#------------------------------------------------------------------------------
#$Date: 2016-12-21 14:01:06 +0200 (Wed, 21 Dec 2016) $
#$Revision: 189301 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/72/4307233.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_4307233
loop_
_publ_author_name
'Richard E. Wilson'
'S. Skanthakumar'
'Ginger Sigmon'
'Peter C. Burns'
'L. Soderholm'
_publ_contact_author_address
;Chemistry Division 
Argonne National Laboratory
9700 South Cass Avenue
Argonne, Illinois 60302
;
_publ_contact_author_email       ls@anl.gov
_publ_contact_author_name        'L. Soderholm'
_publ_contact_author_phone       630-252-4364
_publ_section_title
;
 Structures of Dimeric Hydrolysis Products of Thorium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2368
_journal_page_last               2372
_journal_paper_doi               10.1021/ic0617691
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'H16 N6 O26 Th2'
_chemical_formula_weight         980.27
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.714(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.792(2)
_cell_length_b                   11.710(4)
_cell_length_c                   13.778(5)
_cell_measurement_reflns_used    2363
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.31
_cell_volume                     1069.0(6)
_computing_cell_refinement       'APEX II, SAINT+ (Bruker, 2004)'
_computing_data_collection       'APEX II (Bruker, 2004)'
_computing_data_reduction        'SAINT+ (Bruker, 2004)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '0.3 wide w/exposures'
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8459
_diffrn_reflns_theta_full        27.29
_diffrn_reflns_theta_max         27.29
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    14.028
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'elongated plate'
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.576
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0357
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                1648
_reflns_number_total             2363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0617691si20060918_012949_2.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-21
;
_cod_original_cell_volume        1068.9(6)
_cod_database_code               4307233
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Th1 Th 0.03890(6) 0.14924(4) 0.43630(3) 0.01993(17) Uani 1 1 d . . . 0
O8 O 0.4392(15) 0.1429(9) 0.5348(7) 0.039(2) Uani 1 1 d . . . 0
O7 O 0.2162(13) 0.1739(8) 0.6214(6) 0.032(2) Uani 1 1 d . . . 0
O3 O 0.1659(15) 0.3492(8) 0.4647(7) 0.037(2) Uani 1 1 d . . . 2
O4 O 0.3126(13) 0.1607(9) 0.3386(6) 0.036(2) Uani 1 1 d . . . 2
O9 O -0.0103(13) 0.0230(8) 0.2702(6) 0.032(2) Uani 1 1 d . . . 0
O10 O -0.2791(13) 0.0721(8) 0.3126(6) 0.036(2) Uani 1 1 d . . . 0
O2 O -0.0524(13) 0.2683(9) 0.2764(6) 0.034(2) Uani 1 1 d . . . 2
O6 O -0.1175(14) 0.2800(9) 0.5628(6) 0.036(2) Uani 1 1 d . . . 0
O5 O -0.2937(13) 0.2630(8) 0.4138(6) 0.032(2) Uani 1 1 d . . . 0
N3 N 0.4046(17) 0.1631(10) 0.6200(7) 0.033(3) Uani 1 1 d . . . 0
O11 O 0.5372(17) 0.1730(11) 0.6937(7) 0.060(3) Uani 1 1 d . . . 0
O1 O 0.1564(12) -0.0381(8) 0.4755(6) 0.0258(18) Uani 1 1 d . . . 1
O12 O -0.3033(14) -0.0325(9) 0.1831(6) 0.040(2) Uani 1 1 d . . . 0
N2 N -0.2721(17) 0.3123(9) 0.4983(7) 0.029(2) Uani 1 1 d . . . 0
O13 O -0.3883(16) 0.3821(11) 0.5157(8) 0.053(3) Uani 1 1 d . . . 0
N1 N -0.2005(15) 0.0185(8) 0.2526(7) 0.023(2) Uiso 1 1 d . . . 0
O14 O 0.2809(14) 0.4502(9) 0.6501(7) 0.042(2) Uiso 1 1 d . . . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
H H 0.0000 0.0000 '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
O1 Th1 O1 64.6(3) . 3_556 ?
O1 Th1 O3 138.5(3) . . ?
O1 Th1 O3 130.3(3) 3_556 . ?
O1 Th1 O4 85.4(3) . . ?
O1 Th1 O4 149.4(3) 3_556 . ?
O3 Th1 O4 76.4(3) . . ?
O1 Th1 O2 135.1(3) . . ?
O1 Th1 O2 132.9(3) 3_556 . ?
O3 Th1 O2 68.6(3) . . ?
O4 Th1 O2 65.2(3) . . ?
O1 Th1 O5 138.7(3) . . ?
O1 Th1 O5 76.8(3) 3_556 . ?
O3 Th1 O5 78.3(3) . . ?
