#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/77/2017799.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_2017799
loop_
_publ_author_name
'Nazarenko, Olga M.'
'Rusanova, Julia A.'
'Krautscheid, Harald'
'Domasevitch, Konstantin V.'
_publ_section_title
;
 catena-Poly[thorium(IV)-tetrakis(μ₂-3-carboxyadamantane-1-carboxylato)]:
 a quadruple helical strand driven by a synergy of coordination and
 hydrogen bonding
;
_journal_coeditor_code           EG3060
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m276
_journal_page_last               m279
_journal_paper_doi               10.1107/S0108270110034785
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Th (C12 H15 O4)4]'
_chemical_formula_moiety         'Th 4+ , 4C12 H15 O4 -'
_chemical_formula_sum            'C48 H60 O16 Th'
_chemical_formula_weight         1125.00
_chemical_name_systematic
;
catena-Poly[thorium(IV)-tetrakis(μ₂-3-carboxyadamantane-1-
carboxylato)]
;
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.8182(9)
_cell_length_b                   16.8182(9)
_cell_length_c                   7.5240(4)
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.42
_cell_volume                     2128.2(2)
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Version 1.70.01; Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation 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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6302
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.581
_exptl_absorpt_correction_T_max  0.8138
_exptl_absorpt_correction_T_min  0.6941
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.404
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0186
_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)+(0.0125P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0356
_reflns_number_gt                2472
_reflns_number_total             2498
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            eg3060.cif
_cod_data_source_block           I
_cod_database_code               2017799
_cod_database_fobs_code          2017799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th Th1 0.0000 0.0000 -0.2077 0.01669(5) Uani d S 1 . .
O O1 0.12030(12) -0.00437(14) -0.0466(3) 0.0396(6) Uani d . 1 . .
O O2 0.21529(13) -0.09657(13) -0.0629(3) 0.0405(6) Uani d . 1 . .
O O3 0.09419(12) 0.07342(13) 0.6115(3) 0.0352(6) Uani d . 1 . .
O O4 0.18015(13) 0.16655(12) 0.6858(3) 0.0377(6) Uani d . 1 . .
H H1 0.1509 0.1823 0.7709 0.057 Uiso d R 1 . .
C C1 0.22967(14) 0.00491(15) 0.1581(4) 0.0165(6) Uani d . 1 . .
C C2 0.17111(12) 0.03661(13) 0.2990(10) 0.0195(6) Uani d . 1 . .
H H2A 0.1332 0.0721 0.2430 0.023 Uiso calc R 1 . .
H H2B 0.1419 -0.0074 0.3505 0.023 Uiso calc R 1 . .
C C3 0.21601(15) 0.08140(15) 0.4462(4) 0.0170(6) Uani d . 1 . .
C C4 0.26221(16) 0.15183(15) 0.3634(4) 0.0223(7) Uani d . 1 . .
H H4A 0.2253 0.1884 0.3077 0.027 Uiso calc R 1 . .
H H4B 0.2908 0.1803 0.4556 0.027 Uiso calc R 1 . .
C C5 0.32105(16) 0.12035(16) 0.2245(4) 0.0240(7) Uani d . 1 . .
H H5 0.3498 0.1653 0.1722 0.029 Uiso calc R 1 . .
C C6 0.38035(14) 0.06411(16) 0.3100(10) 0.0285(10) Uani d . 1 . .
H H6A 0.4104 0.0920 0.4007 0.034 Uiso calc R 1 . .
H H6B 0.4174 0.0448 0.2211 0.034 Uiso calc R 1 . .
C C7 0.33568(16) -0.00623(17) 0.3936(4) 0.0249(7) Uani d . 1 . .
H H7 0.3739 -0.0423 0.4499 0.030 Uiso calc R 1 . .
C C8 0.28984(15) -0.05118(15) 0.2484(4) 0.0211(10) Uani d . 1 . .
H H8A 0.2620 -0.0960 0.3006 0.025 Uiso calc R 1 . .
H H8B 0.3268 -0.0715 0.1606 0.025 Uiso calc R 1 . .
C C9 0.27556(16) 0.07592(19) 0.0761(4) 0.0214(6) Uani d . 1 . .
H H9A 0.3127 0.0567 -0.0127 0.026 Uiso calc R 1 . .
H H9B 0.2386 0.1119 0.0184 0.026 Uiso calc R 1 . .
C C10 0.27692(17) 0.02440(19) 0.5344(4) 0.0242(7) Uani d . 1 . .
H H10A 0.3056 0.0523 0.6272 0.029 Uiso calc R 1 . .
H H10B 0.2492 -0.0201 0.5882 0.029 Uiso calc R 1 . .
C C11 0.18510(15) -0.03624(16) 0.0071(4) 0.0215(6) Uani d . 1 . .
