#------------------------------------------------------------------------------
#$Date: 2016-12-21 14:01:06 +0200 (Wed, 21 Dec 2016) $
#$Revision: 189301 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/72/4307234.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_4307234
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            'H18 N6 O26 Th2'
_chemical_formula_weight         982.28
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.3800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9256(3)
_cell_length_b                   7.2067(4)
_cell_length_c                   21.5023(11)
_cell_measurement_reflns_used    4037
_cell_measurement_temperature    298
_cell_measurement_theta_max      33.68
_cell_measurement_theta_min      2.98
_cell_volume                     1066.55(9)
_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 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18949
_diffrn_reflns_theta_full        33.68
_diffrn_reflns_theta_max         33.68
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    14.059
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated plate'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0261
_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)+(0.0292P)²+0.6439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                3257
_reflns_number_total             4037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0617691si20060918_012949_3.cif
_cod_data_source_block           p21n
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-21
;
_cod_database_code               4307234
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Th1 Th 0.960168(19) 0.612135(19) 0.082208(6) 0.01532(4) Uani 1 1 d . . . 0
O1 O 1.1412(4) 0.6051(4) -0.00498(14) 0.0209(6) Uani 1 1 d . . . 1
N1 N 1.2436(5) 0.3174(5) 0.13685(17) 0.0224(7) Uani 1 1 d . . . 0
O5 O 1.0645(5) 0.6337(5) 0.19811(15) 0.0306(8) Uani 1 1 d . . . 2
O4 O 1.2018(5) 0.8681(4) 0.09483(17) 0.0303(7) Uani 1 1 d . . . 2
O2 O 0.7096(4) 0.4584(5) 0.13833(14) 0.0247(6) Uani 1 1 d . . . 2
O9 O 0.5993(5) 0.6738(5) 0.04450(15) 0.0281(7) Uani 1 1 d . . . 0
O3 O 0.8227(5) 0.8966(4) 0.13186(17) 0.0331(8) Uani 1 1 d . . . 2
O8 O 0.7942(5) 0.8324(5) -0.00571(15) 0.0274(7) Uani 1 1 d . . . 0
N2 N 0.6197(5) 0.7833(5) -0.00002(17) 0.0226(7) Uani 1 1 d . . . 0
O7 O 1.3012(4) 0.4726(4) 0.11613(14) 0.0242(6) Uani 1 1 d . . . 0
O10 O 0.4843(5) 0.8363(5) -0.03569(17) 0.0363(8) Uani 1 1 d . . . 0
O11 O 1.3559(5) 0.2064(5) 0.16209(16) 0.0324(8) Uani 1 1 d . . . 0
O6 O 1.0619(4) 0.2911(5) 0.12846(15) 0.0276(7) Uani 1 1 d . . . 0
O12 O 1.7247(5) 0.7055(5) 0.26598(16) 0.0358(8) Uani 1 1 d . . . 0
O13 O 1.4394(6) 0.5787(6) 0.25283(19) 0.0423(9) Uani 1 1 d . . . 0
N3 N 1.5550(6) 0.6989(6) 0.23834(19) 0.0300(9) Uani 1 1 d . . . 0
O14 O 1.5044(6) 0.8124(6) 0.19598(19) 0.0424(9) Uiso 1 1 d . . . 0
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 64.28(11) 3_765 . ?
O1 Th1 O2 82.84(10) 3_765 . ?
O1 Th1 O2 146.65(10) . . ?
O1 Th1 O4 136.18(11) 3_765 . ?
O1 Th1 O4 72.14(11) . . ?
O2 Th1 O4 140.98(11) . . ?
O1 Th1 O5 140.84(11) 3_765 . ?
O1 Th1 O5 131.68(10) . . ?
O2 Th1 O5 71.69(11) . . ?
O4 Th1 O5 74.39(12) . . ?
O1 Th1 O3 137.93(11) 3_765 . ?
O1 Th1 O3 127.23(11) . . ?
O2 Th1 O3 80.86(11) . . ?
O4 Th1 O3 68.59(12) . . ?
O5 Th1 O3 67.37(11) . . ?
O1 Th1 O9 71.78(11) 3_765 . ?
O1 Th1 O9 109.54(10) . . ?
O2 Th1 O9 61.59(10) . . ?
O4 Th1 O9 121.58(11) . . ?
O5 Th1 O9 117.48(10) . . ?
O3 Th1 O9 66.32(11) . . ?
