#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:16:32 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179529 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/26/4342615.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_4342615
loop_
_publ_author_name
'Falaise, Clément'
'Charles, Jean-Sébastien'
'Volkringer, Christophe'
'Loiseau, Thierry'
_publ_section_title
;
 Thorium Terephthalates Coordination Polymers Synthesized in Solvothermal
 DMF/H2O System.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2235
_journal_paper_doi               10.1021/ic502725y
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C22 H22 N2 O10 Th'
_chemical_formula_weight         706.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 101.7130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3843(2)
_cell_length_b                   11.58720(10)
_cell_length_c                   13.4949(2)
_cell_measurement_reflns_used    8633
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.651
_cell_measurement_theta_min      2.217
_cell_volume                     2355.52(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29179
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    6.390
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.512
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0242
_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)+(0.0293P)²+0.3432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                3161
_reflns_number_total             3598
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic502725y_si_002.cif
_cod_data_source_block           cc2c
_cod_database_code               4342615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
O11A O 0.55421(16) 0.36449(19) 0.08265(18) 0.0287(5) Uani 1 1 d .
O12B O 0.47511(17) 0.1753(2) 0.16754(18) 0.0304(5) Uani 1 1 d .
C1B C 0.5000 0.1222(4) 0.2500 0.0269(9) Uani 1 2 d S
C5B C 0.5000 0.7531(4) 0.2500 0.0269(10) Uani 1 2 d S
C6B C 0.5000 0.6245(4) 0.2500 0.0260(9) Uani 1 2 d S
O12A O 0.64539(16) 0.3013(2) 0.21781(17) 0.0336(5) Uani 1 1 d .
C2B C 0.5000 -0.0076(4) 0.2500 0.0286(10) Uani 1 2 d S
O62B O 0.54719(17) 0.57052(19) 0.19933(19) 0.0334(6) Uani 1 1 d .
O1D O 0.37985(16) 0.4186(2) 0.11180(18) 0.0347(6) Uani 1 1 d .
C3B C 0.5187(3) -0.0666(3) 0.1684(3) 0.0342(8) Uani 1 1 d .
H3B H 0.5296 -0.0262 0.1126 0.041 Uiso 1 1 calc R
C4B C 0.5216(3) -0.1866(3) 0.1691(3) 0.0346(8) Uani 1 1 d .
H4B H 0.5378 -0.2264 0.1158 0.042 Uiso 1 1 calc R
C2A C 0.6911(2) 0.2827(3) 0.0600(2) 0.0246(6) Uani 1 1 d .
N1D N 0.2747(2) 0.4183(3) -0.0298(2) 0.0332(6) Uani 1 1 d .
C7A C 0.6706(2) 0.3029(3) -0.0430(3) 0.0297(7) Uani 1 1 d .
H7A H 0.6172 0.3383 -0.0720 0.036 Uiso 1 1 calc R
C1A C 0.6269(2) 0.3184(3) 0.1236(3) 0.0257(6) Uani 1 1 d .
C1D C 0.3577(2) 0.4170(3) 0.0176(3) 0.0300(7) Uani 1 1 d .
H1D H 0.4019 0.4148 -0.0202 0.036 Uiso 1 1 calc R
C3A C 0.7703(2) 0.2297(3) 0.1032(3) 0.0322(8) Uani 1 1 d .
H3A H 0.7839 0.2160 0.1725 0.039 Uiso 1 1 calc R
C2D C 0.2034(3) 0.4219(5) 0.0254(4) 0.0570(13) Uani 1 1 d .
H2D1 H 0.1474 0.4226 -0.0216 0.086 Uiso 1 1 calc R
H2D2 H 0.2088 0.4904 0.0662 0.086 Uiso 1 1 calc R
H2D3 H 0.2066 0.3552 0.0681 0.086 Uiso 1 1 calc R
C3D C 0.2507(3) 0.4230(5) -0.1402(3) 0.0537(12) Uani 1 1 d .
