# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_b
_database_code_depnum_ccdc_archive 'CCDC 1421126'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Thorium carboxylate'
_chemical_name_common            Th(TPO)(OH)(H2O)
_chemical_melting_point          N/A
_chemical_formula_moiety         Th(C21H12PO7)(OH)(H2O)9
_chemical_formula_sum            'C21 H12 O17 P Th'
_chemical_formula_weight         799.32

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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.797(2)
_cell_length_b                   12.889(2)
_cell_length_c                   14.037(3)
_cell_angle_alpha                66.065(4)
_cell_angle_beta                 78.731(4)
_cell_angle_gamma                69.924(4)
_cell_volume                     1828.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    8380
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             758
_exptl_absorpt_coefficient_mu    4.180
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   SHELTXPREP

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48307
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         27.56
_reflns_number_total             8380
_reflns_number_gt                7888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       smart
_computing_cell_refinement       'smart saint'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1355P)²+69.5604P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8380
_refine_ls_number_parameters     361
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.2353
_refine_ls_wR_factor_gt          0.2289
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.53975(3) 0.55039(3) 0.60113(3) 0.01684(15) Uani 1 1 d . . .
P1 P 0.7234(2) 0.6557(3) 0.7215(2) 0.0166(5) Uani 1 1 d . . .
O8 O 0.5308(7) 0.3908(7) 0.5662(6) 0.0149(14) Uani 1 1 d . . .
O1 O 0.6658(8) 0.5981(8) 0.6786(6) 0.0228(17) Uani 1 1 d . . .
O9 O 0.7165(9) 0.3653(9) 0.6861(8) 0.034(2) Uani 1 1 d . . .
C1 C 0.6671(11) 0.8141(10) 0.6641(9) 0.021(2) Uani 1 1 d . . .
C8 C 0.8830(10) 0.6107(11) 0.6927(9) 0.022(2) Uani 1 1 d . . .
C2 C 0.5466(11) 0.8704(10) 0.6877(9) 0.024(2) Uani 1 1 d . . .
H2A H 0.4984 0.8261 0.7358 0.029 Uiso 1 1 calc R . .
C17 C 0.6814(13) 0.4983(12) 0.9147(10) 0.029(3) Uani 1 1 d . . .
H17A H 0.6992 0.4457 0.8804 0.034 Uiso 1 1 calc R . .
C16 C 0.6897(10) 0.6132(11) 0.8592(9) 0.021(2) Uani 1 1 d . . .
C6 C 0.7378(12) 0.8793(12) 0.5897(11) 0.031(3) Uani 1 1 d . . .
H6A H 0.8174 0.8416 0.5732 0.038 Uiso 1 1 calc R . .
C21 C 0.6642(13) 0.6921(12) 0.9099(10) 0.029(3) Uani 1 1 d . . .
H21A H 0.6715 0.7682 0.8735 0.035 Uiso 1 1 calc R . .
C9 C 0.9620(13) 0.6462(18) 0.7249(14) 0.046(4) Uani 1 1 d . . .
H9B H 0.9333 0.6918 0.7664 0.055 Uiso 1 1 calc R . .
C13 C 0.9280(12) 0.5379(17) 0.6375(15) 0.046(4) Uani 1 1 d . . .
H13A H 0.8769 0.5070 0.6213 0.055 Uiso 1 1 calc R . .
O2 O 0.4167(8) 1.2450(8) 0.5317(7) 0.0265(18) Uani 1 1 d . . .
O3 O 0.5920(9) 1.2418(8) 0.4425(8) 0.032(2) Uani 1 1 d . . .
C7 C 0.5217(12) 1.1877(11) 0.5103(11) 0.028(3) Uani 1 1 d . . .
C3 C 0.5000(11) 0.9908(11) 0.6396(10) 0.026(2) Uani 1 1 d . . .
H3A H 0.4209 1.0290 0.6569 0.031 Uiso 1 1 calc R . .
C4 C 0.5712(11) 1.0558(11) 0.5650(9) 0.024(2) Uani 1 1 d . . .
C5 C 0.6895(13) 1.0007(12) 0.5398(12) 0.036(3) Uani 1 1 d . . .
