#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:13:21 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179472 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/69/4336997.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_4336997
loop_
_publ_author_name
'David D. Schnaars'
'Richard E. Wilson'
_publ_contact_author_address
;CSE/200 
Argonne National Laboratory
9600 S. Cass Avenue
Argonne, IL 60439
;
_publ_contact_author_email       rewilson@anl.gov
_publ_contact_author_name        'Richard E. Wilson'
_publ_contact_author_phone       630-252-1288
_publ_section_title
;
 Structural and Vibrational Properties of U(VI)O2Cl42- and Pu(VI)O2Cl42-
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14138
_journal_page_last               14147
_journal_paper_doi               10.1021/ic401991n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Cl4 H4 O4 Rb2 U'
_chemical_formula_weight         618.80
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.1910(10)
_cell_angle_beta                 101.6700(10)
_cell_angle_gamma                118.8110(10)
_cell_formula_units_Z            1
_cell_length_a                   6.7500(7)
_cell_length_b                   6.8991(7)
_cell_length_c                   7.4230(7)
_cell_measurement_reflns_used    2005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      4.27
_cell_volume                     292.90(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 deg w/ exposures'
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4828
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         4.27
_exptl_absorpt_coefficient_mu    22.993
_exptl_absorpt_correction_T_max  0.4049
_exptl_absorpt_correction_T_min  0.0818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow-Green
_exptl_crystal_density_diffrn    3.508
_exptl_crystal_description       Plate
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.430
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         2005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0194
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0445
_reflns_number_gt                1933
_reflns_number_total             2005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401991n_si_002_1.cif
_cod_data_source_block           U_Rb
_cod_database_code               4336997
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
_atom_site_refinement_flags
U1 U 0.5000 0.0000 0.5000 0.00828(5) Uani 1 2 d S
Rb1 Rb 0.93134(5) -0.24703(5) 0.75873(4) 0.01233(6) Uani 1 1 d .
Cl1 Cl 0.29161(13) -0.22754(13) 0.15512(10) 0.01484(14) Uani 1 1 d .
Cl2 Cl 0.66586(13) 0.38179(12) 0.35927(10) 0.01381(14) Uani 1 1 d .
O2W O 1.2408(5) 0.2265(5) 0.9223(4) 0.0175(5) Uani 1 1 d .
O1 O 0.7549(4) -0.0117(4) 0.4925(3) 0.0131(4) Uani 1 1 d .
H1 H 1.340(9) 0.236(9) 0.922(7) 0.028(15) Uiso 1 1 d .
H2 H 1.239(8) 0.308(9) 0.868(7) 0.026(13) Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.00887(7) 0.01036(7) 0.00677(7) 0.00257(5) 0.00275(5) 0.00533(5)
Rb1 0.01419(13) 0.01314(13) 0.00930(14) 0.00225(11) 0.00331(10) 0.00639(11)
Cl1 0.0176(3) 0.0163(3) 0.0082(3) 0.0008(3) 0.0010(3) 0.0075(3)
Cl2 0.0171(3) 0.0126(3) 0.0113(3) 0.0047(3) 0.0043(3) 0.0067(3)
O2W 0.0206(13) 0.0208(12) 0.0160(12) 0.0062(10) 0.0087(10) 0.0123(10)
O1 0.0130(10) 0.0173(10) 0.0122(10) 0.0039(9) 0.0045(8) 0.0095(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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'
Rb Rb -0.9393 2.9676 '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
O1 U1 O1 179.999(1) 2_656 .
O1 U1 Cl1 90.47(8) 2_656 2_656
O1 U1 Cl1 89.52(8) . 2_656
O1 U1 Cl1 89.53(8) 2_656 .
O1 U1 Cl1 90.47(8) . .
Cl1 U1 Cl1 180.0 2_656 .
O1 U1 Cl2 89.88(7) 2_656 2_656
O1 U1 Cl2 90.12(7) . 2_656
Cl1 U1 Cl2 89.40(2) 2_656 2_656
Cl1 U1 Cl2 90.60(2) . 2_656
O1 U1 Cl2 90.12(7) 2_656 .
O1 U1 Cl2 89.88(7) . .
Cl1 U1 Cl2 90.60(2) 2_656 .
Cl1 U1 Cl2 89.40(2) . .
Cl2 U1 Cl2 180.0 2_656 .
H1 O2W H2 102(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.773(2) 2_656
U1 O1 1.773(2) .
U1 Cl1 2.6654(8) 2_656
U1 Cl1 2.6654(8) .
U1 Cl2 2.6691(7) 2_656
U1 Cl2 2.6691(7) .
Rb1 H1 3.11(5) .
O2W H1 0.64(5) .
O2W H2 0.71(5) .