O1 Th1 O6 73.79(10) 3_765 . ?
O1 Th1 O6 98.03(10) . . ?
O2 Th1 O6 65.73(10) . . ?
O4 Th1 O6 118.10(11) . . ?
O5 Th1 O6 68.83(11) . . ?
O3 Th1 O6 131.17(11) . . ?
O9 Th1 O6 119.23(10) . . ?
O1 Th1 O7 97.62(10) 3_765 . ?
O1 Th1 O7 70.67(10) . . ?
O2 Th1 O7 110.74(10) . . ?
O4 Th1 O7 71.11(10) . . ?
O5 Th1 O7 66.07(10) . . ?
O3 Th1 O7 124.43(11) . . ?
O9 Th1 O7 167.10(10) . . ?
O6 Th1 O7 49.06(9) . . ?
O1 Th1 O8 79.67(11) 3_765 . ?
O1 Th1 O8 70.85(10) . . ?
O2 Th1 O8 110.18(10) . . ?
O4 Th1 O8 82.29(11) . . ?
O5 Th1 O8 136.62(11) . . ?
O3 Th1 O8 70.22(11) . . ?
O9 Th1 O8 48.69(10) . . ?
O6 Th1 O8 153.44(10) . . ?
O7 Th1 O8 138.27(9) . . ?
O1 Th1 N1 86.36(10) 3_765 . ?
O1 Th1 N1 85.12(10) . . ?
O2 Th1 N1 87.51(10) . . ?
O4 Th1 N1 94.50(11) . . ?
O5 Th1 N1 63.83(10) . . ?
O3 Th1 N1 131.05(11) . . ?
O9 Th1 N1 143.50(10) . . ?
O6 Th1 N1 24.34(9) . . ?
O7 Th1 N1 24.78(9) . . ?
O8 Th1 N1 155.63(10) . . ?
O1 Th1 N2 72.92(10) 3_765 . ?
O1 Th1 N2 89.60(10) . . ?
O2 Th1 N2 85.69(10) . . ?
O4 Th1 N2 103.37(11) . . ?
O5 Th1 N2 131.83(10) . . ?
O3 Th1 N2 67.40(11) . . ?
O9 Th1 N2 24.10(10) . . ?
O6 Th1 N2 138.23(10) . . ?
O7 Th1 N2 160.27(10) . . ?
O8 Th1 N2 24.66(10) . . ?
N1 Th1 N2 158.83(10) . . ?
Th1 O1 Th1 115.72(11) 3_765 . ?
O11 N1 O6 123.2(4) . . ?
O11 N1 O7 121.7(4) . . ?
O6 N1 O7 115.1(3) . . ?
O11 N1 Th1 175.8(3) . . ?
O6 N1 Th1 57.3(2) . . ?
O7 N1 Th1 57.93(19) . . ?
N2 O9 Th1 99.2(2) . . ?
N2 O8 Th1 96.1(2) . . ?
O10 N2 O9 122.5(4) . . ?
O10 N2 O8 121.9(4) . . ?
O9 N2 O8 115.6(3) . . ?
O10 N2 Th1 174.0(3) . . ?
O9 N2 Th1 56.7(2) . . ?
O8 N2 Th1 59.2(2) . . ?
N1 O7 Th1 97.3(2) . . ?
N1 O6 Th1 98.3(2) . . ?
O13 N3 O14 120.3(4) . . ?
O13 N3 O12 120.2(4) . . ?
O14 N3 O12 119.5(4) . . ?
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 2.333(3) 3_765 ?
Th1 O1 2.369(3) . ?
Th1 O2 2.482(3) . ?
Th1 O4 2.485(3) . ?
Th1 O5 2.521(3) . ?
Th1 O3 2.544(3) . ?
Th1 O9 2.579(3) . ?
Th1 O6 2.585(3) . ?
Th1 O7 2.596(3) . ?
Th1 O8 2.633(3) . ?
Th1 N1 3.039(4) . ?
Th1 N2 3.047(4) . ?
O1 Th1 2.333(3) 3_765 ?
N1 O11 1.202(5) . ?
N1 O6 1.266(5) . ?
N1 O7 1.284(5) . ?
O9 N2 1.261(5) . ?
O8 N2 1.278(5) . ?
N2 O10 1.205(5) . ?
O12 N3 1.258(5) . ?
O13 N3 1.243(6) . ?
N3 O14 1.245(6) . ?
