#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:05:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179230 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/50/4315099.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_4315099
loop_
_publ_author_name
'Daniel E. Bugaris'
'Roy Copping'
'Tolek Tyliszczak'
'David K. Shuh'
'James A. Ibers'
_publ_contact_author_address
;
        Department of Chemistry
        Northwestern University
        2145 Sheridan Road
        Evanston, IL 60208-3113, USA
;
_publ_contact_author_email       ibers@chem.northwestern.edu
_publ_contact_author_fax         '+1 847 491 2976'
_publ_contact_author_name        'James A. Ibers'
_publ_contact_author_phone       '+1 847 491 5449'
_publ_section_title
;
 La2U2Se9: An Ordered Lanthanide/Actinide Chalcogenide with a Novel
 Structure Type
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2568
_journal_page_last               2575
_journal_paper_doi               10.1021/ic902503n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'La2 Se9 U2'
_chemical_formula_sum            'La2 Se9 U2'
_chemical_formula_weight         1464.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           51
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_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            2
_cell_length_a                   10.920(2)
_cell_length_b                   5.6100(11)
_cell_length_c                   10.703(2)
_cell_measurement_reflns_used    4484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.66
_cell_volume                     655.7(2)
_computing_cell_refinement       'APEX2 version v2009.5-1 (Bruker, 2009)'
_computing_data_collection       'SMART version 5.054 (Bruker, 2000)'
_computing_data_reduction        'SAINT version 7.34a (Bruker, 2009)'
_computing_molecular_graphics    'CrystalMaker version 2.2.1 (Palmer, 2009)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7471
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    55.938
_exptl_absorpt_correction_T_max  0.0613
_exptl_absorpt_correction_T_min  0.0039
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
'face indexed; SADABS version 2008/1 (Sheldrick, 2006)'
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.096
_refine_diff_density_max         2.977
_refine_diff_density_min         -2.682
_refine_diff_density_rms         0.501
_refine_ls_extinction_coef       0.00042(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0264
_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
 [1.00000]/[σ²(Fo²)+(0.0200Fo²)²] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                849
_reflns_number_total             926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902503n_si_001.cif
_cod_data_source_block           finalst
_cod_database_code               4315099
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z'
'-x-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.00609(4) 0.0000 0.25077(4) 0.00772(17) Uani 1 2 d S . .
La1 La 0.2500 0.5000 0.57171(9) 0.0058(2) Uani 1 4 d S . .
La2 La 0.2500 0.5000 0.02688(10) 0.0083(2) Uani 1 4 d S . .
Se1 Se 0.2500 0.0000 0.68054(16) 0.0071(3) Uani 1 4 d S . .
Se2 Se 0.55502(11) 0.5000 0.18873(11) 0.0083(3) Uani 1 2 d S . .
Se3 Se 0.12419(12) 0.0000 0.00021(11) 0.0082(3) Uani 1 2 d S . .
Se4 Se 0.0000 0.2498(2) 0.5000 0.0101(3) Uani 1 2 d S . .
Se5 Se 0.2500 0.2492(2) 0.28919(11) 0.0115(3) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
_geom_angle_publ_flag
Se1 U1 Se2 80.73(3) 5_556 2 ?
Se1 U1 Se2 80.73(3) 5_556 2_565 ?
Se2 U1 Se2 142.89(5) 2 2_565 ?
Se1 U1 Se3 130.41(4) 5_556 . ?
Se2 U1 Se3 84.00(3) 2 . ?
Se2 U1 Se3 84.00(3) 2_565 . ?
Se1 U1 Se4 75.74(3) 5_556 . ?
Se2 U1 Se4 129.38(4) 2 . ?
Se2 U1 Se4 75.69(3) 2_565 . ?
Se3 U1 Se4 143.82(3) . . ?
Se1 U1 Se4 75.74(3) 5_556 5_556 ?
Se2 U1 Se4 75.69(3) 2 5_556 ?
Se2 U1 Se4 129.38(4) 2_565 5_556 ?
Se3 U1 Se4 143.82(3) . 5_556 ?
Se4 U1 Se4 55.41(5) . 5_556 ?
