#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:08:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179502 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/99/4339955.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_4339955
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 U8 V'
_chemical_formula_sum            'Se17 U8 V'
_chemical_formula_weight         3297.50
_chemical_name_systematic
'Vanadium(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                 101.5610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9192(4)
_cell_length_b                   8.7569(2)
_cell_length_c                   10.8758(3)
_cell_measurement_reflns_used    5002
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0975
_cell_measurement_theta_min      3.208
_cell_volume                     1298.75(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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14653
_diffrn_reflns_theta_full        33.18
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    73.836
_exptl_absorpt_correction_T_max  0.3199
_exptl_absorpt_correction_T_min  0.0719
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face-indexed, SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    8.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2674
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.875
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.456
_refine_ls_extinction_coef       0.00072(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         2623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.002
_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+(0.0204P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                2429
_reflns_number_total             2623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500721d_si_001.cif
_cod_data_source_block           VU8Se17
_cod_depositor_comments
'Adding full bibliography for 4339953--4339960.cif.'
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4339955
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 0.440972(13) 0.257160(19) 0.294640(16) 0.00447(5) Uani 1 1 d .
U2 U 0.202484(18) 0.0000 0.45755(2) 0.00437(6) Uani 1 2 d S
U3 U 0.681490(18) 0.0000 0.01711(2) 0.00448(6) Uani 1 2 d S
Se1 Se 0.12713(3) 0.30642(5) 0.46683(5) 0.00476(9) Uani 1 1 d .
Se2 Se 0.36518(4) 0.30985(5) 0.02692(4) 0.00467(9) Uani 1 1 d .
Se3 Se 0.05973(5) 0.0000 0.22802(7) 0.00563(12) Uani 1 2 d S
Se4 Se 0.21135(5) 0.0000 0.72338(6) 0.00468(12) Uani 1 2 d S
Se5 Se 0.30232(5) 0.0000 0.24670(6) 0.00441(12) Uani 1 2 d S
Se6 Se 0.52070(5) 0.0000 0.16810(6) 0.00465(12) Uani 1 2 d S
Se7 Se 0.0000 0.0000 0.5000 0.00505(16) Uani 1 4 d S
V1 V 0.0000 0.0000 0.0000 0.0069(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
V V 0.3005 0.5294 '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 Se2 75.138(17) 3 .
Se3 U1 Se1 79.751(17) 3 8
Se2 U1 Se1 139.618(15) . 8
Se3 U1 Se5 155.68(2) 3 .
Se2 U1 Se5 81.468(16) . .
Se1 U1 Se5 115.610(15) 8 .
Se3 U1 Se6 99.039(15) 3 .
Se2 U1 Se6 75.648(16) . .
Se1 U1 Se6 77.716(17) 8 .
Se5 U1 Se6 68.297(16) . .
Se3 U1 Se4 83.861(15) 3 7_556
Se2 U1 Se4 73.291(16) . 7_556
Se1 U1 Se4 134.720(16) 8 7_556
Se5 U1 Se4 95.835(15) . 7_556
Se6 U1 Se4 146.902(19) . 7_556
Se3 U1 Se1 130.955(17) 3 7_556
Se2 U1 Se1 141.186(15) . 7_556
Se1 U1 Se1 78.663(15) 8 7_556
Se5 U1 Se1 72.563(16) . 7_556
Se6 U1 Se1 118.324(15) . 7_556
Se4 U1 Se1 81.072(16) 7_556 7_556
Se3 U1 Se7 65.658(13) 3 3
Se2 U1 Se7 127.163(11) . 3
Se1 U1 Se7 66.031(10) 8 3
Se5 U1 Se7 136.736(14) . 3
Se6 U1 Se7 142.320(14) . 3
Se4 U1 Se7 68.737(12) 7_556 3
Se1 U1 Se7 65.362(10) 7_556 3
Se3 U2 Se4 139.56(2) . .
Se3 U2 Se1 80.622(12) . 6
Se4 U2 Se1 84.690(12) . 6
Se3 U2 Se1 80.623(12) . .
Se4 U2 Se1 84.689(12) . .
Se1 U2 Se1 136.38(2) 6 .
