#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:55:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179496 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/93/4339373.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4339373
loop_
_publ_author_name
'Karimova, Oxana V.'
'Burns, Peter C.'
_publ_section_title
;
 Structural units in three uranyl perrhenates.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10108
_journal_page_last               10113
_journal_paper_doi               10.1021/ic701128b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'H6 O23 Re4 U2'
_chemical_formula_weight         1594.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.180(2)
_cell_angle_beta                 99.131(3)
_cell_angle_gamma                94.114(2)
_cell_formula_units_Z            2
_cell_length_a                   5.2771(7)
_cell_length_b                   13.0997(17)
_cell_length_c                   15.476(2)
_cell_measurement_temperature    273(2)
_cell_volume                     1001.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker PLATFORM with APEX CCD detector'
_diffrn_measurement_method       ω
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12687
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    40.305
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.601
_refine_diff_density_min         -2.484
_refine_diff_density_rms         0.512
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0152P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                3464
_reflns_number_total             4952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701128b-file002.cif
_cod_data_source_block           comp1
_cod_database_code               4339373
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
U1 U 0.23941(8) 0.64455(3) 0.16746(3) 0.01176(10) Uani 1 1 d
U2 U -0.24850(8) 0.79742(3) 0.68538(3) 0.01223(11) Uani 1 1 d
Re1 Re 0.00428(9) 0.50202(4) 0.65300(4) 0.01315(11) Uani 1 1 d
Re2 Re -0.02480(9) 0.85859(4) 0.37095(4) 0.01460(12) Uani 1 1 d
Re3 Re -0.40283(10) 1.06368(4) 0.87380(4) 0.01576(12) Uani 1 1 d
Re4 Re 0.47795(10) 0.36108(4) 0.06217(4) 0.01495(12) Uani 1 1 d
O1 O -0.3496(16) 0.6755(6) 0.5327(6) 0.018(2) Uani 1 1 d
O2 O -0.9351(15) -0.6342(6) -1.6844(7) 0.021(2) Uani 1 1 d
O3 O -0.2600(17) 1.0599(7) 0.9801(7) 0.027(2) Uani 1 1 d
O4 O 0.2979(18) 0.2391(6) 0.0207(7) 0.029(2) Uani 1 1 d
O5 O 0.5251(15) 1.2570(6) 1.2862(6) 0.0138(18) Uani 1 1 d
O6 O 0.2075(16) 0.9589(6) 0.4407(7) 0.022(2) Uani 1 1 d
O7 O 0.2913(16) 0.4580(7) 0.1158(6) 0.019(2) Uani 1 1 d
O8 O 0.3255(17) 0.8089(6) 0.1338(7) 0.022(2) Uani 1 1 d
O9 O -1.0831(17) 1.4354(6) 0.7288(7) 0.024(2) Uani 1 1 d
O10 O 0.0058(16) 0.8154(7) 0.8374(7) 0.023(2) Uani 1 1 d
O11 O -1.1647(16) 0.4349(6) 0.5453(7) 0.023(2) Uani 1 1 d
O12 O -0.7277(17) 1.0340(7) 0.8602(7) 0.028(2) Uani 1 1 d
O13 O -0.5117(16) 0.8858(7) 0.5945(6) 0.019(2) Uani 1 1 d
O14 O -0.7196(17) 1.0862(7) 0.6676(7) 0.028(2) Uani 1 1 d
O15 O 0.5536(14) 0.6690(6) 0.2338(6) 0.0128(18) Uani 1 1 d
O16 O -0.3261(16) 0.5005(7) 0.3494(7) 0.026(2) Uani 1 1 d
O17 O -0.1148(17) 0.7760(6) 0.4313(6) 0.023(2) Uani 1 1 d
O18 O -0.0699(16) 0.6172(7) 0.0994(6) 0.019(2) Uani 1 1 d
O19 O -0.2923(17) 0.9693(7) 0.7920(7) 0.026(2) Uani 1 1 d
O20 O 0.8911(16) 0.2147(6) 0.7196(7) 0.023(2) Uani 1 1 d
O21 O 0.6062(16) 0.3925(7) -0.0262(6) 0.019(2) Uani 1 1 d
O22 O 0.0201(15) 0.8537(6) 0.6530(7) 0.017(2) Uani 1 1 d
O23 O 0.7297(18) 0.3538(8) 0.1413(8) 0.039(3) Uani 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O18 U1 O15 178.4(4) . .
O18 U1 O20 91.1(4) . 2_666
O15 U1 O20 90.5(3) . 2_666
O18 U1 O9 89.9(3) . 2_476
O15 U1 O9 90.5(3) . 2_476
O20 U1 O9 73.8(3) 2_666 2_476
O18 U1 O21 85.9(3) . 2_665
O15 U1 O21 92.9(3) . 2_665
O20 U1 O21 141.9(3) 2_666 2_665
O9 U1 O21 144.0(3) 2_476 2_665
O18 U1 O7 90.2(3) . .
