#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/03/2100396.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_2100396
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 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                   21.4344(15)
_cell_length_b                   21.7929(15)
_cell_length_c                   14.7782(10)
_cell_measurement_reflns_used    7236
_cell_measurement_temperature    165(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.67
_cell_volume                     6903.2(8)
_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      165(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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0337
_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            24887
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    9.480
_exptl_absorpt_correction_T_max  0.4507
_exptl_absorpt_correction_T_min  0.3305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_meas      0
_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         2.332
_refine_diff_density_min         -1.209
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0227P)²+46.4030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                6171
_reflns_number_total             6428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ws5025.cif
_cod_data_source_block           Iat165
_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_sg_symbol_H-M      Cmc2(1)
_cod_database_code               2100396
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 0.748665(16) 0.70241(3) 0.01972(9) Uani d S 1 . . U
Re1 0.854642(15) 0.762088(15) 0.87518(2) 0.03206(9) Uani d . 1 . . Re
Re2 1.0000 0.59180(2) 0.55403(3) 0.02911(11) Uani d S 1 . . Re
Re3 1.0000 0.87773(2) 0.50691(3) 0.02897(11) Uani d S 1 . . Re
P1 0.84170(10) 0.73947(11) 0.59145(15) 0.0319(5) Uani d . 1 . . P
P2 1.0000 0.61055(18) 0.8492(3) 0.0606(12) Uani d SD 1 . . P
P3 1.0000 0.91022(14) 0.7943(2) 0.0391(8) Uani d S 1 . . P
O1 0.9298(3) 0.7540(3) 0.8311(4) 0.0441(16) Uani d . 1 . . O
O2 0.8064(3) 0.7095(4) 0.8319(6) 0.064(2) Uani d . 1 . . O
O3 0.8573(3) 0.7524(4) 0.9895(5) 0.057(2) Uani d . 1 . . O
O4 0.8262(4) 0.8328(4) 0.8510(5) 0.068(2) Uani d . 1 . . O
O5 0.8997(3) 0.7497(3) 0.6491(4) 0.0359(14) Uani d . 1 . . O
O6 1.0000 0.6688(3) 0.5899(5) 0.037(2) Uani d S 1 . . O
O7 1.0000 0.5895(5) 0.4374(6) 0.061(3) Uani d S 1 . . O
O8 0.9351(4) 0.5555(3) 0.5909(6) 0.064(2) Uani d . 1 . . O
