#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:08:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179502 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/99/4339954.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_4339954
loop_
_publ_author_name
'Ward, Matthew D.'
'Mesbah, Adel'
'Minasian, Stefan G.'
'Shuh, David K.'
'Tyliszczak, Tolek'
'Lee, Minseong'
'Choi, Eun Sang'
'Lebègue, Sébastien'
'Ibers, James A.'
_publ_section_title
;
 Synthesis and Characterization of Eight Compounds of the MU8Q17 Family:
 ScU8S17, CoU8S17, NiU8S17, TiU8Se17, VU8Se17, CrU8Se17, CoU8Se17, and
 NiU8Se17.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6920
_journal_page_last               6927
_journal_paper_doi               10.1021/ic500721d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Se17 Ti U8'
_chemical_formula_sum            'Se17 Ti U8'
_chemical_formula_weight         3294.46
_chemical_name_systematic
'Titanium(II) octauranium(IV) heptadecaselenide'
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-08-14 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.3690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8890(4)
_cell_length_b                   8.8141(2)
_cell_length_c                   10.8876(3)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.122
_cell_measurement_theta_min      2.753
_cell_volume                     1306.70(6)
_computing_cell_refinement       'APEX2 (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008c)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008c)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       'φ and 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2640
_diffrn_reflns_theta_full        33.19
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    73.335
_exptl_absorpt_correction_T_max  0.435326
_exptl_absorpt_correction_T_min  0.158917
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008b)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    8.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.011
_refine_diff_density_max         2.049
_refine_diff_density_min         -3.701
_refine_diff_density_rms         0.531
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         2640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0230
_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 
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0357P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                2535
_reflns_number_total             2640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500721d_si_001.cif
_cod_data_source_block           TiU8Se17
_cod_depositor_comments
'Adding full bibliography for 4339953--4339960.cif.'
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4339954
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 0.440687(15) 0.25693(2) 0.296238(18) 0.00471(6) Uani 1 1 d .
U2 U 0.20325(2) 0.0000 0.45914(3) 0.00449(6) Uani 1 2 d S
U3 U 0.68034(2) 0.0000 0.01656(3) 0.00473(7) Uani 1 2 d S
Se1 Se 0.12752(4) 0.30615(6) 0.46596(5) 0.00523(10) Uani 1 1 d .
Se2 Se 0.36543(4) 0.30927(6) 0.02554(5) 0.00499(10) Uani 1 1 d .
Se3 Se 0.06045(6) 0.0000 0.22899(7) 0.00564(13) Uani 1 2 d S
Se4 Se 0.21200(6) 0.0000 0.72515(7) 0.00520(13) Uani 1 2 d S
Se5 Se 0.30210(6) 0.0000 0.24632(7) 0.00536(13) Uani 1 2 d S
Se6 Se 0.52070(6) 0.0000 0.16690(7) 0.00538(13) Uani 1 2 d S
Se7 Se 0.0000 0.0000 0.5000 0.00486(18) Uani 1 4 d S
Ti1 Ti 0.0000 0.0000 0.0000 0.0054(3) Uani 1 4 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
Se3 U1 Se1 79.520(19) 3 8
Se3 U1 Se5 155.20(2) 3 .
Se1 U1 Se5 115.798(18) 8 .
Se3 U1 Se2 74.968(19) 3 .
Se1 U1 Se2 138.821(16) 8 .
Se5 U1 Se2 81.197(18) . .
Se3 U1 Se1 130.933(18) 3 7_556
Se1 U1 Se1 79.053(17) 8 7_556
Se5 U1 Se1 73.104(18) . 7_556
Se2 U1 Se1 141.563(17) . 7_556
Se3 U1 Se4 83.342(17) 3 7_556
Se1 U1 Se4 135.393(18) 8 7_556
Se5 U1 Se4 96.234(18) . 7_556
Se2 U1 Se4 72.863(18) . 7_556
Se1 U1 Se4 81.914(18) 7_556 7_556
Se3 U1 Se6 98.966(17) 3 .
Se1 U1 Se6 77.771(19) 8 .
Se5 U1 Se6 67.802(19) . .
Se2 U1 Se6 74.974(17) . .
Se1 U1 Se6 118.597(16) 7_556 .
Se4 U1 Se6 145.93(2) 7_556 .
Se3 U1 Se7 65.255(14) 3 3
Se1 U1 Se7 66.364(11) 8 3
Se5 U1 Se7 137.637(16) . 3
Se2 U1 Se7 126.912(11) . 3
Se1 U1 Se7 65.748(11) 7_556 3
Se4 U1 Se7 69.046(14) 7_556 3
Se6 U1 Se7 142.586(16) . 3
Se3 U2 Se4 139.78(2) . .
