#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/09/2230973.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230973
loop_
_publ_author_name
'Oh, George N.'
'Ibers, James A.'
_publ_section_title
;
 Manganese(II) octauranium(IV) heptadecasulfide
;
_journal_coeditor_code           WM2512
_journal_issue                   9
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              i46
_journal_page_last               i46
_journal_paper_doi               10.1107/S1600536811030546
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'Mn U8 S17'
_chemical_formula_structural     'Mn U8 S17'
_chemical_formula_sum            'Mn S17 U8'
_chemical_formula_weight         2504.20
_chemical_name_systematic
;
Manganese(II) octauranium(IV) heptadecasulfide
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.658(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3549(6)
_cell_length_b                   8.3893(4)
_cell_length_c                   10.4927(5)
_cell_measurement_reflns_used    8717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.496
_cell_measurement_theta_min      2.884
_cell_volume                     1151.33(9)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8422
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    58.100
_exptl_absorpt_correction_T_max  0.0846
_exptl_absorpt_correction_T_min  0.0430
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'face indexed (SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             2066
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.899
_refine_diff_density_min         -1.940
_refine_ls_extinction_coef       0.00082(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008a)'
_refine_ls_goodness_of_fit_ref   2.098
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.098
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0259
_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)+(0.0161Fo²)²]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                1578
_reflns_number_total             1609
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2512.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2230973
_cod_database_fobs_code          2230973
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.44179(2) 0.25549(3) 0.29633(3) 0.00531(11) Uani d . 1 1 . .
U U2 0.20440(3) 0.0000 0.45685(4) 0.00510(12) Uani d S 1 2 . .
U U3 0.68285(3) 0.0000 0.02025(4) 0.00541(12) Uani d S 1 2 . .
Mn Mn1 0.0000 0.0000 0.0000 0.0058(5) Uani d S 1 4 . .
S S1 0.12730(15) 0.3047(2) 0.46870(18) 0.0065(4) Uani d . 1 1 . .
S S2 0.36424(15) 0.3062(2) 0.03492(18) 0.0064(4) Uani d . 1 1 . .
S S3 0.0598(2) 0.0000 0.2314(3) 0.0066(5) Uani d S 1 2 . .
S S4 0.2086(2) 0.0000 0.7197(3) 0.0061(5) Uani d S 1 2 . .
S S5 0.3030(2) 0.0000 0.2463(3) 0.0058(5) Uani d S 1 2 . .
S S6 0.5211(2) 0.0000 0.1694(3) 0.0061(5) Uani d S 1 2 . .
S S7 0.0000 0.0000 0.5000 0.0056(7) Uani d S 1 4 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S3 U1 S2 3 . 76.01(7) ?
S3 U1 S1 3 8 79.55(7) ?
S2 U1 S1 . 8 140.70(6) ?
S3 U1 S5 3 . 155.43(8) ?
S2 U1 S5 . . 80.28(7) ?
S1 U1 S5 8 . 116.52(6) ?
S3 U1 S6 3 . 99.20(7) ?
S2 U1 S6 . . 75.58(7) ?
S1 U1 S6 8 . 78.56(7) ?
S5 U1 S6 . . 68.37(7) ?
S3 U1 S1 3 7_556 130.39(7) ?
S2 U1 S1 . 7_556 139.93(6) ?
S1 U1 S1 8 7_556 78.93(6) ?
S5 U1 S1 . 7_556 73.14(7) ?
S6 U1 S1 . 7_556 119.29(6) ?
S3 U1 S4 3 7_556 83.16(6) ?
S2 U1 S4 . 7_556 73.29(7) ?
S1 U1 S4 8 7_556 133.46(7) ?
S5 U1 S4 . 7_556 96.17(6) ?
S6 U1 S4 . 7_556 147.19(8) ?
S1 U1 S4 7_556 7_556 80.27(7) ?
S3 U1 S7 3 3 65.25(5) ?
S2 U1 S7 . 3 127.10(4) ?
S1 U1 S7 8 3 65.71(4) ?
S5 U1 S7 . 3 137.07(6) ?
S6 U1 S7 . 3 142.74(6) ?
S1 U1 S7 7_556 3 65.18(4) ?
S4 U1 S7 7_556 3 67.79(5) ?
S3 U1 U3 3 5_655 110.77(6) ?
S2 U1 U3 . 5_655 41.58(4) ?
S1 U1 U3 8 5_655 126.98(4) ?
