#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/03/2100395.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_2100395
loop_
_publ_author_name
'M. Helliwell'
'D. Collison'
'G. H. John'
'I. May'
'M. J. Sarsfield'
'C. A. Sharrad'
'A. D. Sutton'
_publ_contact_author
;
    ENTER NAME
 ENTER ADDRESS
;
_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 U'
_chemical_formula_weight         2112.05
_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                   21.5289(15)
_cell_length_b                   21.9148(16)
_cell_length_c                   14.8288(11)
_cell_measurement_reflns_used    5703
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.65
_cell_volume                     6996.3(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25273
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    9.354
_exptl_absorpt_correction_T_max  0.4548
_exptl_absorpt_correction_T_min  0.3343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.233
_refine_diff_density_min         -1.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6529
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0273
_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)+(0.0273P)²+21.6652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                6180
_reflns_number_total             6529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ws5025.cif
_cod_data_source_block           Iat230
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               2100395
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
U1 1.0000 0.748499(15) 0.70272(3) 0.02929(9) Uani d SU 1 . . U
Re1 0.855048(15) 0.760328(15) 0.87493(2) 0.04713(10) Uani d U 1 . . Re
Re2 1.0000 0.59478(2) 0.55071(3) 0.04392(12) Uani d SU 1 . . Re
Re3 1.0000 0.87951(2) 0.51085(3) 0.04368(12) Uani d SU 1 . . Re
P1 0.84363(11) 0.73937(12) 0.59017(17) 0.0530(6) Uani d U 1 . . P
P2 1.0000 0.60898(17) 0.8435(3) 0.0723(11) Uani d SDU 1 . . P
P3 1.0000 0.90773(15) 0.7991(2) 0.0585(9) Uani d SU 1 . . P
O1 0.9299(3) 0.7516(3) 0.8307(4) 0.0598(14) Uani d U 1 . . O
O2 0.8071(3) 0.7078(4) 0.8317(6) 0.083(2) Uani d U 1 . . O
O3 0.8576(4) 0.7521(4) 0.9881(5) 0.083(2) Uani d U 1 . . O
O4 0.8267(4) 0.8306(3) 0.8506(5) 0.085(2) Uani d U 1 . . O
O5 0.9002(3) 0.7491(3) 0.6483(4) 0.0594(14) Uani d U 1 . . O
O6 1.0000 0.6717(4) 0.5867(5) 0.0562(18) Uani d SU 1 . . O
O7 1.0000 0.5926(5) 0.4359(7) 0.092(3) Uani d SU 1 . . O
O8 0.9353(4) 0.5585(3) 0.5865(6) 0.087(2) Uani d U 1 . . O
O9 1.0000 0.6545(4) 0.7673(6) 0.064(2) Uani d SU 1 A . O
O10 1.0000 0.8097(4) 0.5690(6) 0.0577(18) Uani d SU 1 . . O
O11 0.9372(5) 0.9205(4) 0.5343(5) 0.109(3) Uani d U 1 . . O
O12 1.0000 0.8672(4) 0.3992(6) 0.081(3) Uani d SU 1 . . O
O13 1.0000 0.8465(4) 0.7505(7) 0.067(2) Uani d SU 1 . . O
