#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/03/2100399.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_2100399
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                   21.721(3)
_cell_length_b                   21.738(3)
_cell_length_c                   14.8793(19)
_cell_measurement_reflns_used    5355
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      22.97
_cell_measurement_theta_min      2.65
_cell_volume                     7025.6(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      230(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18098
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    9.127
_exptl_absorpt_correction_T_max  0.4622
_exptl_absorpt_correction_T_min  0.2904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_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         1.134
_refine_diff_density_min         -1.554
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.037(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6391
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0359
_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)+(0.0314P)²+8.8462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                6029
_reflns_number_total             6391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ws5025.cif
_cod_data_source_block           IIat230
_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        7025.4(16)
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               2100399
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 0.25227(3) 0.29686(6) 0.02841(13) Uani d SU 1 . . Th
Re1 0.14631(3) 0.23960(3) 0.12490(4) 0.04611(17) Uani d U 1 . . Re
Re2 0.0000 0.40884(4) 0.44881(5) 0.0425(2) Uani d SU 1 . . Re
Re3 0.0000 0.12049(4) 0.49115(5) 0.0436(2) Uani d SU 1 . . Re
P1 0.15854(18) 0.2620(2) 0.4101(3) 0.0498(9) Uani d U 1 . . P
P2 0.0000 0.3924(3) 0.1503(4) 0.0676(16) Uani d SDU 1 . . P
P3 0.0000 0.0902(3) 0.2015(4) 0.0569(14) Uani d SU 1 . . P
O1 0.0733(5) 0.2466(5) 0.1686(8) 0.060(2) Uani d U 1 . . O
O2 0.1922(6) 0.2943(6) 0.1683(9) 0.077(3) Uani d U 1 . . O
O3 0.1427(6) 0.2490(5) 0.0106(7) 0.076(3) Uani d U 1 . . O
O4 0.1735(7) 0.1686(5) 0.1485(8) 0.085(3) Uani d U 1 . . O
O5 0.1013(5) 0.2508(4) 0.3546(8) 0.0570(18) Uani d U 1 . . O
O6 0.0000 0.3338(6) 0.4117(9) 0.051(3) Uani d SU 1 . . O
O7 0.0000 0.4072(7) 0.5671(9) 0.088(6) Uani d SU 1 . . O
O8 0.0659(7) 0.4441(6) 0.4148(10) 0.096(5) Uani d U 1 . . O
O9 0.0000 0.3457(8) 0.2273(10) 0.065(2) Uani d SU 1 A . O
O10 0.0000 0.1902(6) 0.4385(10) 0.052(3) Uani d SU 1 . . O
O11 0.0571(8) 0.0811(6) 0.4670(8) 0.095(4) Uani d U 1 . . O
O12 0.0000 0.1315(8) 0.6050(9) 0.086(5) Uani d SU 1 . . O
