#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/04/2100401.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2100401
loop_
_publ_author_name
'M. Helliwell'
'D. Collison'
'G. H. John'
'I. May'
'M. J. Sarsfield'
'C. A. Sharrad'
'A. D. Sutton'
_publ_section_title
;
 Temperature-resolved study of three
 [M(M'O₄)₄(TBPO)₄] complexes (MM' = URe,
 ThRe, ThTc)
;
_journal_coeditor_code           WS5025
_journal_date_accepted           2005-11-09
_journal_date_recd_electronic    2005-02-24
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              68
_journal_page_last               85
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768105036931
_journal_volume                  62
_journal_year                    2006
_chemical_formula_sum            'C48 H108 O20 P4 Re4 Th'
_chemical_formula_weight         2106.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   21.535(3)
_cell_length_b                   21.548(3)
_cell_length_c                   14.7950(19)
_cell_measurement_reflns_used    8488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.67
_cell_volume                     6865.4(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24358
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    9.340
_exptl_absorpt_correction_T_max  0.4552
_exptl_absorpt_correction_T_min  0.2842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4024
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.615
_refine_diff_density_min         -1.343
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0121P)²+76.2392P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                6376
_reflns_number_total             6390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ws5025.cif
_cod_data_source_block           IIat100
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6865.4(15)
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               2100401
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Th1 0.0000 0.25213(3) 0.29653(4) 0.00999(11) Uani d SU 1 . . Th
Re1 0.14695(2) 0.23760(2) 0.12466(3) 0.01727(9) Uani d U 1 . . Re
Re2 0.0000 0.41287(3) 0.44558(4) 0.01414(13) Uani d SU 1 . . Re
Re3 0.0000 0.12284(3) 0.49589(4) 0.01718(14) Uani d SU 1 . . Re
P1 0.16069(13) 0.26198(15) 0.40888(18) 0.0186(6) Uani d U 1 . . P
P2 0.0000 0.3906(2) 0.1422(3) 0.0461(13) Uani d SDU 1 . . P
P3 0.0000 0.0869(2) 0.2075(3) 0.0317(10) Uani d SU 1 . . P
O1 0.0710(4) 0.2456(4) 0.1663(6) 0.0335(16) Uani d U 1 . . O
O2 0.1934(5) 0.2931(5) 0.1709(7) 0.043(2) Uani d U 1 . . O
O3 0.1453(4) 0.2475(4) 0.0100(5) 0.036(2) Uani d U 1 . . O
O4 0.1769(6) 0.1669(4) 0.1490(5) 0.049(3) Uani d U 1 . . O
O5 0.1030(4) 0.2511(4) 0.3523(5) 0.0266(13) Uani d U 1 . . O
O6 0.0000 0.3363(5) 0.4090(7) 0.0165(18) Uani d SU 1 . . O
O7 0.0000 0.4134(6) 0.5634(7) 0.047(4) Uani d SU 1 . . O
O8 0.0636(5) 0.4502(4) 0.4112(7) 0.040(2) Uani d U 1 . . O
