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#$Date: 2021-04-30 12:13:07 +0300 (Fri, 30 Apr 2021) $
#$Revision: 264724 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/23/1562323.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_1562323
loop_
_publ_author_name
'Oh, George N.'
'Burns, Peter C.'
_publ_section_title
;
 Solid-state actinide acid phosphites from phosphorous acid melts
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              50
_journal_page_last               56
_journal_paper_doi               10.1016/j.jssc.2014.03.029
_journal_volume                  215
_journal_year                    2014
_chemical_formula_sum            'H8 O12 P4 Th'
_chemical_formula_weight         555.98
_chemical_name_systematic
; 
Alpha-Thorium (IV) tetra(hydrogenphosphanate)  
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.466(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.896(3)
_cell_length_b                   13.631(5)
_cell_length_c                   12.518(5)
_cell_measurement_temperature    296(2)
_cell_volume                     1160.7(8)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'CrystalMaker(R) (Palmer, 2011)'
_computing_publication_material  .
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker QUAZAR'
_diffrn_measurement_method       sphere
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13388
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    13.454
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1016
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0410
_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 
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0395P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                1944
_reflns_number_total             2735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-215-50.cif
_cod_data_source_block           thhp
_cod_original_cell_volume        1160.6(8)
_cod_original_sg_symbol_Hall     '-P 2yac'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1562323
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
Th1 Th 0.63627(5) 0.65303(3) 0.18022(3) 0.01365(12) Uani 1 1 d . . .
P1 P 0.1781(4) 0.6601(2) 0.2943(2) 0.0222(6) Uani 1 1 d . . .
P2 P 0.2787(4) 0.4494(2) 0.0873(2) 0.0203(6) Uani 1 1 d . . .
P3 P 0.7489(5) 0.4210(2) 0.3393(2) 0.0245(6) Uani 1 1 d . . .
P4 P 0.7506(4) 0.7513(2) 0.4595(2) 0.0236(6) Uani 1 1 d . . .
O1 O 0.0715(12) 0.4537(7) 0.1194(7) 0.045(2) Uani 1 1 d . . .
O2 O 0.2388(15) 0.5638(7) 0.3573(8) 0.057(3) Uani 1 1 d . . .
O3 O 0.3561(10) 0.6997(6) 0.2554(6) 0.0273(18) Uani 1 1 d . . .
O4 O 0.3712(11) 0.5492(5) 0.0971(6) 0.0240(17) Uani 1 1 d . . .
O5 O 0.4371(10) 0.7545(5) 0.0391(6) 0.0261(17) Uani 1 1 d . . .
O6 O 0.4974(10) 0.1416(6) 0.2922(6) 0.0257(17) Uani 1 1 d . . .
O7 O 0.5370(15) 0.9360(7) 0.1008(8) 0.058(3) Uani 1 1 d . . .
O8 O 0.5674(12) 0.7409(7) 0.5151(7) 0.046(2) Uani 1 1 d . . .
O9 O 0.7069(11) 0.4938(5) 0.2493(6) 0.0262(18) Uani 1 1 d . . .
O10 O 0.7313(12) 0.3152(5) 0.3067(7) 0.0301(19) Uani 1 1 d . . .
O11 O 0.7398(12) 0.5994(6) 0.0206(6) 0.031(2) Uani 1 1 d . . .
O12 O 0.7427(10) 0.6765(5) 0.3721(6) 0.0229(17) 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
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 '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
O11 Th1 O9 87.3(3) . .
O11 Th1 O3 143.5(3) . .
O9 Th1 O3 103.5(3) . .
O11 Th1 O10 100.4(3) . 2_655
O9 Th1 O10 140.7(3) . 2_655
O3 Th1 O10 93.0(3) . 2_655
O11 Th1 O4 76.4(3) . .
O9 Th1 O4 73.4(3) . .
O3 Th1 O4 73.7(2) . .
O10 Th1 O4 145.9(3) 2_655 .
O11 Th1 O12 143.4(3) . .
O9 Th1 O12 75.3(2) . .
O3 Th1 O12 72.8(2) . .
O10 Th1 O12 76.0(3) 2_655 .
O4 Th1 O12 126.3(2) . .
O11 Th1 O5 77.1(3) . .
O9 Th1 O5 146.5(3) . .
O3 Th1 O5 74.9(3) . .
O10 Th1 O5 72.1(3) 2_655 .
O4 Th1 O5 74.2(2) . .
O12 Th1 O5 132.7(2) . .
O11 Th1 O6 69.9(3) . 2_655
O9 Th1 O6 75.5(3) . 2_655
O3 Th1 O6 146.5(2) . 2_655
O10 Th1 O6 71.4(3) 2_655 2_655
O4 Th1 O6 134.6(2) . 2_655
O12 Th1 O6 74.7(2) . 2_655
O5 Th1 O6 124.3(2) . 2_655
O3 P1 O6 115.6(4) . 2
O3 P1 O2 107.7(5) . .
O6 P1 O2 109.9(5) 2 .
O11 P2 O4 116.7(4) 3_665 .
O11 P2 O1 107.9(5) 3_665 .
O4 P2 O1 110.0(5) . .
O9 P3 O10 116.0(5) . .
O9 P3 O7 109.1(5) . 2_645
O10 P3 O7 106.6(5) . 2_645
O12 P4 O5 112.2(4) . 4_676
O12 P4 O8 109.5(5) . .
O5 P4 O8 111.9(5) 4_676 .
P1 O3 Th1 143.1(5) . .
P2 O4 Th1 148.3(4) . .
P4 O5 Th1 139.7(4) 4_575 .
P1 O6 Th1 139.8(4) 2_545 2_645
P3 O9 Th1 153.1(5) . .
P3 O10 Th1 149.3(5) . 2_645
P2 O11 Th1 156.5(5) 3_665 .
P4 O12 Th1 142.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 O11 2.347(7) .
Th1 O9 2.357(7) .
Th1 O3 2.371(7) .
Th1 O10 2.387(7) 2_655
Th1 O4 2.408(7) .
Th1 O12 2.415(7) .
Th1 O5 2.474(7) .
Th1 O6 2.498(7) 2_655
P1 O3 1.494(8) .
P1 O6 1.507(7) 2
P1 O2 1.552(9) .
P2 O11 1.492(7) 3_665
P2 O4 1.500(7) .
P2 O1 1.548(8) .
P3 O9 1.493(8) .
P3 O10 1.498(8) .
P3 O7 1.555(10) 2_645
P4 O12 1.489(7) .
P4 O5 1.494(7) 4_676
P4 O8 1.545(9) .
O5 P4 1.494(7) 4_575
O6 P1 1.507(7) 2_545
O6 Th1 2.498(7) 2_645
O7 P3 1.555(10) 2_655
O10 Th1 2.387(7) 2_645
O11 P2 1.492(7) 3_665