O13 0.0000 0.1499(7) 0.2491(10) 0.059(3) Uani d SU 1 . . O
C1 0.1483(9) 0.2425(8) 0.5274(10) 0.077(4) Uani d DU 1 . . C
H1A 0.1343 0.2002 0.5317 0.092 Uiso calc R 1 . . H
H1B 0.1877 0.2453 0.5577 0.092 Uiso calc R 1 . . H
C2 0.1028(9) 0.2834(9) 0.5749(10) 0.081(4) Uani d DU 1 . . C
H2A 0.0644 0.2833 0.5416 0.098 Uiso calc R 1 . . H
H2B 0.1184 0.3252 0.5749 0.098 Uiso calc R 1 . . H
C3 0.0898(8) 0.2637(9) 0.6728(10) 0.079(4) Uani d DU 1 . . C
H3A 0.0570 0.2890 0.6971 0.095 Uiso calc R 1 . . H
H3B 0.0760 0.2213 0.6734 0.095 Uiso calc R 1 . . H
C4 0.1460(9) 0.2699(10) 0.7313(12) 0.094(5) Uani d DU 1 . . C
H4A 0.1772 0.2418 0.7111 0.140 Uiso calc R 1 . . H
H4B 0.1354 0.2605 0.7924 0.140 Uiso calc R 1 . . H
H4C 0.1614 0.3112 0.7279 0.140 Uiso calc R 1 . . H
C5 0.1858(6) 0.3380(7) 0.3939(11) 0.057(3) Uani d DU 1 . . C
H5A 0.1940 0.3431 0.3303 0.069 Uiso calc R 1 . . H
H5B 0.1524 0.3658 0.4090 0.069 Uiso calc R 1 . . H
C6 0.2428(6) 0.3596(6) 0.4448(11) 0.060(3) Uani d DU 1 . . C
H6A 0.2362 0.3529 0.5086 0.072 Uiso calc R 1 . . H
H6B 0.2775 0.3343 0.4268 0.072 Uiso calc R 1 . . H
C7 0.2592(7) 0.4254(6) 0.4305(13) 0.066(4) Uani d DU 1 . . C
H7A 0.2249 0.4506 0.4506 0.080 Uiso calc R 1 . . H
H7B 0.2642 0.4323 0.3666 0.080 Uiso calc R 1 . . H
C8 0.3177(9) 0.4474(8) 0.4786(12) 0.085(6) Uani d DU 1 . . C
H8A 0.3172 0.4915 0.4831 0.128 Uiso calc R 1 . . H
H8B 0.3533 0.4346 0.4451 0.128 Uiso calc R 1 . . H
H8C 0.3193 0.4299 0.5378 0.128 Uiso calc R 1 . . H
C9 0.2171(6) 0.2111(6) 0.3780(10) 0.051(2) Uani d DU 1 . . C
H9A 0.2295 0.2214 0.3172 0.062 Uiso calc R 1 . . H
H9B 0.2523 0.2182 0.4167 0.062 Uiso calc R 1 . . H
C10 0.2018(7) 0.1434(6) 0.3808(12) 0.063(3) Uani d DU 1 . . C
H10A 0.1897 0.1329 0.4417 0.075 Uiso calc R 1 . . H
H10B 0.1665 0.1362 0.3423 0.075 Uiso calc R 1 . . H
C11 0.2525(7) 0.1006(7) 0.3526(11) 0.069(3) Uani d DU 1 . . C
H11A 0.2661 0.1121 0.2928 0.083 Uiso calc R 1 . . H
H11B 0.2361 0.0592 0.3491 0.083 Uiso calc R 1 . . H
C12 0.3075(8) 0.1004(9) 0.4145(14) 0.089(5) Uani d DU 1 . . C
H12A 0.3303 0.1379 0.4069 0.134 Uiso calc R 1 . . H
H12B 0.3334 0.0659 0.4004 0.134 Uiso calc R 1 . . H
H12C 0.2937 0.0972 0.4757 0.134 Uiso calc R 1 . . H
C13A -0.0489(12) 0.4566(10) 0.165(2) 0.078(3) Uani d PDU 0.61(2) A 1 C
H13A -0.0331 0.4822 0.2127 0.094 Uiso calc PR 0.61(2) A 1 H
H13B -0.0491 0.4809 0.1099 0.094 Uiso calc PR 0.61(2) A 1 H
C14A -0.1130(13) 0.4378(12) 0.186(2) 0.085(3) Uani d PDU 0.61(2) A 1 C
H14A -0.1118 0.4133 0.2408 0.102 Uiso calc PR 0.61(2) A 1 H
H14B -0.1274 0.4112 0.1384 0.102 Uiso calc PR 0.61(2) A 1 H
C15A -0.1609(13) 0.4890(13) 0.200(2) 0.084(3) Uani d PDU 0.61(2) A 1 C
H15A -0.2014 0.4704 0.1950 0.101 Uiso calc PR 0.61(2) A 1 H
H15B -0.1567 0.5041 0.2607 0.101 Uiso calc PR 0.61(2) A 1 H
