#------------------------------------------------------------------------------
#$Date: 2021-02-18 12:14:41 +0200 (Thu, 18 Feb 2021) $
#$Revision: 262065 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560470.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_1560470
loop_
_publ_author_name
'Iyer, Abishek K.'
'Yin, Wenlong'
'Lee, Emma J.'
'Lin, Xinsong'
'Mar, Arthur'
_publ_section_title
;
 Quaternary rare-earth sulfides RE 3 M 0.5 GeS 7 (RE=La--Nd, Sm; M=Co, Ni)
 and Y 3 Pd 0.5 SiS 7
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              14
_journal_page_last               23
_journal_paper_doi               10.1016/j.jssc.2017.03.009
_journal_volume                  250
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_structural     'Nd3 Ni0.50 Ge S7'
_chemical_formula_sum            'Ge Nd3 Ni0.5 S7'
_chemical_formula_weight         759.09
_chemical_name_common
'neodymium nickel germanium sulfide (3/0.5/1/7)'
_chemical_name_systematic
'neodymium nickel germanium sulfide (3/0.5/1/7)'
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.0760(3)
_cell_length_b                   10.0760(3)
_cell_length_c                   5.7605(2)
_cell_measurement_reflns_used    7588
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.33
_cell_volume                     506.49(3)
_computing_cell_refinement       'Bruker SAINT 8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT 8.34A'
_computing_molecular_graphics    'ATOMS 5.1 (Dowty, 1999)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PLATFORM/SMART APEX II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7287
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.137
_diffrn_reflns_theta_min         2.334
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.332
_exptl_absorpt_correction_T_max  0.461
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXL-2014/7 (Sheldrick, 2014)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.977
_exptl_crystal_description       irregular
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.009(17)
_refine_ls_extinction_coef       0.0122(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1286
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0129
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0116P)²+0.3902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0298
_refine_ls_wR_factor_ref         0.0299
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1270
_reflns_number_total             1286
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc20.cif
_cod_data_source_block           9
_cod_original_formula_sum        'Ge Nd3 Ni0.50 S7'
_cod_database_code               1560470
_shelx_shelxl_version_number     2014/7
_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   0.311
_shelx_estimated_absorpt_t_max   0.370
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd Nd 0.12870(2) 0.35583(2) 0.01764(8) 0.00860(6) Uani 1 1 d . . . . .
NiA Ni 0.0000 0.0000 0.2490(5) 0.0094(4) Uani 0.474(2) 3 d S T P . .
NiB Ni 0.0000 0.0000 -0.002(8) 0.0094(4) Uani 0.026(2) 3 d S T P . .
Ge Ge 0.3333 0.6667 0.59932(13) 0.00835(14) Uani 1 3 d S T P . .
S1 S 0.24320(10) 0.15487(10) 0.0000(3) 0.01269(18) Uani 1 1 d . . . . .
S2 S 0.51982(11) 0.10186(11) 0.25117(18) 0.00949(17) Uani 1 1 d . . . . .
S3 S 0.3333 0.6667 0.2227(3) 0.0096(3) Uani 1 3 d S T P . .
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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
S1 Nd S1 83.83(4) 2 .
S1 Nd S2 106.91(3) 2 5_564
S1 Nd S2 142.60(4) . 5_564
S1 Nd S1 77.56(3) 2 6
S1 Nd S1 77.45(3) . 6
S2 Nd S1 139.38(3) 5_564 6
S1 Nd S2 140.30(4) 2 6_554
S1 Nd S2 74.76(3) . 6_554
S2 Nd S2 74.75(4) 5_564 6_554
S1 Nd S2 127.63(3) 6 6_554
S1 Nd S3 149.64(3) 2 .
S1 Nd S3 117.03(2) . .
S2 Nd S3 70.73(3) 5_564 .
S1 Nd S3 85.49(4) 6 .
S2 Nd S3 69.54(3) 6_554 .