C1 0.8557(5) 0.7557(6) 0.4746(7) 0.079(3) Uani d DU 1 . . C
H1A 0.8153 0.7538 0.4441 0.094 Uiso calc R 1 . . H
H1B 0.8705 0.7979 0.4698 0.094 Uiso calc R 1 . . H
C2 0.8995(7) 0.7161(7) 0.4245(8) 0.104(4) Uani d DU 1 . . C
H2A 0.8833 0.6743 0.4238 0.125 Uiso calc R 1 . . H
H2B 0.9395 0.7156 0.4562 0.125 Uiso calc R 1 . . H
C3 0.9102(7) 0.7380(6) 0.3247(8) 0.101(4) Uani d DU 1 . . C
H3A 0.9216 0.7813 0.3248 0.121 Uiso calc R 1 . . H
H3B 0.9448 0.7150 0.2984 0.121 Uiso calc R 1 . . H
C4 0.8544(8) 0.7293(9) 0.2687(12) 0.131(6) Uani d DU 1 . . C
H4A 0.8222 0.7574 0.2881 0.197 Uiso calc R 1 . . H
H4B 0.8396 0.6877 0.2751 0.197 Uiso calc R 1 . . H
H4C 0.8645 0.7371 0.2060 0.197 Uiso calc R 1 . . H
C5 0.8160(4) 0.6626(4) 0.6086(7) 0.063(2) Uani d DU 1 . . C
H5A 0.8497 0.6343 0.5931 0.075 Uiso calc R 1 . . H
H5B 0.8076 0.6577 0.6731 0.075 Uiso calc R 1 . . H
C6 0.7587(4) 0.6432(4) 0.5573(8) 0.066(2) Uani d DU 1 . . C
H6A 0.7666 0.6463 0.4924 0.080 Uiso calc R 1 . . H
H6B 0.7243 0.6708 0.5721 0.080 Uiso calc R 1 . . H
C7 0.7401(5) 0.5777(5) 0.5804(8) 0.077(3) Uani d DU 1 . . C
H7A 0.7317 0.5748 0.6452 0.092 Uiso calc R 1 . . H
H7B 0.7747 0.5503 0.5663 0.092 Uiso calc R 1 . . H
C8 0.6824(7) 0.5571(6) 0.5281(9) 0.114(5) Uani d DU 1 . . C
H8A 0.6823 0.5130 0.5232 0.171 Uiso calc R 1 . . H
H8B 0.6830 0.5750 0.4682 0.171 Uiso calc R 1 . . H
H8C 0.6453 0.5704 0.5597 0.171 Uiso calc R 1 . . H
C9 0.7818(4) 0.7903(4) 0.6221(7) 0.0598(19) Uani d DU 1 . . C
H9A 0.7461 0.7833 0.5823 0.072 Uiso calc R 1 . . H
H9B 0.7687 0.7806 0.6838 0.072 Uiso calc R 1 . . H
C10 0.7998(5) 0.8571(4) 0.6175(8) 0.075(2) Uani d DU 1 . . C
H10A 0.8126 0.8668 0.5557 0.090 Uiso calc R 1 . . H
H10B 0.8356 0.8640 0.6569 0.090 Uiso calc R 1 . . H
C11 0.7478(5) 0.9002(5) 0.6450(9) 0.088(3) Uani d DU 1 . . C
H11A 0.7324 0.8883 0.7046 0.106 Uiso calc R 1 . . H
H11B 0.7645 0.9417 0.6497 0.106 Uiso calc R 1 . . H
C12 0.6949(6) 0.9000(6) 0.5794(11) 0.113(5) Uani d DU 1 . . C
H12A 0.6714 0.8625 0.5861 0.169 Uiso calc R 1 . . H
H12B 0.7110 0.9027 0.5185 0.169 Uiso calc R 1 . . H
H12C 0.6681 0.9346 0.5912 0.169 Uiso calc R 1 . . H
C13A 1.0468(7) 0.5465(7) 0.8263(14) 0.088(5) Uiso d PDU 0.637(15) A 1 C
H13A 1.0411 0.5167 0.8749 0.105 Uiso calc PR 0.637(15) A 1 H
H13B 1.0365 0.5268 0.7688 0.105 Uiso calc PR 0.637(15) A 1 H
C14A 1.1123(7) 0.5691(7) 0.8250(13) 0.081(5) Uiso d PDU 0.637(15) A 1 C
H14A 1.1231 0.5846 0.8850 0.097 Uiso calc PR 0.637(15) A 1 H
H14B 1.1156 0.6030 0.7822 0.097 Uiso calc PR 0.637(15) A 1 H
C15A 1.1593(9) 0.5188(8) 0.7981(14) 0.090(6) Uiso d PDU 0.637(15) A 1 C
H15A 1.1487 0.5037 0.7378 0.108 Uiso calc PR 0.637(15) A 1 H
H15B 1.2009 0.5369 0.7946 0.108 Uiso calc PR 0.637(15) A 1 H
C16A 1.1611(10) 0.4651(9) 0.8634(15) 0.094(6) Uiso d PDU 0.637(15) A 1 C
H16A 1.1351 0.4324 0.8405 0.140 Uiso calc PR 0.637(15) A 1 H