C16A -0.1595(18) 0.5443(13) 0.137(3) 0.085(5) Uani d PDU 0.61(2) A 1 C
H16A -0.1334 0.5756 0.1621 0.128 Uiso calc PR 0.61(2) A 1 H
H16B -0.2004 0.5603 0.1300 0.128 Uiso calc PR 0.61(2) A 1 H
H16C -0.1437 0.5321 0.0795 0.128 Uiso calc PR 0.61(2) A 1 H
C13B -0.0764(11) 0.4274(18) 0.135(3) 0.078(3) Uani d PDU 0.39(2) A 2 C
H13C -0.0711 0.4683 0.1604 0.094 Uiso calc PR 0.39(2) A 2 H
H13D -0.0788 0.4337 0.0708 0.094 Uiso calc PR 0.39(2) A 2 H
C14B -0.1428(16) 0.4112(16) 0.161(3) 0.085(3) Uani d PDU 0.39(2) A 2 C
H14C -0.1426 0.3776 0.2036 0.102 Uiso calc PR 0.39(2) A 2 H
H14D -0.1648 0.3977 0.1076 0.102 Uiso calc PR 0.39(2) A 2 H
C15B -0.176(2) 0.4672(19) 0.202(3) 0.084(3) Uani d PDU 0.39(2) A 2 C
H15C -0.2184 0.4563 0.2144 0.101 Uiso calc PR 0.39(2) A 2 H
H15D -0.1565 0.4776 0.2587 0.101 Uiso calc PR 0.39(2) A 2 H
C16B -0.175(3) 0.5233(18) 0.140(4) 0.085(5) Uani d PDU 0.39(2) A 2 C
H16D -0.1454 0.5526 0.1629 0.128 Uiso calc PR 0.39(2) A 2 H
H16E -0.2147 0.5418 0.1384 0.128 Uiso calc PR 0.39(2) A 2 H
H16F -0.1628 0.5108 0.0809 0.128 Uiso calc PR 0.39(2) A 2 H
C17 0.0000 0.3565(11) 0.0448(12) 0.074(4) Uani d SDU 1 A . C
H17A 0.0359 0.3301 0.0418 0.089 Uiso calc PR 0.50 . . H
H17B -0.0359 0.3301 0.0418 0.089 Uiso calc PR 0.50 . . H
C18 0.0000 0.3971(9) -0.0395(10) 0.076(4) Uani d SDU 1 . . C
H18A 0.0361 0.4233 -0.0391 0.091 Uiso calc PR 0.50 A . H
H18B -0.0361 0.4233 -0.0391 0.091 Uiso calc PR 0.50 . . H
C19 0.0000 0.3574(9) -0.1266(11) 0.080(5) Uani d SDU 1 A . C
H19A 0.0363 0.3314 -0.1285 0.096 Uiso calc PR 0.50 . . H
H19B -0.0363 0.3314 -0.1285 0.096 Uiso calc PR 0.50 . . H
C20 0.0000 0.4020(12) -0.2062(14) 0.098(7) Uani d SDU 1 . . C
H20A 0.0000 0.3791 -0.2614 0.147 Uiso calc SR 1 A . H
H20B 0.0361 0.4274 -0.2036 0.147 Uiso calc PR 0.50 . . H
H20C -0.0361 0.4274 -0.2036 0.147 Uiso calc PR 0.50 . . H
C21 -0.0697(9) 0.0525(8) 0.2342(13) 0.090(4) Uani d DU 1 . . C
H21A -0.0678 0.0446 0.2983 0.108 Uiso calc R 1 . . H
H21B -0.1036 0.0806 0.2240 0.108 Uiso calc R 1 . . H
C22 -0.0840(7) -0.0069(8) 0.1875(13) 0.091(4) Uani d DU 1 . . C
H22A -0.0517 -0.0364 0.2004 0.109 Uiso calc R 1 . . H
H22B -0.0846 0.0000 0.1231 0.109 Uiso calc R 1 . . H
C23 -0.1460(8) -0.0337(8) 0.2168(13) 0.097(5) Uani d DU 1 . . C
H23A -0.1446 -0.0418 0.2809 0.117 Uiso calc R 1 . . H
H23B -0.1778 -0.0032 0.2065 0.117 Uiso calc R 1 . . H
C24 -0.1636(10) -0.0922(9) 0.1686(15) 0.114(7) Uani d DU 1 . . C
H24A -0.2052 -0.1030 0.1837 0.172 Uiso calc R 1 . . H
H24B -0.1364 -0.1248 0.1867 0.172 Uiso calc R 1 . . H
H24C -0.1603 -0.0861 0.1049 0.172 Uiso calc R 1 . . H
C25 -0.025(3) 0.0916(16) 0.0871(17) 0.155(11) Uani d PDU 0.50 . . C
H25A -0.0169 0.0516 0.0613 0.186 Uiso calc PR 0.50 . . H
H25B -0.0698 0.0966 0.0876 0.186 Uiso calc PR 0.50 . . H
