#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/91/2239179.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_2239179
loop_
_publ_author_name
'Ward, Matthew D.'
'Ibers, James A.'
_publ_section_title
;
 Nickel(II) uranium(IV) trisulfide
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i4
_journal_paper_doi               10.1107/S1600536813033680
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Ni U S3'
_chemical_formula_structural     'Ni U S3'
_chemical_formula_sum            'Ni S3 U'
_chemical_formula_weight         392.92
_chemical_name_systematic
;
Nickel(II) uranium(IV) trisulfide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8924(3)
_cell_length_b                   8.7570(4)
_cell_length_c                   6.0758(2)
_cell_measurement_reflns_used    3973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1815
_cell_measurement_theta_min      4.082
_cell_volume                     366.72(3)
_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  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7334
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.225
_diffrn_reflns_theta_min         4.082
_exptl_absorpt_coefficient_mu    50.683
_exptl_absorpt_correction_T_max  0.1082
_exptl_absorpt_correction_T_min  0.0933
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.117
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.079
_refine_diff_density_max         2.801
_refine_diff_density_min         -1.151
_refine_ls_extinction_coef       0.0039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 2013)'
_refine_ls_goodness_of_fit_ref   1.356
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[σ²(Fo²)+(0.0149Fo²)²]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                728
_reflns_number_total             748
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2789sup1.cf
_cod_data_source_block           I
_cod_database_code               2239179
_cod_database_fobs_code          2239179
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.093
_shelx_estimated_absorpt_t_max   0.108
_shelxl_version_number           2.013
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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_occupancy
U U1 0.38141(3) 0.2500 0.05064(3) 0.00770(8) Uani d 1
Ni Ni1 0.0000 0.0000 0.0000 0.00778(13) Uani d 1
S S1 0.18039(14) 0.05448(9) 0.33217(13) 0.00731(15) Uani d 1
S S2 0.52930(19) 0.2500 0.63121(19) 0.0085(2) Uani d 1
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'
Ni Ni 0.3393 1.1124 '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
S2 U1 S2 6_556 1_554 87.32(2)
S2 U1 S1 6_556 4 141.532(18)
S2 U1 S1 1_554 4 87.85(3)
S2 U1 S1 6_556 6_656 141.532(18)
S2 U1 S1 1_554 6_656 87.85(3)
S1 U1 S1 4 6_656 76.29(3)
S2 U1 S1 6_556 7_565 78.58(3)
S2 U1 S1 1_554 7_565 138.939(19)