H5A H 0.7364 1.0448 0.4895 0.044 Uiso 1 1 calc R . .
C12 C 1.0508(12) 0.5093(18) 0.6049(16) 0.049(5) Uani 1 1 d . . .
H12A H 1.0803 0.4612 0.5657 0.059 Uiso 1 1 calc R . .
C10 C 1.0840(12) 0.6135(17) 0.6950(14) 0.042(4) Uani 1 1 d . . .
H10A H 1.1374 0.6343 0.7197 0.051 Uiso 1 1 calc R . .
C11 C 1.1275(10) 0.5513(10) 0.6301(9) 0.020(2) Uani 1 1 d . . .
C14 C 1.2569(10) 0.5269(10) 0.5880(9) 0.019(2) Uani 1 1 d . . .
O4 O 1.3263(7) 0.5569(8) 0.6221(7) 0.0235(17) Uani 1 1 d . . .
O5 O 1.2825(8) 0.4870(10) 0.5174(7) 0.033(2) Uani 1 1 d U . .
O6 O 0.5705(8) 0.4023(8) 1.2342(7) 0.0253(17) Uani 1 1 d . . .
O7 O 0.5153(9) 0.5888(8) 1.2187(7) 0.0295(19) Uani 1 1 d . . .
C20 C 0.6160(10) 0.5425(11) 1.0699(9) 0.022(2) Uani 1 1 d . . .
C15 C 0.5669(11) 0.5070(11) 1.1823(9) 0.023(2) Uani 1 1 d . . .
C18 C 0.6473(12) 0.4620(12) 1.0196(10) 0.027(2) Uani 1 1 d . . .
H18A H 0.6451 0.3843 1.0568 0.033 Uiso 1 1 calc R . .
C19 C 0.6272(13) 0.6561(12) 1.0163(10) 0.030(3) Uani 1 1 d . . .
H19A H 0.6102 0.7082 1.0511 0.036 Uiso 1 1 calc R . .
O1W O 0.6035(18) 0.7570(13) 1.2445(11) 0.071(5) Uani 1 1 d . . .
O2W O 0.7709(14) 0.2030(13) 0.5924(12) 0.062(4) Uani 1 1 d . . .
O3W O 0.753(2) 0.1945(19) 0.8881(15) 0.102(7) Uani 1 1 d . . .
O4W O 0.493(3) 0.990(2) 1.1054(16) 0.110(8) Uani 1 1 d . . .
O5W O 0.749(3) 0.1888(18) 1.236(2) 0.154(14) Uani 1 1 d . . .
O6W O 1.182(3) 0.207(2) 0.623(3) 0.153(13) Uani 1 1 d . . .
O7W O 0.659(3) 0.111(3) 1.090(2) 0.155(13) Uani 1 1 d . . .
O8W O 0.275(3) 0.963(3) 1.203(2) 0.165(14) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O8 2.339(7) . ?
Th1 O1 2.362(8) . ?
Th1 O8 2.382(7) 2_666 ?
Th1 O5 2.448(8) 2_766 ?
Th1 O4 2.454(8) 1_455 ?
Th1 O3 2.479(9) 2_676 ?
Th1 O7 2.552(9) 2_667 ?
Th1 O9 2.590(10) . ?
Th1 O6 2.614(8) 2_667 ?
Th1 O2 2.695(9) 2_676 ?
Th1 C15 2.948(12) 2_667 ?
Th1 C7 2.974(13) 2_676 ?
P1 O1 1.498(8) . ?
P1 C16 1.784(12) . ?
P1 C8 1.785(12) . ?
P1 C1 1.789(12) . ?
O8 Th1 2.382(7) 2_666 ?
C1 C6 1.386(16) . ?
C1 C2 1.399(16) . ?
C8 C13 1.361(17) . ?
C8 C9 1.380(18) . ?
C2 C3 1.370(17) . ?
C17 C18 1.374(17) . ?
C17 C16 1.394(17) . ?
C16 C21 1.387(17) . ?
C6 C5 1.385(18) . ?
C21 C19 1.400(17) . ?
C9 C10 1.385(17) . ?