H16B 1.1458 0.4780 0.9219 0.140 Uiso calc PR 0.637(15) A 1 H
H16C 1.2035 0.4506 0.8694 0.140 Uiso calc PR 0.637(15) A 1 H
C13B 1.0821(9) 0.5819(11) 0.847(2) 0.070(7) Uiso d PDU 0.363(15) A 2 C
H13C 1.0998 0.5929 0.7881 0.084 Uiso calc PR 0.363(15) A 2 H
H13D 1.1029 0.6081 0.8912 0.084 Uiso calc PR 0.363(15) A 2 H
C14B 1.1050(12) 0.5184(11) 0.866(2) 0.089(7) Uiso d PDU 0.363(15) A 2 C
H14C 1.0758 0.4895 0.8384 0.107 Uiso calc PR 0.363(15) A 2 H
H14D 1.1038 0.5118 0.9311 0.107 Uiso calc PR 0.363(15) A 2 H
C15B 1.1709(13) 0.5027(15) 0.832(3) 0.094(9) Uiso d PDU 0.363(15) A 2 C
H15C 1.1726 0.5050 0.7662 0.113 Uiso calc PR 0.363(15) A 2 H
H15D 1.2011 0.5315 0.8571 0.113 Uiso calc PR 0.363(15) A 2 H
C16B 1.1857(19) 0.4379(16) 0.864(4) 0.133(14) Uiso d PDU 0.363(15) A 2 C
H16D 1.1531 0.4104 0.8440 0.200 Uiso calc PR 0.363(15) A 2 H
H16E 1.1884 0.4372 0.9290 0.200 Uiso calc PR 0.363(15) A 2 H
H16F 1.2250 0.4250 0.8382 0.200 Uiso calc PR 0.363(15) A 2 H
C17 1.0000 0.6438(6) 0.9514(8) 0.073(4) Uani d SDU 1 A . C
H17A 1.0367 0.6701 0.9557 0.088 Uiso calc PR 0.50 . . H
H17B 0.9633 0.6701 0.9557 0.088 Uiso calc PR 0.50 . . H
C18 1.0000 0.6010(6) 1.0319(7) 0.072(4) Uani d SDU 1 . . C
H18A 1.0369 0.5748 1.0298 0.086 Uiso calc PR 0.50 A . H
H18B 0.9631 0.5748 1.0298 0.086 Uiso calc PR 0.50 . . H
C19 1.0000 0.6380(7) 1.1199(8) 0.091(5) Uani d SDU 1 A . C
H19A 1.0369 0.6641 1.1229 0.109 Uiso calc PR 0.50 . . H
H19B 0.9631 0.6641 1.1229 0.109 Uiso calc PR 0.50 . . H
C20 1.0000 0.5928(8) 1.1978(10) 0.115(7) Uani d SDU 1 . . C
H20A 1.0000 0.6149 1.2545 0.173 Uiso calc SR 1 A . H
H20B 1.0368 0.5674 1.1942 0.173 Uiso calc PR 0.50 . . H
H20C 0.9632 0.5674 1.1942 0.173 Uiso calc PR 0.50 . . H
C21 1.0675(5) 0.9465(5) 0.7688(9) 0.086(3) Uani d DU 1 . . C
H21A 1.1023 0.9179 0.7755 0.103 Uiso calc R 1 . . H
H21B 1.0644 0.9563 0.7045 0.103 Uiso calc R 1 . . H
C22 1.0851(4) 1.0049(5) 0.8179(9) 0.083(3) Uani d DU 1 . . C
H22A 1.0872 0.9965 0.8828 0.100 Uiso calc R 1 . . H
H22B 1.0525 1.0353 0.8082 0.100 Uiso calc R 1 . . H
C23 1.1469(5) 1.0312(6) 0.7872(11) 0.104(4) Uani d DU 1 . . C
H23A 1.1797 1.0011 0.7983 0.125 Uiso calc R 1 . . H
H23B 1.1452 1.0386 0.7220 0.125 Uiso calc R 1 . . H
C24 1.1635(6) 1.0894(6) 0.8338(13) 0.141(7) Uani d DU 1 . . C
H24A 1.2058 1.1006 0.8187 0.211 Uiso calc R 1 . . H
H24B 1.1600 1.0839 0.8985 0.211 Uiso calc R 1 . . H
H24C 1.1355 1.1215 0.8145 0.211 Uiso calc R 1 . . H
C25 1.0227(14) 0.9056(10) 0.9130(13) 0.116(8) Uani d PDU 0.50 . . C
H25A 1.0681 0.9032 0.9136 0.139 Uiso calc PR 0.50 . . H
H25B 1.0117 0.9453 0.9390 0.139 Uiso calc PR 0.50 . . H
C26 1.0000 0.8589(10) 0.9760(10) 0.135(7) Uani d SDU 1 . . C
H26A 1.0254 0.8222 0.9680 0.163 Uiso calc PR 0.50 . . H
H26B 0.9574 0.8484 0.9588 0.163 Uiso calc PR 0.50 . . H