O9 1.0000 0.6548(4) 0.7699(6) 0.053(3) Uani d S 1 A . O
O10 1.0000 0.8075(4) 0.5641(5) 0.039(2) Uani d S 1 . . O
O11 0.9373(5) 0.9194(4) 0.5316(6) 0.090(3) Uani d . 1 . . O
O12 1.0000 0.8653(4) 0.3935(6) 0.062(3) Uani d S 1 . . O
O13 1.0000 0.8482(4) 0.7462(6) 0.050(2) Uani d S 1 . . O
C1 0.8548(4) 0.7545(5) 0.4730(6) 0.041(2) Uani d . 1 . . C
H1A 0.8142 0.7518 0.4412 0.049 Uiso calc R 1 . . H
H1B 0.8698 0.7973 0.4667 0.049 Uiso calc R 1 . . H
C2 0.9000(5) 0.7132(5) 0.4261(7) 0.052(3) Uani d . 1 . . C
H2A 0.8838 0.6706 0.4271 0.062 Uiso calc R 1 . . H
H2B 0.9402 0.7137 0.4589 0.062 Uiso calc R 1 . . H
C3 0.9108(6) 0.7334(6) 0.3261(7) 0.064(3) Uani d . 1 . . C
H3A 0.9256 0.7764 0.3255 0.077 Uiso calc R 1 . . H
H3B 0.9441 0.7076 0.2995 0.077 Uiso calc R 1 . . H
C4 0.8546(6) 0.7286(6) 0.2692(10) 0.073(4) Uani d . 1 . . C
H4A 0.8230 0.7577 0.2908 0.109 Uiso calc R 1 . . H
H4B 0.8379 0.6868 0.2727 0.109 Uiso calc R 1 . . H
H4C 0.8653 0.7382 0.2063 0.109 Uiso calc R 1 . . H
C5 0.8157(4) 0.6619(4) 0.6081(6) 0.038(2) Uani d . 1 . . C
H5A 0.8506 0.6341 0.5923 0.045 Uiso calc R 1 . . H
H5B 0.8071 0.6562 0.6734 0.045 Uiso calc R 1 . . H
C6 0.7585(4) 0.6410(4) 0.5559(7) 0.045(2) Uani d . 1 . . C
H6A 0.7229 0.6680 0.5715 0.054 Uiso calc R 1 . . H
H6B 0.7666 0.6454 0.4903 0.054 Uiso calc R 1 . . H
C7 0.7413(5) 0.5757(5) 0.5759(8) 0.058(3) Uani d . 1 . . C
H7A 0.7318 0.5719 0.6413 0.069 Uiso calc R 1 . . H
H7B 0.7776 0.5491 0.5626 0.069 Uiso calc R 1 . . H
C8 0.6852(7) 0.5531(6) 0.5215(10) 0.090(5) Uani d . 1 . . C
H8A 0.6863 0.5082 0.5177 0.135 Uiso calc R 1 . . H
H8B 0.6866 0.5705 0.4605 0.135 Uiso calc R 1 . . H
H8C 0.6466 0.5659 0.5516 0.135 Uiso calc R 1 . . H
C9 0.7800(4) 0.7911(4) 0.6246(6) 0.038(2) Uani d . 1 . . C
H9A 0.7434 0.7839 0.5853 0.045 Uiso calc R 1 . . H
H9B 0.7676 0.7817 0.6876 0.045 Uiso calc R 1 . . H
C10 0.7985(5) 0.8582(4) 0.6185(7) 0.046(2) Uani d . 1 . . C
H10A 0.8354 0.8653 0.6574 0.055 Uiso calc R 1 . . H
H10B 0.8106 0.8677 0.5554 0.055 Uiso calc R 1 . . H
C11 0.7467(5) 0.9018(4) 0.6473(8) 0.053(3) Uani d . 1 . . C
H11A 0.7314 0.8896 0.7079 0.064 Uiso calc R 1 . . H
H11B 0.7639 0.9439 0.6521 0.064 Uiso calc R 1 . . H
C12 0.6931(6) 0.9023(6) 0.5827(11) 0.080(4) Uani d . 1 . . C
H12A 0.6691 0.8643 0.5893 0.121 Uiso calc R 1 . . H
H12B 0.7089 0.9055 0.5206 0.121 Uiso calc R 1 . . H
H12C 0.6662 0.9376 0.5957 0.121 Uiso calc R 1 . . H
C13A 1.0483(7) 0.5488(7) 0.8327(12) 0.063(4) Uani d PDU 0.687(16) A 1 C