Se1 U1 Se5 144.49(3) 5_556 2 ?
Se2 U1 Se5 77.98(3) 2 2 ?
Se2 U1 Se5 131.67(4) 2_565 2 ?
Se3 U1 Se5 75.04(3) . 2 ?
Se4 U1 Se5 96.52(3) . 2 ?
Se4 U1 Se5 71.66(2) 5_556 2 ?
Se1 U1 Se5 144.49(3) 5_556 . ?
Se2 U1 Se5 131.67(4) 2 . ?
Se2 U1 Se5 77.98(3) 2_565 . ?
Se3 U1 Se5 75.04(3) . . ?
Se4 U1 Se5 71.66(2) . . ?
Se4 U1 Se5 96.52(3) 5_556 . ?
Se5 U1 Se5 54.83(5) 2 . ?
Se1 U1 Se3 76.82(4) 5_556 5 ?
Se2 U1 Se3 72.31(2) 2 5 ?
Se2 U1 Se3 72.31(2) 2_565 5 ?
Se3 U1 Se3 53.59(5) . 5 ?
Se4 U1 Se3 140.52(3) . 5 ?
Se4 U1 Se3 140.52(3) 5_556 5 ?
Se5 U1 Se3 122.02(3) 2 5 ?
Se5 U1 Se3 122.02(3) . 5 ?
Se1 La1 Se1 134.90(7) 1_565 . ?
Se1 La1 Se4 71.54(3) 1_565 2_565 ?
Se1 La1 Se4 120.18(2) . 2_565 ?
Se1 La1 Se4 71.54(3) 1_565 5_566 ?
Se1 La1 Se4 120.18(2) . 5_566 ?
Se4 La1 Se4 119.26(4) 2_565 5_566 ?
Se1 La1 Se4 120.18(2) 1_565 6_656 ?
Se1 La1 Se4 71.54(3) . 6_656 ?
Se4 La1 Se4 52.67(5) 2_565 6_656 ?
Se4 La1 Se4 151.92(3) 5_566 6_656 ?
Se1 La1 Se4 120.18(2) 1_565 . ?
Se1 La1 Se4 71.54(3) . . ?
Se4 La1 Se4 151.92(3) 2_565 . ?
Se4 La1 Se4 52.67(5) 5_566 . ?
Se4 La1 Se4 119.26(4) 6_656 . ?
Se1 La1 Se2 72.84(3) 1_565 5_666 ?
Se1 La1 Se2 72.84(3) . 5_666 ?
Se4 La1 Se2 68.62(2) 2_565 5_666 ?
Se4 La1 Se2 137.54(3) 5_566 5_666 ?
Se4 La1 Se2 68.62(2) 6_656 5_666 ?
Se4 La1 Se2 137.54(3) . 5_666 ?
Se1 La1 Se2 72.84(3) 1_565 6_556 ?
Se1 La1 Se2 72.84(3) . 6_556 ?
Se4 La1 Se2 137.54(3) 2_565 6_556 ?
Se4 La1 Se2 68.62(2) 5_566 6_556 ?
Se4 La1 Se2 137.54(3) 6_656 6_556 ?
Se4 La1 Se2 68.62(2) . 6_556 ?
Se2 La1 Se2 79.41(5) 5_666 6_556 ?
Se1 La1 Se5 87.60(4) 1_565 2_565 ?
Se1 La1 Se5 137.51(5) . 2_565 ?
Se4 La1 Se5 65.979(17) 2_565 2_565 ?
Se4 La1 Se5 65.979(17) 5_566 2_565 ?
Se4 La1 Se5 88.12(3) 6_656 2_565 ?
Se4 La1 Se5 88.12(3) . 2_565 ?
Se2 La1 Se5 134.23(2) 5_666 2_565 ?
Se2 La1 Se5 134.23(2) 6_556 2_565 ?
Se1 La1 Se5 137.51(5) 1_565 . ?
Se1 La1 Se5 87.60(4) . . ?
Se4 La1 Se5 88.12(3) 2_565 . ?
Se4 La1 Se5 88.12(3) 5_566 . ?