C13 C12 1.397(18) . ?
O2 C7 1.256(16) . ?
O2 Th1 2.695(9) 2_676 ?
O3 C7 1.276(16) . ?
O3 Th1 2.479(9) 2_676 ?
C7 C4 1.502(17) . ?
C7 Th1 2.974(13) 2_676 ?
C3 C4 1.390(17) . ?
C4 C5 1.381(18) . ?
C12 C11 1.361(17) . ?
C10 C11 1.366(17) . ?
C11 C14 1.499(15) . ?
C14 O5 1.237(14) . ?
C14 O4 1.252(14) . ?
O4 Th1 2.454(8) 1_655 ?
O5 Th1 2.448(8) 2_766 ?
O6 C15 1.236(16) . ?
O6 Th1 2.614(8) 2_667 ?
O7 C15 1.272(15) . ?
O7 Th1 2.552(9) 2_667 ?
C20 C19 1.388(18) . ?
C20 C18 1.393(16) . ?
C20 C15 1.507(16) . ?
C15 Th1 2.948(11) 2_667 ?

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
O8 Th1 O1 139.9(3) . . ?
O8 Th1 O8 67.0(3) . 2_666 ?
O1 Th1 O8 138.7(3) . 2_666 ?
O8 Th1 O5 75.5(3) . 2_766 ?
O1 Th1 O5 84.6(3) . 2_766 ?
O8 Th1 O5 72.7(3) 2_666 2_766 ?
O8 Th1 O4 72.8(3) . 1_455 ?
O1 Th1 O4 136.5(3) . 1_455 ?
O8 Th1 O4 70.9(3) 2_666 1_455 ?
O5 Th1 O4 138.7(3) 2_766 1_455 ?
O8 Th1 O3 132.3(3) . 2_676 ?
O1 Th1 O3 87.8(3) . 2_676 ?
O8 Th1 O3 73.6(3) 2_666 2_676 ?
O5 Th1 O3 117.3(4) 2_766 2_676 ?
O4 Th1 O3 69.7(3) 1_455 2_676 ?
O8 Th1 O7 77.4(3) . 2_667 ?
O1 Th1 O7 89.4(3) . 2_667 ?
O8 Th1 O7 131.7(3) 2_666 2_667 ?
O5 Th1 O7 128.9(4) 2_766 2_667 ?
O4 Th1 O7 68.0(3) 1_455 2_667 ?
O3 Th1 O7 113.1(3) 2_676 2_667 ?
O8 Th1 O9 71.0(3) . . ?
O1 Th1 O9 69.0(3) . . ?
O8 Th1 O9 126.1(3) 2_666 . ?
O5 Th1 O9 65.1(4) 2_766 . ?
O4 Th1 O9 125.5(3) 1_455 . ?
O3 Th1 O9 156.6(3) 2_676 . ?
O7 Th1 O9 65.4(3) 2_667 . ?
O8 Th1 O6 123.0(3) . 2_667 ?
O1 Th1 O6 68.8(3) . 2_667 ?
O8 Th1 O6 130.6(3) 2_666 2_667 ?
O5 Th1 O6 153.1(3) 2_766 2_667 ?
O4 Th1 O6 68.2(3) 1_455 2_667 ?
O3 Th1 O6 67.0(3) 2_676 2_667 ?
O7 Th1 O6 50.2(3) 2_667 2_667 ?
O9 Th1 O6 100.3(3) . 2_667 ?
O8 Th1 O2 129.5(3) . 2_676 ?
O1 Th1 O2 70.9(3) . 2_676 ?
O8 Th1 O2 68.9(3) 2_666 2_676 ?
O5 Th1 O2 68.9(3) 2_766 2_676 ?
O4 Th1 O2 114.0(3) 1_455 2_676 ?
O3 Th1 O2 50.0(3) 2_676 2_676 ?
O7 Th1 O2 153.0(3) 2_667 2_676 ?
O9 Th1 O2 120.4(3) . 2_676 ?
O6 Th1 O2 104.1(3) 2_667 2_676 ?
O8 Th1 C15 100.5(3) . 2_667 ?
O1 Th1 C15 78.5(3) . 2_667 ?