H13A 1.0443 0.5195 0.8835 0.076 Uiso calc PR 0.687(16) A 1 H
H13B 1.0372 0.5273 0.7759 0.076 Uiso calc PR 0.687(16) A 1 H
C14A 1.1110(9) 0.5715(8) 0.8276(13) 0.066(4) Uani d PU 0.687(16) A 1 C
H14A 1.1222 0.5897 0.8868 0.080 Uiso calc PR 0.687(16) A 1 H
H14B 1.1127 0.6046 0.7818 0.080 Uiso calc PR 0.687(16) A 1 H
C15A 1.1603(11) 0.5221(9) 0.8029(14) 0.063(4) Uani d PU 0.687(16) A 1 C
H15A 1.1546 0.5104 0.7387 0.075 Uiso calc PR 0.687(16) A 1 H
H15B 1.2024 0.5404 0.8089 0.075 Uiso calc PR 0.687(16) A 1 H
C16A 1.1576(10) 0.4651(11) 0.8598(17) 0.065(5) Uani d PU 0.687(16) A 1 C
H16A 1.1302 0.4349 0.8308 0.097 Uiso calc PR 0.687(16) A 1 H
H16B 1.1413 0.4752 0.9198 0.097 Uiso calc PR 0.687(16) A 1 H
H16C 1.1996 0.4478 0.8658 0.097 Uiso calc PR 0.687(16) A 1 H
C13B 1.0810(10) 0.5803(16) 0.860(3) 0.061(6) Uani d PDU 0.313(16) A 2 C
H13C 1.1023 0.5966 0.8056 0.074 Uiso calc PR 0.313(16) A 2 H
H13D 1.0984 0.6036 0.9115 0.074 Uiso calc PR 0.313(16) A 2 H
C14B 1.1061(17) 0.5231(17) 0.870(3) 0.066(5) Uani d PU 0.313(16) A 2 C
H14C 1.0754 0.4942 0.8439 0.079 Uiso calc PR 0.313(16) A 2 H
H14D 1.1066 0.5150 0.9361 0.079 Uiso calc PR 0.313(16) A 2 H
C15B 1.170(3) 0.503(3) 0.834(4) 0.070(6) Uani d PU 0.313(16) A 2 C
H15C 1.1703 0.5029 0.7675 0.084 Uiso calc PR 0.313(16) A 2 H
H15D 1.2030 0.5312 0.8559 0.084 Uiso calc PR 0.313(16) A 2 H
C16B 1.181(3) 0.448(2) 0.864(4) 0.076(9) Uani d PU 0.313(16) A 2 C
H16D 1.1478 0.4199 0.8444 0.115 Uiso calc PR 0.313(16) A 2 H
H16E 1.1828 0.4481 0.9306 0.115 Uiso calc PR 0.313(16) A 2 H
H16F 1.2212 0.4330 0.8404 0.115 Uiso calc PR 0.313(16) A 2 H
C17 1.0000 0.6464(6) 0.9574(9) 0.045(3) Uani d SU 1 A . C
H17A 1.0372 0.6731 0.9618 0.054 Uiso calc PR 0.50 . . H
H17B 0.9628 0.6731 0.9618 0.054 Uiso calc PR 0.50 . . H
C18 1.0000 0.6031(6) 1.0370(8) 0.047(3) Uani d SU 1 . . C
H18A 0.9627 0.5765 1.0338 0.056 Uiso calc PR 0.50 A . H
H18B 1.0373 0.5765 1.0338 0.056 Uiso calc PR 0.50 . . H
C19 1.0000 0.6365(7) 1.1246(10) 0.066(4) Uani d SU 1 A . C
H19A 0.9626 0.6630 1.1284 0.080 Uiso calc PR 0.50 . . H
H19B 1.0374 0.6630 1.1284 0.080 Uiso calc PR 0.50 . . H
C20 1.0000 0.5914(8) 1.2030(11) 0.081(6) Uani d SU 1 . . C
H20A 1.0000 0.6141 1.2603 0.121 Uiso calc SR 1 A . H
H20B 1.0373 0.5656 1.1996 0.121 Uiso calc PR 0.50 . . H
H20C 0.9627 0.5656 1.1996 0.121 Uiso calc PR 0.50 . . H
C21 1.0683(6) 0.9487(6) 0.7648(10) 0.084(5) Uani d . 1 . . C
H21A 1.1034 0.9198 0.7737 0.100 Uiso calc R 1 . . H
H21B 1.0661 0.9577 0.6992 0.100 Uiso calc R 1 . . H