Se3 U2 Se1 129.000(16) . 7_556
Se4 U2 Se1 81.097(18) . 7_556
Se3 U2 Se1 129.000(16) . 4_546
Se4 U2 Se1 81.097(18) . 4_546
Se1 U2 Se1 72.48(2) 7_556 4_546
Se3 U2 Se1 80.268(13) . .
Se4 U2 Se1 85.283(13) . .
Se1 U2 Se1 73.848(17) 7_556 .
Se1 U2 Se1 145.191(15) 4_546 .
Se3 U2 Se1 80.268(13) . 6
Se4 U2 Se1 85.283(13) . 6
Se1 U2 Se1 145.192(15) 7_556 6
Se1 U2 Se1 73.849(17) 4_546 6
Se1 U2 Se1 136.78(2) . 6
Se3 U2 Se5 70.08(2) . .
Se4 U2 Se5 150.15(2) . .
Se1 U2 Se5 74.941(17) 7_556 .
Se1 U2 Se5 74.941(17) 4_546 .
Se1 U2 Se5 104.479(12) . .
Se1 U2 Se5 104.479(12) 6 .
Se3 U2 Se7 67.294(17) . .
Se4 U2 Se7 72.483(17) . .
Se1 U2 Se7 135.094(12) 7_556 .
Se1 U2 Se7 135.094(12) 4_546 .
Se1 U2 Se7 68.463(12) . .
Se1 U2 Se7 68.463(12) 6 .
Se5 U2 Se7 137.371(19) . .
Se2 U3 Se2 150.93(2) 5_655 2_655
Se2 U3 Se4 102.333(12) 5_655 5_656
Se2 U3 Se4 102.333(12) 2_655 5_656
Se2 U3 Se5 84.276(12) 5_655 5_655
Se2 U3 Se5 84.276(12) 2_655 5_655
Se4 U3 Se5 145.09(2) 5_656 5_655
Se2 U3 Se6 85.496(13) 5_655 .
Se2 U3 Se6 85.496(13) 2_655 .
Se4 U3 Se6 76.56(2) 5_656 .
Se5 U3 Se6 138.35(2) 5_655 .
Se2 U3 Se2 134.347(14) 5_655 8
Se2 U3 Se2 68.553(18) 2_655 8
Se4 U3 Se2 72.585(17) 5_656 8
Se5 U3 Se2 78.416(17) 5_655 8
Se6 U3 Se2 133.538(15) . 8
Se2 U3 Se2 68.553(18) 5_655 3_545
Se2 U3 Se2 134.347(14) 2_655 3_545
Se4 U3 Se2 72.585(17) 5_656 3_545
Se5 U3 Se2 78.416(17) 5_655 3_545
Se6 U3 Se2 133.538(15) . 3_545
Se2 U3 Se2 66.72(2) 8 3_545
Se2 U3 Se6 75.465(12) 5_655 5_655
Se2 U3 Se6 75.465(12) 2_655 5_655
Se4 U3 Se6 148.07(2) 5_656 5_655
Se5 U3 Se6 66.84(2) 5_655 5_655
Se6 U3 Se6 71.51(2) . 5_655
Se2 U3 Se6 131.788(15) 8 5_655
Se2 U3 Se6 131.788(15) 3_545 5_655
U2 Se1 U2 106.152(17) 7_556 .
U2 Se1 U1 149.42(2) 7_556 8_455
U2 Se1 U1 95.043(16) . 8_455
U2 Se1 U1 104.202(18) 7_556 7_556
U2 Se1 U1 91.585(16) . 7_556
U1 Se1 U1 96.833(16) 8_455 7_556
Ti1 Se2 U3 139.59(2) 3 5_655
Ti1 Se2 U1 95.051(17) 3 .
U3 Se2 U1 92.021(16) 5_655 .
Ti1 Se2 U3 105.175(17) 3 3_455
U3 Se2 U3 111.448(17) 5_655 3_455
U1 Se2 U3 104.300(17) . 3_455
Ti1 Se3 U2 156.88(3) . .
Ti1 Se3 U1 99.06(2) . 3_445
U2 Se3 U1 96.42(2) . 3_445
Ti1 Se3 U1 99.06(2) . 8_455
U2 Se3 U1 96.42(2) . 8_455
U1 Se3 U1 95.53(2) 3_445 8_455
U2 Se4 U3 152.16(3) . 5_656
U2 Se4 U1 91.894(19) . 4_546
U3 Se4 U1 107.233(19) 5_656 4_546
U2 Se4 U1 91.894(19) . 7_556
U3 Se4 U1 107.233(19) 5_656 7_556
U1 Se4 U1 91.50(2) 4_546 7_556
U2 Se5 U3 157.22(3) . 5_655
U2 Se5 U1 104.220(19) . 6
U3 Se5 U1 90.175(18) 5_655 6
U2 Se5 U1 104.220(19) . .