O9 0.0000 0.3452(6) 0.2221(9) 0.047(2) Uani d SU 1 A . O
O10 0.0000 0.1944(5) 0.4394(8) 0.0204(18) Uani d SU 1 . . O
O11 0.0619(7) 0.0806(5) 0.4699(7) 0.067(4) Uani d U 1 . . O
O12 0.0000 0.1341(5) 0.6090(7) 0.035(3) Uani d SU 1 . . O
O13 0.0000 0.1500(5) 0.2530(8) 0.033(2) Uani d SU 1 . . O
C1 0.1482(5) 0.2474(5) 0.5266(7) 0.021(2) Uani d DU 1 . . C
H1A 0.1343 0.2038 0.5336 0.025 Uiso calc R 1 . . H
H1B 0.1885 0.2514 0.5583 0.025 Uiso calc R 1 . . H
C2 0.1009(5) 0.2895(5) 0.5740(7) 0.024(2) Uani d DU 1 . . C
H2A 0.0613 0.2886 0.5400 0.029 Uiso calc R 1 . . H
H2B 0.1165 0.3327 0.5735 0.029 Uiso calc R 1 . . H
C3 0.0889(5) 0.2694(6) 0.6720(7) 0.025(2) Uani d DU 1 . . C
H3A 0.0561 0.2963 0.6979 0.030 Uiso calc R 1 . . H
H3B 0.0730 0.2263 0.6720 0.030 Uiso calc R 1 . . H
C4 0.1460(6) 0.2726(6) 0.7325(8) 0.029(3) Uani d DU 1 . . C
H4A 0.1774 0.2434 0.7105 0.043 Uiso calc R 1 . . H
H4B 0.1344 0.2617 0.7945 0.043 Uiso calc R 1 . . H
H4C 0.1629 0.3148 0.7314 0.043 Uiso calc R 1 . . H
C5 0.1837(5) 0.3397(5) 0.3959(8) 0.025(2) Uani d DU 1 . . C
H5A 0.1917 0.3471 0.3308 0.030 Uiso calc R 1 . . H
H5B 0.1483 0.3664 0.4134 0.030 Uiso calc R 1 . . H
C6 0.2416(5) 0.3618(4) 0.4493(8) 0.0263(19) Uani d DU 1 . . C
H6A 0.2348 0.3546 0.5146 0.032 Uiso calc R 1 . . H
H6B 0.2781 0.3370 0.4305 0.032 Uiso calc R 1 . . H
C7 0.2550(6) 0.4299(5) 0.4337(10) 0.037(3) Uani d DU 1 . . C
H7A 0.2190 0.4549 0.4537 0.044 Uiso calc R 1 . . H
H7B 0.2612 0.4374 0.3683 0.044 Uiso calc R 1 . . H
C8 0.3131(7) 0.4506(6) 0.4854(11) 0.054(4) Uani d DU 1 . . C
H8A 0.3133 0.4959 0.4906 0.081 Uiso calc R 1 . . H
H8B 0.3503 0.4370 0.4528 0.081 Uiso calc R 1 . . H
H8C 0.3128 0.4321 0.5460 0.081 Uiso calc R 1 . . H
C9 0.2192(5) 0.2102(4) 0.3757(7) 0.0177(17) Uani d DU 1 . . C
H9A 0.2306 0.2195 0.3122 0.021 Uiso calc R 1 . . H
H9B 0.2564 0.2181 0.4133 0.021 Uiso calc R 1 . . H
C10 0.2032(5) 0.1419(5) 0.3824(8) 0.021(2) Uani d DU 1 . . C
H10A 0.1934 0.1322 0.4462 0.026 Uiso calc R 1 . . H
H10B 0.1651 0.1342 0.3465 0.026 Uiso calc R 1 . . H
C11 0.2531(5) 0.0978(5) 0.3505(8) 0.024(2) Uani d DU 1 . . C
H11A 0.2356 0.0554 0.3459 0.029 Uiso calc R 1 . . H
H11B 0.2673 0.1104 0.2896 0.029 Uiso calc R 1 . . H
C12 0.3073(6) 0.0971(5) 0.4138(9) 0.033(3) Uani d DU 1 . . C
H12A 0.3312 0.1355 0.4066 0.050 Uiso calc R 1 . . H
H12B 0.3339 0.0614 0.4001 0.050 Uiso calc R 1 . . H
H12C 0.2923 0.0940 0.4762 0.050 Uiso calc R 1 . . H
C13A -0.0531(12) 0.4509(10) 0.1595(18) 0.051(2) Uani d PDU 0.491(15) A 1 C
H13A -0.0297 0.4833 0.1926 0.061 Uiso calc PR 0.491(15) A 1 H
H13B -0.0613 0.4683 0.0987 0.061 Uiso calc PR 0.491(15) A 1 H
C14A -0.1158(12) 0.4479(12) 0.2051(18) 0.050(2) Uani d PDU 0.491(15) A 1 C
H14A -0.1309 0.4050 0.1956 0.060 Uiso calc PR 0.491(15) A 1 H
H14B -0.1074 0.4518 0.2707 0.060 Uiso calc PR 0.491(15) A 1 H
C15A -0.1700(13) 0.4891(12) 0.187(2) 0.049(2) Uani d PDU 0.491(15) A 1 C
H15A -0.1933 0.4948 0.2437 0.059 Uiso calc PR 0.491(15) A 1 H