C27 1.0000 0.8749(11) 1.0745(11) 0.150(7) Uani d SDU 1 . . C
H27A 1.0366 0.9004 1.0858 0.180 Uiso calc PR 0.50 . . H
H27B 0.9634 0.9004 1.0858 0.180 Uiso calc PR 0.50 . . H
C28 1.0000 0.8271(15) 1.1404(18) 0.252(14) Uani d SDU 1 . . C
H28A 1.0000 0.8448 1.2003 0.379 Uiso calc SR 1 . . H
H28B 1.0368 0.8021 1.1327 0.379 Uiso calc PR 0.50 . . H
H28C 0.9632 0.8021 1.1327 0.379 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'
U U -9.6767 9.6646 '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
O13 U1 O9 . . 136.8(3)
O13 U1 O5 . 4_755 96.00(18)
O9 U1 O5 . 4_755 98.84(18)
O13 U1 O5 . . 96.00(18)
O9 U1 O5 . . 98.84(18)
O5 U1 O5 4_755 . 138.8(3)
O13 U1 O10 . . 74.2(3)
O9 U1 O10 . . 149.0(3)
O5 U1 O10 4_755 . 72.86(17)
O5 U1 O10 . . 72.86(17)
O13 U1 O6 . . 152.6(3)
O9 U1 O6 . . 70.6(3)
O5 U1 O6 4_755 . 75.69(17)
O5 U1 O6 . . 75.68(17)
O10 U1 O6 . . 78.4(3)
O13 U1 O1 . 4_755 74.2(2)
O9 U1 O1 . 4_755 72.3(2)
O5 U1 O1 4_755 4_755 72.1(2)
O5 U1 O1 . 4_755 149.0(2)
O10 U1 O1 . 4_755 129.2(2)
O6 U1 O1 . 4_755 125.4(2)
O13 U1 O1 . . 74.2(2)
O9 U1 O1 . . 72.3(2)
O5 U1 O1 4_755 . 149.0(2)
O5 U1 O1 . . 72.1(2)
O10 U1 O1 . . 129.2(2)
O6 U1 O1 . . 125.4(2)
O1 U1 O1 4_755 . 77.0(3)
O2 Re1 O3 . . 109.1(4)
O2 Re1 O4 . . 108.7(4)
O3 Re1 O4 . . 108.7(4)
O2 Re1 O1 . . 110.5(3)
O3 Re1 O1 . . 109.3(3)
O4 Re1 O1 . . 110.5(4)
O8 Re2 O8 . 4_755 111.0(6)
O8 Re2 O7 . . 107.5(4)
O8 Re2 O7 4_755 . 107.5(4)
O8 Re2 O6 . . 110.7(3)
O8 Re2 O6 4_755 . 110.7(3)
O7 Re2 O6 . . 109.1(4)
O11 Re3 O11 4_755 . 109.1(8)
O11 Re3 O12 4_755 . 107.1(3)
O11 Re3 O12 . . 107.1(3)
O11 Re3 O10 4_755 . 111.6(3)
O11 Re3 O10 . . 111.6(3)
O12 Re3 O10 . . 110.2(4)
O5 P1 C1 . . 114.0(5)
O5 P1 C9 . . 111.1(4)
C1 P1 C9 . . 103.7(5)
O5 P1 C5 . . 108.2(4)
C1 P1 C5 . . 112.5(5)
C9 P1 C5 . . 107.1(4)
O9 P2 C13A . 4_755 114.6(7)
O9 P2 C13A . . 114.6(7)
C13A P2 C13A 4_755 . 71.7(11)
O9 P2 C17 . . 113.1(5)
C13A P2 C17 4_755 . 118.5(8)
C13A P2 C17 . . 118.5(8)
O9 P2 C13B . . 103.3(8)
C13A P2 C13B 4_755 . 107.8(10)
C13A P2 C13B . . 36.5(9)
C17 P2 C13B . . 96.5(10)
O9 P2 C13B . 4_755 103.3(8)
C13A P2 C13B 4_755 4_755 36.5(9)
C13A P2 C13B . 4_755 107.8(10)
C17 P2 C13B . 4_755 96.5(10)
C13B P2 C13B . 4_755 142.8(16)
O13 P3 C21 . . 107.9(4)
O13 P3 C21 . 4_755 107.9(4)
C21 P3 C21 . 4_755 113.1(9)
O13 P3 C25 . . 115.5(8)
C21 P3 C25 . . 91.6(10)
C21 P3 C25 4_755 . 119.5(10)
O13 P3 C25 . 4_755 115.5(8)
C21 P3 C25 . 4_755 119.5(10)
C21 P3 C25 4_755 4_755 91.6(10)
C25 P3 C25 . 4_755 32.2(19)
Re1 O1 U1 . . 150.4(4)
P1 O5 U1 . . 163.1(4)
Re2 O6 U1 . . 151.9(4)
P2 O9 U1 . . 156.4(6)
Re3 O10 U1 . . 153.5(5)
P3 O13 U1 . . 170.1(7)
C2 C1 P1 . . 117.4(9)
C2 C1 H1A . . 108.0
P1 C1 H1A . . 108.0
C2 C1 H1B . . 108.0
P1 C1 H1B . . 108.0
H1A C1 H1B . . 107.2
C1 C2 C3 . . 112.7(11)
C1 C2 H2A . . 109.0
C3 C2 H2A . . 109.0