C22 1.0850(5) 1.0084(5) 0.8131(9) 0.065(3) Uani d . 1 . . C
H22A 1.0519 1.0390 0.8013 0.078 Uiso calc R 1 . . H
H22B 1.0862 1.0008 0.8791 0.078 Uiso calc R 1 . . H
C23 1.1462(6) 1.0345(7) 0.7843(12) 0.094(6) Uani d . 1 . . C
H23A 1.1793 1.0042 0.7983 0.112 Uiso calc R 1 . . H
H23B 1.1455 1.0401 0.7178 0.112 Uiso calc R 1 . . H
C24 1.1628(6) 1.0928(7) 0.8262(13) 0.109(7) Uani d . 1 . . C
H24A 1.2059 1.1034 0.8101 0.163 Uiso calc R 1 . . H
H24B 1.1593 1.0893 0.8921 0.163 Uiso calc R 1 . . H
H24C 1.1346 1.1250 0.8045 0.163 Uiso calc R 1 . . H
C25 1.0227(10) 0.9061(10) 0.9119(12) 0.059(5) Uani d PU 0.50 . . C
H25A 1.0686 0.9014 0.9124 0.071 Uiso calc PR 0.50 . . H
H25B 1.0138 0.9470 0.9381 0.071 Uiso calc PR 0.50 . . H
C26 1.0000 0.8641(9) 0.9724(9) 0.084(5) Uani d SDU 1 . . C
H26A 1.0233 0.8255 0.9620 0.101 Uiso calc PR 0.50 . . H
H26B 0.9562 0.8559 0.9549 0.101 Uiso calc PR 0.50 . . H
C27 1.0000 0.8748(8) 1.0714(9) 0.087(5) Uani d SDU 1 . . C
H27A 1.0370 0.9003 1.0849 0.104 Uiso calc PR 0.50 . . H
H27B 0.9630 0.9003 1.0849 0.104 Uiso calc PR 0.50 . . H
C28 1.0000 0.8245(12) 1.1371(16) 0.191(12) Uani d SDU 1 . . C
H28A 1.0000 0.8415 1.1986 0.287 Uiso calc SR 1 . . H
H28B 1.0373 0.7993 1.1284 0.287 Uiso calc PR 0.50 . . H
H28C 0.9627 0.7993 1.1284 0.287 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 . . 137.4(3)
O13 U1 O5 . . 95.11(17)
O9 U1 O5 . . 99.17(17)
O13 U1 O5 . 4_755 95.11(17)
O9 U1 O5 . 4_755 99.17(17)
O5 U1 O5 . 4_755 139.8(3)
O13 U1 O6 . . 152.9(3)
O9 U1 O6 . . 69.7(3)
O5 U1 O6 . . 76.67(16)
O5 U1 O6 4_755 . 76.67(16)
O13 U1 O10 . . 74.5(3)
O9 U1 O10 . . 148.1(3)
O5 U1 O10 . . 72.76(15)
O5 U1 O10 4_755 . 72.76(15)
O6 U1 O10 . . 78.4(3)
O13 U1 O1 . 4_755 74.3(2)
O9 U1 O1 . 4_755 72.5(2)
O5 U1 O1 . 4_755 148.3(2)
O5 U1 O1 4_755 4_755 71.8(2)
O6 U1 O1 . 4_755 125.2(2)
O10 U1 O1 . 4_755 129.6(2)
O13 U1 O1 . . 74.3(2)
O9 U1 O1 . . 72.5(2)
O5 U1 O1 . . 71.8(2)
O5 U1 O1 4_755 . 148.3(2)
O6 U1 O1 . . 125.2(2)
O10 U1 O1 . . 129.6(2)
O1 U1 O1 4_755 . 76.6(3)
O2 Re1 O4 . . 108.7(4)
O2 Re1 O3 . . 108.3(4)
O4 Re1 O3 . . 109.5(4)
O2 Re1 O1 . . 111.0(3)
O4 Re1 O1 . . 110.1(4)
O3 Re1 O1 . . 109.1(3)
O8 Re2 O8 . 4_755 110.7(5)
O8 Re2 O7 . . 108.0(3)
O8 Re2 O7 4_755 . 108.0(3)
O8 Re2 O6 . . 110.4(3)
O8 Re2 O6 4_755 . 110.4(3)
O7 Re2 O6 . . 109.2(4)
O11 Re3 O11 4_755 . 107.9(8)
O11 Re3 O12 4_755 . 107.7(4)
O11 Re3 O12 . . 107.7(4)
O11 Re3 O10 4_755 . 111.8(3)
O11 Re3 O10 . . 111.8(3)
O12 Re3 O10 . . 109.7(4)