S5 U1 U3 . 5_655 44.95(6) ?
S6 U1 U3 . 5_655 48.80(6) ?
S1 U1 U3 7_556 5_655 117.93(4) ?
S4 U1 U3 7_556 5_655 99.54(5) ?
S7 U1 U3 3 5_655 166.765(10) ?
S3 U1 U2 3 7_556 98.80(5) ?
S2 U1 U2 . 7_556 114.83(4) ?
S1 U1 U2 8 7_556 98.88(4) ?
S5 U1 U2 . 7_556 96.86(5) ?
S6 U1 U2 . 7_556 161.01(4) ?
S1 U1 U2 7_556 7_556 42.42(4) ?
S4 U1 U2 7_556 7_556 42.01(5) ?
S7 U1 U2 3 7_556 44.218(7) ?
U3 U1 U2 5_655 7_556 128.230(12) ?
S3 U2 S4 . . 137.38(8) ?
S3 U2 S1 . 7_556 129.53(6) ?
S4 U2 S1 . 7_556 82.29(6) ?
S3 U2 S1 . 4_546 129.53(6) ?
S4 U2 S1 . 4_546 82.29(6) ?
S1 U2 S1 7_556 4_546 72.72(8) ?
S3 U2 S1 . . 80.49(5) ?
S4 U2 S1 . . 83.52(5) ?
S1 U2 S1 7_556 . 74.25(7) ?
S1 U2 S1 4_546 . 145.44(5) ?
S3 U2 S1 . 6 80.49(5) ?
S4 U2 S1 . 6 83.52(5) ?
S1 U2 S1 7_556 6 145.44(5) ?
S1 U2 S1 4_546 6 74.25(7) ?
S1 U2 S1 . 6 134.89(9) ?
S3 U2 S5 . . 71.28(8) ?
S4 U2 S5 . . 151.35(9) ?
S1 U2 S5 7_556 . 74.75(6) ?
S1 U2 S5 4_546 . 74.75(6) ?
S1 U2 S5 . . 105.95(4) ?
S1 U2 S5 6 . 105.95(4) ?
S3 U2 S7 . . 66.83(6) ?
S4 U2 S7 . . 70.55(6) ?
S1 U2 S7 7_556 . 134.75(4) ?
S1 U2 S7 4_546 . 134.75(4) ?
S1 U2 S7 . . 67.46(4) ?
S1 U2 S7 6 . 67.46(4) ?
S5 U2 S7 . . 138.10(6) ?
S3 U2 U1 . 7_556 101.73(5) ?
S4 U2 U1 . 7_556 44.00(4) ?
S1 U2 U1 7_556 7_556 89.36(4) ?
S1 U2 U1 4_546 7_556 125.64(4) ?
S1 U2 U1 . 7_556 43.93(4) ?
S1 U2 U1 6 7_556 101.83(4) ?
S5 U2 U1 . 7_556 149.546(11) ?
S7 U2 U1 . 7_556 46.101(7) ?
S3 U2 U1 . 4_546 101.73(5) ?
S4 U2 U1 . 4_546 44.00(4) ?
S1 U2 U1 7_556 4_546 125.64(4) ?
S1 U2 U1 4_546 4_546 89.36(4) ?
S1 U2 U1 . 4_546 101.83(4) ?
S1 U2 U1 6 4_546 43.93(4) ?
S5 U2 U1 . 4_546 149.546(10) ?
S7 U2 U1 . 4_546 46.101(7) ?
U1 U2 U1 7_556 4_546 60.118(10) ?
S2 U3 S2 5_655 2_655 146.88(9) ?
S2 U3 S4 5_655 5_656 105.15(4) ?
S2 U3 S4 2_655 5_656 105.15(4) ?
S2 U3 S5 5_655 5_655 81.18(4) ?
S2 U3 S5 2_655 5_655 81.18(4) ?
S4 U3 S5 5_656 5_655 146.02(8) ?
S2 U3 S2 5_655 8 134.99(5) ?
S2 U3 S2 2_655 8 68.31(7) ?
S4 U3 S2 5_656 8 71.79(6) ?
S5 U3 S2 5_655 8 80.27(6) ?
S2 U3 S2 5_655 3_545 68.31(7) ?
S2 U3 S2 2_655 3_545 134.99(5) ?
S4 U3 S2 5_656 3_545 71.79(6) ?