O8 Th1 C15 136.0(3) 2_666 2_667 ?
O5 Th1 C15 147.8(4) 2_766 2_667 ?
O4 Th1 C15 65.1(3) 1_455 2_667 ?
O3 Th1 C15 89.5(3) 2_676 2_667 ?
O7 Th1 C15 25.5(3) 2_667 2_667 ?
O9 Th1 C15 83.1(3) . 2_667 ?
O6 Th1 C15 24.8(3) 2_667 2_667 ?
O2 Th1 C15 128.6(3) 2_676 2_667 ?
O8 Th1 C7 135.7(3) . 2_676 ?
O1 Th1 C7 78.9(3) . 2_676 ?
O8 Th1 C7 68.7(3) 2_666 2_676 ?
O5 Th1 C7 92.9(4) 2_766 2_676 ?
O4 Th1 C7 91.7(3) 1_455 2_676 ?
O3 Th1 C7 25.0(3) 2_676 2_676 ?
O7 Th1 C7 135.4(3) 2_667 2_676 ?
O9 Th1 C7 142.1(3) . 2_676 ?
O6 Th1 C7 85.8(3) 2_667 2_676 ?
O2 Th1 C7 25.0(3) 2_676 2_676 ?
C15 Th1 C7 110.2(4) 2_667 2_676 ?
O1 P1 C16 110.1(5) . . ?
O1 P1 C8 108.6(5) . . ?
C16 P1 C8 110.4(6) . . ?
O1 P1 C1 110.9(5) . . ?
C16 P1 C1 107.7(6) . . ?
C8 P1 C1 109.1(6) . . ?
Th1 O8 Th1 113.0(3) . 2_666 ?
P1 O1 Th1 166.6(6) . . ?
C6 C1 C2 120.1(11) . . ?
C6 C1 P1 120.5(9) . . ?
C2 C1 P1 119.1(9) . . ?
C13 C8 C9 119.0(11) . . ?
C13 C8 P1 118.4(10) . . ?
C9 C8 P1 122.6(9) . . ?
C3 C2 C1 119.8(11) . . ?
C18 C17 C16 120.7(11) . . ?
C21 C16 C17 120.1(11) . . ?
C21 C16 P1 122.4(9) . . ?
C17 C16 P1 117.4(9) . . ?
C5 C6 C1 119.8(12) . . ?
C16 C21 C19 119.3(12) . . ?
C8 C9 C10 119.7(12) . . ?
C8 C13 C12 120.2(13) . . ?
C7 O2 Th1 90.1(8) . 2_676 ?
C7 O3 Th1 99.8(8) . 2_676 ?
O2 C7 O3 120.1(12) . . ?
O2 C7 C4 122.2(12) . . ?
O3 C7 C4 117.6(11) . . ?
O2 C7 Th1 65.0(7) . 2_676 ?
O3 C7 Th1 55.2(6) . 2_676 ?
C4 C7 Th1 171.8(9) . 2_676 ?
C2 C3 C4 119.8(11) . . ?
C5 C4 C3 120.8(12) . . ?
C5 C4 C7 118.4(11) . . ?
C3 C4 C7 120.9(11) . . ?
C4 C5 C6 119.6(12) . . ?
C11 C12 C13 120.8(13) . . ?
C11 C10 C9 121.2(12) . . ?
C12 C11 C10 118.4(11) . . ?
C12 C11 C14 119.9(11) . . ?
C10 C11 C14 121.7(11) . . ?
O5 C14 O4 126.3(10) . . ?
O5 C14 C11 116.4(10) . . ?
O4 C14 C11 117.1(10) . . ?
C14 O4 Th1 139.2(7) . 1_655 ?
C14 O5 Th1 135.1(7) . 2_766 ?
C15 O6 Th1 92.9(7) . 2_667 ?
C15 O7 Th1 95.0(7) . 2_667 ?
C19 C20 C18 120.3(11) . . ?
C19 C20 C15 119.9(11) . . ?
C18 C20 C15 119.8(11) . . ?
O6 C15 O7 121.8(11) . . ?
O6 C15 C20 120.1(11) . . ?