H15B -0.1979 0.4676 0.1436 0.059 Uiso calc PR 0.491(15) A 1 H
C16A -0.1548(18) 0.5531(12) 0.148(2) 0.046(4) Uani d PDU 0.491(15) A 1 C
H16A -0.1265 0.5748 0.1893 0.069 Uiso calc PR 0.491(15) A 1 H
H16B -0.1932 0.5771 0.1418 0.069 Uiso calc PR 0.491(15) A 1 H
H16C -0.1351 0.5484 0.0889 0.069 Uiso calc PR 0.491(15) A 1 H
C13B -0.0725(9) 0.4303(10) 0.1138(16) 0.051(2) Uani d PDU 0.509(15) A 2 C
H13C -0.0643 0.4755 0.1127 0.061 Uiso calc PR 0.509(15) A 2 H
H13D -0.0845 0.4178 0.0518 0.061 Uiso calc PR 0.509(15) A 2 H
C14B -0.1235(13) 0.4196(10) 0.1712(17) 0.050(2) Uani d PDU 0.509(15) A 2 C
H14C -0.1075 0.3984 0.2258 0.060 Uiso calc PR 0.509(15) A 2 H
H14D -0.1512 0.3898 0.1401 0.060 Uiso calc PR 0.509(15) A 2 H
C15B -0.1633(16) 0.4732(11) 0.2028(17) 0.049(2) Uani d PDU 0.509(15) A 2 C
H15C -0.1465 0.4880 0.2613 0.059 Uiso calc PR 0.509(15) A 2 H
H15D -0.2056 0.4573 0.2143 0.059 Uiso calc PR 0.509(15) A 2 H
C16B -0.1684(18) 0.5288(11) 0.1394(19) 0.046(4) Uani d PDU 0.509(15) A 2 C
H16D -0.1392 0.5611 0.1585 0.069 Uiso calc PR 0.509(15) A 2 H
H16E -0.2108 0.5453 0.1415 0.069 Uiso calc PR 0.509(15) A 2 H
H16F -0.1586 0.5158 0.0776 0.069 Uiso calc PR 0.509(15) A 2 H
C17 0.0000 0.3542(9) 0.0371(10) 0.039(3) Uani d SDU 1 A . C
H17A 0.0370 0.3270 0.0339 0.046 Uiso calc PR 0.50 . . H
H17B -0.0370 0.3270 0.0339 0.046 Uiso calc PR 0.50 . . H
C18 0.0000 0.3959(7) -0.0458(9) 0.038(3) Uani d SDU 1 . . C
H18A -0.0372 0.4229 -0.0440 0.046 Uiso calc PR 0.50 A . H
H18B 0.0372 0.4229 -0.0440 0.046 Uiso calc PR 0.50 . . H
C19 0.0000 0.3596(8) -0.1333(10) 0.048(4) Uani d SDU 1 A . C
H19A -0.0372 0.3327 -0.1357 0.058 Uiso calc PR 0.50 . . H
H19B 0.0372 0.3327 -0.1357 0.058 Uiso calc PR 0.50 . . H
C20 0.0000 0.4039(9) -0.2157(11) 0.061(6) Uani d SDU 1 . . C
H20A 0.0000 0.3795 -0.2716 0.092 Uiso calc SR 1 A . H
H20B 0.0372 0.4302 -0.2138 0.092 Uiso calc PR 0.50 . . H
H20C -0.0372 0.4302 -0.2138 0.092 Uiso calc PR 0.50 . . H
C21 -0.0694(7) 0.0472(6) 0.2409(10) 0.046(3) Uani d DU 1 . . C
H21A -0.0663 0.0382 0.3064 0.055 Uiso calc R 1 . . H
H21B -0.1047 0.0760 0.2326 0.055 Uiso calc R 1 . . H
C22 -0.0851(6) -0.0134(6) 0.1925(11) 0.054(3) Uani d DU 1 . . C
H22A -0.0864 -0.0059 0.1265 0.065 Uiso calc R 1 . . H
H22B -0.0521 -0.0442 0.2046 0.065 Uiso calc R 1 . . H
C23 -0.1467(6) -0.0391(7) 0.2232(12) 0.063(4) Uani d DU 1 . . C
H23A -0.1791 -0.0071 0.2140 0.076 Uiso calc R 1 . . H
H23B -0.1444 -0.0479 0.2888 0.076 Uiso calc R 1 . . H
C24 -0.1661(7) -0.0979(7) 0.1742(13) 0.065(5) Uani d DU 1 . . C
H24A -0.2090 -0.1083 0.1905 0.097 Uiso calc R 1 . . H
H24B -0.1386 -0.1321 0.1918 0.097 Uiso calc R 1 . . H
H24C -0.1633 -0.0914 0.1088 0.097 Uiso calc R 1 . . H
C25 -0.0307(13) 0.0904(11) 0.0910(13) 0.038(4) Uani d PDU 0.50 . . C
H25A -0.0270 0.0486 0.0638 0.046 Uiso calc PR 0.50 . . H
H25B -0.0755 0.1005 0.0942 0.046 Uiso calc PR 0.50 . . H