S5 U3 S2 5_655 3_545 80.27(6) ?
S2 U3 S2 8 3_545 68.33(8) ?
S2 U3 S6 5_655 . 87.07(5) ?
S2 U3 S6 2_655 . 87.07(5) ?
S4 U3 S6 5_656 . 76.83(8) ?
S5 U3 S6 5_655 . 137.15(8) ?
S2 U3 S6 8 . 132.44(5) ?
S2 U3 S6 3_545 . 132.44(5) ?
S2 U3 S6 5_655 5_655 73.60(4) ?
S2 U3 S6 2_655 5_655 73.60(4) ?
S4 U3 S6 5_656 5_655 148.59(8) ?
S5 U3 S6 5_655 5_655 65.38(8) ?
S2 U3 S6 8 5_655 131.75(5) ?
S2 U3 S6 3_545 5_655 131.75(5) ?
S6 U3 S6 . 5_655 71.77(8) ?
S2 U3 U1 5_655 5_655 43.17(4) ?
S2 U3 U1 2_655 5_655 107.02(4) ?
S4 U3 U1 5_656 5_655 147.748(6) ?
S5 U3 U1 5_655 5_655 44.40(4) ?
S2 U3 U1 8 5_655 123.06(4) ?
S2 U3 U1 3_545 5_655 86.95(4) ?
S6 U3 U1 . 5_655 102.46(5) ?
S6 U3 U1 5_655 5_655 44.81(3) ?
S2 U3 U1 5_655 2_655 107.02(4) ?
S2 U3 U1 2_655 2_655 43.17(4) ?
S4 U3 U1 5_656 2_655 147.748(6) ?
S5 U3 U1 5_655 2_655 44.40(4) ?
S2 U3 U1 8 2_655 86.95(4) ?
S2 U3 U1 3_545 2_655 123.06(4) ?
S6 U3 U1 . 2_655 102.46(5) ?
S6 U3 U1 5_655 2_655 44.81(3) ?
U1 U3 U1 5_655 2_655 64.432(10) ?
S3 Mn1 S3 . 5 180.0 ?
S3 Mn1 S2 . 3_445 87.41(7) ?
S3 Mn1 S2 5 3_445 92.59(7) ?
S3 Mn1 S2 . 7 92.59(7) ?
S3 Mn1 S2 5 7 87.41(7) ?
S2 Mn1 S2 3_445 7 180.00(11) ?
S3 Mn1 S2 . 4_545 92.59(7) ?
S3 Mn1 S2 5 4_545 87.41(7) ?
S2 Mn1 S2 3_445 4_545 99.50(9) ?
S2 Mn1 S2 7 4_545 80.50(9) ?
S3 Mn1 S2 . 8_455 87.41(7) ?
S3 Mn1 S2 5 8_455 92.59(7) ?
S2 Mn1 S2 3_445 8_455 80.50(9) ?
S2 Mn1 S2 7 8_455 99.50(9) ?
S2 Mn1 S2 4_545 8_455 180.00(9) ?
U2 S1 U2 7_556 . 105.75(7) ?
U2 S1 U1 7_556 8_455 148.40(8) ?
U2 S1 U1 . 8_455 95.33(6) ?
U2 S1 U1 7_556 7_556 104.35(6) ?
U2 S1 U1 . 7_556 93.65(6) ?
U1 S1 U1 8_455 7_556 97.35(6) ?
Mn1 S2 U3 3 5_655 137.09(8) ?
Mn1 S2 U1 3 . 96.17(6) ?
U3 S2 U1 5_655 . 95.25(6) ?
Mn1 S2 U3 3 3_455 104.41(7) ?
U3 S2 U3 5_655 3_455 111.68(7) ?
U1 S2 U3 . 3_455 106.32(6) ?
Mn1 S3 U2 . . 155.27(12) ?
Mn1 S3 U1 . 3_445 99.23(8) ?
U2 S3 U1 . 3_445 97.20(7) ?
Mn1 S3 U1 . 8_455 99.23(8) ?
U2 S3 U1 . 8_455 97.20(7) ?
U1 S3 U1 3_445 8_455 96.26(9) ?
U2 S4 U3 . 5_656 150.90(11) ?
U2 S4 U1 . 4_546 93.99(7) ?
U3 S4 U1 5_656 4_546 105.98(7) ?
U2 S4 U1 . 7_556 93.99(7) ?
U3 S4 U1 5_656 7_556 105.98(7) ?