C C12 0.15917(15) 0.10853(15) 0.5907(4) 0.0199(6) Uani d . 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Th1 O1 3 2 74.71(6) n
O1 Th1 O1 3 . 74.71(6) y
O1 Th1 O1 2 . 118.20(13) y
O1 Th1 O1 3 4 118.20(13) n
O1 Th1 O1 2 4 74.71(6) n
O1 Th1 O1 . 4 74.71(6) n
O1 Th1 O3 3 2_554 138.14(8) n
O1 Th1 O3 2 2_554 75.16(9) n
O1 Th1 O3 . 2_554 146.32(8) y
O1 Th1 O3 4 2_554 80.28(8) n
O1 Th1 O3 3 3_554 75.16(9) n
O1 Th1 O3 2 3_554 80.28(8) n
O1 Th1 O3 . 3_554 138.14(8) y
O1 Th1 O3 4 3_554 146.31(8) n
O3 Th1 O3 2_554 3_554 71.67(6) n
O1 Th1 O3 3 1_554 80.28(8) n
O1 Th1 O3 2 1_554 146.32(8) n
O1 Th1 O3 . 1_554 75.16(9) y
O1 Th1 O3 4 1_554 138.14(8) n
O3 Th1 O3 2_554 1_554 111.78(11) n
O3 Th1 O3 3_554 1_554 71.67(6) y
O1 Th1 O3 3 4_554 146.31(8) n
O1 Th1 O3 2 4_554 138.14(8) n
O1 Th1 O3 . 4_554 80.28(8) y
O1 Th1 O3 4 4_554 75.16(9) n
O3 Th1 O3 2_554 4_554 71.67(6) n
O3 Th1 O3 3_554 4_554 111.78(11) n
O3 Th1 O3 1_554 4_554 71.67(6) y
C11 O1 Th1 . . 154.85(19) n
C12 O3 Th1 . 1_556 151.7(2) n
C12 O4 H1 . . 120.4 n
C11 C1 C8 . . 111.9(2) n
C11 C1 C2 . . 110.8(2) n
C8 C1 C2 . . 109.1(3) n
C11 C1 C9 . . 107.3(2) n
C8 C1 C9 . . 108.7(2) n
C2 C1 C9 . . 109.0(2) n
C3 C2 C1 . . 110.54(18) n
C3 C2 H2A . . 109.5 n
C1 C2 H2A . . 109.5 n
C3 C2 H2B . . 109.5 n
C1 C2 H2B . . 109.5 n
H2A C2 H2B . . 108.1 n
C12 C3 C2 . . 110.7(2) n
C12 C3 C4 . . 112.0(2) n
C2 C3 C4 . . 109.3(3) n
C12 C3 C10 . . 107.2(2) n
C2 C3 C10 . . 109.2(2) n
C4 C3 C10 . . 108.3(2) n
C5 C4 C3 . . 109.5(2) n
C5 C4 H4A . . 109.8 n
C3 C4 H4A . . 109.8 n
C5 C4 H4B . . 109.8 n
C3 C4 H4B . . 109.8 n
H4A C4 H4B . . 108.2 n
C6 C5 C4 . . 110.5(4) n
C6 C5 C9 . . 109.3(3) n
C4 C5 C9 . . 109.9(2) n
C6 C5 H5 . . 109.0 n
C4 C5 H5 . . 109.0 n
C9 C5 H5 . . 109.1 n
C5 C6 C7 . . 109.40(19) n
C5 C6 H6A . . 109.8 n
C7 C6 H6A . . 109.8 n
C5 C6 H6B . . 109.8 n
C7 C6 H6B . . 109.8 n
H6A C6 H6B . . 108.2 n
C8 C7 C6 . . 109.4(3) n
C8 C7 C10 . . 109.4(2) n
C6 C7 C10 . . 109.8(3) n
C8 C7 H7 . . 109.4 n
C6 C7 H7 . . 109.4 n
C10 C7 H7 . . 109.4 n
C7 C8 C1 . . 110.0(2) n
C7 C8 H8A . . 109.7 n
C1 C8 H8A . . 109.7 n
C7 C8 H8B . . 109.7 n
C1 C8 H8B . . 109.7 n
H8A C8 H8B . . 108.2 n
C5 C9 C1 . . 109.3(2) n
C5 C9 H9A . . 109.8 n
C1 C9 H9A . . 109.8 n
C5 C9 H9B . . 109.8 n
C1 C9 H9B . . 109.8 n
H9A C9 H9B . . 108.3 n
C7 C10 C3 . . 109.7(3) n
C7 C10 H10A . . 109.7 n
C3 C10 H10A . . 109.7 n
C7 C10 H10B . . 109.7 n
C3 C10 H10B . . 109.7 n
H10A C10 H10B . . 108.2 n
O2 C11 O1 . . 123.5(3) n
O2 C11 C1 . . 118.8(2) n
O1 C11 C1 . . 117.6(2) n
O3 C12 O4 . . 122.6(3) n
O3 C12 C3 . . 119.8(2) n
O4 C12 C3 . . 117.6(2) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Th1 O1 3 2.359(2) n
Th1 O1 2 2.359(2) n
Th1 O1 . 2.359(2) y
Th1 O1 4 2.359(2) ?