C1 C2 H2B . . 109.0
C3 C2 H2B . . 109.0
H2A C2 H2B . . 107.8
C4 C3 C2 . . 111.8(13)
C4 C3 H3A . . 109.3
C2 C3 H3A . . 109.3
C4 C3 H3B . . 109.3
C2 C3 H3B . . 109.3
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 . . 117.0(7)
C6 C5 H5A . . 108.0
P1 C5 H5A . . 108.0
C6 C5 H5B . . 108.0
P1 C5 H5B . . 108.0
H5A C5 H5B . . 107.3
C5 C6 C7 . . 111.4(8)
C5 C6 H6A . . 109.3
C7 C6 H6A . . 109.3
C5 C6 H6B . . 109.3
C7 C6 H6B . . 109.3
H6A C6 H6B . . 108.0
C6 C7 C8 . . 112.1(8)
C6 C7 H7A . . 109.2
C8 C7 H7A . . 109.2
C6 C7 H7B . . 109.2
C8 C7 H7B . . 109.2
H7A C7 H7B . . 107.9
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 . . 113.4(7)
C10 C9 H9A . . 108.9
P1 C9 H9A . . 108.9
C10 C9 H9B . . 108.9
P1 C9 H9B . . 108.9
H9A C9 H9B . . 107.7
C9 C10 C11 . . 113.6(9)
C9 C10 H10A . . 108.9
C11 C10 H10A . . 108.9
C9 C10 H10B . . 108.9
C11 C10 H10B . . 108.9
H10A C10 H10B . . 107.7
C12 C11 C10 . . 112.6(10)
C12 C11 H11A . . 109.1
C10 C11 H11A . . 109.1
C12 C11 H11B . . 109.1
C10 C11 H11B . . 109.1
H11A C11 H11B . . 107.8
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 . . 106.9(11)
C14A C13A H13A . . 110.3
P2 C13A H13A . . 110.3
C14A C13A H13B . . 110.3
P2 C13A H13B . . 110.3
H13A C13A H13B . . 108.6
C13A C14A C15A . . 112.6(14)
C13A C14A H14A . . 109.1
C15A C14A H14A . . 109.1
C13A C14A H14B . . 109.1
C15A C14A H14B . . 109.1
H14A C14A H14B . . 107.8
C16A C15A C14A . . 113.7(15)
C16A C15A H15A . . 108.8
C14A C15A H15A . . 108.8
C16A C15A H15B . . 108.8
C14A C15A H15B . . 108.8
H15A C15A H15B . . 107.7
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 . . 127.5(18)
C14B C13B H13C . . 105.4
P2 C13B H13C . . 105.4
C14B C13B H13D . . 105.4
P2 C13B H13D . . 105.4
H13C C13B H13D . . 106.0
C13B C14B C15B . . 117(2)
C13B C14B H14C . . 108.2
C15B C14B H14C . . 108.2
C13B C14B H14D . . 108.2
C15B C14B H14D . . 108.2
H14C C14B H14D . . 107.3
C16B C15B C14B . . 107(2)
C16B C15B H15C . . 110.2
C14B C15B H15C . . 110.2
C16B C15B H15D . . 110.2
C14B C15B H15D . . 110.2
H15C C15B H15D . . 108.5
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 . . 116.4(10)
C18 C17 H17A . . 108.2
P2 C17 H17A . . 108.2
C18 C17 H17B . . 108.2
P2 C17 H17B . . 108.2
H17A C17 H17B . . 107.3
C17 C18 C19 . . 110.0(11)
C17 C18 H18A . . 109.7
C19 C18 H18A . . 109.7
C17 C18 H18B . . 109.7
C19 C18 H18B . . 109.7
H18A C18 H18B . . 108.2
C20 C19 C18 . . 107.5(12)
C20 C19 H19A . . 110.2
C18 C19 H19A . . 110.2
C20 C19 H19B . . 110.2
C18 C19 H19B . . 110.2
H19A C19 H19B . . 108.5
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 . . 119.6(8)
C22 C21 H21A . . 107.4
P3 C21 H21A . . 107.4
C22 C21 H21B . . 107.4
P3 C21 H21B . . 107.4
H21A C21 H21B . . 106.9
C21 C22 C23 . . 113.2(9)
C21 C22 H22A . . 108.9
C23 C22 H22A . . 108.9
C21 C22 H22B . . 108.9
C23 C22 H22B . . 108.9