O7 C15 C20 117.9(11) . . ?
O6 C15 Th1 62.3(6) . 2_667 ?
O7 C15 Th1 59.6(6) . 2_667 ?
C20 C15 Th1 176.9(9) . 2_667 ?
C17 C18 C20 119.5(12) . . ?
C20 C19 C21 119.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         6.978
_refine_diff_density_min         -3.449
_refine_diff_density_rms         0.385
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a
_database_code_depnum_ccdc_archive 'CCDC 1421127'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Thorium Caroboxylate'
_chemical_name_common            Th(TPO)Cl2
_chemical_melting_point          N/A
_chemical_formula_moiety         Th(C21H12PO7)Cl2
_chemical_formula_sum            'C21 H12 Cl2 O7 P Th'
_chemical_formula_weight         710.22
_chemical_absolute_configuration 'unk '

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   21.735(2)
_cell_length_b                   23.205(2)
_cell_length_c                   10.5286(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5310.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    12083
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      27.43

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1332
_exptl_absorpt_coefficient_mu    2.956
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   SHELTXPREP

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34916
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.43
_reflns_number_total             12083
_reflns_number_gt                10319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       smart
_computing_cell_refinement       'smart saint'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1264P)²+8.5658P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.470(14)
_refine_ls_number_reflns         12083
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1956
_refine_ls_wR_factor_gt          0.1810
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.031610(15) 0.282680(16) 1.01490(3) 0.03072(12) Uani 1 1 d . . .
P1 P -0.09407(11) 0.34976(12) 0.8066(2) 0.0299(5) Uani 1 1 d . . .
O1 O -0.0508(3) 0.3158(3) 0.8868(7) 0.0365(17) Uani 1 1 d . . .
C4 C -0.0361(5) 0.3255(5) 0.3936(9) 0.035(2) Uani 1 1 d . . .
C9 C -0.0844(5) 0.4401(5) 0.9748(11) 0.041(2) Uani 1 1 d . . .
H9A H -0.0841 0.4116 1.0370 0.049 Uiso 1 1 calc R . .
C1 C -0.0743(5) 0.3411(5) 0.6416(9) 0.035(2) Uani 1 1 d . . .
C3 C -0.0928(6) 0.3432(6) 0.4177(11) 0.049(3) Uani 1 1 d . . .
H3A H -0.1189 0.3518 0.3503 0.059 Uiso 1 1 calc R . .
C10 C -0.0787(5) 0.4963(5) 1.0077(11) 0.047(3) Uani 1 1 d . . .
H10A H -0.0752 0.5065 1.0929 0.057 Uiso 1 1 calc R . .
C2 C -0.1149(5) 0.3492(6) 0.5436(10) 0.046(3) Uani 1 1 d . . .
H2A H -0.1558 0.3583 0.5593 0.055 Uiso 1 1 calc R . .
C6 C -0.0133(5) 0.3277(8) 0.6150(11) 0.061(4) Uani 1 1 d . . .
H6A H 0.0150 0.3237 0.6806 0.073 Uiso 1 1 calc R . .
C5 C 0.0046(5) 0.3207(8) 0.4936(12) 0.068(4) Uani 1 1 d . . .
H5A H 0.0456 0.3123 0.4766 0.081 Uiso 1 1 calc R . .
C8 C -0.0908(4) 0.4251(5) 0.8460(10) 0.032(2) Uani 1 1 d . . .
C14 C -0.0674(4) 0.6018(5) 0.9513(9) 0.034(2) Uani 1 1 d . . .
C11 C -0.0780(4) 0.5395(5) 0.9131(10) 0.034(2) Uani 1 1 d . . .
O3 O -0.0508(3) 0.6129(3) 1.0625(8) 0.0421(19) Uani 1 1 d . . .
O2 O -0.0735(3) 0.6416(4) 0.8684(7) 0.0424(19) Uani 1 1 d . . .
Cl1 Cl 0.0680(2) 0.2228(2) 0.8020(4) 0.0827(12) Uani 1 1 d . . .
Cl2 Cl -0.04615(17) 0.19135(17) 1.0553(5) 0.0794(13) Uani 1 1 d . . .