C26 0.0000 0.1383(14) 0.0259(13) 0.161(11) Uani d SDU 1 . . C
H26A 0.0421 0.1466 0.0439 0.193 Uiso calc PR 0.50 . . H
H26B -0.0232 0.1761 0.0339 0.193 Uiso calc PR 0.50 . . H
C27 0.0000 0.1226(13) -0.0728(13) 0.167(11) Uani d SDU 1 . . C
H27A -0.0359 0.0974 -0.0848 0.200 Uiso calc PR 0.50 . . H
H27B 0.0359 0.0974 -0.0848 0.200 Uiso calc PR 0.50 . . H
C28 0.0000 0.1751(16) -0.139(2) 0.196(13) Uani d SDU 1 . . C
H28A 0.0000 0.1589 -0.1993 0.295 Uiso calc SR 1 . . H
H28B 0.0361 0.1998 -0.1304 0.295 Uiso calc PR 0.50 . . H
H28C -0.0361 0.1998 -0.1304 0.295 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 . . 135.3(6)
O9 Th1 O5 . 4 100.2(3)
O13 Th1 O5 . 4 95.6(3)
O9 Th1 O5 . . 100.2(3)
O13 Th1 O5 . . 95.6(3)
O5 Th1 O5 4 . 137.3(6)
O9 Th1 O6 . . 70.9(5)
O13 Th1 O6 . . 153.7(5)
O5 Th1 O6 4 . 76.0(3)
O5 Th1 O6 . . 76.0(3)
O9 Th1 O1 . 4 72.3(4)
O13 Th1 O1 . 4 73.7(4)
O5 Th1 O1 4 4 71.5(4)
O5 Th1 O1 . 4 151.0(4)
O6 Th1 O1 . 4 124.6(3)
O9 Th1 O1 . . 72.3(4)
O13 Th1 O1 . . 73.7(4)
O5 Th1 O1 4 . 151.0(4)
O5 Th1 O1 . . 71.5(4)
O6 Th1 O1 . . 124.6(3)
O1 Th1 O1 4 . 79.6(5)
O9 Th1 O10 . . 149.6(5)
O13 Th1 O10 . . 75.1(5)
O5 Th1 O10 4 . 71.7(3)
O5 Th1 O10 . . 71.7(3)
O6 Th1 O10 . . 78.7(4)
O1 Th1 O10 4 . 128.3(3)
O1 Th1 O10 . . 128.3(3)
O2 Re1 O4 . . 111.1(7)
O2 Re1 O3 . . 108.9(6)
O4 Re1 O3 . . 109.3(5)
O2 Re1 O1 . . 109.8(6)
O4 Re1 O1 . . 108.9(6)
O3 Re1 O1 . . 108.8(6)
O8 Re2 O8 . 4 114.6(12)
O8 Re2 O6 . . 109.4(5)
O8 Re2 O6 4 . 109.4(5)
O8 Re2 O7 . . 107.9(6)
O8 Re2 O7 4 . 107.9(6)
O6 Re2 O7 . . 107.5(7)
O11 Re3 O11 4 . 106.4(13)
O11 Re3 O10 4 . 112.6(6)
O11 Re3 O10 . . 112.6(6)
O11 Re3 O12 4 . 107.9(5)
O11 Re3 O12 . . 107.9(5)
O10 Re3 O12 . . 109.3(8)
O5 P1 C9 . . 110.3(6)
O5 P1 C5 . . 110.5(6)
C9 P1 C5 . . 108.0(7)
O5 P1 C1 . . 112.8(8)
C9 P1 C1 . . 101.8(7)
C5 P1 C1 . . 113.0(8)
O9 P2 C17 . . 112.1(9)
O9 P2 C13A . . 115.6(11)
C17 P2 C13A . . 117.3(13)
O9 P2 C13A . 4 115.6(11)
C17 P2 C13A . 4 117.3(13)
C13A P2 C13A . 4 74(2)
O9 P2 C13B . 4 111.4(13)
C17 P2 C13B . 4 94.3(17)
C13A P2 C13B . 4 103.3(19)
C13A P2 C13B 4 4 31.2(15)
O9 P2 C13B . . 111.4(13)
C17 P2 C13B . . 94.3(17)
C13A P2 C13B . . 31.2(15)
C13A P2 C13B 4 . 103.3(19)
C13B P2 C13B 4 . 129(3)
O13 P3 C21 . . 105.8(6)
O13 P3 C21 . 4 105.8(6)
C21 P3 C21 . 4 115.6(16)
O13 P3 C25 . . 116.1(15)
C21 P3 C25 . . 90.3(17)
C21 P3 C25 4 . 122(2)
O13 P3 C25 . 4 116.1(15)
C21 P3 C25 . 4 122(2)
C21 P3 C25 4 4 90.3(17)
C25 P3 C25 . 4 36(4)
Re1 O1 Th1 . . 152.1(6)
P1 O5 Th1 . . 164.2(7)
Re2 O6 Th1 . . 154.7(7)
P2 O9 Th1 . . 158.5(11)
Re3 O10 Th1 . . 149.9(8)
P3 O13 Th1 . . 169.0(11)
C2 C1 P1 . . 113.3(11)
C2 C1 H1A . . 108.9
P1 C1 H1A . . 108.9
C2 C1 H1B . . 108.9
P1 C1 H1B . . 108.9
H1A C1 H1B . . 107.7
C1 C2 C3 . . 113.5(14)