H22A C22 H22B . . 107.8
C24 C23 C22 . . 113.2(10)
C24 C23 H23A . . 108.9
C22 C23 H23A . . 108.9
C24 C23 H23B . . 108.9
C22 C23 H23B . . 108.9
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 . . 122.5(16)
C26 C25 H25A . . 106.7
P3 C25 H25A . . 106.7
C26 C25 H25B . . 106.7
P3 C25 H25B . . 106.7
H25A C25 H25B . . 106.6
C25 C26 C27 . . 117.2(16)
C25 C26 H26A . . 108.0
C27 C26 H26A . . 108.0
C25 C26 H26B . . 108.0
C27 C26 H26B . . 108.0
H26A C26 H26B . . 107.3
C28 C27 C26 . . 120(2)
C28 C27 H27A . . 107.4
C26 C27 H27A . . 107.4
C28 C27 H27B . . 107.4
C26 C27 H27B . . 107.4
H27A C27 H27B . . 107.0
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
U1 O13 . 2.262(8)
U1 O9 . 2.271(8)
U1 O5 4_755 2.294(6)
U1 O5 . 2.294(6)
U1 O10 . 2.393(8)
U1 O6 . 2.407(8)
U1 O1 4_755 2.426(6)
U1 O1 . 2.426(6)
Re1 O2 . 1.674(8)
Re1 O3 . 1.688(8)
Re1 O4 . 1.696(7)
Re1 O1 . 1.750(6)
Re2 O8 . 1.689(7)
Re2 O8 4_755 1.689(7)
Re2 O7 . 1.703(10)
Re2 O6 . 1.769(8)
Re3 O11 4_755 1.661(8)
Re3 O11 . 1.661(8)
Re3 O12 . 1.677(9)
Re3 O10 . 1.757(8)
P1 O5 . 1.508(6)
P1 C1 . 1.770(12)
P1 C9 . 1.801(10)
P1 C5 . 1.806(10)
P2 O9 . 1.508(9)
P2 C13A 4_755 1.719(14)
P2 C13A . 1.719(14)
P2 C17 . 1.773(14)
P2 C13B . 1.865(16)
P2 C13B 4_755 1.865(16)
P3 O13 . 1.523(8)
P3 C21 . 1.742(11)
P3 C21 4_755 1.742(11)
P3 C25 . 1.76(2)
P3 C25 4_755 1.76(2)
C1 C2 . 1.481(13)
C1 H1A . 0.9800
C1 H1B . 0.9800
C2 C3 . 1.573(13)
C2 H2A . 0.9800
C2 H2B . 0.9800
C3 C4 . 1.474(14)
C3 H3A . 0.9800
C3 H3B . 0.9800
C4 H4A . 0.9700
C4 H4B . 0.9700
C4 H4C . 0.9700
C5 C6 . 1.512(10)
C5 H5A . 0.9800
C5 H5B . 0.9800
C6 C7 . 1.528(11)
C6 H6A . 0.9800
C6 H6B . 0.9800
C7 C8 . 1.532(12)
C7 H7A . 0.9800
C7 H7B . 0.9800
C8 H8A . 0.9700
C8 H8B . 0.9700
C8 H8C . 0.9700
C9 C10 . 1.516(11)
C9 H9A . 0.9800
C9 H9B . 0.9800
C10 C11 . 1.520(12)
C10 H10A . 0.9800
C10 H10B . 0.9800
C11 C12 . 1.498(13)
C11 H11A . 0.9800
C11 H11B . 0.9800
C12 H12A . 0.9700
C12 H12B . 0.9700
C12 H12C . 0.9700
C13A C14A . 1.497(16)
C13A H13A . 0.9800
C13A H13B . 0.9800
C14A C15A . 1.548(16)
C14A H14A . 0.9800
C14A H14B . 0.9800
C15A C16A . 1.526(17)
C15A H15A . 0.9800
C15A H15B . 0.9800
C16A H16A . 0.9700
C16A H16B . 0.9700
C16A H16C . 0.9700
C13B C14B . 1.504(18)
C13B H13C . 0.9800
C13B H13D . 0.9800
C14B C15B . 1.543(19)
C14B H14C . 0.9800
C14B H14D . 0.9800
C15B C16B . 1.527(19)
C15B H15C . 0.9800
C15B H15D . 0.9800
C16B H16D . 0.9700
C16B H16E . 0.9700
C16B H16F . 0.9700
C17 C18 . 1.518(12)
C17 H17A . 0.9800
C17 H17B . 0.9800
C18 C19 . 1.537(14)
C18 H18A . 0.9800
C18 H18B . 0.9800
C19 C20 . 1.521(15)
C19 H19A . 0.9800
C19 H19B . 0.9800
C20 H20A . 0.9700
C20 H20B . 0.9700
C20 H20C . 0.9700
C21 C22 . 1.521(11)
C21 H21A . 0.9800
C21 H21B . 0.9800
C22 C23 . 1.521(12)
C22 H22A . 0.9800
C22 H22B . 0.9800
C23 C24 . 1.494(13)
C23 H23A . 0.9800