C26 0.0000 0.1361(9) 0.0287(9) 0.049(4) Uani d SDU 1 . . C
H26A -0.0201 0.1769 0.0382 0.059 Uiso calc PR 0.50 . . H
H26B 0.0438 0.1404 0.0482 0.059 Uiso calc PR 0.50 . . H
C27 0.0000 0.1233(9) -0.0709(9) 0.053(4) Uani d SDU 1 . . C
H27A -0.0371 0.0980 -0.0854 0.064 Uiso calc PR 0.50 . . H
H27B 0.0371 0.0980 -0.0854 0.064 Uiso calc PR 0.50 . . H
C28 0.0000 0.1796(12) -0.1317(16) 0.099(8) Uani d SDU 1 . . C
H28A 0.0000 0.1662 -0.1950 0.148 Uiso calc SR 1 . . H
H28B 0.0372 0.2045 -0.1197 0.148 Uiso calc PR 0.50 . . H
H28C -0.0372 0.2045 -0.1197 0.148 Uiso calc PR 0.50 . . H
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'
Re Re -1.0185 7.2310 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O9 Th1 O13 . . 134.9(5)
O9 Th1 O5 . . 100.1(2)
O13 Th1 O5 . . 95.1(2)
O9 Th1 O5 . 4 100.2(2)
O13 Th1 O5 . 4 95.1(2)
O5 Th1 O5 . 4 139.2(4)
O9 Th1 O10 . . 149.3(4)
O13 Th1 O10 . . 75.8(4)
O5 Th1 O10 . . 72.2(2)
O5 Th1 O10 4 . 72.2(2)
O9 Th1 O6 . . 71.3(4)
O13 Th1 O6 . . 153.8(4)
O5 Th1 O6 . . 76.8(2)
O5 Th1 O6 4 . 76.8(2)
O10 Th1 O6 . . 78.0(3)
O9 Th1 O1 . 4 70.9(3)
O13 Th1 O1 . 4 74.1(3)
O5 Th1 O1 . 4 148.6(3)
O5 Th1 O1 4 4 72.0(3)
O10 Th1 O1 . 4 130.2(3)
O6 Th1 O1 . 4 124.8(3)
O9 Th1 O1 . . 70.9(3)
O13 Th1 O1 . . 74.1(3)
O5 Th1 O1 . . 72.0(3)
O5 Th1 O1 4 . 148.6(3)
O10 Th1 O1 . . 130.2(3)
O6 Th1 O1 . . 124.8(3)
O1 Th1 O1 4 . 76.7(4)
O4 Re1 O2 . . 108.8(5)
O4 Re1 O3 . . 109.4(4)
O2 Re1 O3 . . 108.8(4)
O4 Re1 O1 . . 111.6(5)
O2 Re1 O1 . . 109.7(5)
O3 Re1 O1 . . 108.4(4)
O8 Re2 O8 . 4 110.5(7)
O8 Re2 O6 . . 111.3(4)
O8 Re2 O6 4 . 111.3(4)
O8 Re2 O7 . . 107.6(4)
O8 Re2 O7 4 . 107.6(4)
O6 Re2 O7 . . 108.5(5)
O11 Re3 O11 4 . 106.9(11)
O11 Re3 O12 4 . 107.9(4)
O11 Re3 O12 . . 107.9(4)
O11 Re3 O10 4 . 111.8(4)
O11 Re3 O10 . . 111.8(4)
O12 Re3 O10 . . 110.2(5)
O5 P1 C9 . . 109.6(5)
O5 P1 C5 . . 108.6(5)
C9 P1 C5 . . 111.9(5)
O5 P1 C1 . . 112.8(5)
C9 P1 C1 . . 105.6(5)
C5 P1 C1 . . 108.5(5)
O9 P2 C17 . . 113.5(8)
O9 P2 C13A . 4 111.2(10)
C17 P2 C13A . 4 117.7(10)
O9 P2 C13A . . 111.2(10)
C17 P2 C13A . . 117.7(10)
C13A P2 C13A 4 . 82(2)
O9 P2 C13B . 4 118.4(8)
C17 P2 C13B . 4 90.3(9)
C13A P2 C13B 4 4 29.4(10)
C13A P2 C13B . 4 104.2(13)
O9 P2 C13B . . 118.4(8)
C17 P2 C13B . . 90.3(9)
C13A P2 C13B 4 . 104.2(13)
C13A P2 C13B . . 29.4(10)
C13B P2 C13B 4 . 117.3(15)
O13 P3 C21 . 4 107.8(4)
O13 P3 C21 . . 107.8(4)
C21 P3 C21 4 . 113.1(11)
O13 P3 C25 . . 112.2(9)
C21 P3 C25 4 . 125.1(10)
C21 P3 C25 . . 88.8(9)
O13 P3 C25 . 4 112.2(9)
C21 P3 C25 4 4 88.8(9)
C21 P3 C25 . 4 125.1(10)
C25 P3 C25 . 4 41.9(17)
Re1 O1 Th1 . . 149.1(5)
P1 O5 Th1 . . 163.5(5)
Re2 O6 Th1 . . 155.6(6)
P2 O9 Th1 . . 158.4(9)
Re3 O10 Th1 . . 148.9(6)
P3 O13 Th1 . . 170.0(7)
C2 C1 P1 . . 116.1(8)
C2 C1 H1A . . 108.3
P1 C1 H1A . . 108.3
C2 C1 H1B . . 108.3
P1 C1 H1B . . 108.3
H1A C1 H1B . . 107.4
C1 C2 C3 . . 112.2(9)
C1 C2 H2A . . 109.2
C3 C2 H2A . . 109.2
C1 C2 H2B . . 109.2
C3 C2 H2B . . 109.2