O5 P1 C5 . . 108.2(4)
O5 P1 C1 . . 112.9(4)
C5 P1 C1 . . 110.6(4)
O5 P1 C9 . . 110.8(4)
C5 P1 C9 . . 108.8(4)
C1 P1 C9 . . 105.3(5)
O9 P2 C13A . 4_755 112.9(7)
O9 P2 C13A . . 112.9(7)
C13A P2 C13A 4_755 . 74.3(12)
O9 P2 C17 . . 114.5(6)
C13A P2 C17 4_755 . 118.2(7)
C13A P2 C17 . . 118.2(7)
O9 P2 C13B . . 106.9(13)
C13A P2 C13B 4_755 . 107.3(14)
C13A P2 C13B . . 34.1(12)
C17 P2 C13B . . 94.5(13)
O9 P2 C13B . 4_755 106.9(13)
C13A P2 C13B 4_755 4_755 34.1(12)
C13A P2 C13B . 4_755 107.3(14)
C17 P2 C13B . 4_755 94.5(13)
C13B P2 C13B . 4_755 137(2)
O13 P3 C21 . 4_755 108.0(4)
O13 P3 C21 . . 108.0(4)
C21 P3 C21 4_755 . 114.3(11)
O13 P3 C25 . . 113.8(8)
C21 P3 C25 4_755 . 119.4(8)
C21 P3 C25 . . 92.2(9)
O13 P3 C25 . 4_755 113.8(8)
C21 P3 C25 4_755 4_755 92.2(9)
C21 P3 C25 . 4_755 119.4(8)
C25 P3 C25 . 4_755 31.2(14)
Re1 O1 U1 . . 150.3(4)
P1 O5 U1 . . 163.2(4)
Re2 O6 U1 . . 153.9(4)
P2 O9 U1 . . 155.5(6)
Re3 O10 U1 . . 151.0(5)
P3 O13 U1 . . 168.9(6)
C2 C1 P1 . . 116.2(8)
C2 C1 H1A . . 108.2
P1 C1 H1A . . 108.2
C2 C1 H1B . . 108.2
P1 C1 H1B . . 108.2
H1A C1 H1B . . 107.4
C1 C2 C3 . . 111.5(9)
C1 C2 H2A . . 109.3
C3 C2 H2A . . 109.3
C1 C2 H2B . . 109.3
C3 C2 H2B . . 109.3
H2A C2 H2B . . 108.0
C4 C3 C2 . . 113.5(11)
C4 C3 H3A . . 108.9
C2 C3 H3A . . 108.9
C4 C3 H3B . . 108.9
C2 C3 H3B . . 108.9
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 . . 117.5(6)
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 . . 112.4(8)
C7 C6 H6A . . 109.1
C5 C6 H6A . . 109.1
C7 C6 H6B . . 109.1
C5 C6 H6B . . 109.1
H6A C6 H6B . . 107.9
C6 C7 C8 . . 113.3(9)
C6 C7 H7A . . 108.9
C8 C7 H7A . . 108.9
C6 C7 H7B . . 108.9
C8 C7 H7B . . 108.9
H7A C7 H7B . . 107.7
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 . . 113.2(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
C11 C10 C9 . . 113.3(8)
C11 C10 H10A . . 108.9
C9 C10 H10A . . 108.9
C11 C10 H10B . . 108.9
C9 C10 H10B . . 108.9
H10A C10 H10B . . 107.7
C12 C11 C10 . . 112.8(10)
C12 C11 H11A . . 109.0
C10 C11 H11A . . 109.0
C12 C11 H11B . . 109.0
C10 C11 H11B . . 109.0
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 . . 107.6(13)
C14A C13A H13A . . 110.2
P2 C13A H13A . . 110.2
C14A C13A H13B . . 110.2
P2 C13A H13B . . 110.2
H13A C13A H13B . . 108.5
C13A C14A C15A . . 114.2(16)
C13A C14A H14A . . 108.7
C15A C14A H14A . . 108.7
C13A C14A H14B . . 108.7
C15A C14A H14B . . 108.7
H14A C14A H14B . . 107.6
C16A C15A C14A . . 114.6(16)
C16A C15A H15A . . 108.6
C14A C15A H15A . . 108.6