Se3 U2 Se1 129.297(15) . 7_556
Se4 U2 Se1 81.170(16) . 7_556
Se1 U2 Se1 144.640(13) 6 7_556
Se1 U2 Se1 74.279(15) . 7_556
Se3 U2 Se1 129.297(15) . 4_546
Se4 U2 Se1 81.170(16) . 4_546
Se1 U2 Se1 74.279(15) 6 4_546
Se1 U2 Se1 144.639(13) . 4_546
Se1 U2 Se1 71.62(2) 7_556 4_546
Se3 U2 Se5 70.75(2) . .
Se4 U2 Se5 149.69(2) . .
Se1 U2 Se5 105.158(11) 6 .
Se1 U2 Se5 105.158(11) . .
Se1 U2 Se5 74.373(15) 7_556 .
Se1 U2 Se5 74.373(15) 4_546 .
Se3 U2 Se7 67.537(15) . .
Se4 U2 Se7 72.023(15) . .
Se1 U2 Se7 68.236(11) 6 .
Se1 U2 Se7 68.236(11) . .
Se1 U2 Se7 135.238(11) 7_556 .
Se1 U2 Se7 135.238(11) 4_546 .
Se5 U2 Se7 138.289(16) . .
Se2 U3 Se2 150.05(2) 5_655 2_655
Se2 U3 Se4 102.767(11) 5_655 5_656
Se2 U3 Se4 102.767(11) 2_655 5_656
Se2 U3 Se5 83.876(12) 5_655 5_655
Se2 U3 Se5 83.876(12) 2_655 5_655
Se4 U3 Se5 145.59(2) 5_656 5_655
Se2 U3 Se6 85.507(12) 5_655 .
Se2 U3 Se6 85.507(12) 2_655 .
Se4 U3 Se6 76.438(19) 5_656 .
Se5 U3 Se6 137.97(2) 5_655 .
Se2 U3 Se2 134.460(13) 5_655 8
Se2 U3 Se2 68.927(16) 2_655 8
Se4 U3 Se2 72.666(15) 5_656 8
Se5 U3 Se2 78.721(15) 5_655 8
Se6 U3 Se2 133.594(14) . 8
Se2 U3 Se2 68.927(16) 5_655 3_545
Se2 U3 Se2 134.460(13) 2_655 3_545
Se4 U3 Se2 72.666(15) 5_656 3_545
Se5 U3 Se2 78.721(15) 5_655 3_545
Se6 U3 Se2 133.594(14) . 3_545
Se2 U3 Se2 66.544(18) 8 3_545
Se2 U3 Se6 75.028(11) 5_655 5_655
Se2 U3 Se6 75.028(11) 2_655 5_655
Se4 U3 Se6 147.82(2) 5_656 5_655
Se5 U3 Se6 66.588(19) 5_655 5_655
Se6 U3 Se6 71.38(2) . 5_655
Se2 U3 Se6 131.931(14) 8 5_655
Se2 U3 Se6 131.931(14) 3_545 5_655
U2 Se1 U2 105.721(15) . 7_556
U2 Se1 U1 94.699(15) . 8_455
U2 Se1 U1 149.470(19) 7_556 8_455
U2 Se1 U1 92.167(14) . 7_556
U2 Se1 U1 104.284(16) 7_556 7_556
U1 Se1 U1 97.224(15) 8_455 7_556
V1 Se2 U3 139.11(2) 3 5_655
V1 Se2 U1 95.143(15) 3 .
U3 Se2 U1 92.421(15) 5_655 .
V1 Se2 U3 105.655(15) 3 3_455
U3 Se2 U3 111.074(16) 5_655 3_455
U1 Se2 U3 104.746(16) . 3_455
V1 Se3 U2 156.54(3) . .
V1 Se3 U1 99.169(19) . 3_445
U2 Se3 U1 96.544(18) . 3_445
V1 Se3 U1 99.169(19) . 8_455
U2 Se3 U1 96.544(18) . 8_455
U1 Se3 U1 95.45(2) 3_445 8_455
U2 Se4 U3 152.34(3) . 5_656
U2 Se4 U1 92.715(17) . 4_546
U3 Se4 U1 106.420(17) 5_656 4_546
U2 Se4 U1 92.715(17) . 7_556
U3 Se4 U1 106.420(17) 5_656 7_556
U1 Se4 U1 91.00(2) 4_546 7_556
U2 Se5 U3 156.44(3) . 5_655
U2 Se5 U1 105.079(17) . 6
U3 Se5 U1 89.831(16) 5_655 6
U2 Se5 U1 105.078(17) . .
U3 Se5 U1 89.832(16) 5_655 .
