#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:01:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179463 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/60/4336078.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_4336078
loop_
_publ_author_name
'Andrew C. Behrle'
'Charles L. Barnes'
'Nikolas Kaltsoyannis'
'Justin R. Walensky'
_publ_section_title
;
 Systematic Investigation of Thorium(IV)- and Uranium(IV)-Ligand Bonding
 in Dithiophosphonate, Thioselenophosphinate, and Diselenophosphonate
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10623
_journal_page_last               10631
_journal_paper_doi               10.1021/ic401642a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C28 H32 O4 P4 Se8 Th'
_chemical_formula_weight         1420.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1065(4)
_cell_length_b                   19.1065(4)
_cell_length_c                   10.8977(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3978.30(16)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker ApexII CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Incoatec Cu Helios multi-layer optics'
_diffrn_radiation_source         'micro-focus tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0107
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22490
_diffrn_reflns_theta_full        71.74
_diffrn_reflns_theta_max         71.74
_diffrn_reflns_theta_min         4.63
_exptl_absorpt_coefficient_mu    22.248
_exptl_absorpt_correction_T_max  0.4025
_exptl_absorpt_correction_T_min  0.2691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;
_exptl_crystal_density_diffrn    2.371
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.344
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1935
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0238
_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)+(0.0398P)²+18.1903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                1877
_reflns_number_total             1935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401642a_si_002.cif
_cod_data_source_block           u:\walens~2\andrew~1\th_se2~1\selma
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4336078
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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
Th1 Th 0.5000 0.2500 0.3750 0.02407(10) Uani 1 4 d SU
Se1 Se 0.53340(2) 0.32845(2) 0.13934(4) 0.03058(13) Uani 1 1 d U
Se2 Se 0.54027(2) 0.39785(2) 0.43947(4) 0.03220(13) Uani 1 1 d U
P1 P 0.54677(5) 0.42152(5) 0.24659(10) 0.0297(2) Uani 1 1 d U
O1 O 0.61942(16) 0.46027(15) 0.2161(3) 0.0392(7) Uani 1 1 d U
C1 C 0.4838(2) 0.4874(2) 0.2037(4) 0.0336(9) Uani 1 1 d U
C5 C 0.4440(3) 0.6063(2) 0.2053(5) 0.0454(11) Uani 1 1 d U
H5 H 0.4517 0.6531 0.2244 0.055 Uiso 1 1 calc R
C6 C 0.4942(2) 0.5566(2) 0.2357(5) 0.0397(10) Uani 1 1 d U
H6 H 0.5346 0.5699 0.2772 0.048 Uiso 1 1 calc R
C7 C 0.6836(2) 0.4229(3) 0.2393(6) 0.0512(13) Uani 1 1 d U
H7A H 0.6831 0.4049 0.3216 0.077 Uiso 1 1 calc R
H7B H 0.7226 0.4542 0.2297 0.077 Uiso 1 1 calc R
H7C H 0.6879 0.3849 0.1823 0.077 Uiso 1 1 calc R
C4 C 0.3831(3) 0.5869(3) 0.1473(5) 0.0485(12) Uani 1 1 d U
H4 H 0.3493 0.6203 0.1291 0.058 Uiso 1 1 calc R
C2 C 0.4224(3) 0.4679(3) 0.1430(6) 0.0528(14) Uani 1 1 d U
H2 H 0.4153 0.4214 0.1208 0.063 Uiso 1 1 calc R
C3 C 0.3722(3) 0.5179(3) 0.1161(5) 0.0573(15) Uani 1 1 d U
H3 H 0.3310 0.5048 0.0769 0.069 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -4.1491 12.3296 '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
Se2 Th1 Se2 93.121(4) 3_655 12_656
Se2 Th1 Se2 93.121(4) 3_655 10_666
Se2 Th1 Se2 153.011(18) 12_656 10_666
Se2 Th1 Se2 153.012(18) 3_655 .
Se2 Th1 Se2 93.122(4) 12_656 .
Se2 Th1 Se2 93.121(4) 10_666 .
Se2 Th1 Se1 135.484(12) 3_655 .
Se2 Th1 Se1 82.753(12) 12_656 .
Se2 Th1 Se1 74.457(12) 10_666 .
Se2 Th1 Se1 71.400(12) . .
Se2 Th1 Se1 74.457(12) 3_655 10_666
Se2 Th1 Se1 135.485(12) 12_656 10_666
Se2 Th1 Se1 71.399(12) 10_666 10_666
Se2 Th1 Se1 82.754(12) . 10_666
Se1 Th1 Se1 135.486(11) . 10_666
Se2 Th1 Se1 82.754(12) 3_655 12_656
Se2 Th1 Se1 71.399(12) 12_656 12_656
Se2 Th1 Se1 135.485(12) 10_666 12_656
Se2 Th1 Se1 74.458(12) . 12_656
Se1 Th1 Se1 135.486(11) . 12_656
Se1 Th1 Se1 64.777(16) 10_666 12_656
Se2 Th1 Se1 71.399(12) 3_655 3_655
Se2 Th1 Se1 74.457(12) 12_656 3_655
Se2 Th1 Se1 82.753(12) 10_666 3_655
Se2 Th1 Se1 135.485(12) . 3_655
Se1 Th1 Se1 64.776(16) . 3_655
Se1 Th1 Se1 135.485(11) 10_666 3_655
Se1 Th1 Se1 135.485(11) 12_656 3_655
P1 Se1 Th1 88.48(3) . .
P1 Se2 Th1 89.09(3) . .
O1 P1 C1 101.60(18) . .
O1 P1 Se1 111.85(13) . .
C1 P1 Se1 111.00(15) . .
O1 P1 Se2 110.38(13) . .
C1 P1 Se2 111.16(15) . .
Se1 P1 Se2 110.56(5) . .
C7 O1 P1 118.1(3) . .
C6 C1 C2 119.7(4) . .
C6 C1 P1 120.5(3) . .
C2 C1 P1 119.8(4) . .
C4 C5 C6 120.6(5) . .
C1 C6 C5 119.6(4) . .
C5 C4 C3 120.0(5) . .
C3 C2 C1 119.8(5) . .
C4 C3 C2 120.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 Se2 3.0109(4) 3_655
Th1 Se2 3.0109(4) 12_656
Th1 Se2 3.0109(4) 10_666
Th1 Se2 3.0109(4) .
Th1 Se1 3.0413(4) .
Th1 Se1 3.0413(4) 10_666
Th1 Se1 3.0413(4) 12_656
Th1 Se1 3.0413(4) 3_655
Se1 P1 2.1433(11) .
Se2 P1 2.1536(12) .
P1 O1 1.608(3) .
P1 C1 1.803(4) .
O1 C7 1.442(6) .
C1 C6 1.382(6) .
C1 C2 1.397(7) .
C5 C4 1.375(8) .
C5 C6 1.389(7) .
C4 C3 1.377(8) .
C2 C3 1.385(8) .
