C19 110.3(2) . .
O1 C18 C19 110.5(2) 5_675 .
C19 C18 C19 109.2(5) 5_675 .
O1 C18 Th1 53.1(2) . .
O1 C18 Th1 53.1(2) 5_675 .
C19 C18 Th1 125.4(3) 5_675 .
C19 C18 Th1 125.4(3) . .
C24 C19 C20 119.0(5) . .
C24 C19 C18 121.6(4) . .
C20 C19 C18 119.4(4) . .
C21 C20 C19 120.1(6) . .
C21 C20 H20 120.0 . .
C19 C20 H20 120.0 . .
C22 C21 C20 120.0(6) . .
C22 C21 H21 120.0 . .
C20 C21 H21 120.0 . .
C23 C22 C21 120.2(5) . .
C23 C22 H22 119.9 . .
C21 C22 H22 119.9 . .
C22 C23 C24 120.2(6) . .
C22 C23 H23 119.9 . .
C24 C23 H23 119.9 . .
C19 C24 C23 120.5(5) . .
C19 C24 H24 119.8 . .
C23 C24 H24 119.8 . .
C18 O1 Th1 95.7(2) . .
O1 Th1 O1 62.39(15) . 5_675
O1 Th1 C18 31.19(7) . .
O1 Th1 C18 31.19(7) 5_675 .
O1 Th1 C4 115.63(11) . .
O1 Th1 C4 99.10(12) 5_675 .
C18 Th1 C4 110.20(8) . .
O1 Th1 C4 99.10(12) . 5_675
O1 Th1 C4 115.63(11) 5_675 5_675
C18 Th1 C4 110.20(8) . 5_675
C4 Th1 C4 139.60(17) . 5_675
O1 Th1 C5 87.23(11) . .
O1 Th1 C5 91.74(12) 5_675 .
C18 Th1 C5 89.40(9) . .
C4 Th1 C5 29.08(11) . .
C4 Th1 C5 151.79(12) 5_675 .
O1 Th1 C5 91.74(12) . 5_675
O1 Th1 C5 87.23(11) 5_675 5_675
C18 Th1 C5 89.40(9) . 5_675
C4 Th1 C5 151.79(12) . 5_675
C4 Th1 C5 29.08(11) 5_675 5_675
C5 Th1 C5 178.80(18) . 5_675
O1 Th1 C3 128.04(11) . .
O1 Th1 C3 127.65(12) 5_675 .
C18 Th1 C3 135.82(8) . .
C4 Th1 C3 28.79(11) . .
C4 Th1 C3 112.41(12) 5_675 .
C5 Th1 C3 46.62(12) . .
C5 Th1 C3 134.58(12) 5_675 .
O1 Th1 C3 127.65(12) . 5_675
O1 Th1 C3 128.04(11) 5_675 5_675
C18 Th1 C3 135.82(8) . 5_675
C4 Th1 C3 112.41(12) . 5_675
C4 Th1 C3 28.79(11) 5_675 5_675
C5 Th1 C3 134.58(12) . 5_675
C5 Th1 C3 46.62(12) 5_675 5_675
C3 Th1 C3 88.35(17) . 5_675
O1 Th1 C1 81.82(10) . .
O1 Th1 C1 113.01(10) 5_675 .
C18 Th1 C1 98.35(8) . .
C4 Th1 C1 47.58(11) . .
C4 Th1 C1 125.04(11) 5_675 .
C5 Th1 C1 28.36(10) . .
C5 Th1 C1 152.01(10) 5_675 .
C3 Th1 C1 46.35(11) . .
C3 Th1 C1 118.81(11) 5_675 .
O1 Th1 C1 113.01(11) . 5_675
O1 Th1 C1 81.82(10) 5_675 5_675
C18 Th1 C1 98.35(8) . 5_675
C4 Th1 C1 125.04(11) . 5_675
C4 Th1 C1 47.58(11) 5_675 5_675
C5 Th1 C1 152.01(10) . 5_675
C5 Th1 C1 28.36(10) 5_675 5_675
C3 Th1 C1 118.81(11) . 5_675
C3 Th1 C1 46.35(11) 5_675 5_675
C1 Th1 C1 163.29(16) . 5_675
O1 Th1 C2 105.38(10) . .
O1 Th1 C2 137.98(11) 5_675 .
C18 Th1 C2 126.11(7) . .
C4 Th1 C2 47.26(11) . .
C4 Th1 C2 105.77(11) 5_675 .
C5 Th1 C2 46.34(11) . .
C5 Th1 C2 134.64(11) 5_675 .
C3 Th1 C2 28.05(10) . .
C3 Th1 C2 92.13(11) 5_675 .
C1 Th1 C2 27.93(10) . .
C1 Th1 C2 135.42(12) 5_675 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C5 1.419(5) .
C1 C2 1.440(5) .
C1 C6 1.542(5) .
C1 Th1 2.962(4) .
C2 C3 1.426(5) .
C2 C10 1.548(5) .
C2 Th1 3.001(4) .
C3 C4 1.402(5) .
C3 Th1 2.852(4) .
C3 H3 0.9300 .
C4 C5 1.399(5) .
C4 C14 1.531(5) .
C4 Th1 2.785(4) .
C5 Th1 2.790(3) .
C5 H5 0.9300 .
C6 C7 1.530(6) .
C6 C8 1.532(5) .
C6 C9 1.540(5) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C13 1.531(6) .
C10 C11 1.536(6) .
C10 C12 1.541(5) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C17 1.507(6) .
C14 C16 1.525(5) .
C14 C15 1.527(6) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 O1 1.427(4) .
C18 O1 1.427(4) 5_675
C18 C19 1.528(5) 5_675
C18 C19 1.528(5) .
C18 Th1 2.741(6) .
C19 C24 1.364(7) .
C19 C20 1.394(6) .
C20 C21 1.386(7) .
C20 H20 0.9300 .
C21 C22 1.372(8) .
C21 H21 0.9300 .
C22 C23 1.358(8) .
C22 H22 0.9300 .
C23 C24 1.395(6) .
C23 H23 0.9300 .
C24 H24 0.9300 .
O1 Th1 2.202(3) .
Th1 O1 2.202(3) 5_675
Th1 C4 2.785(4) 5_675
Th1 C5 2.790(3) 5_675
Th1 C3 2.852(4) 5_675
Th1 C1 2.962(4) 5_675