O4 O -0.0506(3) 0.3218(4) 0.1674(7) 0.0374(18) Uani 1 1 d . . .
C7 C -0.0158(5) 0.3129(5) 0.2641(10) 0.037(2) Uani 1 1 d . . .
C12 C -0.0875(6) 0.5255(5) 0.7884(11) 0.047(3) Uani 1 1 d . . .
H12A H -0.0903 0.5541 0.7269 0.056 Uiso 1 1 calc R . .
C16 C -0.2217(5) 0.3576(5) 0.8037(12) 0.044(3) Uani 1 1 d . . .
H16A H -0.2162 0.3940 0.7686 0.053 Uiso 1 1 calc R . .
C13 C -0.0930(6) 0.4675(5) 0.7547(11) 0.048(3) Uani 1 1 d . . .
H13A H -0.0983 0.4575 0.6698 0.058 Uiso 1 1 calc R . .
C15 C -0.1708(4) 0.3246(5) 0.8325(10) 0.035(2) Uani 1 1 d . . .
O5 O 0.0388(3) 0.2934(4) 0.2480(6) 0.0447(19) Uani 1 1 d . . .
C18 C -0.2872(5) 0.2827(6) 0.8812(10) 0.039(2) Uani 1 1 d . . .
C17 C -0.2810(5) 0.3375(5) 0.8259(11) 0.044(3) Uani 1 1 d . . .
H17A H -0.3153 0.3595 0.8049 0.053 Uiso 1 1 calc R . .
C21 C -0.3519(5) 0.2601(5) 0.9103(10) 0.038(2) Uani 1 1 d . . .
C19 C -0.2367(5) 0.2519(6) 0.9183(16) 0.054(4) Uani 1 1 d . . .
H19A H -0.2417 0.2176 0.9625 0.065 Uiso 1 1 calc R . .
O6 O -0.3545(3) 0.2101(4) 0.9573(8) 0.0468(19) Uani 1 1 d . . .
O7 O -0.3962(3) 0.2936(4) 0.8992(8) 0.048(2) Uani 1 1 d . . .
C20 C -0.1780(6) 0.2718(6) 0.8901(15) 0.058(4) Uani 1 1 d . . .
H20A H -0.1437 0.2496 0.9101 0.069 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 2.371(7) . ?
Th1 O5 2.472(7) 1_556 ?
Th1 O6 2.499(6) 4_557 ?
Th1 O3 2.509(8) 2_565 ?
Th1 O2 2.509(8) 2_565 ?
Th1 O7 2.532(8) 4_557 ?
Th1 O4 2.568(7) 1_556 ?
Th1 Cl2 2.744(4) . ?
Th1 Cl1 2.754(4) . ?
Th1 C21 2.831(10) 4_557 ?
Th1 C14 2.871(11) 2_565 ?
Th1 C7 2.905(11) 1_556 ?
P1 O1 1.489(8) . ?
P1 C15 1.788(10) . ?
P1 C1 1.801(10) . ?
P1 C8 1.797(11) . ?
C4 C3 1.324(16) . ?
C4 C5 1.379(15) . ?
C4 C7 1.463(14) . ?
C9 C10 1.356(15) . ?
C9 C8 1.407(15) . ?
C1 C2 1.370(14) . ?
C1 C6 1.390(16) . ?
C3 C2 1.416(16) . ?
C10 C11 1.414(16) . ?
C6 C5 1.346(17) . ?
C8 C13 1.378(15) . ?
C14 O3 1.253(12) . ?
C14 O2 1.278(13) . ?
C14 C11 1.517(16) . ?
C14 Th1 2.871(11) 2_565 ?
C11 C12 1.369(15) . ?
O3 Th1 2.509(8) 2_565 ?
O2 Th1 2.509(8) 2_565 ?
O4 C7 1.287(12) . ?
O4 Th1 2.568(7) 1_554 ?
C7 O5 1.281(13) . ?
C7 Th1 2.905(11) 1_554 ?
C12 C13 1.396(16) . ?
C16 C15 1.379(15) . ?
C16 C17 1.391(15) . ?
C15 C20 1.375(17) . ?
