#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:55:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179496 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/93/4339371.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_4339371
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            'H4 Na O14 Re3 U'
_chemical_formula_weight         1047.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.366(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.311(3)
_cell_length_b                   22.651(6)
_cell_length_c                   5.4896(14)
_cell_measurement_temperature    273(2)
_cell_volume                     1444.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.1510
_diffrn_reflns_av_sigmaI/netI    0.1175
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13139
_diffrn_reflns_theta_full        34.71
_diffrn_reflns_theta_max         34.71
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    36.330
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   "SADABS' "
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flattened prism'
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.302
_refine_diff_density_min         -2.669
_refine_diff_density_rms         0.479
_refine_ls_extinction_coef       0.00067(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.778
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         3068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.778
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0402
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                1919
_reflns_number_total             3068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701128b-file004.cif
_cod_data_source_block           comp3
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4339371
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_refinement_flags
U1 U 0.22453(4) 0.0000 0.29378(8) 0.02211(11) Uani 1 2 d S
Re1 Re 0.0000 0.10892(2) 0.5000 0.02545(12) Uani 1 2 d S
Re2 Re 0.29975(3) 0.171422(15) 0.33237(6) 0.02671(10) Uani 1 1 d .
Na1 Na 0.0000 0.2414(2) 0.0000 0.0340(12) Uani 1 2 d S
O1 O 0.0982(5) 0.0649(3) 0.4245(11) 0.0357(15) Uani 1 1 d .
O3 O 0.1334(8) 0.0000 -0.0271(16) 0.039(2) Uani 1 2 d S
O4 O 0.3949(7) 0.1752(4) 0.6434(13) 0.051(2) Uani 1 1 d .
O5 O 0.3135(8) 0.0000 0.6137(16) 0.044(3) Uani 1 2 d S
O6 O 0.3533(6) 0.2095(3) 0.1347(14) 0.0444(17) Uani 1 1 d .
O7 O 1.6025(7) 0.0000 0.8171(15) 0.0290(18) Uani 1 2 d S
O8 O 0.2826(6) 0.0971(3) 0.2400(13) 0.0444(17) Uani 1 1 d .
O9 O 0.0703(6) 0.1524(4) 0.7570(12) 0.0458(18) Uani 1 1 d .
O10 O 0.1724(5) 0.2001(3) 0.3278(12) 0.0358(15) Uani 1 1 d .
O2 O 0.4849(18) 0.0878(5) -0.034(4) 0.108(4) Uiso 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'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 '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
O5 U1 O3 179.3(4) . .
O5 U1 O8 90.6(2) . .
O3 U1 O8 89.6(2) . .
O5 U1 O8 90.6(2) . 6
O3 U1 O8 89.6(2) . 6
O8 U1 O8 137.3(3) . 6
O5 U1 O7 86.6(4) . 5_756
O3 U1 O7 94.1(4) . 5_756
O8 U1 O7 68.75(15) . 5_756
O8 U1 O7 68.75(15) 6 5_756
O5 U1 O1 87.2(3) . .
O3 U1 O1 92.2(3) . .
O8 U1 O1 73.8(2) . .
O8 U1 O1 148.8(2) 6 .
O7 U1 O1 141.98(16) 5_756 .
O5 U1 O1 87.2(3) . 6
O3 U1 O1 92.2(3) . 6
O8 U1 O1 148.8(2) . 6
O8 U1 O1 73.8(2) 6 6
O7 U1 O1 141.98(16) 5_756 6
O1 U1 O1 75.0(3) . 6
O9 Re1 O9 109.3(5) . 2_556
O9 Re1 O1 109.9(3) . 2_556
O9 Re1 O1 109.3(3) 2_556 2_556
O9 Re1 O1 109.3(3) . .
O9 Re1 O1 109.9(3) 2_556 .
O1 Re1 O1 109.2(4) 2_556 .
O6 Re2 O10 110.7(3) . .
O6 Re2 O4 109.3(4) . .
O10 Re2 O4 108.6(3) . .
O6 Re2 O8 110.0(3) . .
O10 Re2 O8 110.1(3) . .
O4 Re2 O8 108.2(4) . .
O6 Na1 O6 125.6(4) 7 8_455
O6 Na1 O10 119.8(2) 7 2
O6 Na1 O10 81.3(2) 8_455 2
O6 Na1 O10 81.3(2) 7 .
O6 Na1 O10 119.8(2) 8_455 .
O10 Na1 O10 135.4(4) 2 .
O6 Na1 O9 78.5(2) 7 1_554
O6 Na1 O9 151.4(3) 8_455 1_554
O10 Na1 O9 72.4(2) 2 1_554
O10 Na1 O9 74.9(2) . 1_554
O6 Na1 O9 151.4(3) 7 2_556
O6 Na1 O9 78.5(2) 8_455 2_556
O10 Na1 O9 74.9(2) 2 2_556
O10 Na1 O9 72.4(2) . 2_556
O9 Na1 O9 84.0(4) 1_554 2_556
O6 Na1 O4 71.2(3) 7 7_556
O6 Na1 O4 71.8(3) 8_455 7_556
O10 Na1 O4 151.3(3) 2 7_556
O10 Na1 O4 69.5(2) . 7_556
O9 Na1 O4 135.8(2) 1_554 7_556
O9 Na1 O4 108.4(2) 2_556 7_556
O6 Na1 O4 71.8(3) 7 8_454
O6 Na1 O4 71.2(3) 8_455 8_454
O10 Na1 O4 69.5(2) 2 8_454
O10 Na1 O4 151.3(3) . 8_454
O9 Na1 O4 108.4(2) 1_554 8_454
O9 Na1 O4 135.8(2) 2_556 8_454
O4 Na1 O4 92.0(4) 7_556 8_454
Re1 O1 U1 175.8(4) . .
Re2 O4 Na1 138.8(4) . 7_556
Re2 O6 Na1 156.7(4) . 7
Re2 O8 U1 150.7(3) . .
Re1 O9 Na1 132.9(4) . 1_556
Re2 O10 Na1 136.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O5 1.735(8) .
U1 O3 1.747(8) .
U1 O8 2.362(7) .
U1 O8 2.362(7) 6
U1 O7 2.402(7) 5_756
U1 O1 2.416(6) .
U1 O1 2.416(6) 6
Re1 O9 1.703(7) .
Re1 O9 1.703(7) 2_556
Re1 O1 1.720(6) 2_556
Re1 O1 1.720(6) .
Re2 O6 1.682(6) .
Re2 O10 1.689(6) .
Re2 O4 1.723(7) .
Re2 O8 1.750(7) .
Na1 O6 2.436(7) 7
Na1 O6 2.436(7) 8_455
Na1 O10 2.467(7) 2
Na1 O10 2.467(7) .
Na1 O9 2.712(9) 1_554
Na1 O9 2.712(9) 2_556
Na1 O4 2.719(9) 7_556
Na1 O4 2.719(9) 8_454
O4 Na1 2.719(9) 7_556
O6 Na1 2.436(7) 7
O7 U1 2.402(7) 5_756
O9 Na1 2.712(9) 1_556