Se4 La1 Se5 65.979(17) 6_656 . ?
Se4 La1 Se5 65.979(17) . . ?
Se2 La1 Se5 134.23(2) 5_666 . ?
Se2 La1 Se5 134.23(2) 6_556 . ?
Se5 La1 Se5 49.91(5) 2_565 . ?
Se3 La2 Se3 169.56(6) . 2_565 ?
Se3 La2 Se3 51.96(4) . 2 ?
Se3 La2 Se3 126.85(4) 2_565 2 ?
Se3 La2 Se3 126.85(4) . 1_565 ?
Se3 La2 Se3 51.96(4) 2_565 1_565 ?
Se3 La2 Se3 169.56(6) 2 1_565 ?
Se3 La2 Se2 68.66(2) . 6 ?
Se3 La2 Se2 103.30(3) 2_565 6 ?
Se3 La2 Se2 103.30(3) 2 6 ?
Se3 La2 Se2 68.66(2) 1_565 6 ?
Se3 La2 Se2 103.30(3) . 5_665 ?
Se3 La2 Se2 68.66(2) 2_565 5_665 ?
Se3 La2 Se2 68.66(2) 2 5_665 ?
Se3 La2 Se2 103.30(3) 1_565 5_665 ?
Se2 La2 Se2 85.39(5) 6 5_665 ?
Se3 La2 Se5 71.38(3) . . ?
Se3 La2 Se5 118.82(4) 2_565 . ?
Se3 La2 Se5 71.38(3) 2 . ?
Se3 La2 Se5 118.82(4) 1_565 . ?
Se2 La2 Se5 131.08(2) 6 . ?
Se2 La2 Se5 131.08(2) 5_665 . ?
Se3 La2 Se5 118.82(4) . 2_565 ?
Se3 La2 Se5 71.38(3) 2_565 2_565 ?
Se3 La2 Se5 118.82(4) 2 2_565 ?
Se3 La2 Se5 71.38(3) 1_565 2_565 ?
Se2 La2 Se5 131.08(2) 6 2_565 ?
Se2 La2 Se5 131.08(2) 5_665 2_565 ?
Se5 La2 Se5 53.24(5) . 2_565 ?
U1 Se1 U1 150.54(7) 6_656 5_556 ?
U1 Se1 La1 95.596(8) 6_656 1_545 ?
U1 Se1 La1 95.596(8) 5_556 1_545 ?
U1 Se1 La1 95.596(8) 6_656 . ?
U1 Se1 La1 95.596(8) 5_556 . ?
La1 Se1 La1 134.90(7) 1_545 . ?
U1 Se2 U1 142.89(5) 2_565 2 ?
U1 Se2 La2 108.54(2) 2_565 5_665 ?
U1 Se2 La2 108.54(2) 2 5_665 ?
U1 Se2 La1 88.36(3) 2_565 5_666 ?
U1 Se2 La1 88.36(3) 2 5_666 ?
La2 Se2 La1 97.60(4) 5_665 5_666 ?
Se3 Se3 Se3 179.90(5) 5 2 ?
Se3 Se3 U1 64.41(5) 5 . ?
Se3 Se3 U1 115.68(3) 2 . ?
Se3 Se3 U1 62.00(4) 5 5 ?
Se3 Se3 U1 117.91(3) 2 5 ?
U1 Se3 U1 126.41(5) . 5 ?
Se3 Se3 La2 115.99(2) 5 . ?
Se3 Se3 La2 64.02(2) 2 . ?
U1 Se3 La2 96.19(3) . . ?
U1 Se3 La2 106.58(3) 5 . ?
Se3 Se3 La2 115.99(2) 5 1_545 ?
Se3 Se3 La2 64.02(2) 2 1_545 ?
U1 Se3 La2 96.19(3) . 1_545 ?
U1 Se3 La2 106.58(3) 5 1_545 ?
La2 Se3 La2 126.85(4) . 1_545 ?
Se4 Se4 Se4 180.0 5_556 5_566 ?
Se4 Se4 U1 62.29(2) 5_556 5_556 ?