U1 Se5 U1 99.82(2) 6 .
U1 Se6 U1 98.71(2) 6 .
U1 Se6 U3 129.555(11) 6 .
U1 Se6 U3 129.555(11) . .
U1 Se6 U3 85.788(15) 6 5_655
U1 Se6 U3 85.788(15) . 5_655
U3 Se6 U3 108.62(2) . 5_655
U2 Se7 U2 180.0 5_556 .
U2 Se7 U1 89.373(5) 5_556 3_445
U2 Se7 U1 90.627(5) . 3_445
U2 Se7 U1 90.627(5) 5_556 7_556
U2 Se7 U1 89.373(5) . 7_556
U1 Se7 U1 180.0 3_445 7_556
U2 Se7 U1 90.627(5) 5_556 4_546
U2 Se7 U1 89.373(5) . 4_546
U1 Se7 U1 92.460(7) 3_445 4_546
U1 Se7 U1 87.540(7) 7_556 4_546
U2 Se7 U1 89.373(5) 5_556 8_455
U2 Se7 U1 90.627(5) . 8_455
U1 Se7 U1 87.540(7) 3_445 8_455
U1 Se7 U1 92.460(7) 7_556 8_455
U1 Se7 U1 180.0 4_546 8_455
Se3 V1 Se3 180.0 5 .
Se3 V1 Se2 90.453(16) 5 3_445
Se3 V1 Se2 89.547(16) . 3_445
Se3 V1 Se2 89.547(16) 5 7
Se3 V1 Se2 90.453(16) . 7
Se2 V1 Se2 180.00(3) 3_445 7
Se3 V1 Se2 89.547(16) 5 4_545
Se3 V1 Se2 90.454(16) . 4_545
Se2 V1 Se2 99.20(2) 3_445 4_545
Se2 V1 Se2 80.80(2) 7 4_545
Se3 V1 Se2 90.453(16) 5 8_455
Se3 V1 Se2 89.546(16) . 8_455
Se2 V1 Se2 80.80(2) 3_445 8_455
Se2 V1 Se2 99.20(2) 7 8_455
Se2 V1 Se2 180.00(3) 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 2.8740(5) 3
U1 Se2 2.9278(5) .
U1 Se1 2.9302(5) 8
U1 Se5 2.9435(5) .
U1 Se6 2.9680(5) .
U1 Se4 2.9815(5) 7_556
U1 Se1 2.9873(5) 7_556
U1 Se7 3.07408(18) 3
U2 Se3 2.8621(7) .
U2 Se4 2.8688(7) .
U2 Se1 2.8902(5) 6
U2 Se1 2.8902(5) .
U2 Se1 2.8971(5) 7_556
U2 Se1 2.8971(5) 4_546
U2 Se5 2.9098(7) .
U2 Se7 2.9458(3) .
U3 Se2 2.8087(5) 5_655
U3 Se2 2.8087(5) 2_655
U3 Se4 2.9161(7) 5_656
U3 Se5 2.9226(7) 5_655
U3 Se6 3.0297(7) .
U3 Se2 3.0351(5) 8
U3 Se2 3.0351(5) 3_545
U3 Se6 3.1153(7) 5_655
Se1 U2 2.8971(5) 7_556
Se1 U1 2.9302(5) 8_455
Se1 U1 2.9873(5) 7_556
Se2 V1 2.5691(5) 3
Se2 U3 2.8087(5) 5_655
Se2 U3 3.0352(5) 3_455
Se3 V1 2.4525(7) .
Se3 U1 2.8740(5) 3_445
Se3 U1 2.8740(5) 8_455
Se4 U3 2.9161(7) 5_656
Se4 U1 2.9815(5) 4_546
Se4 U1 2.9815(5) 7_556
Se5 U3 2.9227(7) 5_655
Se5 U1 2.9435(5) 6
Se6 U1 2.9679(5) 6
Se6 U3 3.1153(7) 5_655
Se7 U2 2.9458(3) 5_556
Se7 U1 3.07411(18) 3_445
Se7 U1 3.07411(18) 7_556
Se7 U1 3.07411(18) 4_546
Se7 U1 3.07411(18) 8_455
V1 Se3 2.4525(7) 5
V1 Se2 2.5691(5) 3_445
V1 Se2 2.5691(5) 7
V1 Se2 2.5691(5) 4_545
V1 Se2 2.5691(5) 8_455