C16A C15A H15B . . 108.6
C14A C15A H15B . . 108.6
H15A C15A H15B . . 107.6
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 . . 134(3)
C14B C13B H13C . . 103.6
P2 C13B H13C . . 103.6
C14B C13B H13D . . 103.6
P2 C13B H13D . . 103.6
H13C C13B H13D . . 105.3
C13B C14B C15B . . 125(4)
C13B C14B H14C . . 106.0
C15B C14B H14C . . 106.0
C13B C14B H14D . . 106.0
C15B C14B H14D . . 106.0
H14C C14B H14D . . 106.3
C16B C15B C14B . . 108(5)
C16B C15B H15C . . 110.1
C14B C15B H15C . . 110.1
C16B C15B H15D . . 110.0
C14B C15B H15D . . 110.1
H15C C15B H15D . . 108.4
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 . . 115.2(9)
C18 C17 H17A . . 108.5
P2 C17 H17A . . 108.5
C18 C17 H17B . . 108.5
P2 C17 H17B . . 108.5
H17A C17 H17B . . 107.5
C19 C18 C17 . . 111.9(11)
C19 C18 H18A . . 109.2
C17 C18 H18A . . 109.2
C19 C18 H18B . . 109.2
C17 C18 H18B . . 109.2
H18A C18 H18B . . 107.9
C18 C19 C20 . . 110.4(13)
C18 C19 H19A . . 109.6
C20 C19 H19A . . 109.6
C18 C19 H19B . . 109.6
C20 C19 H19B . . 109.6
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 . . 119.4(9)
C22 C21 H21A . . 107.5
P3 C21 H21A . . 107.5
C22 C21 H21B . . 107.5
P3 C21 H21B . . 107.5
H21A C21 H21B . . 107.0
C23 C22 C21 . . 113.4(9)
C23 C22 H22A . . 108.9
C21 C22 H22A . . 108.9
C23 C22 H22B . . 108.9
C21 C22 H22B . . 108.9
H22A C22 H22B . . 107.7
C24 C23 C22 . . 115.2(11)
C24 C23 H23A . . 108.5
C22 C23 H23A . . 108.5
C24 C23 H23B . . 108.5
C22 C23 H23B . . 108.5
H23A C23 H23B . . 107.5
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 . . 124.5(15)
C26 C25 H25A . . 106.2
P3 C25 H25A . . 106.2
C26 C25 H25B . . 106.2
P3 C25 H25B . . 106.2
H25A C25 H25B . . 106.4
C25 C26 C27 . . 122.7(16)
C25 C26 H26A . . 106.7
C27 C26 H26A . . 106.7
C25 C26 H26B . . 106.7
C27 C26 H26B . . 106.7
H26A C26 H26B . . 106.6
C28 C27 C26 . . 123(2)
C28 C27 H27A . . 106.7
C26 C27 H27A . . 106.7
C28 C27 H27B . . 106.7
C26 C27 H27B . . 106.7
H27A C27 H27B . . 106.6
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 . 2.263(9)
U1 O9 . 2.275(9)
U1 O5 . 2.289(6)
U1 O5 4_755 2.289(6)
U1 O6 . 2.406(7)
U1 O10 . 2.413(8)
U1 O1 4_755 2.428(6)
U1 O1 . 2.428(6)
Re1 O2 . 1.670(8)
Re1 O4 . 1.695(8)
Re1 O3 . 1.703(7)
Re1 O1 . 1.747(7)
Re2 O8 . 1.691(8)
Re2 O8 4_755 1.691(8)
Re2 O7 . 1.724(9)
Re2 O6 . 1.760(7)
Re3 O11 4_755 1.663(9)
Re3 O11 . 1.663(9)
Re3 O12 . 1.697(9)
Re3 O10 . 1.748(8)
P1 O5 . 1.524(6)
P1 C5 . 1.798(9)
P1 C1 . 1.803(9)
P1 C9 . 1.803(9)
P2 O9 . 1.518(9)
P2 C13A 4_755 1.716(14)
P2 C13A . 1.716(14)