Th1 O3 2_554 2.426(2) n
Th1 O3 3_554 2.426(2) n
Th1 O3 1_554 2.426(2) y
Th1 O3 4_554 2.426(2) n
O1 C11 . 1.280(3) n
O2 C11 . 1.251(3) n
O3 C12 . 1.252(3) n
O3 Th1 1_556 2.426(2) n
O4 C12 . 1.260(3) n
O4 H1 . 0.8500 n
C1 C11 . 1.527(4) n
C1 C8 . 1.541(4) n
C1 C2 . 1.542(5) n
C1 C9 . 1.550(4) n
C2 C3 . 1.538(6) n
C2 H2A . 0.9700 n
C2 H2B . 0.9700 n
C3 C12 . 1.518(4) n
C3 C4 . 1.548(4) n
C3 C10 . 1.552(4) n
C4 C5 . 1.533(4) n
C4 H4A . 0.9700 n
C4 H4B . 0.9700 n
C5 C6 . 1.517(5) n
C5 C9 . 1.546(4) n
C5 H5 . 0.9800 n
C6 C7 . 1.536(5) n
C6 H6A . 0.9700 n
C6 H6B . 0.9700 n
C7 C8 . 1.536(4) n
C7 C10 . 1.537(4) n
C7 H7 . 0.9800 n
C8 H8A . 0.9700 n
C8 H8B . 0.9700 n
C9 H9A . 0.9700 n
C9 H9B . 0.9700 n
C10 H10A . 0.9700 n
C10 H10B . 0.9700 n
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 Th1 O1 C11 3 . . . 177.0(5) n
O1 Th1 O1 C11 2 . . . 114.2(6) n
O1 Th1 O1 C11 4 . . . 51.4(6) n
O3 Th1 O1 C11 2_554 . . . 7.9(6) n
O3 Th1 O1 C11 3_554 . . . -137.7(5) n
O3 Th1 O1 C11 1_554 . . . -99.2(5) n
O3 Th1 O1 C11 4_554 . . . -25.8(5) n
C11 C1 C2 C3 . . . . -177.3(3) n
C8 C1 C2 C3 . . . . 59.0(3) n
C9 C1 C2 C3 . . . . -59.5(4) n
C1 C2 C3 C12 . . . . -176.7(3) n
C1 C2 C3 C4 . . . . 59.4(3) n
C1 C2 C3 C10 . . . . -58.9(4) n
C12 C3 C4 C5 . . . . 177.6(2) n
C2 C3 C4 C5 . . . . -59.3(3) n
C10 C3 C4 C5 . . . . 59.6(3) n
C3 C4 C5 C6 . . . . -60.5(3) n
C3 C4 C5 C9 . . . . 60.2(3) n
C4 C5 C6 C7 . . . . 59.7(4) n
C9 C5 C6 C7 . . . . -61.3(5) n
C5 C6 C7 C8 . . . . 60.7(4) n
C5 C6 C7 C10 . . . . -59.4(5) n
C6 C7 C8 C1 . . . . -59.9(3) n
C10 C7 C8 C1 . . . . 60.5(3) n
C11 C1 C8 C7 . . . . 177.5(2) n
C2 C1 C8 C7 . . . . -59.5(3) n
C9 C1 C8 C7 . . . . 59.2(3) n
C6 C5 C9 C1 . . . . 61.1(3) n
C4 C5 C9 C1 . . . . -60.4(3) n
C11 C1 C9 C5 . . . . 179.3(2) n
C8 C1 C9 C5 . . . . -59.5(3) n
C2 C1 C9 C5 . . . . 59.3(3) n
C8 C7 C10 C3 . . . . -60.1(3) n
C6 C7 C10 C3 . . . . 60.1(4) n
C12 C3 C10 C7 . . . . 179.2(2) n
C2 C3 C10 C7 . . . . 59.2(3) n
C4 C3 C10 C7 . . . . -59.8(3) n
Th1 O1 C11 O2 . . . . 14.4(8) n
Th1 O1 C11 C1 . . . . -169.1(4) n
C8 C1 C11 O2 . . . . -21.4(4) n
C2 C1 C11 O2 . . . . -143.5(3) n
C9 C1 C11 O2 . . . . 97.7(3) n
C8 C1 C11 O1 . . . . 161.9(3) n
C2 C1 C11 O1 . . . . 39.9(4) n
C9 C1 C11 O1 . . . . -79.0(3) n
Th1 O3 C12 O4 1_556 . . . -57.4(5) n
Th1 O3 C12 C3 1_556 . . . 122.6(4) n
C2 C3 C12 O3 . . . . 23.2(4) n
C4 C3 C12 O3 . . . . 145.5(3) n
C10 C3 C12 O3 . . . . -95.9(3) n
C2 C3 C12 O4 . . . . -156.8(3) n
C4 C3 C12 O4 . . . . -34.4(4) n
C10 C3 C12 O4 . . . . 84.2(3) n