C1 C2 H2A . . 108.9
C3 C2 H2A . . 108.9
C1 C2 H2B . . 108.9
C3 C2 H2B . . 108.9
H2A C2 H2B . . 107.7
C4 C3 C2 . . 111.9(15)
C4 C3 H3A . . 109.2
C2 C3 H3A . . 109.2
C4 C3 H3B . . 109.2
C2 C3 H3B . . 109.2
H3A C3 H3B . . 107.9
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 . . 119.3(10)
C6 C5 H5A . . 107.5
P1 C5 H5A . . 107.5
C6 C5 H5B . . 107.5
P1 C5 H5B . . 107.5
H5A C5 H5B . . 107.0
C7 C6 C5 . . 114.7(11)
C7 C6 H6A . . 108.6
C5 C6 H6A . . 108.6
C7 C6 H6B . . 108.6
C5 C6 H6B . . 108.6
H6A C6 H6B . . 107.6
C6 C7 C8 . . 115.5(12)
C6 C7 H7A . . 108.4
C8 C7 H7A . . 108.4
C6 C7 H7B . . 108.4
C8 C7 H7B . . 108.4
H7A C7 H7B . . 107.5
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 . . 116.6(10)
C10 C9 H9A . . 108.1
P1 C9 H9A . . 108.1
C10 C9 H9B . . 108.1
P1 C9 H9B . . 108.1
H9A C9 H9B . . 107.3
C11 C10 C9 . . 115.8(13)
C11 C10 H10A . . 108.3
C9 C10 H10A . . 108.3
C11 C10 H10B . . 108.3
C9 C10 H10B . . 108.3
H10A C10 H10B . . 107.4
C10 C11 C12 . . 114.3(14)
C10 C11 H11A . . 108.7
C12 C11 H11A . . 108.7
C10 C11 H11B . . 108.7
C12 C11 H11B . . 108.7
H11A C11 H11B . . 107.6
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 . . 111.8(16)
C14A C13A H13A . . 109.3
P2 C13A H13A . . 109.3
C14A C13A H13B . . 109.3
P2 C13A H13B . . 109.3
H13A C13A H13B . . 107.9
C13A C14A C15A . . 117.5(19)
C13A C14A H14A . . 107.9
C15A C14A H14A . . 107.9
C13A C14A H14B . . 107.9
C15A C14A H14B . . 107.9
H14A C14A H14B . . 107.2
C16A C15A C14A . . 119(2)
C16A C15A H15A . . 107.6
C14A C15A H15A . . 107.6
C16A C15A H15B . . 107.6
C14A C15A H15B . . 107.6
H15A C15A H15B . . 107.1
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 . . 136(3)
C14B C13B H13C . . 103.1
P2 C13B H13C . . 103.1
C14B C13B H13D . . 103.1
P2 C13B H13D . . 103.1
H13C C13B H13D . . 105.1
C13B C14B C15B . . 111(2)
C13B C14B H14C . . 109.5
C15B C14B H14C . . 109.5
C13B C14B H14D . . 109.5
C15B C14B H14D . . 109.5
H14C C14B H14D . . 108.1
C16B C15B C14B . . 112(2)
C16B C15B H15C . . 109.1
C14B C15B H15C . . 109.1
C16B C15B H15D . . 109.1
C14B C15B H15D . . 109.1
H15C C15B H15D . . 107.9
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 . . 118.5(16)
C18 C17 H17A . . 107.7
P2 C17 H17A . . 107.7
C18 C17 H17B . . 107.7
P2 C17 H17B . . 107.7
H17A C17 H17B . . 107.1
C17 C18 C19 . . 111.2(15)
C17 C18 H18A . . 109.4
C19 C18 H18A . . 109.4
C17 C18 H18B . . 109.4
C19 C18 H18B . . 109.4
H18A C18 H18B . . 108.0
C20 C19 C18 . . 107.0(16)
C20 C19 H19A . . 110.3
C18 C19 H19A . . 110.3
C20 C19 H19B . . 110.3
C18 C19 H19B . . 110.3
H19A C19 H19B . . 108.6
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 . . 116.4(12)
C22 C21 H21A . . 108.2
P3 C21 H21A . . 108.2
C22 C21 H21B . . 108.2
P3 C21 H21B . . 108.2
H21A C21 H21B . . 107.3