S1 Nd S2 72.07(3) 2 2
S1 Nd S2 144.11(4) . 2
S2 Nd S2 71.628(17) 5_564 2
S1 Nd S2 71.75(3) 6 2
S2 Nd S2 139.71(3) 6_554 2
S3 Nd S2 78.80(2) . 2
S1 Nd S1 74.38(3) 2 6_554
S1 Nd S1 74.29(3) . 6_554
S2 Nd S1 74.51(3) 5_564 6_554
S1 Nd S1 141.81(3) 6 6_554
S2 Nd S1 67.87(3) 6_554 6_554
S3 Nd S1 130.37(4) . 6_554
S2 Nd S1 121.68(3) 2 6_554
S1 Nd NiB 41.94(2) 2 .
S1 Nd NiB 41.91(2) . .
S2 Nd NiB 137.5(7) 5_564 .
S1 Nd NiB 72.3(9) 6 .
S2 Nd NiB 110.3(5) 6_554 .
S3 Nd NiB 151.7(7) . .
S2 Nd NiB 109.4(4) 2 .
S1 Nd NiB 69.5(9) 6_554 .
S1 Nd NiA 47.94(3) 2 .
S1 Nd NiA 47.91(3) . .
S2 Nd NiA 154.84(3) 5_564 .
S1 Nd NiA 47.32(5) 6 .
S2 Nd NiA 122.64(3) 6_554 .
S3 Nd NiA 130.13(5) . .
S2 Nd NiA 96.70(3) 2 .
S1 Nd NiA 94.50(5) 6_554 .
NiB Nd NiA 25.0(9) . .
S1 Nd NiA 46.94(3) 2 4_554
S1 Nd NiA 46.91(3) . 4_554
S2 Nd NiA 116.27(5) 5_564 4_554
S1 Nd NiA 96.49(5) 6 4_554
S2 Nd NiA 95.71(3) 6_554 4_554
S3 Nd NiA 162.104(11) . 4_554
S2 Nd NiA 118.76(2) 2 4_554
S1 Nd NiA 45.32(5) 6_554 4_554
NiB Nd NiA 24.2(9) . 4_554
NiA Nd NiA 49.174(4) . 4_554
NiB NiA NiB 180.000(12) 4 .
NiB NiA S1 123.72(6) 4 3
NiB NiA S1 56.28(6) . 3
NiB NiA S1 123.72(6) 4 2
NiB NiA S1 56.28(6) . 2
S1 NiA S1 92.16(9) 3 2
NiB NiA S1 123.72(6) 4 .
NiB NiA S1 56.28(6) . .
S1 NiA S1 92.16(9) 3 .
S1 NiA S1 92.16(9) 2 .
NiB NiA S1 56.06(6) 4 6
NiB NiA S1 123.94(6) . 6
S1 NiA S1 179.78(12) 3 6
S1 NiA S1 87.994(15) 2 6
S1 NiA S1 87.994(15) . 6
NiB NiA S1 56.06(6) 4 5
NiB NiA S1 123.94(6) . 5
S1 NiA S1 87.994(15) 3 5
S1 NiA S1 179.78(12) 2 5
S1 NiA S1 87.995(15) . 5
S1 NiA S1 91.85(9) 6 5
NiB NiA S1 56.06(6) 4 4
NiB NiA S1 123.94(6) . 4
S1 NiA S1 87.994(15) 3 4
S1 NiA S1 87.994(15) 2 4
S1 NiA S1 179.78(12) . 4
S1 NiA S1 91.85(9) 6 4
S1 NiA S1 91.85(9) 5 4
NiB NiA NiA 180.0 4 4_554
NiB NiA NiA 0.0 . 4_554
S1 NiA NiA 56.28(6) 3 4_554
S1 NiA NiA 56.28(6) 2 4_554
S1 NiA NiA 56.28(6) . 4_554
S1 NiA NiA 123.94(6) 6 4_554
S1 NiA NiA 123.94(6) 5 4_554
S1 NiA NiA 123.94(6) 4 4_554
NiB NiA NiA 0.000(7) 4 4
NiB NiA NiA 180.0 . 4
S1 NiA NiA 123.72(6) 3 4
S1 NiA NiA 123.72(6) 2 4
S1 NiA NiA 123.72(6) . 4
S1 NiA NiA 56.06(6) 6 4
S1 NiA NiA 56.06(6) 5 4
S1 NiA NiA 56.06(6) 4 4
NiA NiA NiA 180.0 4_554 4
NiB NiA Nd 112.97(5) 4 .