U1 S4 U1 4_546 7_556 91.99(8) ?
U2 S5 U1 . . 104.51(7) ?
U2 S5 U1 . 6 104.51(7) ?
U1 S5 U1 . 6 99.28(9) ?
U2 S5 U3 . 5_655 156.22(12) ?
U1 S5 U3 . 5_655 90.65(7) ?
U1 S5 U3 6 5_655 90.65(7) ?
U1 S6 U1 6 . 98.05(8) ?
U1 S6 U3 6 . 129.76(5) ?
U1 S6 U3 . . 129.76(5) ?
U1 S6 U3 6 5_655 86.39(7) ?
U1 S6 U3 . 5_655 86.39(7) ?
U3 S6 U3 . 5_655 108.23(8) ?
U2 S7 U2 . 5_556 180.0 ?
U2 S7 U1 . 3_445 90.317(8) ?
U2 S7 U1 5_556 3_445 89.682(8) ?
U2 S7 U1 . 7_556 89.683(8) ?
U2 S7 U1 5_556 7_556 90.318(8) ?
U1 S7 U1 3_445 7_556 180.0 ?
U2 S7 U1 . 4_546 89.683(8) ?
U2 S7 U1 5_556 4_546 90.318(8) ?
U1 S7 U1 3_445 4_546 91.925(11) ?
U1 S7 U1 7_556 4_546 88.075(11) ?
U2 S7 U1 . 8_455 90.317(8) ?
U2 S7 U1 5_556 8_455 89.682(8) ?
U1 S7 U1 3_445 8_455 88.075(11) ?
U1 S7 U1 7_556 8_455 91.925(11) ?
U1 S7 U1 4_546 8_455 180.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 S3 3 2.7546(19) ?
U1 S2 . 2.7621(19) ?
U1 S1 8 2.802(2) ?
U1 S5 . 2.8129(19) ?
U1 S6 . 2.8390(18) ?
U1 S1 7_556 2.8469(19) ?
U1 S4 7_556 2.852(2) ?
U1 S7 3 2.9509(3) ?
U1 U3 5_655 4.0206(4) ?
U1 U2 7_556 4.0951(5) ?
U2 S3 . 2.735(3) ?
U2 S4 . 2.747(3) ?
U2 S1 7_556 2.763(2) ?
U2 S1 4_546 2.763(2) ?
U2 S1 . 2.768(2) ?
U2 S1 6 2.768(2) ?
U2 S5 . 2.791(3) ?
U2 S7 . 2.8559(4) ?
U2 U1 7_556 4.0952(5) ?
U2 U1 4_546 4.0952(5) ?
U3 S2 5_655 2.680(2) ?
U3 S2 2_655 2.680(2) ?
U3 S4 5_656 2.819(3) ?
U3 S5 5_655 2.841(3) ?
U3 S2 8 2.896(2) ?
U3 S2 3_545 2.896(2) ?
U3 S6 . 2.912(3) ?
U3 S6 5_655 3.031(3) ?
U3 U1 5_655 4.0205(4) ?
U3 U1 2_655 4.0205(4) ?
Mn1 S3 . 2.398(3) ?
Mn1 S3 5 2.398(3) ?
Mn1 S2 3_445 2.5168(19) ?
Mn1 S2 7 2.5168(19) ?
Mn1 S2 4_545 2.5168(19) ?
Mn1 S2 8_455 2.5168(19) ?
S1 U2 7_556 2.763(2) ?
S1 U1 8_455 2.802(2) ?
S1 U1 7_556 2.8469(19) ?
S2 Mn1 3 2.5168(19) ?
S2 U3 5_655 2.680(2) ?
S2 U3 3_455 2.896(2) ?
S3 U1 3_445 2.7546(19) ?
S3 U1 8_455 2.7546(19) ?
S4 U3 5_656 2.819(3) ?
S4 U1 4_546 2.852(2) ?
S4 U1 7_556 2.852(2) ?
S5 U1 6 2.8130(19) ?
S5 U3 5_655 2.841(3) ?
S6 U1 6 2.8390(18) ?
S6 U3 5_655 3.031(3) ?
S7 U2 5_556 2.8559(4) ?
S7 U1 3_445 2.9509(3) ?
S7 U1 7_556 2.9509(3) ?
S7 U1 4_546 2.9509(3) ?
S7 U1 8_455 2.9509(3) ?