H3D1 H 0.1872 0.4237 -0.1613 0.081 Uiso 1 1 calc R
H3D2 H 0.2743 0.3567 -0.1682 0.081 Uiso 1 1 calc R
H3D3 H 0.2748 0.4918 -0.1637 0.081 Uiso 1 1 calc R
Th1 Th 0.5000 0.371689(12) 0.2500 0.01773(5) 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'
N N 0.0061 0.0033 '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
C1A O11A Th1 92.61(19) . .
C1B O12B Th1 93.4(2) . .
O12B C1B O12B 121.5(4) 2_655 .
O12B C1B C2B 119.2(2) 2_655 .
O12B C1B C2B 119.2(2) . .
O12B C1B Th1 60.8(2) 2_655 .
O12B C1B Th1 60.8(2) . .
C2B C1B Th1 180.0 . .
C4B C5B C4B 119.8(4) 2_665 1_565
C4B C5B C6B 120.1(2) 2_665 .
C4B C5B C6B 120.1(2) 1_565 .
O62B C6B O62B 120.5(4) 2_655 .
O62B C6B C5B 119.8(2) 2_655 .
O62B C6B C5B 119.8(2) . .
O62B C6B Th1 60.2(2) 2_655 .
O62B C6B Th1 60.2(2) . .
C5B C6B Th1 180.000(1) . .
C1A O12A Th1 95.57(19) . .
C3B C2B C3B 120.4(4) 2_655 .
C3B C2B C1B 119.8(2) 2_655 .
C3B C2B C1B 119.8(2) . .
C6B O62B Th1 94.4(2) . .
C1D O1D Th1 142.6(2) . .
C2B C3B C4B 120.2(3) . .
C3B C4B C5B 119.7(3) . 1_545
C7A C2A C3A 120.2(3) . .
C7A C2A C1A 119.2(3) . .
C3A C2A C1A 120.6(3) . .
C1D N1D C2D 121.1(3) . .
C1D N1D C3D 121.3(3) . .
C2D N1D C3D 117.6(3) . .
C2A C7A C3A 119.9(3) . 7_655
O12A C1A O11A 120.5(3) . .
O12A C1A C2A 119.7(3) . .
O11A C1A C2A 119.8(3) . .
O12A C1A Th1 58.87(16) . .
O11A C1A Th1 61.72(16) . .
C2A C1A Th1 176.2(2) . .
O1D C1D N1D 122.4(3) . .
C2A C3A C7A 120.0(3) . 7_655
O1D Th1 O1D 153.89(13) 2_655 .
O1D Th1 O12A 120.83(8) 2_655 2_655
O1D Th1 O12A 68.58(8) . 2_655
O1D Th1 O12A 68.58(8) 2_655 .
O1D Th1 O12A 120.83(8) . .
O12A Th1 O12A 141.94(12) 2_655 .
O1D Th1 O12B 124.64(9) 2_655 .
O1D Th1 O12B 80.69(8) . .
O12A Th1 O12B 73.86(8) 2_655 .
O12A Th1 O12B 72.00(8) . .
O1D Th1 O12B 80.69(8) 2_655 2_655
O1D Th1 O12B 124.64(9) . 2_655
O12A Th1 O12B 72.00(8) 2_655 2_655
O12A Th1 O12B 73.86(8) . 2_655
O12B Th1 O12B 51.64(11) . 2_655
O1D Th1 O62B 78.69(9) 2_655 2_655
O1D Th1 O62B 77.77(9) . 2_655
O12A Th1 O62B 86.25(8) 2_655 2_655
O12A Th1 O62B 130.89(8) . 2_655
O12B Th1 O62B 154.86(9) . 2_655
O12B Th1 O62B 136.14(8) 2_655 2_655
O1D Th1 O62B 77.77(9) 2_655 .
O1D Th1 O62B 78.69(9) . .