H2A C2 H2B . . 107.9
C4 C3 C2 . . 113.9(10)
C4 C3 H3A . . 108.8
C2 C3 H3A . . 108.8
C4 C3 H3B . . 108.8
C2 C3 H3B . . 108.8
H3A C3 H3B . . 107.7
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C6 C5 P1 . . 117.6(8)
C6 C5 H5A . . 107.9
P1 C5 H5A . . 107.9
C6 C5 H5B . . 107.9
P1 C5 H5B . . 107.9
H5A C5 H5B . . 107.2
C7 C6 C5 . . 111.9(9)
C7 C6 H6A . . 109.2
C5 C6 H6A . . 109.2
C7 C6 H6B . . 109.2
C5 C6 H6B . . 109.2
H6A C6 H6B . . 107.9
C6 C7 C8 . . 111.2(10)
C6 C7 H7A . . 109.4
C8 C7 H7A . . 109.4
C6 C7 H7B . . 109.4
C8 C7 H7B . . 109.4
H7A C7 H7B . . 108.0
C7 C8 H8A . . 109.5
C7 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C7 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
C10 C9 P1 . . 115.8(8)
C10 C9 H9A . . 108.3
P1 C9 H9A . . 108.3
C10 C9 H9B . . 108.3
P1 C9 H9B . . 108.3
H9A C9 H9B . . 107.4
C11 C10 C9 . . 115.4(9)
C11 C10 H10A . . 108.4
C9 C10 H10A . . 108.4
C11 C10 H10B . . 108.4
C9 C10 H10B . . 108.4
H10A C10 H10B . . 107.5
C12 C11 C10 . . 111.4(9)
C12 C11 H11A . . 109.3
C10 C11 H11A . . 109.3
C12 C11 H11B . . 109.3
C10 C11 H11B . . 109.3
H11A C11 H11B . . 108.0
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
C14A C13A P2 . . 128.1(18)
C14A C13A H13A . . 105.3
P2 C13A H13A . . 105.3
C14A C13A H13B . . 105.3
P2 C13A H13B . . 105.3
H13A C13A H13B . . 106.0
C15A C14A C13A . . 126.3(19)
C15A C14A H14A . . 105.7
C13A C14A H14A . . 105.8
C15A C14A H14B . . 105.8
C13A C14A H14B . . 105.8
H14A C14A H14B . . 106.2
C14A C15A C16A . . 116(2)
C14A C15A H15A . . 108.3
C16A C15A H15A . . 108.3
C14A C15A H15B . . 108.3
C16A C15A H15B . . 108.3
H15A C15A H15B . . 107.4
C15A C16A H16A . . 109.5
C15A C16A H16B . . 109.5
H16A C16A H16B . . 109.5
C15A C16A H16C . . 109.5
H16A C16A H16C . . 109.5
H16B C16A H16C . . 109.5
C14B C13B P2 . . 116.9(17)
C14B C13B H13C . . 108.1
P2 C13B H13C . . 108.1
C14B C13B H13D . . 108.1
P2 C13B H13D . . 108.1
H13C C13B H13D . . 107.3
C13B C14B C15B . . 120.3(19)
C13B C14B H14C . . 107.2
C15B C14B H14C . . 107.2
C13B C14B H14D . . 107.3
C15B C14B H14D . . 107.3
H14C C14B H14D . . 106.9
C14B C15B C16B . . 116.8(19)
C14B C15B H15C . . 108.1
C16B C15B H15C . . 108.1
C14B C15B H15D . . 108.1
C16B C15B H15D . . 108.1
H15C C15B H15D . . 107.3
C15B C16B H16D . . 109.5
C15B C16B H16E . . 109.5
H16D C16B H16E . . 109.5
C15B C16B H16F . . 109.5
H16D C16B H16F . . 109.5
H16E C16B H16F . . 109.5
C18 C17 P2 . . 117.0(13)
C18 C17 H17A . . 108.1
P2 C17 H17A . . 108.1
C18 C17 H17B . . 108.1
P2 C17 H17B . . 108.1
H17A C17 H17B . . 107.3
C19 C18 C17 . . 112.6(12)
C19 C18 H18A . . 109.1
C17 C18 H18A . . 109.1
C19 C18 H18B . . 109.1
C17 C18 H18B . . 109.1
H18A C18 H18B . . 107.8
C18 C19 C20 . . 110.8(14)
C18 C19 H19A . . 109.5
C20 C19 H19A . . 109.5
C18 C19 H19B . . 109.5
C20 C19 H19B . . 109.5
H19A C19 H19B . . 108.1
C19 C20 H20A . . 109.5
C19 C20 H20B . . 109.5
H20A C20 H20B . . 109.5
C19 C20 H20C . . 109.5
H20A C20 H20C . . 109.5