S1 U1 S1 4 7_565 80.362(19)
S1 U1 S1 6_656 7_565 126.225(15)
S2 U1 S1 6_556 . 78.58(3)
S2 U1 S1 1_554 . 138.939(19)
S1 U1 S1 4 . 126.225(15)
S1 U1 S1 6_656 . 80.362(19)
S1 U1 S1 7_565 . 75.75(3)
S2 U1 S1 6_556 2_554 71.84(2)
S2 U1 S1 1_554 2_554 69.082(18)
S1 U1 S1 4 2_554 139.987(15)
S1 U1 S1 6_656 2_554 70.81(3)
S1 U1 S1 7_565 2_554 138.102(15)
S1 U1 S1 . 2_554 69.890(12)
S2 U1 S1 6_556 8_665 71.84(2)
S2 U1 S1 1_554 8_665 69.082(18)
S1 U1 S1 4 8_665 70.81(3)
S1 U1 S1 6_656 8_665 139.987(15)
S1 U1 S1 7_565 8_665 69.890(12)
S1 U1 S1 . 8_665 138.102(15)
S1 U1 S1 2_554 8_665 124.80(3)
S2 U1 Ni1 6_556 . 42.805(10)
S2 U1 Ni1 1_554 . 101.60(2)
S1 U1 Ni1 4 . 170.255(18)
S1 U1 Ni1 6_656 . 101.436(18)
S1 U1 Ni1 7_565 . 93.784(19)
S1 U1 Ni1 . . 44.224(18)
S1 U1 Ni1 2_554 . 44.546(18)
S1 U1 Ni1 8_665 . 114.642(18)
S2 U1 Ni1 6_556 3 42.805(10)
S2 U1 Ni1 1_554 3 101.60(2)
S1 U1 Ni1 4 3 101.436(18)
S1 U1 Ni1 6_656 3 170.255(18)
S1 U1 Ni1 7_565 3 44.224(18)
S1 U1 Ni1 . 3 93.784(19)
S1 U1 Ni1 2_554 3 114.642(18)
S1 U1 Ni1 8_665 3 44.546(18)
Ni1 U1 Ni1 . 3 79.190(5)
S2 Ni1 S2 6_556 2_554 180.0
S2 Ni1 S1 6_556 5 86.82(3)
S2 Ni1 S1 2_554 5 93.18(3)
S2 Ni1 S1 6_556 . 93.18(3)
S2 Ni1 S1 2_554 . 86.82(3)
S1 Ni1 S1 5 . 180.00(4)
S2 Ni1 S1 6_556 6_556 92.11(4)
S2 Ni1 S1 2_554 6_556 87.89(4)
S1 Ni1 S1 5 6_556 85.654(14)
S1 Ni1 S1 . 6_556 94.346(14)
S2 Ni1 S1 6_556 2_554 87.89(4)
S2 Ni1 S1 2_554 2_554 92.11(4)
S1 Ni1 S1 5 2_554 94.346(14)
S1 Ni1 S1 . 2_554 85.654(14)
S1 Ni1 S1 6_556 2_554 180.0
S2 Ni1 U1 6_556 5 129.21(3)
S2 Ni1 U1 2_554 5 50.79(3)
S1 Ni1 U1 5 5 53.55(2)
S1 Ni1 U1 . 5 126.45(2)
S1 Ni1 U1 6_556 5 58.556(19)
S1 Ni1 U1 2_554 5 121.444(19)
S2 Ni1 U1 6_556 . 50.79(3)
S2 Ni1 U1 2_554 . 129.21(3)
S1 Ni1 U1 5 . 126.45(2)
S1 Ni1 U1 . . 53.55(2)
S1 Ni1 U1 6_556 . 121.444(19)
S1 Ni1 U1 2_554 . 58.556(19)
U1 Ni1 U1 5 . 180.0
Ni1 S1 Ni1 . 2 139.81(4)
Ni1 S1 U1 . 6_556 87.36(3)
Ni1 S1 U1 2 6_556 132.47(3)
Ni1 S1 U1 . . 82.22(2)
Ni1 S1 U1 2 . 85.92(3)
U1 S1 U1 6_556 . 98.49(2)
Ni1 S1 U1 . 2 96.93(3)
Ni1 S1 U1 2 2 76.90(2)
U1 S1 U1 6_556 2 109.19(3)
U1 S1 U1 . 2 152.25(3)
Ni1 S2 Ni1 2 4 138.82(6)
Ni1 S2 U1 2 6_656 86.41(3)
Ni1 S2 U1 4 6_656 86.41(3)
Ni1 S2 U1 2 1_556 106.53(3)
Ni1 S2 U1 4 1_556 106.53(3)
U1 S2 U1 6_656 1_556 136.28(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
U1 S2 6_556 2.6666(13)
U1 S2 1_554 2.7446(12)
U1 S1 4 2.7721(9)
U1 S1 6_656 2.7721(9)
U1 S1 7_565 2.7888(8)
U1 S1 . 2.7888(8)
U1 S1 2_554 3.0088(8)
U1 S1 8_665 3.0088(8)
U1 Ni1 . 3.43488(18)
U1 Ni1 3 3.43488(18)
Ni1 S2 6_556 2.3386(4)
Ni1 S2 2_554 2.3386(4)
Ni1 S1 5 2.4180(8)
Ni1 S1 . 2.4180(8)
Ni1 S1 6_556 2.4739(9)
Ni1 S1 2_554 2.4739(9)
Ni1 U1 5 3.43487(18)
S1 Ni1 2 2.4739(9)
S1 U1 6_556 2.7722(9)
S1 U1 2 3.0088(8)
S2 Ni1 2 2.3386(4)
S2 Ni1 4 2.3386(4)
S2 U1 6_656 2.6666(13)
S2 U1 1_556 2.7446(12)