O5 Th1 2.472(7) 1_554 ?
C18 C19 1.366(17) . ?
C18 C17 1.406(17) . ?
C18 C21 1.532(14) . ?
C21 O7 1.244(14) . ?
C21 O6 1.262(14) . ?
C21 Th1 2.831(10) 4_457 ?
C19 C20 1.389(16) . ?
O6 Th1 2.499(6) 4_457 ?
O7 Th1 2.532(8) 4_457 ?

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 O5 125.5(2) . 1_556 ?
O1 Th1 O6 142.5(3) . 4_557 ?
O5 Th1 O6 79.3(3) 1_556 4_557 ?
O1 Th1 O3 85.8(3) . 2_565 ?
O5 Th1 O3 72.2(3) 1_556 2_565 ?
O6 Th1 O3 75.4(3) 4_557 2_565 ?
O1 Th1 O2 72.4(2) . 2_565 ?
O5 Th1 O2 121.1(3) 1_556 2_565 ?
O6 Th1 O2 70.4(2) 4_557 2_565 ?
O3 Th1 O2 52.1(3) 2_565 2_565 ?
O1 Th1 O7 153.9(3) . 4_557 ?
O5 Th1 O7 71.1(3) 1_556 4_557 ?
O6 Th1 O7 52.5(3) 4_557 4_557 ?
O3 Th1 O7 120.1(3) 2_565 4_557 ?
O2 Th1 O7 119.0(2) 2_565 4_557 ?
O1 Th1 O4 73.4(2) . 1_556 ?
O5 Th1 O4 52.3(2) 1_556 1_556 ?
O6 Th1 O4 126.4(3) 4_557 1_556 ?
O3 Th1 O4 69.5(2) 2_565 1_556 ?
O2 Th1 O4 112.9(2) 2_565 1_556 ?
O7 Th1 O4 117.1(3) 4_557 1_556 ?
O1 Th1 Cl2 82.7(2) . . ?
O5 Th1 Cl2 87.9(2) 1_556 . ?
O6 Th1 Cl2 130.1(2) 4_557 . ?
O3 Th1 Cl2 144.80(19) 2_565 . ?
O2 Th1 Cl2 149.3(2) 2_565 . ?
O7 Th1 Cl2 77.7(2) 4_557 . ?
O4 Th1 Cl2 75.4(2) 1_556 . ?
O1 Th1 Cl1 85.3(2) . . ?
O5 Th1 Cl1 147.3(2) 1_556 . ?
O6 Th1 Cl1 81.1(2) 4_557 . ?
O3 Th1 Cl1 127.0(2) 2_565 . ?
O2 Th1 Cl1 75.4(2) 2_565 . ?
O7 Th1 Cl1 76.1(2) 4_557 . ?
O4 Th1 Cl1 152.5(2) 1_556 . ?
Cl2 Th1 Cl1 85.02(16) . . ?
O1 Th1 C21 161.4(3) . 4_557 ?
O5 Th1 C21 72.7(3) 1_556 4_557 ?
O6 Th1 C21 26.5(3) 4_557 4_557 ?
O3 Th1 C21 97.7(3) 2_565 4_557 ?
O2 Th1 C21 95.3(3) 2_565 4_557 ?
O7 Th1 C21 26.1(3) 4_557 4_557 ?
O4 Th1 C21 124.9(3) 1_556 4_557 ?
Cl2 Th1 C21 103.7(3) . 4_557 ?
Cl1 Th1 C21 78.1(2) . 4_557 ?
O1 Th1 C14 76.7(3) . 2_565 ?
O5 Th1 C14 96.9(3) 1_556 2_565 ?
O6 Th1 C14 72.3(3) 4_557 2_565 ?
O3 Th1 C14 25.8(3) 2_565 2_565 ?
O2 Th1 C14 26.4(3) 2_565 2_565 ?
O7 Th1 C14 124.6(3) 4_557 2_565 ?
O4 Th1 C14 90.3(3) 1_556 2_565 ?
Cl2 Th1 C14 157.6(2) . 2_565 ?
Cl1 Th1 C14 101.7(2) . 2_565 ?
C21 Th1 C14 98.6(3) 4_557 2_565 ?