C23 H23B . 0.9800
C24 H24A . 0.9700
C24 H24B . 0.9700
C24 H24C . 0.9700
C25 C26 . 1.469(17)
C25 H25A . 0.9800
C25 H25B . 0.9800
C26 C27 . 1.501(17)
C26 H26A . 0.9800
C26 H26B . 0.9800
C27 C28 . 1.432(18)
C27 H27A . 0.9800
C27 H27B . 0.9800
C28 H28A . 0.9700
C28 H28B . 0.9700
C28 H28C . 0.9700
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
C18 H18A O8 2_765 0.98 3.10 3.849(13) 134.4
C18 H18B O8 3_565 0.98 3.10 3.849(13) 134.4
C2 H2B O6 . 0.98 2.52 3.377(15) 145.6
C2 H2B O10 . 0.98 2.96 3.670(17) 130.5
C3 H3A O12 . 0.98 2.76 3.603(17) 144.5
C5 H5A O8 . 0.98 2.48 3.450(12) 168.6
C5 H5B O2 . 0.98 2.60 3.460(13) 147.1
C9 H9B O2 . 0.98 2.84 3.637(13) 139.5
C9 H9B O4 . 0.98 2.98 3.632(12) 125.2
C10 H10A O11 . 0.98 2.95 3.492(15) 116.2
C10 H10B O4 . 0.98 2.97 3.552(14) 119.2
C10 H10B O5 . 0.98 2.88 3.238(12) 102.7
C14A H14B O9 . 0.98 2.74 3.176(17) 107.5
C14A H14B O9 . 0.98 2.74 3.176(17) 107.5
C17 H17B O1 . 0.98 2.67 3.327(12) 124.4
C17 H17B O3 . 0.98 2.94 3.915(11) 174.0
C26 H26B O1 . 0.98 2.91 3.529(18) 122.3
C4 H4A O2 6_664 0.97 2.96 3.854(19) 154.2
C6 H6A O4 6_664 0.98 2.95 3.620(12) 126.4
C6 H6B O3 6_664 0.98 2.74 3.548(12) 139.8
C8 H8B O4 6_664 0.97 2.71 3.608(14) 153.4
C9 H9A O3 6_664 0.98 2.75 3.717(11) 170.8
C12 H12A O3 6_664 0.97 2.97 3.771(15) 140.9
C14B H14C O7 2_765 0.98 2.83 3.48(3) 124.7
C14B H14D O8 2_765 0.98 2.90 3.78(3) 150.7
C13A H13A O7 2_765 0.98 2.71 3.60(2) 151.0
C13A H13A O7 2_765 0.98 2.71 3.60(2) 151.0
C14B H14C O7 2_765 0.98 2.83 3.48(3) 124.7
C13A H13A O7 3_565 0.98 2.71 3.60(2) 151.0
C14B H14C O7 3_565 0.98 2.83 3.48(3) 124.7
C13A H13A O7 3_565 0.98 2.71 3.60(2) 151.0
C14B H14C O7 3_565 0.98 2.83 3.48(3) 124.7
C17 H17A O1 4_755 0.98 2.67 3.327(12) 124.4
C17 H17A O3 4_755 0.98 2.94 3.915(12) 174.0
C13A H13B O8 4_755 0.98 2.86 3.59(2) 131.9
C13B H13D O2 4_755 0.98 3.05 3.65(3) 121.0
C21 H21A O4 4_755 0.98 2.69 3.620(15) 158.4
C21 H21B O11 4_755 0.98 2.64 3.524(15) 149.9
C25 H25A O4 4_755 0.98 2.92 3.75(3) 143.2
C26 H26A O1 4_755 0.98 2.73 3.529(18) 138.7
C26 H26A O3 4_755 0.98 2.97 3.861(15) 152.5
C14A H14B O2 4_755 0.98 2.93 3.502(18) 118.3
C20 H20A O7 1_556 0.97 2.73 3.531(18) 139.8
C28 H28A O12 1_556 0.97 2.99 3.94(3) 165.9
C20 H20A O7 4_756 0.97 2.73 3.531(18) 139.8
C28 H28A O12 4_756 0.97 2.99 3.94(3) 165.9
C22 H22A O11 2_775 0.98 2.94 3.634(13) 128.8
C22 H22B O12 2_775 0.98 2.77 3.559(13) 138.3
C24 H24B O11 2_775 0.97 2.91 3.69(2) 138.3
C22 H22B O12 3_575 0.98 2.77 3.559(13) 138.3
C16B H16F O4 5_545 0.97 3.02 3.84(3) 144.0
C16A H16A O7 2_765 0.97 3.28 3.84(2) 118.9
C16A H16B O8 2_765 0.97 3.11 3.94(2) 144.9
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 U1 . 59.0(8)
O3 Re1 O1 U1 . 179.0(7)
O4 Re1 O1 U1 . -61.4(8)
O13 U1 O1 Re1 . 91.9(7)
O9 U1 O1 Re1 . -115.8(7)
O5 U1 O1 Re1 4_755 166.8(5)
O5 U1 O1 Re1 . -10.0(7)