O12A Th1 O62B 130.89(8) 2_655 .
O12A Th1 O62B 86.25(8) . .
O12B Th1 O62B 136.14(8) . .
O12B Th1 O62B 154.86(9) 2_655 .
O62B Th1 O62B 50.79(10) 2_655 .
O1D Th1 O11A 110.74(8) 2_655 .
O1D Th1 O11A 70.16(8) . .
O12A Th1 O11A 127.24(8) 2_655 .
O12A Th1 O11A 51.22(7) . .
O12B Th1 O11A 68.29(7) . .
O12B Th1 O11A 108.14(7) 2_655 .
O62B Th1 O11A 115.28(7) 2_655 .
O62B Th1 O11A 68.40(7) . .
O1D Th1 O11A 70.16(8) 2_655 2_655
O1D Th1 O11A 110.74(8) . 2_655
O12A Th1 O11A 51.22(7) 2_655 2_655
O12A Th1 O11A 127.24(8) . 2_655
O12B Th1 O11A 108.14(7) . 2_655
O12B Th1 O11A 68.29(7) 2_655 2_655
O62B Th1 O11A 68.40(7) 2_655 2_655
O62B Th1 O11A 115.28(7) . 2_655
O11A Th1 O11A 176.27(10) . 2_655
O1D Th1 C1B 103.05(7) 2_655 .
O1D Th1 C1B 103.05(7) . .
O12A Th1 C1B 70.97(6) 2_655 .
O12A Th1 C1B 70.97(6) . .
O12B Th1 C1B 25.82(5) . .
O12B Th1 C1B 25.82(5) 2_655 .
O62B Th1 C1B 154.60(5) 2_655 .
O62B Th1 C1B 154.60(5) . .
O11A Th1 C1B 88.14(5) . .
O11A Th1 C1B 88.14(5) 2_655 .
O1D Th1 C1A 90.06(9) 2_655 .
O1D Th1 C1A 95.44(9) . .
O12A Th1 C1A 139.79(9) 2_655 .
O12A Th1 C1A 25.57(8) . .
O12B Th1 C1A 67.07(8) . .
O12B Th1 C1A 90.43(9) 2_655 .
O62B Th1 C1A 127.64(8) 2_655 .
O62B Th1 C1A 76.87(8) . .
O11A Th1 C1A 25.67(8) . .
O11A Th1 C1A 152.56(9) 2_655 .
C1B Th1 C1A 77.75(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O11A C1A 1.261(4) .
O11A Th1 2.563(2) .
O12B C1B 1.262(3) .
O12B Th1 2.528(2) .
C1B O12B 1.262(3) 2_655
C1B C2B 1.503(6) .
C1B Th1 2.891(4) .
C5B C4B 1.392(4) 2_665
C5B C4B 1.392(4) 1_565
C5B C6B 1.490(6) .
C6B O62B 1.260(3) 2_655
C6B O62B 1.260(3) .
C6B Th1 2.930(4) .
O12A C1A 1.261(4) .
O12A Th1 2.500(2) .
C2B C3B 1.376(4) 2_655
C2B C3B 1.376(4) .
O62B Th1 2.550(2) .
O1D C1D 1.247(4) .
O1D Th1 2.406(2) .
C3B C4B 1.392(5) .
C4B C5B 1.392(4) 1_545
C2A C7A 1.381(5) .
C2A C3A 1.382(5) .
C2A C1A 1.494(4) .
N1D C1D 1.308(4) .
N1D C2D 1.447(5) .
N1D C3D 1.461(5) .
C7A C3A 1.390(4) 7_655
C1A Th1 2.907(3) .
C3A C7A 1.390(4) 7_655
Th1 O1D 2.406(2) 2_655
Th1 O12A 2.500(2) 2_655
Th1 O12B 2.528(2) 2_655
Th1 O62B 2.550(2) 2_655
Th1 O11A 2.563(2) 2_655