H20B C20 H20C . . 109.5
C22 C21 P3 . . 117.6(9)
C22 C21 H21A . . 107.9
P3 C21 H21A . . 107.9
C22 C21 H21B . . 107.9
P3 C21 H21B . . 107.9
H21A C21 H21B . . 107.2
C23 C22 C21 . . 111.6(10)
C23 C22 H22A . . 109.3
C21 C22 H22A . . 109.3
C23 C22 H22B . . 109.3
C21 C22 H22B . . 109.3
H22A C22 H22B . . 108.0
C22 C23 C24 . . 114.0(11)
C22 C23 H23A . . 108.8
C24 C23 H23A . . 108.8
C22 C23 H23B . . 108.8
C24 C23 H23B . . 108.8
H23A C23 H23B . . 107.7
C23 C24 H24A . . 109.5
C23 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C23 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
C26 C25 P3 . . 116.2(15)
C26 C25 H25A . . 108.2
P3 C25 H25A . . 108.2
C26 C25 H25B . . 108.2
P3 C25 H25B . . 108.2
H25A C25 H25B . . 107.4
C27 C26 C25 . . 118.8(15)
C27 C26 H26A . . 107.6
C25 C26 H26A . . 107.6
C27 C26 H26B . . 107.6
C25 C26 H26B . . 107.6
H26A C26 H26B . . 107.0
C26 C27 C28 . . 116.0(16)
C26 C27 H27A . . 108.3
C28 C27 H27A . . 108.3
C26 C27 H27B . . 108.3
C28 C27 H27B . . 108.3
H27A C27 H27B . . 107.4
C27 C28 H28A . . 109.5
C27 C28 H28B . . 109.5
H28A C28 H28B . . 109.5
C27 C28 H28C . . 109.5
H28A C28 H28C . . 109.5
H28B C28 H28C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Th1 O9 . 2.287(12)
Th1 O13 . 2.293(11)
Th1 O5 . 2.368(8)
Th1 O5 4 2.368(8)
Th1 O10 . 2.454(11)
Th1 O6 . 2.461(11)
Th1 O1 4 2.464(8)
Th1 O1 . 2.464(8)
Re1 O4 . 1.693(9)
Re1 O2 . 1.703(9)
Re1 O3 . 1.711(8)
Re1 O1 . 1.756(9)
Re2 O8 . 1.668(9)
Re2 O8 4 1.668(9)
Re2 O6 . 1.737(11)
Re2 O7 . 1.743(11)
Re3 O11 4 1.660(11)
Re3 O11 . 1.660(11)
Re3 O12 . 1.691(10)
Re3 O10 . 1.753(10)
P1 O5 . 1.515(8)
P1 C9 . 1.754(11)
P1 C5 . 1.758(12)
P1 C1 . 1.791(10)
P2 O9 . 1.535(12)
P2 C17 . 1.742(17)
P2 C13A 4 1.749(16)
P2 C13A . 1.750(16)
P2 C13B 4 1.828(17)
P2 C13B . 1.828(17)
P3 O13 . 1.518(12)
P3 C21 4 1.791(14)
P3 C21 . 1.792(14)
P3 C25 . 1.85(2)
P3 C25 4 1.85(2)
C1 C2 . 1.533(12)
C1 H1A . 0.9900
C1 H1B . 0.9900
C2 C3 . 1.536(12)
C2 H2A . 0.9900
C2 H2B . 0.9900
C3 C4 . 1.522(13)
C3 H3A . 0.9900
C3 H3B . 0.9900
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
C5 C6 . 1.551(12)
C5 H5A . 0.9900
C5 H5B . 0.9900
C6 C7 . 1.514(12)
C6 H6A . 0.9900
C6 H6B . 0.9900
C7 C8 . 1.531(14)
C7 H7A . 0.9900
C7 H7B . 0.9900
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 0.9800
C9 C10 . 1.515(12)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 C11 . 1.511(13)
C10 H10A . 0.9900
C10 H10B . 0.9900
C11 C12 . 1.498(13)
C11 H11A . 0.9900
C11 H11B . 0.9900
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C13A C14A . 1.510(18)
C13A H13A . 0.9900
C13A H13B . 0.9900
C14A C15A . 1.492(18)
C14A H14A . 0.9900
C14A H14B . 0.9900
C15A C16A . 1.526(18)
C15A H15A . 0.9900
C15A H15B . 0.9900
C16A H16A . 0.9800
C16A H16B . 0.9800
C16A H16C . 0.9800
C13B C14B . 1.406(18)
C13B H13C . 0.9900
C13B H13D . 0.9900
C14B C15B . 1.512(18)
C14B H14C . 0.9900
C14B H14D . 0.9900
C15B C16B . 1.525(17)
C15B H15C . 0.9900