O10 U1 O1 Re1 . 38.4(8)
O6 U1 O1 Re1 . -66.8(8)
O1 U1 O1 Re1 4_755 168.9(6)
C1 P1 O5 U1 . -46.2(16)
C9 P1 O5 U1 . -162.9(13)
C5 P1 O5 U1 . 79.8(15)
O13 U1 O5 P1 . 137.7(14)
O9 U1 O5 P1 . -83.0(14)
O5 U1 O5 P1 4_755 31.4(18)
O10 U1 O5 P1 . 66.2(14)
O6 U1 O5 P1 . -15.8(14)
O1 U1 O5 P1 4_755 -153.2(12)
O1 U1 O5 P1 . -151.1(15)
O8 Re2 O6 U1 . 61.8(3)
O8 Re2 O6 U1 4_755 -61.8(3)
O7 Re2 O6 U1 . 180.000(2)
O13 U1 O6 Re2 . 180.0
O9 U1 O6 Re2 . 0.000(3)
O5 U1 O6 Re2 4_755 104.97(17)
O5 U1 O6 Re2 . -104.96(17)
O10 U1 O6 Re2 . 180.000(4)
O1 U1 O6 Re2 4_755 49.8(2)
O1 U1 O6 Re2 . -49.8(2)
C13A P2 O9 U1 4_755 139.9(7)
C13A P2 O9 U1 . -139.9(7)
C17 P2 O9 U1 . 0.000(5)
C13B P2 O9 U1 . -103.1(9)
C13B P2 O9 U1 4_755 103.1(9)
O13 U1 O9 P2 . 0.000(5)
O5 U1 O9 P2 4_755 108.68(17)
O5 U1 O9 P2 . -108.68(17)
O10 U1 O9 P2 . 180.000(3)
O6 U1 O9 P2 . 180.000(4)
O1 U1 O9 P2 4_755 40.78(17)
O1 U1 O9 P2 . -40.78(17)
O11 Re3 O10 U1 4_755 61.2(4)
O11 Re3 O10 U1 . -61.2(4)
O12 Re3 O10 U1 . 180.000(3)
O13 U1 O10 Re3 . 0.000(3)
O9 U1 O10 Re3 . 180.0
O5 U1 O10 Re3 4_755 -101.59(18)
O5 U1 O10 Re3 . 101.59(18)
O6 U1 O10 Re3 . 180.000(3)
O1 U1 O10 Re3 4_755 -53.4(2)
O1 U1 O10 Re3 . 53.4(2)
C21 P3 O13 U1 . 118.7(5)
C21 P3 O13 U1 4_755 -118.7(5)
C25 P3 O13 U1 . 17.9(11)
C25 P3 O13 U1 4_755 -17.9(11)
O9 U1 O13 P3 . 0.000(15)
O5 U1 O13 P3 4_755 -109.74(17)
O5 U1 O13 P3 . 109.74(17)
O10 U1 O13 P3 . 180.000(13)
O6 U1 O13 P3 . 180.000(10)
O1 U1 O13 P3 4_755 -40.29(17)
O1 U1 O13 P3 . 40.29(17)
O5 P1 C1 C2 . 65.8(11)
C9 P1 C1 C2 . -173.3(10)
C5 P1 C1 C2 . -57.8(12)
P1 C1 C2 C3 . -175.7(9)
C1 C2 C3 C4 . -69.1(17)
O5 P1 C5 C6 . 179.3(7)
C1 P1 C5 C6 . -53.9(10)
C9 P1 C5 C6 . 59.5(9)
P1 C5 C6 C7 . -179.2(8)
C5 C6 C7 C8 . -179.3(11)
O5 P1 C9 C10 . 57.5(8)
C1 P1 C9 C10 . -65.4(8)
C5 P1 C9 C10 . 175.4(7)
P1 C9 C10 C11 . -179.6(8)
C9 C10 C11 C12 . -67.7(14)
O9 P2 C13A C14A . 66.3(15)
C13A P2 C13A C14A 4_755 175.6(9)
C17 P2 C13A C14A . -71.3(15)
C13B P2 C13A C14A . -12.5(18)
C13B P2 C13A C14A 4_755 -179.3(14)
P2 C13A C14A C15A . -172.8(13)
C13A C14A C15A C16A . -62(2)
O9 P2 C13B C14B . -143(3)
C13A P2 C13B C14B 4_755 -21(3)
C13A P2 C13B C14B . -29(2)
C17 P2 C13B C14B . 102(3)
C13B P2 C13B C14B 4_755 -8(5)
P2 C13B C14B C15B . 159(3)
C13B C14B C15B C16B . 177(3)
O9 P2 C17 C18 . 180.000(4)
C13A P2 C17 C18 4_755 41.8(6)
C13A P2 C17 C18 . -41.8(6)
C13B P2 C17 C18 . -72.5(8)
C13B P2 C17 C18 4_755 72.5(8)
P2 C17 C18 C19 . 180.000(6)
C17 C18 C19 C20 . 180.000(7)
O13 P3 C21 C22 . -170.7(10)
C21 P3 C21 C22 4_755 70.0(14)
C25 P3 C21 C22 . -53.1(14)
C25 P3 C21 C22 4_755 -36.0(15)
P3 C21 C22 C23 . 176.9(10)
C21 C22 C23 C24 . 178.6(14)
O13 P3 C25 C26 . -44(2)
C21 P3 C25 C26 . -155(2)
C21 P3 C25 C26 4_755 87(2)
C25 P3 C25 C26 4_755 54(2)
P3 C25 C26 C27 . -155.5(13)
C25 C26 C27 C28 . -158.1(15)