NiB NiA Nd 67.03(5) . .
S1 NiA Nd 123.31(11) 3 .
S1 NiA Nd 53.08(3) 2 .
S1 NiA Nd 53.25(3) . .
S1 NiA Nd 56.91(3) 6 .
S1 NiA Nd 126.94(2) 5 .
S1 NiA Nd 126.77(3) 4 .
NiA NiA Nd 67.03(5) 4_554 .
NiA NiA Nd 112.97(5) 4 .
NiB NiA Nd 112.97(5) 4 2
NiB NiA Nd 67.03(5) . 2
S1 NiA Nd 53.08(3) 3 2
S1 NiA Nd 53.25(3) 2 2
S1 NiA Nd 123.31(11) . 2
S1 NiA Nd 126.94(2) 6 2
S1 NiA Nd 126.77(3) 5 2
S1 NiA Nd 56.91(3) 4 2
NiA NiA Nd 67.03(5) 4_554 2
NiA NiA Nd 112.97(5) 4 2
Nd NiA Nd 105.76(5) . 2
NiA NiB NiA 180.0 4_554 .
NiA NiB S1 90.3(13) 4_554 3
NiA NiB S1 89.7(13) . 3
NiA NiB S1 90.3(13) 4_554 2
NiA NiB S1 89.7(13) . 2
S1 NiB S1 120.00(2) 3 2
NiA NiB S1 90.3(13) 4_554 .
NiA NiB S1 89.7(13) . .
S1 NiB S1 120.00(2) 3 .
S1 NiB S1 120.00(2) 2 .
NiA NiB NiB 0.0 4_554 4_554
NiA NiB NiB 180.0 . 4_554
S1 NiB NiB 90.3(13) 3 4_554
S1 NiB NiB 90.3(13) 2 4_554
S1 NiB NiB 90.3(13) . 4_554
NiA NiB NiB 180.0 4_554 4
NiA NiB NiB 0.0 . 4
S1 NiB NiB 89.7(13) 3 4
S1 NiB NiB 89.7(13) 2 4
S1 NiB NiB 89.7(13) . 4
NiB NiB NiB 180.0 4_554 4
NiA NiB Nd 92.0(9) 4_554 .
NiA NiB Nd 88.0(9) . .
S1 NiB Nd 178(2) 3 .
S1 NiB Nd 59.91(4) 2 .
S1 NiB Nd 60.11(4) . .
NiB NiB Nd 92.0(9) 4_554 .
NiB NiB Nd 88.0(9) 4 .
NiA NiB Nd 92.0(9) 4_554 2
NiA NiB Nd 88.0(9) . 2
S1 NiB Nd 59.91(4) 3 2
S1 NiB Nd 60.11(4) 2 2
S1 NiB Nd 178(2) . 2
NiB NiB Nd 92.0(9) 4_554 2
NiB NiB Nd 88.0(9) 4 2
Nd NiB Nd 119.88(11) . 2
NiA NiB Nd 92.0(9) 4_554 3
NiA NiB Nd 88.0(9) . 3
S1 NiB Nd 60.11(4) 3 3
S1 NiB Nd 178(2) 2 3
S1 NiB Nd 59.91(4) . 3
NiB NiB Nd 92.0(9) 4_554 3
NiB NiB Nd 88.0(9) 4 3
Nd NiB Nd 119.88(11) . 3
Nd NiB Nd 119.88(11) 2 3
S3 Ge S2 113.17(3) . 4_665
S3 Ge S2 113.17(3) . 5_565
S2 Ge S2 105.53(4) 4_665 5_565
S3 Ge S2 113.17(3) . 6
S2 Ge S2 105.53(4) 4_665 6
S2 Ge S2 105.53(4) 5_565 6
NiB S1 NiA 34.0(13) . .