C15B H15D . 0.9900
C16B H16D . 0.9800
C16B H16E . 0.9800
C16B H16F . 0.9800
C17 C18 . 1.521(15)
C17 H17A . 0.9900
C17 H17B . 0.9900
C18 C19 . 1.513(15)
C18 H18A . 0.9900
C18 H18B . 0.9900
C19 C20 . 1.549(16)
C19 H19A . 0.9900
C19 H19B . 0.9900
C20 H20A . 0.9800
C20 H20B . 0.9800
C20 H20C . 0.9800
C21 C22 . 1.526(13)
C21 H21A . 0.9900
C21 H21B . 0.9900
C22 C23 . 1.508(14)
C22 H22A . 0.9900
C22 H22B . 0.9900
C23 C24 . 1.519(14)
C23 H23A . 0.9900
C23 H23B . 0.9900
C24 H24A . 0.9800
C24 H24B . 0.9800
C24 H24C . 0.9800
C25 C26 . 1.502(17)
C25 H25A . 0.9900
C25 H25B . 0.9900
C26 C27 . 1.500(16)
C26 H26A . 0.9900
C26 H26B . 0.9900
C27 C28 . 1.510(17)
C27 H27A . 0.9900
C27 H27B . 0.9900
C28 H28A . 0.9800
C28 H28B . 0.9800
C28 H28C . 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C2 H2A O6 . 0.99 2.56 3.421(14) 145.2
C2 H2A O10 . 0.99 2.84 3.590(15) 132.8
C3 H3B O12 . 0.99 2.70 3.611(15) 153.1
C5 H5B O8 . 0.99 2.57 3.522(17) 162.3
C5 H5A O2 . 0.99 2.64 3.483(16) 143.5
C9 H9A O2 . 0.99 2.74 3.561(14) 140.1
C9 H9A O4 . 0.99 2.91 3.598(13) 127.6
C10 H10A O11 . 0.99 3.06 3.561(18) 112.5
C10 H10B O4 . 0.99 3.02 3.539(14) 114.2
C10 H10B O5 . 0.99 2.85 3.222(13) 103.0
C14A H14A O9 . 0.99 3.12 3.34(2) 94.0
C14A H14A O9 . 0.99 3.12 3.34(2) 94.0
C17 H17A O1 . 0.99 2.73 3.386(18) 124.1
C17 H17A O3 . 0.99 2.91 3.903(15) 175.8
C26 H26B O1 . 0.99 2.92 3.471(18) 115.9
C4 H4A O2 6 0.98 2.95 3.847(18) 152.7
C6 H6A O4 6 0.99 2.79 3.491(15) 128.3
C6 H6B O3 6 0.99 2.72 3.505(13) 136.1
C8 H8C O4 6 0.98 2.63 3.509(15) 149.1
C9 H9B O3 6 0.99 2.66 3.646(14) 173.7
C12 H12A O3 6 0.98 2.99 3.778(14) 138.1
C13A H13B O7 2_564 0.99 2.92 3.45(3) 114.3
C13A H13B O7 2_564 0.99 2.92 3.45(3) 114.3
C13B H13C O7 2_564 0.99 2.86 3.79(3) 156.2
C13A H13B O7 3_564 0.99 2.92 3.45(3) 114.3
C13A H13B O7 3_564 0.99 2.92 3.45(3) 114.3
C13A H13B O7 3_564 0.99 2.92 3.45(3) 114.3
C13B H13C O7 3_564 0.99 2.86 3.79(3) 156.2
C18 H18A O8 2_564 0.99 2.87 3.645(18) 135.6
C18 H18B O8 3_564 0.99 2.87 3.645(18) 135.6
C17 H17B O1 4 0.99 2.73 3.386(18) 124.1
C17 H17B O3 4 0.99 2.91 3.903(15) 175.8
C13A H13A O8 4 0.99 3.39 3.73(3) 102.4
C14A H14B O8 4 0.99 2.28 3.25(3) 165.0
C21 H21B O4 4 0.99 2.79 3.72(2) 157.5
C21 H21A O11 4 0.99 2.59 3.467(17) 148.1
C25 H25B O4 4 0.99 2.73 3.66(3) 155.2
C26 H26A O1 4 0.99 2.64 3.471(18) 141.3
C26 H26A O3 4 0.99 3.12 3.953(16) 142.4
C14A H14A O2 4 0.99 2.79 3.76(3) 170.3
C20 H20A O7 1_554 0.98 2.55 3.275(19) 130.9
C28 H28A O12 1_554 0.98 2.98 3.96(3) 176.4
C20 H20A O7 4_554 0.98 2.55 3.275(19) 130.9
C28 H28A O12 4_554 0.98 2.98 3.96(3) 176.4
C22 H22A O11 2_554 0.99 2.87 3.632(16) 134.4
C22 H22B O12 2_554 0.99 2.65 3.413(15) 134.4
C24 H24C O11 2_554 0.98 3.01 3.78(2) 137.0
C22 H22B O12 3_554 0.99 2.65 3.413(15) 134.4
C16B H16D O7 2_564 0.98 3.36 4.00(4) 124.7
C16A H16C O7 2_564 0.98 3.05 3.64(4) 119.9
C16A H16C O8 2_564 0.98 3.05 4.02(4) 172.2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