U3 Se5 U1 90.175(18) 5_655 .
U1 Se5 U1 100.18(3) 6 .
U1 Se6 U1 98.30(2) . 6
U1 Se6 U3 129.679(13) . .
U1 Se6 U3 129.679(13) 6 .
U1 Se6 U3 86.116(18) . 5_655
U1 Se6 U3 86.116(18) 6 5_655
U3 Se6 U3 108.49(2) . 5_655
U2 Se7 U2 180.0 5_556 .
U2 Se7 U1 88.885(6) 5_556 3_445
U2 Se7 U1 91.116(5) . 3_445
U2 Se7 U1 91.115(5) 5_556 7_556
U2 Se7 U1 88.884(5) . 7_556
U1 Se7 U1 180.000(5) 3_445 7_556
U2 Se7 U1 91.115(5) 5_556 4_546
U2 Se7 U1 88.884(5) . 4_546
U1 Se7 U1 91.753(7) 3_445 4_546
U1 Se7 U1 88.247(7) 7_556 4_546
U2 Se7 U1 88.885(5) 5_556 8_455
U2 Se7 U1 91.116(5) . 8_455
U1 Se7 U1 88.247(7) 3_445 8_455
U1 Se7 U1 91.753(7) 7_556 8_455
U1 Se7 U1 180.0 4_546 8_455
Se3 Ti1 Se3 180.0 5 .
Se3 Ti1 Se2 89.971(18) 5 3_445
Se3 Ti1 Se2 90.029(18) . 3_445
Se3 Ti1 Se2 90.029(18) 5 7
Se3 Ti1 Se2 89.971(18) . 7
Se2 Ti1 Se2 180.00(3) 3_445 7
Se3 Ti1 Se2 90.029(18) 5 4_545
Se3 Ti1 Se2 89.971(18) . 4_545
Se2 Ti1 Se2 98.27(2) 3_445 4_545
Se2 Ti1 Se2 81.73(2) 7 4_545
Se3 Ti1 Se2 89.971(18) 5 8_455
Se3 Ti1 Se2 90.029(18) . 8_455
Se2 Ti1 Se2 81.73(2) 3_445 8_455
Se2 Ti1 Se2 98.27(2) 7 8_455
Se2 Ti1 Se2 180.00(2) 4_545 8_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 Se3 2.8936(6) 3
U1 Se1 2.9269(6) 8
U1 Se5 2.9524(6) .
U1 Se2 2.9626(6) .
U1 Se1 2.9794(6) 7_556
U1 Se4 2.9911(6) 7_556
U1 Se6 2.9939(5) .
U1 Se7 3.07729(19) 3
U2 Se3 2.8729(9) .
U2 Se4 2.8747(8) .
U2 Se1 2.8902(6) 7_556
U2 Se1 2.8902(6) 4_546
U2 Se1 2.9024(5) .
U2 Se1 2.9025(5) 6
U2 Se5 2.9168(8) .
U2 Se7 2.9431(3) .
U3 Se2 2.8161(5) 5_655
U3 Se2 2.8161(5) 2_655
U3 Se4 2.9132(8) 5_656
U3 Se5 2.9200(8) 5_655
U3 Se6 3.0045(8) .
U3 Se2 3.0570(6) 8
U3 Se2 3.0570(6) 3_545
U3 Se6 3.0964(8) 5_655
Se1 U2 2.8902(6) 7_556
Se1 U1 2.9270(6) 8_455
Se1 U1 2.9794(6) 7_556
Se2 Ti1 2.5693(5) 3
Se2 U3 2.8161(5) 5_655
Se2 U3 3.0569(6) 3_455
Se3 Ti1 2.4688(8) .
Se3 U1 2.8937(6) 3_445
Se3 U1 2.8937(6) 8_455
Se4 U3 2.9131(8) 5_656
Se4 U1 2.9911(6) 4_546
Se4 U1 2.9911(6) 7_556
Se5 U3 2.9200(8) 5_655
Se5 U1 2.9524(6) 6
Se6 U1 2.9939(5) 6
Se6 U3 3.0964(8) 5_655
Se7 U2 2.9431(3) 5_556
Se7 U1 3.07730(19) 3_445
Se7 U1 3.07730(19) 7_556
Se7 U1 3.07730(19) 4_546
Se7 U1 3.07730(19) 8_455
Ti1 Se3 2.4688(8) 5
Ti1 Se2 2.5693(5) 3_445
Ti1 Se2 2.5693(5) 7
Ti1 Se2 2.5693(5) 4_545
Ti1 Se2 2.5693(5) 8_455