P2 C17 . 1.780(14)
P2 C13B . 1.863(19)
P2 C13B 4_755 1.863(19)
P3 O13 . 1.528(9)
P3 C21 4_755 1.743(12)
P3 C21 . 1.743(12)
P3 C25 . 1.807(19)
P3 C25 4_755 1.807(19)
C1 C2 . 1.494(14)
C1 H1A . 0.9900
C1 H1B . 0.9900
C2 C3 . 1.559(14)
C2 H2A . 0.9900
C2 H2B . 0.9900
C3 C4 . 1.474(17)
C3 H3A . 0.9900
C3 H3B . 0.9900
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
C5 C6 . 1.519(12)
C5 H5A . 0.9900
C5 H5B . 0.9900
C6 C7 . 1.500(13)
C6 H6A . 0.9900
C6 H6B . 0.9900
C7 C8 . 1.529(15)
C7 H7A . 0.9900
C7 H7B . 0.9900
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 0.9800
C9 C10 . 1.518(12)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 C11 . 1.522(14)
C10 H10A . 0.9900
C10 H10B . 0.9900
C11 C12 . 1.493(15)
C11 H11A . 0.9900
C11 H11B . 0.9900
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C13A C14A . 1.43(2)
C13A H13A . 0.9900
C13A H13B . 0.9900
C14A C15A . 1.55(3)
C14A H14A . 0.9900
C14A H14B . 0.9900
C15A C16A . 1.50(3)
C15A H15A . 0.9900
C15A H15B . 0.9900
C16A H16A . 0.9800
C16A H16B . 0.9800
C16A H16C . 0.9800
C13B C14B . 1.37(5)
C13B H13C . 0.9900
C13B H13D . 0.9900
C14B C15B . 1.54(6)
C14B H14C . 0.9900
C14B H14D . 0.9900
C15B C16B . 1.30(7)
C15B H15C . 0.9900
C15B H15D . 0.9900
C16B H16D . 0.9800
C16B H16E . 0.9800
C16B H16F . 0.9800
C17 C18 . 1.508(16)
C17 H17A . 0.9900
C17 H17B . 0.9900
C18 C19 . 1.49(2)
C18 H18A . 0.9900
C18 H18B . 0.9900
C19 C20 . 1.52(2)
C19 H19A . 0.9900
C19 H19B . 0.9900
C20 H20A . 0.9800
C20 H20B . 0.9800
C20 H20C . 0.9800
C21 C22 . 1.527(14)
C21 H21A . 0.9900
C21 H21B . 0.9900
C22 C23 . 1.490(16)
C22 H22A . 0.9900
C22 H22B . 0.9900
C23 C24 . 1.459(17)
C23 H23A . 0.9900
C23 H23B . 0.9900
C24 H24A . 0.9800
C24 H24B . 0.9800
C24 H24C . 0.9800
C25 C26 . 1.37(3)
C25 H25A . 0.9900
C25 H25B . 0.9900
C26 C27 . 1.481(15)
C26 H26A . 0.9900
C26 H26B . 0.9900
C27 C28 . 1.463(17)
C27 H27A . 0.9900
C27 H27B . 0.9900
C28 H28A . 0.9800
C28 H28B . 0.9800
C28 H28C . 0.9800
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 . 55.6(8)
O4 Re1 O1 U1 . -64.9(8)
O3 Re1 O1 U1 . 175.0(7)
O13 U1 O1 Re1 . 93.8(8)
O9 U1 O1 Re1 . -113.4(8)
O5 U1 O1 Re1 . -7.1(7)
O5 U1 O1 Re1 4_755 167.7(6)
O6 U1 O1 Re1 . -65.2(8)
O10 U1 O1 Re1 . 40.2(9)
O1 U1 O1 Re1 4_755 171.0(6)
C5 P1 O5 U1 . 76.3(14)
C1 P1 O5 U1 . -46.6(14)
C9 P1 O5 U1 . -164.5(12)
O13 U1 O5 P1 . 138.0(13)
O9 U1 O5 P1 . -82.3(13)
O5 U1 O5 P1 4_755 33.9(17)
O6 U1 O5 P1 . -15.8(13)
O10 U1 O5 P1 . 66.0(13)
O1 U1 O5 P1 4_755 -153.8(12)
O1 U1 O5 P1 . -150.4(14)