O4 Re1 O1 Th1 . 65.9(10)
O2 Re1 O1 Th1 . -54.8(11)
O3 Re1 O1 Th1 . -173.5(9)
O9 Th1 O1 Re1 . 114.0(10)
O13 Th1 O1 Re1 . -94.9(10)
O5 Th1 O1 Re1 . 6.0(9)
O5 Th1 O1 Re1 4 -168.0(7)
O10 Th1 O1 Re1 . -40.0(12)
O6 Th1 O1 Re1 . 64.7(11)
O1 Th1 O1 Re1 4 -171.9(8)
C9 P1 O5 Th1 . 166.6(17)
C5 P1 O5 Th1 . -70.9(19)
C1 P1 O5 Th1 . 49(2)
O9 Th1 O5 P1 . 82.0(19)
O13 Th1 O5 P1 . -140.6(18)
O5 Th1 O5 P1 4 -37(2)
O10 Th1 O5 P1 . -67.3(18)
O6 Th1 O5 P1 . 14.1(18)
O1 Th1 O5 P1 4 151.9(16)
O1 Th1 O5 P1 . 148.0(19)
O8 Re2 O6 Th1 . -61.8(4)
O8 Re2 O6 Th1 4 61.8(4)
O7 Re2 O6 Th1 . 180.000(3)
O9 Th1 O6 Re2 . 0.0000(10)
O13 Th1 O6 Re2 . 180.0
O5 Th1 O6 Re2 . 105.7(2)
O5 Th1 O6 Re2 4 -105.7(2)
O10 Th1 O6 Re2 . 180.000(2)
O1 Th1 O6 Re2 4 -49.1(3)
O1 Th1 O6 Re2 . 49.1(3)
C17 P2 O9 Th1 . 0.000(5)
C13A P2 O9 Th1 4 -135.5(11)
C13A P2 O9 Th1 . 135.5(11)
C13B P2 O9 Th1 4 -104.0(10)
C13B P2 O9 Th1 . 104.0(10)
O13 Th1 O9 P2 . 0.000(4)
O5 Th1 O9 P2 . 107.8(2)
O5 Th1 O9 P2 4 -107.8(2)
O10 Th1 O9 P2 . 180.000(2)
O6 Th1 O9 P2 . 180.000(3)
O1 Th1 O9 P2 4 -41.0(2)
O1 Th1 O9 P2 . 41.0(2)
O11 Re3 O10 Th1 4 -59.9(6)
O11 Re3 O10 Th1 . 59.9(6)
O12 Re3 O10 Th1 . 180.0000(10)
O9 Th1 O10 Re3 . 180.0
O13 Th1 O10 Re3 . 0.0000(10)
O5 Th1 O10 Re3 . -100.2(2)
O5 Th1 O10 Re3 4 100.2(2)
O6 Th1 O10 Re3 . 180.000(2)
O1 Th1 O10 Re3 4 54.3(3)
O1 Th1 O10 Re3 . -54.3(3)
C21 P3 O13 Th1 4 118.8(6)
C21 P3 O13 Th1 . -118.8(6)
C25 P3 O13 Th1 . -22.7(9)
C25 P3 O13 Th1 4 22.7(9)
O9 Th1 O13 P3 . 0.000(5)
O5 Th1 O13 P3 . -109.8(2)
O5 Th1 O13 P3 4 109.8(2)
O10 Th1 O13 P3 . 180.000(5)
O6 Th1 O13 P3 . 180.000(4)
O1 Th1 O13 P3 4 40.2(2)
O1 Th1 O13 P3 . -40.2(2)
O5 P1 C1 C2 . -63.5(9)
C9 P1 C1 C2 . 176.9(8)
C5 P1 C1 C2 . 56.8(10)
P1 C1 C2 C3 . 174.5(8)
C1 C2 C3 C4 . 62.3(13)
O5 P1 C5 C6 . 179.0(9)
C9 P1 C5 C6 . -59.9(11)
C1 P1 C5 C6 . 56.2(11)
P1 C5 C6 C7 . -178.5(9)
C5 C6 C7 C8 . -178.9(12)
O5 P1 C9 C10 . -58.1(9)
C5 P1 C9 C10 . -178.6(8)
C1 P1 C9 C10 . 63.6(9)
P1 C9 C10 C11 . 177.9(8)
C9 C10 C11 C12 . 70.2(13)
O9 P2 C13A C14A . -36(3)
C17 P2 C13A C14A . 98(3)
C13A P2 C13A C14A 4 -145(2)
C13B P2 C13A C14A 4 -164(2)
C13B P2 C13A C14A . 75(3)
P2 C13A C14A C15A . -152(3)
C13A C14A C15A C16A . -25(4)
O9 P2 C13B C14B . 4(2)
C17 P2 C13B C14B . 121(2)
C13A P2 C13B C14B 4 -120.0(19)
C13A P2 C13B C14B . -79(3)
C13B P2 C13B C14B 4 -148.2(14)
P2 C13B C14B C15B . 135(2)
C13B C14B C15B C16B . 30(5)
O9 P2 C17 C18 . 180.0000(10)
C13A P2 C17 C18 4 -47.6(11)
C13A P2 C17 C18 . 47.6(11)
C13B P2 C17 C18 4 -58.6(8)
C13B P2 C17 C18 . 58.6(8)
P2 C17 C18 C19 . 180.000(2)
C17 C18 C19 C20 . 180.000(2)
O13 P3 C21 C22 . 170.7(13)
C21 P3 C21 C22 4 -70.3(17)
C25 P3 C21 C22 . 57.8(16)
C25 P3 C21 C22 4 35.5(19)
P3 C21 C22 C23 . -176.1(13)
C21 C22 C23 C24 . 177.4(16)
O13 P3 C25 C26 . 55(2)
C21 P3 C25 C26 4 -79(2)
C21 P3 C25 C26 . 163.2(19)
C25 P3 C25 C26 4 -44(2)
P3 C25 C26 C27 . 152.4(12)
C25 C26 C27 C28 . 149.9(15)