O4 Th1 O5 129.5(3) . . ?
O2 Th1 O5 65.0(3) . . ?
O1 Th1 O7 79.5(3) . . ?
O1 Th1 O7 75.4(3) 3_556 . ?
O3 Th1 O7 70.8(3) . . ?
O4 Th1 O7 106.4(3) . . ?
O2 Th1 O7 139.3(3) . . ?
O5 Th1 O7 105.4(3) . . ?
O1 Th1 O10 91.0(3) . . ?
O1 Th1 O10 70.6(3) 3_556 . ?
O3 Th1 O10 129.6(3) . . ?
O4 Th1 O10 105.8(3) . . ?
O2 Th1 O10 67.5(3) . . ?
O5 Th1 O10 61.4(3) . . ?
O7 Th1 O10 145.5(3) . . ?
O1 Th1 O9 69.8(3) . . ?
O1 Th1 O9 99.0(3) 3_556 . ?
O3 Th1 O9 128.6(3) . . ?
O4 Th1 O9 62.8(3) . . ?
O2 Th1 O9 66.8(3) . . ?
O5 Th1 O9 103.9(3) . . ?
O7 Th1 O9 147.8(3) . . ?
O10 Th1 O9 47.2(3) . . ?
O1 Th1 O6 122.7(3) . . ?
O1 Th1 O6 68.8(3) 3_556 . ?
O3 Th1 O6 62.6(3) . . ?
O4 Th1 O6 138.8(3) . . ?
O2 Th1 O6 101.0(3) . . ?
O5 Th1 O6 47.8(2) . . ?
O7 Th1 O6 57.7(3) . . ?
O10 Th1 O6 103.4(3) . . ?
O9 Th1 O6 150.2(3) . . ?
O1 Th1 O8 67.3(3) . . ?
O1 Th1 O8 109.5(3) 3_556 . ?
O3 Th1 O8 71.3(3) . . ?
O4 Th1 O8 60.2(3) . . ?
O2 Th1 O8 117.6(3) . . ?
O5 Th1 O8 144.5(3) . . ?
O7 Th1 O8 47.4(3) . . ?
O10 Th1 O8 154.0(3) . . ?
O9 Th1 O8 109.2(3) . . ?
O6 Th1 O8 100.5(3) . . ?
O1 Th1 Th1 32.46(19) . 3_556 ?
O1 Th1 Th1 32.2(2) 3_556 3_556 ?
O3 Th1 Th1 145.6(2) . 3_556 ?
O4 Th1 Th1 117.7(2) . 3_556 ?
O2 Th1 Th1 145.3(2) . 3_556 ?
O5 Th1 Th1 107.9(2) . 3_556 ?
O7 Th1 Th1 75.1(2) . 3_556 ?
O10 Th1 Th1 79.2(2) . 3_556 ?
O9 Th1 Th1 83.6(2) . 3_556 ?
O6 Th1 Th1 95.9(2) . 3_556 ?
O8 Th1 Th1 88.4(2) . 3_556 ?
N3 O8 Th1 95.0(7) . . ?
N3 O7 Th1 102.9(6) . . ?
N1 O9 Th1 96.7(6) . . ?
N1 O10 Th1 101.2(7) . . ?
N2 O6 Th1 95.7(7) . . ?
N2 O5 Th1 101.7(7) . . ?
O11 N3 O8 122.7(12) . . ?
O11 N3 O7 122.5(11) . . ?
O8 N3 O7 114.7(10) . . ?
Th1 O1 Th1 115.4(3) . 3_556 ?
O13 N2 O6 122.7(11) . . ?
O13 N2 O5 122.9(11) . . ?
O6 N2 O5 114.4(10) . . ?
O12 N1 O10 121.0(10) . . ?
O12 N1 O9 124.1(10) . . ?
O10 N1 O9 114.9(9) . . ?
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 O1 2.356(9) . ?
Th1 O1 2.375(8) 3_556 ?
Th1 O3 2.496(9) . ?
Th1 O4 2.528(9) . ?
Th1 O2 2.566(9) . ?
Th1 O5 2.581(9) . ?
Th1 O7 2.586(8) . ?
Th1 O10 2.601(9) . ?
Th1 O9 2.683(8) . ?
Th1 O6 2.707(9) . ?
Th1 O8 2.760(10) . ?
Th1 Th1 3.9980(14) 3_556 ?
O8 N3 1.270(14) . ?
O7 N3 1.290(14) . ?
O9 N1 1.262(12) . ?
O10 N1 1.248(12) . ?
O6 N2 1.275(13) . ?
O5 N2 1.278(13) . ?
N3 O11 1.205(13) . ?
O1 Th1 2.375(8) 3_556 ?
O12 N1 1.211(12) . ?
N2 O13 1.197(14) . ?