Se4 Se4 U1 117.71(2) 5_566 5_556 ?
Se4 Se4 U1 62.29(2) 5_556 . ?
Se4 Se4 U1 117.71(2) 5_566 . ?
U1 Se4 U1 124.59(5) 5_556 . ?
Se4 Se4 La1 116.34(2) 5_556 . ?
Se4 Se4 La1 63.66(2) 5_566 . ?
U1 Se4 La1 90.608(18) 5_556 . ?
U1 Se4 La1 113.697(18) . . ?
Se4 Se4 La1 116.34(2) 5_556 5_566 ?
Se4 Se4 La1 63.66(2) 5_566 5_566 ?
U1 Se4 La1 113.697(18) 5_556 5_566 ?
U1 Se4 La1 90.607(18) . 5_566 ?
La1 Se4 La1 127.33(5) . 5_566 ?
Se5 Se5 Se5 180.0 2 2_565 ?
Se5 Se5 U1 62.58(2) 2 2 ?
Se5 Se5 U1 117.42(2) 2_565 2 ?
Se5 Se5 U1 62.58(2) 2 . ?
Se5 Se5 U1 117.42(2) 2_565 . ?
U1 Se5 U1 122.63(5) 2 . ?
Se5 Se5 La2 116.62(3) 2 . ?
Se5 Se5 La2 63.38(3) 2_565 . ?
U1 Se5 La2 94.89(3) 2 . ?
U1 Se5 La2 94.89(3) . . ?
Se5 Se5 La1 114.95(3) 2 . ?
Se5 Se5 La1 65.05(3) 2_565 . ?
U1 Se5 La1 108.48(3) 2 . ?
U1 Se5 La1 108.49(3) . . ?
La2 Se5 La1 128.43(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Se1 2.8915(8) 5_556 ?
U1 Se2 2.9588(7) 2 ?
U1 Se2 2.9588(7) 2_565 ?
U1 Se3 2.9757(14) . ?
U1 Se4 3.0140(9) . ?
U1 Se4 3.0140(9) 5_556 ?
U1 Se5 3.0361(9) 2 ?
U1 Se5 3.0361(9) . ?
U1 Se3 3.0398(13) 5 ?
La1 Se1 3.0373(9) 1_565 ?
La1 Se1 3.0373(9) . ?
La1 Se4 3.1642(8) 2_565 ?
La1 Se4 3.1642(8) 5_566 ?
La1 Se4 3.1642(8) 6_656 ?
La1 Se4 3.1642(8) . ?
La1 Se2 3.3328(15) 5_666 ?
La1 Se2 3.3328(15) 6_556 ?
La1 Se5 3.3352(16) 2_565 ?
La1 Se5 3.3352(16) . ?
La2 Se3 3.1364(8) . ?
La2 Se3 3.1364(8) 2_565 ?
La2 Se3 3.1364(8) 2 ?
La2 Se3 3.1364(8) 1_565 ?
La2 Se2 3.1399(15) 6 ?
La2 Se2 3.1399(15) 5_665 ?
La2 Se5 3.1404(16) . ?
La2 Se5 3.1404(16) 2_565 ?
Se1 U1 2.8915(8) 6_656 ?
Se1 U1 2.8915(8) 5_556 ?
Se1 La1 3.0373(9) 1_545 ?
Se2 U1 2.9588(7) 2_565 ?
Se2 U1 2.9588(7) 2 ?
Se2 La2 3.1399(15) 5_665 ?
Se2 La1 3.3328(15) 5_666 ?
Se3 Se3 2.712(3) 5 ?
Se3 Se3 2.748(3) 2 ?
Se3 U1 3.0398(13) 5 ?
Se3 La2 3.1364(8) 1_545 ?
Se4 Se4 2.803(3) 5_556 ?
Se4 Se4 2.807(3) 5_566 ?
Se4 U1 3.0139(9) 5_556 ?
Se4 La1 3.1642(8) 5_566 ?
Se5 Se5 2.796(3) 2 ?
Se5 Se5 2.814(3) 2_565 ?
Se5 U1 3.0360(9) 2 ?