NiB S1 NiA 33.7(13) . 4_554
NiA S1 NiA 67.67(2) . 4_554
NiB S1 Nd 78.15(6) . 3
NiA S1 Nd 78.98(3) . 3
NiA S1 Nd 81.37(3) 4_554 3
NiB S1 Nd 77.99(6) . .
NiA S1 Nd 78.84(3) . .
NiA S1 Nd 81.23(3) 4_554 .
Nd S1 Nd 155.74(4) 3 .
NiB S1 Nd 109.5(13) . 5_554
NiA S1 Nd 143.44(7) . 5_554
NiA S1 Nd 75.77(7) 4_554 5_554
Nd S1 Nd 96.06(4) 3 5_554
Nd S1 Nd 95.90(4) . 5_554
NiB S1 Nd 108.7(13) . 5
NiA S1 Nd 74.75(7) . 5
NiA S1 Nd 142.41(7) 4_554 5
Nd S1 Nd 91.84(4) 3 5
Nd S1 Nd 91.71(4) . 5
Nd S1 Nd 141.81(3) 5_554 5
Ge S2 Nd 91.01(3) 4_664 6_655
Ge S2 Nd 88.70(3) 4_664 5
Nd S2 Nd 109.96(4) 6_655 5
Ge S2 Nd 121.02(4) 4_664 3
Nd S2 Nd 142.50(4) 6_655 3
Nd S2 Nd 91.17(3) 5 3
Ge S3 Nd 113.19(3) . 3_565
Ge S3 Nd 113.19(3) . 2_665
Nd S3 Nd 105.51(4) 3_565 2_665
Ge S3 Nd 113.19(3) . .
Nd S3 Nd 105.51(4) 3_565 .
Nd S3 Nd 105.51(4) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nd S1 2.7817(9) 2
Nd S1 2.7889(9) .
Nd S2 2.8707(10) 5_564
Nd S1 2.9517(15) 6
Nd S2 2.9607(11) 6_554
Nd S3 2.9997(7) .
Nd S2 3.0087(10) 2
Nd S1 3.1438(15) 6_554
Nd NiB 3.1463(17) .
Nd NiA 3.4150(12) .
Nd NiA 3.5047(14) 4_554
NiA NiB 1.44(5) 4
NiA NiB 1.44(5) .
NiA S1 2.583(2) 3
NiA S1 2.583(2) 2
NiA S1 2.583(2) .
NiA S1 2.590(2) 6
NiA S1 2.590(2) 5
NiA S1 2.590(2) 4
NiA NiA 2.88023(10) 4_554
NiA NiA 2.88027(10) 4
NiA Nd 3.4151(12) 2
NiB NiA 1.44(5) 4_554
NiB S1 2.1485(9) 3
NiB S1 2.1485(9) 2
NiB S1 2.1485(9) .
NiB NiB 2.88024(10) 4_554
NiB NiB 2.88026(10) 4
NiB Nd 3.1464(17) 2
NiB Nd 3.1464(17) 3
Ge S3 2.1695(18) .
Ge S2 2.2234(10) 4_665
Ge S2 2.2234(10) 5_565
Ge S2 2.2234(10) 6
S1 NiA 2.590(2) 4_554
S1 Nd 2.7817(9) 3
S1 Nd 2.9517(15) 5_554
S1 Nd 3.1438(15) 5
S2 Ge 2.2234(10) 4_664
S2 Nd 2.8707(10) 6_655
S2 Nd 2.9606(11) 5
S2 Nd 3.0087(10) 3
S3 Nd 2.9997(7) 3_565
S3 Nd 2.9997(7) 2_665
