#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:00:32 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243998 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/27/7702755.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_7702755
loop_
_publ_author_name
'Abrahams, Brendan F.'
'Coleiro, Joseph'
'Ha, Karen'
'Hoskins, Bernard F.'
'Orchard, Simon D.'
'Robson, Richard'
_publ_section_title
;
 Dihydroxybenzoquinone and chloranilic acid derivatives of rare earth
 metals
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1586
_journal_paper_doi               10.1039/b109296k
_journal_year                    2002
_chemical_formula_sum            'C12 H12 Cl4 O14 Th'
_chemical_formula_weight         754.06
_chemical_name_systematic
; 
diaquabis(chloranilato)thorium(IV) hydrate  
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.231(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.884(1)
_cell_length_b                   11.522(1)
_cell_length_c                   12.720(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      5.8
_cell_volume                     2022.8(3)
_computing_cell_refinement       'CAD4 software'
_computing_data_collection       'CAD4 software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       ω:2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2254
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.972
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELX-76 (Sheldrick, 1976)'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated octahedron'
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.070
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0485
_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)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                1439
_reflns_number_total             1781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109296k.txt
_cod_data_source_block           thcanabs97
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7702755
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
Th Th 0.0000 0.26515(5) 0.2500 0.0236(2) Uani 1 2 d S
Cl1 Cl 0.39767(19) 0.2663(4) 0.3266(2) 0.0526(9) Uani 1 1 d .
O1 O 0.1807(5) 0.2879(7) 0.2986(5) 0.0311(18) Uani 1 1 d .
O2 O 0.0630(5) 0.2976(7) 0.4413(6) 0.041(2) Uani 1 1 d .
C1 C 0.2188(7) 0.2730(10) 0.3906(8) 0.030(3) Uani 1 1 d .
C2 C 0.1495(7) 0.2704(11) 0.4744(8) 0.033(3) Uani 1 1 d .
C3 C 0.3182(7) 0.2552(10) 0.4212(8) 0.031(3) Uani 1 1 d .
Cl2 Cl -0.2002(2) 0.1019(3) 0.5586(3) 0.0532(10) Uani 1 1 d .
O3 O 0.0769(5) 0.0848(7) 0.3316(6) 0.0314(19) Uani 1 1 d .
O4 O -0.0913(5) 0.1640(6) 0.3758(6) 0.0302(18) Uani 1 1 d .
C4 C 0.0438(7) 0.0402(10) 0.4101(9) 0.030(3) Uani 1 1 d .
C5 C -0.0525(8) 0.0874(9) 0.4388(9) 0.028(3) Uani 1 1 d .
C6 C -0.0923(8) 0.0468(10) 0.5229(9) 0.032(3) Uani 1 1 d .
O5 O 0.0716(6) 0.4383(7) 0.1738(7) 0.046(2) Uani 1 1 d .
O6 O 0.2679(7) 0.0376(9) 0.2208(8) 0.069(3) Uani 1 1 d .
O7 O 0.4301(7) 0.0810(11) 0.0755(9) 0.080(3) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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
O4 Th O4 123.0(3) 2 .
O4 Th O5 154.3(3) 2 2
O4 Th O5 82.5(3) . 2
O4 Th O5 82.5(3) 2 .
O4 Th O5 154.3(3) . .
O5 Th O5 72.5(4) 2 .
O4 Th O3 64.0(2) 2 2
O4 Th O3 69.4(2) . 2
O5 Th O3 131.2(3) 2 2
O5 Th O3 132.6(3) . 2
O4 Th O3 69.4(2) 2 .
O4 Th O3 64.0(2) . .
O5 Th O3 132.6(3) 2 .
O5 Th O3 131.2(2) . .
O3 Th O3 68.2(3) 2 .
O4 Th O2 123.5(2) 2 .
O4 Th O2 65.7(3) . .
O5 Th O2 67.3(3) 2 .
O5 Th O2 98.4(3) . .
O3 Th O2 127.5(3) 2 .
O3 Th O2 68.7(2) . .
O4 Th O2 65.7(2) 2 2
O4 Th O2 123.5(2) . 2
O5 Th O2 98.4(3) 2 2
O5 Th O2 67.3(3) . 2
O3 Th O2 68.7(2) 2 2
O3 Th O2 127.5(3) . 2
O2 Th O2 163.0(4) . 2
O4 Th O1 117.4(2) 2 2
O4 Th O1 68.8(2) . 2
O5 Th O1 65.3(2) 2 2
O5 Th O1 104.5(3) . 2
O3 Th O1 67.6(2) 2 2
O3 Th O1 123.6(2) . 2
O2 Th O1 116.8(2) . 2
O2 Th O1 61.2(2) 2 2
O4 Th O1 68.8(2) 2 .
O4 Th O1 117.4(2) . .
O5 Th O1 104.5(3) 2 .
O5 Th O1 65.3(2) . .
O3 Th O1 123.6(2) 2 .
O3 Th O1 67.6(2) . .
O2 Th O1 61.2(2) . .
O2 Th O1 116.8(2) 2 .
O1 Th O1 168.1(3) 2 .
C1 O1 Th 121.6(6) . .
C2 O2 Th 120.1(6) . .
O1 C1 C3 125.7(10) . .
O1 C1 C2 115.4(8) . .
C3 C1 C2 118.8(9) . .
O2 C2 C3 124.5(10) . 7_556
O2 C2 C1 114.4(9) . .
C3 C2 C1 121.1(8) 7_556 .
C2 C3 C1 120.0(9) 7_556 .
C2 C3 Cl1 121.3(7) 7_556 .
C1 C3 Cl1 118.6(7) . .
C4 O3 Th 119.5(7) . .
C5 O4 Th 122.0(6) . .
O3 C4 C6 124.8(10) . 5_556
O3 C4 C5 116.8(10) . .
C6 C4 C5 118.3(10) 5_556 .
O4 C5 C6 124.2(11) . .
O4 C5 C4 114.8(10) . .
C6 C5 C4 121.0(10) . .
C5 C6 C4 120.7(10) . 5_556
C5 C6 Cl2 121.6(9) . .
C4 C6 Cl2 117.6(9) 5_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th O4 2.442(7) 2
Th O4 2.442(7) .
Th O5 2.473(8) 2
Th O5 2.473(8) .
Th O3 2.509(7) 2
Th O3 2.509(7) .
Th O2 2.523(7) .
Th O2 2.523(7) 2
Th O1 2.532(6) 2
Th O1 2.532(6) .
Cl1 C3 1.722(10) .
O1 C1 1.242(11) .
O2 C2 1.268(11) .
C1 C3 1.408(13) .
C1 C2 1.511(14) .
C2 C3 1.386(13) 7_556
C3 C2 1.386(13) 7_556
Cl2 C6 1.732(11) .
O3 C4 1.254(13) .
O4 C5 1.272(12) .
C4 C6 1.436(16) 5_556
C4 C5 1.525(15) .
C5 C6 1.340(16) .
C6 C4 1.436(16) 5_556