O8 Re2 O6 U1 . 61.4(3)
O8 Re2 O6 U1 4_755 -61.4(3)
O7 Re2 O6 U1 . 180.000(2)
O13 U1 O6 Re2 . 180.0
O9 U1 O6 Re2 . 0.000(2)
O5 U1 O6 Re2 . -105.21(16)
O5 U1 O6 Re2 4_755 105.21(16)
O10 U1 O6 Re2 . 180.000(3)
O1 U1 O6 Re2 4_755 49.3(2)
O1 U1 O6 Re2 . -49.3(2)
C13A P2 O9 U1 4_755 139.1(7)
C13A P2 O9 U1 . -139.1(7)
C17 P2 O9 U1 . 0.000(7)
C13B P2 O9 U1 . -103.3(13)
C13B P2 O9 U1 4_755 103.3(13)
O13 U1 O9 P2 . 0.000(6)
O5 U1 O9 P2 . -107.99(16)
O5 U1 O9 P2 4_755 107.99(16)
O6 U1 O9 P2 . 180.000(5)
O10 U1 O9 P2 . 180.000(3)
O1 U1 O9 P2 4_755 40.51(17)
O1 U1 O9 P2 . -40.51(17)
O11 Re3 O10 U1 4_755 60.6(4)
O11 Re3 O10 U1 . -60.6(4)
O12 Re3 O10 U1 . 180.000(3)
O13 U1 O10 Re3 . 0.000(2)
O9 U1 O10 Re3 . 180.0
O5 U1 O10 Re3 . 100.54(17)
O5 U1 O10 Re3 4_755 -100.54(17)
O6 U1 O10 Re3 . 180.000(3)
O1 U1 O10 Re3 4_755 -53.6(2)
O1 U1 O10 Re3 . 53.6(2)
C21 P3 O13 U1 4_755 -117.9(6)
C21 P3 O13 U1 . 117.9(6)
C25 P3 O13 U1 . 17.1(8)
C25 P3 O13 U1 4_755 -17.1(8)
O9 U1 O13 P3 . 0.000(12)
O5 U1 O13 P3 . 109.49(15)
O5 U1 O13 P3 4_755 -109.49(15)
O6 U1 O13 P3 . 180.000(8)
O10 U1 O13 P3 . 180.000(11)
O1 U1 O13 P3 4_755 -40.06(17)
O1 U1 O13 P3 . 40.06(17)
O5 P1 C1 C2 . 64.7(9)
C5 P1 C1 C2 . -56.9(9)
C9 P1 C1 C2 . -174.3(8)
P1 C1 C2 C3 . -176.1(8)
C1 C2 C3 C4 . -64.4(14)
O5 P1 C5 C6 . -179.3(7)
C1 P1 C5 C6 . -55.0(9)
C9 P1 C5 C6 . 60.2(8)
P1 C5 C6 C7 . -179.7(8)
C5 C6 C7 C8 . -177.9(11)
O5 P1 C9 C10 . 57.6(7)
C5 P1 C9 C10 . 176.5(6)
C1 P1 C9 C10 . -64.8(7)
P1 C9 C10 C11 . -179.5(7)
C9 C10 C11 C12 . -68.6(12)
O9 P2 C13A C14A . 64.6(14)
C13A P2 C13A C14A 4_755 173.2(10)
C17 P2 C13A C14A . -72.8(14)
C13B P2 C13A C14A . -22(3)
C13B P2 C13A C14A 4_755 -178.0(18)
P2 C13A C14A C15A . -174.1(13)
C13A C14A C15A C16A . -51(3)
O9 P2 C13B C14B . -133(5)
C13A P2 C13B C14B 4_755 -11(5)
C13A P2 C13B C14B . -27(4)
C17 P2 C13B C14B . 110(5)
C13B P2 C13B C14B 4_755 8(8)
P2 C13B C14B C15B . 149(4)
C13B C14B C15B C16B . 174(5)
O9 P2 C17 C18 . 180.000(4)
C13A P2 C17 C18 4_755 43.2(7)
C13A P2 C17 C18 . -43.2(7)
C13B P2 C17 C18 . -69.1(12)
C13B P2 C17 C18 4_755 69.1(12)
P2 C17 C18 C19 . 180.000(7)
C17 C18 C19 C20 . 180.000(7)
O13 P3 C21 C22 . -171.8(11)
C21 P3 C21 C22 4_755 68.0(17)
C25 P3 C21 C22 . -55.8(14)
C25 P3 C21 C22 4_755 -39.6(17)
P3 C21 C22 C23 . 177.0(12)
C21 C22 C23 C24 . 177.7(15)
O13 P3 C25 C26 . -46.8(19)
C21 P3 C25 C26 4_755 82.8(19)
C21 P3 C25 C26 . -157.6(17)
C25 P3 C25 C26 4_755 50.3(18)
P3 C25 C26 C27 . -156.5(10)
C25 C26 C27 C28 . -155.0(13)