C21 C22 C23 . . 112.3(12)
C21 C22 H22A . . 109.1
C23 C22 H22A . . 109.1
C21 C22 H22B . . 109.1
C23 C22 H22B . . 109.1
H22A C22 H22B . . 107.9
C24 C23 C22 . . 114.1(13)
C24 C23 H23A . . 108.7
C22 C23 H23A . . 108.7
C24 C23 H23B . . 108.7
C22 C23 H23B . . 108.7
H23A C23 H23B . . 107.6
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 . . 119(3)
C26 C25 H25A . . 107.6
P3 C25 H25A . . 107.6
C26 C25 H25B . . 107.6
P3 C25 H25B . . 107.6
H25A C25 H25B . . 107.0
C25 C26 C27 . . 117(2)
C25 C26 H26A . . 108.2
C27 C26 H26A . . 108.2
C25 C26 H26B . . 108.2
C27 C26 H26B . . 108.2
H26A C26 H26B . . 107.3
C26 C27 C28 . . 118(2)
C26 C27 H27A . . 107.9
C28 C27 H27A . . 107.9
C26 C27 H27B . . 107.9
C28 C27 H27B . . 107.9
H27A C27 H27B . . 107.2
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 . 2.280(15)
Th1 O13 . 2.337(15)
Th1 O5 4 2.362(11)
Th1 O5 . 2.362(11)
Th1 O6 . 2.462(13)
Th1 O1 4 2.489(11)
Th1 O1 . 2.489(11)
Th1 O10 . 2.502(14)
Re1 O2 . 1.681(11)
Re1 O4 . 1.690(11)
Re1 O3 . 1.715(11)
Re1 O1 . 1.720(11)
Re2 O8 . 1.701(12)
Re2 O8 4 1.701(12)
Re2 O6 . 1.722(13)
Re2 O7 . 1.761(14)
Re3 O11 4 1.550(13)
Re3 O11 . 1.550(13)
Re3 O10 . 1.706(13)
Re3 O12 . 1.711(13)
P1 O5 . 1.513(11)
P1 C9 . 1.751(14)
P1 C5 . 1.772(15)
P1 C1 . 1.809(16)
P2 O9 . 1.531(15)
P2 C17 . 1.75(2)
P2 C13A . 1.767(16)
P2 C13A 4 1.767(16)
P2 C13B 4 1.840(18)
P2 C13B . 1.840(18)
P3 O13 . 1.477(16)
P3 C21 . 1.788(17)
P3 C21 4 1.788(17)
P3 C25 . 1.79(3)
P3 C25 4 1.79(3)
C1 C2 . 1.506(15)
C1 H1A . 0.9700
C1 H1B . 0.9700
C2 C3 . 1.544(15)
C2 H2A . 0.9700
C2 H2B . 0.9700
C3 C4 . 1.506(16)
C3 H3A . 0.9700
C3 H3B . 0.9700
C4 H4A . 0.9600
C4 H4B . 0.9600
C4 H4C . 0.9600
C5 C6 . 1.526(14)
C5 H5A . 0.9700
C5 H5B . 0.9700
C6 C7 . 1.491(14)
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 C8 . 1.536(15)
C7 H7A . 0.9700
C7 H7B . 0.9700
C8 H8A . 0.9600
C8 H8B . 0.9600
C8 H8C . 0.9600
C9 C10 . 1.510(14)
C9 H9A . 0.9700
C9 H9B . 0.9700
C10 C11 . 1.502(15)
C10 H10A . 0.9700
C10 H10B . 0.9700
C11 C12 . 1.508(15)
C11 H11A . 0.9700
C11 H11B . 0.9700
C12 H12A . 0.9600
C12 H12B . 0.9600
C12 H12C . 0.9600
C13A C14A . 1.486(18)
C13A H13A . 0.9700
C13A H13B . 0.9700
C14A C15A . 1.537(18)
C14A H14A . 0.9700
C14A H14B . 0.9700
C15A C16A . 1.522(18)
C15A H15A . 0.9700
C15A H15B . 0.9700
C16A H16A . 0.9600
C16A H16B . 0.9600
C16A H16C . 0.9600
C13B C14B . 1.532(19)
C13B H13C . 0.9700
C13B H13D . 0.9700
C14B C15B . 1.543(19)
C14B H14C . 0.9700
C14B H14D . 0.9700
C15B C16B . 1.528(19)
C15B H15C . 0.9700
C15B H15D . 0.9700
C16B H16D . 0.9600
C16B H16E . 0.9600
C16B H16F . 0.9600
C17 C18 . 1.533(15)
C17 H17A . 0.9700
C17 H17B . 0.9700
C18 C19 . 1.557(17)
C18 H18A . 0.9700
C18 H18B . 0.9700
C19 C20 . 1.530(16)
C19 H19A . 0.9700
C19 H19B . 0.9700