O1 Th1 C7 99.7(3) . 1_556 ?
O5 Th1 C7 26.0(3) 1_556 1_556 ?
O6 Th1 C7 103.3(3) 4_557 1_556 ?
O3 Th1 C7 69.2(3) 2_565 1_556 ?
O2 Th1 C7 121.0(3) 2_565 1_556 ?
O7 Th1 C7 93.8(3) 4_557 1_556 ?
O4 Th1 C7 26.3(3) 1_556 1_556 ?
Cl2 Th1 C7 80.1(3) . 1_556 ?
Cl1 Th1 C7 163.5(2) . 1_556 ?
C21 Th1 C7 98.6(3) 4_557 1_556 ?
C14 Th1 C7 94.7(3) 2_565 1_556 ?
O1 P1 C15 109.2(5) . . ?
O1 P1 C1 109.7(5) . . ?
C15 P1 C1 109.5(5) . . ?
O1 P1 C8 111.0(5) . . ?
C15 P1 C8 108.6(5) . . ?
C1 P1 C8 108.8(5) . . ?
P1 O1 Th1 166.2(5) . . ?
C3 C4 C5 118.4(10) . . ?
C3 C4 C7 121.5(10) . . ?
C5 C4 C7 120.1(10) . . ?
C10 C9 C8 119.6(11) . . ?
C2 C1 C6 119.5(9) . . ?
C2 C1 P1 123.9(8) . . ?
C6 C1 P1 116.5(8) . . ?
C4 C3 C2 121.7(9) . . ?
C9 C10 C11 120.3(11) . . ?
C1 C2 C3 118.2(9) . . ?
C5 C6 C1 119.6(10) . . ?
C6 C5 C4 122.0(10) . . ?
C13 C8 C9 119.9(10) . . ?
C13 C8 P1 122.2(8) . . ?
C9 C8 P1 117.9(8) . . ?
O3 C14 O2 121.3(11) . . ?
O3 C14 C11 119.2(10) . . ?
O2 C14 C11 119.5(9) . . ?
O3 C14 Th1 60.7(6) . 2_565 ?
O2 C14 Th1 60.8(6) . 2_565 ?
C11 C14 Th1 172.9(7) . 2_565 ?
C12 C11 C10 120.3(11) . . ?
C12 C11 C14 120.3(10) . . ?
C10 C11 C14 119.4(9) . . ?
C14 O3 Th1 93.5(7) . 2_565 ?
C14 O2 Th1 92.8(6) . 2_565 ?
C7 O4 Th1 91.6(6) . 1_554 ?
O4 C7 O5 119.8(9) . . ?
O4 C7 C4 121.8(9) . . ?
O5 C7 C4 118.3(9) . . ?
O4 C7 Th1 62.1(5) . 1_554 ?
O5 C7 Th1 57.8(5) . 1_554 ?
C4 C7 Th1 175.9(8) . 1_554 ?
C11 C12 C13 119.1(11) . . ?
C15 C16 C17 121.3(11) . . ?
C8 C13 C12 120.6(10) . . ?
C20 C15 C16 120.0(10) . . ?
C20 C15 P1 117.7(9) . . ?
C16 C15 P1 122.2(9) . . ?
C7 O5 Th1 96.2(6) . 1_554 ?
C19 C18 C17 120.9(10) . . ?
C19 C18 C21 120.1(11) . . ?
C17 C18 C21 118.8(10) . . ?
C18 C17 C16 117.5(10) . . ?
O7 C21 O6 125.2(10) . . ?
O7 C21 C18 118.5(10) . . ?
O6 C21 C18 115.7(10) . . ?
O7 C21 Th1 63.4(5) . 4_457 ?
O6 C21 Th1 61.9(5) . 4_457 ?
C18 C21 Th1 175.3(7) . 4_457 ?
C18 C19 C20 120.3(12) . . ?
C21 O6 Th1 91.6(6) . 4_457 ?
C21 O7 Th1 90.5(6) . 4_457 ?
C15 C20 C19 119.6(12) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.341
_refine_diff_density_min         -2.641
_refine_diff_density_rms         0.237