O15 U1 O7 88.4(3) . .
O20 U1 O7 146.7(3) 2_666 .
O9 U1 O7 72.9(3) 2_476 .
O21 U1 O7 71.4(3) 2_665 .
O18 U1 O8 92.0(3) . .
O15 U1 O8 88.6(3) . .
O20 U1 O8 71.6(3) 2_666 .
O9 U1 O8 145.4(3) 2_476 .
O21 U1 O8 70.6(3) 2_665 .
O7 U1 O8 141.6(3) . .
O5 U2 O22 177.4(4) 2_577 .
O5 U2 O1 91.6(3) 2_577 .
O22 U2 O1 87.2(4) . .
O5 U2 O2 88.2(3) 2_577 2_454
O22 U2 O2 93.6(3) . 2_454
O1 U2 O2 71.4(3) . 2_454
O5 U2 O13 90.6(3) 2_577 .
O22 U2 O13 86.9(3) . .
O1 U2 O13 73.8(3) . .
O2 U2 O13 145.1(3) 2_454 .
O5 U2 O19 88.2(3) 2_577 .
O22 U2 O19 91.7(3) . .
O1 U2 O19 148.5(3) . .
O2 U2 O19 140.0(3) 2_454 .
O13 U2 O19 74.8(3) . .
O5 U2 O10 91.1(3) 2_577 .
O22 U2 O10 91.3(4) . .
O1 U2 O10 140.6(3) . .
O2 U2 O10 69.4(3) 2_454 .
O13 U2 O10 145.5(3) . .
O19 U2 O10 70.8(3) . .
O11 Re1 O16 108.0(4) 1_655 2_566
O11 Re1 O2 109.1(4) 1_655 2_454
O16 Re1 O2 110.1(4) 2_566 2_454
O11 Re1 O9 108.5(4) 1_655 1_645
O16 Re1 O9 109.7(4) 2_566 1_645
O2 Re1 O9 111.4(4) 2_454 1_645
O14 Re2 O6 109.0(4) 2_476 .
O14 Re2 O17 110.6(4) 2_476 .
O6 Re2 O17 109.5(4) . .
O14 Re2 O20 110.9(5) 2_476 2_666
O6 Re2 O20 107.6(4) . 2_666
O17 Re2 O20 109.2(4) . 2_666
O12 Re3 O19 108.9(5) . .
O12 Re3 O3 109.0(4) . .
O19 Re3 O3 108.7(4) . .
O12 Re3 O8 110.6(4) . 2_576
O19 Re3 O8 110.6(4) . 2_576
O3 Re3 O8 108.9(4) . 2_576
O23 Re4 O4 107.8(5) . .
O23 Re4 O21 107.3(4) . .
O4 Re4 O21 110.1(4) . .
O23 Re4 O7 108.9(5) . .
O4 Re4 O7 109.6(4) . .
O21 Re4 O7 113.0(4) . .
Re1 O2 U2 163.1(5) 2_454 2_454
Re4 O7 U1 146.5(4) . .
Re3 O8 U1 171.8(6) 2_576 .
Re1 O9 U1 174.0(5) 1_465 2_476
Re3 O19 U2 160.8(5) . .
Re2 O20 U1 164.0(5) 2_666 2_666
Re4 O21 U1 156.0(5) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O18 1.746(9) .
U1 O15 1.759(8) .
U1 O20 2.364(8) 2_666
U1 O9 2.376(8) 2_476
U1 O21 2.382(8) 2_665
U1 O7 2.387(8) .
U1 O8 2.389(7) .
U2 O5 1.753(7) 2_577
U2 O22 1.760(8) .
U2 O1 2.380(9) .
U2 O2 2.408(7) 2_454
U2 O13 2.413(8) .
U2 O19 2.418(9) .
U2 O10 2.453(10) .
Re1 O11 1.702(10) 1_655
Re1 O16 1.707(8) 2_566
Re1 O2 1.737(8) 2_454
Re1 O9 1.752(8) 1_645
Re2 O14 1.684(9) 2_476
Re2 O6 1.704(9) .
Re2 O17 1.713(8) .
Re2 O20 1.732(9) 2_666
Re3 O12 1.696(9) .
Re3 O19 1.698(9) .
Re3 O3 1.714(10) .
Re3 O8 1.732(7) 2_576
Re4 O23 1.686(11) .
Re4 O4 1.688(8) .
Re4 O21 1.756(8) .
Re4 O7 1.757(8) .
O2 Re1 1.737(8) 2_454
O2 U2 2.408(7) 2_454
O5 U2 1.753(7) 2_577
O8 Re3 1.732(7) 2_576
O9 Re1 1.752(8) 1_465
O9 U1 2.376(8) 2_476
O11 Re1 1.702(10) 1_455
O14 Re2 1.684(9) 2_476
O16 Re1 1.707(8) 2_566
O20 Re2 1.732(9) 2_666
O20 U1 2.364(8) 2_666
O21 U1 2.382(8) 2_665