C20 H20A . 0.9600
C20 H20B . 0.9600
C20 H20C . 0.9600
C21 C22 . 1.498(14)
C21 H21A . 0.9700
C21 H21B . 0.9700
C22 C23 . 1.531(15)
C22 H22A . 0.9700
C22 H22B . 0.9700
C23 C24 . 1.509(15)
C23 H23A . 0.9700
C23 H23B . 0.9700
C24 H24A . 0.9600
C24 H24B . 0.9600
C24 H24C . 0.9600
C25 C26 . 1.471(18)
C25 H25A . 0.9700
C25 H25B . 0.9700
C26 C27 . 1.508(18)
C26 H26A . 0.9700
C26 H26B . 0.9700
C27 C28 . 1.509(18)
C27 H27A . 0.9700
C27 H27B . 0.9700
C28 H28A . 0.9600
C28 H28B . 0.9600
C28 H28C . 0.9600
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 . 0.97 2.63 3.476(19) 146.3
C2 H2A O10 . 0.97 2.90 3.63(2) 133.4
C3 H3B O12 . 0.97 2.75 3.62(2) 148.9
C5 H5B O8 . 0.97 2.54 3.49(2) 168.3
C5 H5A O2 . 0.97 2.63 3.492(19) 147.7
C9 H9A O2 . 0.97 2.84 3.65(2) 140.9
C9 H9A O4 . 0.97 3.02 3.663(19) 125.2
C10 H10A O11 . 0.97 3.11 3.65(2) 116.7
C10 H10B O4 . 0.97 2.97 3.55(2) 119.7
C10 H10B O5 . 0.97 2.87 3.220(17) 102.3
C14A H14A O9 . 0.97 2.84 3.22(3) 104.3
C14A H14A O9 . 0.97 2.84 3.22(3) 104.3
C17 H17A O1 . 0.97 2.74 3.41(2) 126.8
C17 H17A O3 . 0.97 2.95 3.915(19) 173.5
C26 H26A O1 . 0.97 2.94 3.55(3) 122.0
C4 H4A O2 6 0.96 3.01 3.90(3) 153.7
C6 H6A O4 6 0.97 2.90 3.587(19) 128.7
C6 H6B O3 6 0.97 2.80 3.565(18) 136.3
C8 H8C O4 6 0.96 2.71 3.58(2) 151.0
C9 H9B O3 6 0.97 2.77 3.731(18) 172.1
C12 H12A O3 6 0.96 2.96 3.73(2) 138.2
C13A H13B O7 2_564 0.97 2.73 3.46(3) 132.8
C13A H13B O7 2_564 0.97 2.73 3.46(3) 132.8
C13B H13C O7 2_564 0.97 3.41 4.09(4) 128.5
C13A H13B O7 3_564 0.97 2.73 3.46(3) 132.8
C13A H13B O7 3_564 0.97 2.73 3.46(3) 132.8
C13A H13B O7 3_564 0.97 2.73 3.46(3) 132.8
C13B H13C O7 3_564 0.97 3.41 4.09(4) 128.5
C18 H18B O8 2_564 0.97 3.03 3.80(2) 136.8
C18 H18A O8 3_564 0.97 3.03 3.80(2) 136.8
C17 H17B O1 4 0.97 2.74 3.41(2) 126.8
C17 H17B O3 4 0.97 2.95 3.915(19) 173.5
C13A H13A O8 4 0.97 3.20 3.75(3) 117.8
C14A H14A O8 4 0.97 2.85 3.55(4) 129.7
C21 H21B O4 4 0.97 2.69 3.62(3) 160.6
C21 H21A O11 4 0.97 2.64 3.53(2) 152.2
C25 H25B O4 4 0.97 2.89 3.74(6) 146.8
C26 H26B O1 4 0.97 2.75 3.55(3) 140.1
C26 H26B O3 4 0.97 3.06 3.93(2) 149.8
C14A H14B O2 4 0.97 2.94 3.57(3) 124.0
C20 H20A O7 1_554 0.96 2.62 3.37(3) 135.3
C28 H28A O12 1_554 0.96 2.97 3.92(4) 170.1
C20 H20A O7 4_554 0.96 2.62 3.37(3) 135.3
C28 H28A O12 4_554 0.96 2.97 3.92(4) 170.1
C22 H22B O11 2_554 0.97 2.98 3.702(19) 132.6
C22 H22A O12 2_554 0.97 2.75 3.49(2) 133.8
C24 H24C O11 2_554 0.96 3.04 3.79(3) 136.5
C22 H22A O12 3_554 0.97 2.75 3.49(2) 133.8
C16B H16D O7 2_564 0.96 3.57 4.22(6) 127.4
C16A H16A O7 2_564 0.96 3.25 3.77(4) 116.1
C16A H16C O8 2_564 0.96 3.02 3.89(4) 151.0
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
O2 Re1 O1 Th1 . -55.5(14)
O4 Re1 O1 Th1 . 66.3(13)
O3 Re1 O1 Th1 . -174.6(11)
O9 Th1 O1 Re1 . 113.3(13)
O13 Th1 O1 Re1 . -96.1(13)
O5 Th1 O1 Re1 4 -167.7(9)
O5 Th1 O1 Re1 . 5.7(11)
O6 Th1 O1 Re1 . 62.9(13)
O1 Th1 O1 Re1 4 -172.1(10)
O10 Th1 O1 Re1 . -41.0(14)
C9 P1 O5 Th1 . 171(2)
C5 P1 O5 Th1 . -70(3)
C1 P1 O5 Th1 . 58(3)
O9 Th1 O5 P1 . 76(3)
O13 Th1 O5 P1 . -146(2)
O5 Th1 O5 P1 4 -42(3)
O6 Th1 O5 P1 . 9(2)
O1 Th1 O5 P1 4 148(2)
O1 Th1 O5 P1 . 143(3)
O10 Th1 O5 P1 . -74(3)
O8 Re2 O6 Th1 . -63.1(6)
O8 Re2 O6 Th1 4 63.1(6)
O7 Re2 O6 Th1 . 180.000(4)
O9 Th1 O6 Re2 . 0.0000(10)
O13 Th1 O6 Re2 . 180.0
O5 Th1 O6 Re2 4 -106.2(3)
O5 Th1 O6 Re2 . 106.2(3)
O1 Th1 O6 Re2 4 -51.0(4)
O1 Th1 O6 Re2 . 51.0(4)
O10 Th1 O6 Re2 . 180.000(2)
C17 P2 O9 Th1 . 0.000(6)
C13A P2 O9 Th1 . 138.2(12)
C13A P2 O9 Th1 4 -138.2(12)
C13B P2 O9 Th1 4 -104.3(17)
C13B P2 O9 Th1 . 104.3(17)
O13 Th1 O9 P2 . 0.000(5)
O5 Th1 O9 P2 4 -108.8(3)
O5 Th1 O9 P2 . 108.8(3)
O6 Th1 O9 P2 . 180.000(4)
O1 Th1 O9 P2 4 -42.2(3)
O1 Th1 O9 P2 . 42.2(3)
O10 Th1 O9 P2 . 180.000(2)
O11 Re3 O10 Th1 4 -60.2(7)
O11 Re3 O10 Th1 . 60.2(7)
O12 Re3 O10 Th1 . 180.000(2)
O9 Th1 O10 Re3 . 180.0
O13 Th1 O10 Re3 . 0.000(2)
O5 Th1 O10 Re3 4 101.2(3)
O5 Th1 O10 Re3 . -101.2(3)
O6 Th1 O10 Re3 . 180.000(2)
O1 Th1 O10 Re3 4 54.6(4)
O1 Th1 O10 Re3 . -54.6(4)
C21 P3 O13 Th1 . -118.4(8)
C21 P3 O13 Th1 4 118.4(8)
C25 P3 O13 Th1 . -20(2)
C25 P3 O13 Th1 4 20(2)
O9 Th1 O13 P3 . 0.000(6)
O5 Th1 O13 P3 4 110.6(3)
O5 Th1 O13 P3 . -110.6(3)
O6 Th1 O13 P3 . 180.000(4)
O1 Th1 O13 P3 4 41.8(3)
O1 Th1 O13 P3 . -41.8(3)
O10 Th1 O13 P3 . 180.000(6)
O5 P1 C1 C2 . -66.2(17)
C9 P1 C1 C2 . 175.6(15)
C5 P1 C1 C2 . 60.0(17)
P1 C1 C2 C3 . 175.3(13)
C1 C2 C3 C4 . 65(2)
O5 P1 C5 C6 . 179.1(12)
C9 P1 C5 C6 . -60.2(15)
C1 P1 C5 C6 . 51.6(15)
P1 C5 C6 C7 . -176.3(13)
C5 C6 C7 C8 . -178.0(16)
O5 P1 C9 C10 . -55.3(14)
C5 P1 C9 C10 . -176.1(12)
C1 P1 C9 C10 . 64.7(14)
P1 C9 C10 C11 . 179.7(12)
C9 C10 C11 C12 . 66(2)
O9 P2 C13A C14A . -53(3)
C17 P2 C13A C14A . 83(2)
C13A P2 C13A C14A 4 -164.0(18)
C13B P2 C13A C14A 4 -175(3)
C13B P2 C13A C14A . 37(3)
P2 C13A C14A C15A . -179(3)
C13A C14A C15A C16A . 40(5)
O9 P2 C13B C14B . -20(5)
C17 P2 C13B C14B . 95(5)
C13A P2 C13B C14B . -125(7)
C13A P2 C13B C14B 4 -145(5)
C13B P2 C13B C14B 4 -166(3)
P2 C13B C14B C15B . 133(5)
C13B C14B C15B C16B . 56(5)
O9 P2 C17 C18 . 180.000(2)
C13A P2 C17 C18 . 42.6(10)
C13A P2 C17 C18 4 -42.6(10)
C13B P2 C17 C18 4 -64.8(13)
C13B P2 C17 C18 . 64.8(13)
P2 C17 C18 C19 . 180.000(3)
C17 C18 C19 C20 . 180.000(2)
O13 P3 C21 C22 . 174.0(18)
C21 P3 C21 C22 4 -69(2)
C25 P3 C21 C22 . 57(2)
C25 P3 C21 C22 4 38(2)
P3 C21 C22 C23 . -177.1(17)
C21 C22 C23 C24 . 178(2)
O13 P3 C25 C26 . 48(5)
C21 P3 C25 C26 . 156(4)
C21 P3 C25 C26 4 -83(4)
C25 P3 C25 C26 4 -51(4)
P3 C25 C26 C27 . 154(2)
C25 C26 C27 C28 . 155(3)
