#------------------------------------------------------------------------------
#$Date: 2021-02-18 12:04:43 +0200 (Thu, 18 Feb 2021) $
#$Revision: 262062 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560467.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_1560467
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     'La3 Ni0.50 Ge S7'
_chemical_formula_sum            'Ge La3 Ni0.5 S7'
_chemical_formula_weight         743.09
_chemical_name_common
'lanthanum nickel germanium sulfide (3/0.5/1/7)'
_chemical_name_systematic
'lanthanum 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                   10.2983(4)
_cell_length_b                   10.2983(4)
_cell_length_c                   5.8078(2)
_cell_measurement_reflns_used    5800
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.62
_cell_measurement_theta_min      4.19
_cell_volume                     533.42(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 1.000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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            7786
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.008
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    16.718
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXL-2014/7 (Sheldrick, 2014)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.626
_exptl_crystal_description       irregular
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.281
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.0017(3)
_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   1.175
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1341
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0214
_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)+(0.0088P)²+1.8044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1282
_reflns_number_total             1341
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc17.cif
_cod_data_source_block           6
_cod_original_cell_volume        533.42(5)
_cod_original_formula_sum        'Ge La3 Ni0.50 S7'
_cod_database_code               1560467
_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   0.489
_shelx_estimated_absorpt_t_max   0.540
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
La La 0.12671(3) 0.35582(3) 0.01251(11) 0.00969(8) Uani 1 1 d . . . . .
NiA Ni 0.0000 0.0000 0.2489(9) 0.0116(5) Uani 0.478(3) 3 d S T P . .
NiB Ni 0.0000 0.0000 0.020(18) 0.0116(5) Uani 0.022(3) 3 d S T P . .
Ge Ge 0.3333 0.6667 0.59400(19) 0.0103(2) Uani 1 3 d S T P . .
S1 S 0.24042(15) 0.15496(15) 0.0000(4) 0.0149(3) Uani 1 1 d . . . . .
S2 S 0.52159(17) 0.10625(17) 0.2408(3) 0.0116(3) Uani 1 1 d . . . . .
S3 S 0.3333 0.6667 0.2202(5) 0.0121(5) 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'
La La -0.2871 2.4523 '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 La S1 82.91(5) . 2
S1 La S2 142.48(6) . 5_564
S1 La S2 108.98(5) 2 5_564
S1 La S1 76.43(5) . 6
S1 La S1 76.39(5) 2 6
S2 La S1 140.31(4) 5_564 6
S1 La S2 75.61(5) . 6_554
S1 La S2 140.50(6) 2 6_554
S2 La S2 73.20(6) 5_564 6_554
S1 La S2 128.05(4) 6 6_554
S1 La S2 143.77(5) . 2
S1 La S2 71.89(4) 2 2
S2 La S2 72.14(3) 5_564 2
S1 La S2 72.67(4) 6 2
S2 La S2 139.47(4) 6_554 2
S1 La S3 116.49(3) . .
S1 La S3 150.07(5) 2 .
S2 La S3 70.36(5) 5_564 .
S1 La S3 85.97(6) 6 .
S2 La S3 69.11(5) 6_554 .
S2 La S3 79.91(4) 2 .
S1 La S1 74.25(5) . 6_554
S1 La S1 74.21(5) 2 6_554
S2 La S1 75.20(4) 5_564 6_554
S1 La S1 140.46(5) 6 6_554
S2 La S1 68.28(4) 6_554 6_554
S2 La S1 120.87(4) 2 6_554
S3 La S1 131.03(6) . 6_554
S1 La NiB 41.53(10) . .
S1 La NiB 41.52(11) 2 .
S2 La NiB 140.5(16) 5_564 .
S1 La NiB 69.0(19) 6 .
S2 La NiB 111.9(10) 6_554 .
S2 La NiB 108.1(9) 2 .
S3 La NiB 149.1(15) . .
S1 La NiB 71.4(19) 6_554 .
S1 La NiA 47.25(5) . .
S1 La NiA 47.24(5) 2 .
S2 La NiA 156.19(5) 5_564 .
S1 La NiA 46.66(8) 6 .
S2 La NiA 122.83(4) 6_554 .
S2 La NiA 96.93(5) 2 .
S3 La NiA 129.75(9) . .
S1 La NiA 93.80(8) 6_554 .
NiB La NiA 22.4(19) . .
S1 La NiA 46.59(5) . 4_554
S1 La NiA 46.58(5) 2 4_554
S2 La NiA 117.34(8) 5_564 4_554
S1 La NiA 95.23(8) 6 4_554
S2 La NiA 96.17(6) 6_554 4_554
S2 La NiA 118.14(4) 2 4_554
S3 La NiA 161.462(14) . 4_554
S1 La NiA 45.24(8) 6_554 4_554
NiB La NiA 26.2(19) . 4_554
NiA La NiA 48.563(5) . 4_554
NiB NiA NiB 180.000(14) . 4
NiB NiA S1 56.38(10) . 3
NiB NiA S1 123.62(10) 4 3
NiB NiA S1 56.38(10) . 2
NiB NiA S1 123.62(10) 4 2
S1 NiA S1 92.30(14) 3 2
NiB NiA S1 56.38(10) . .
NiB NiA S1 123.62(10) 4 .
S1 NiA S1 92.30(14) 3 .
S1 NiA S1 92.30(14) 2 .
NiB NiA S1 123.86(10) . 6
NiB NiA S1 56.14(10) 4 6
S1 NiA S1 179.8(2) 3 6
S1 NiA S1 87.86(2) 2 6
S1 NiA S1 87.86(2) . 6
NiB NiA S1 123.86(10) . 5
NiB NiA S1 56.14(10) 4 5
S1 NiA S1 87.86(2) 3 5
S1 NiA S1 179.8(2) 2 5
S1 NiA S1 87.86(2) . 5
S1 NiA S1 91.97(14) 6 5
NiB NiA S1 123.86(10) . 4
NiB NiA S1 56.14(10) 4 4
S1 NiA S1 87.86(2) 3 4
S1 NiA S1 87.86(2) 2 4
S1 NiA S1 179.8(2) . 4
S1 NiA S1 91.97(14) 6 4
S1 NiA S1 91.97(14) 5 4
NiB NiA NiA 0.000(1) . 4_554
NiB NiA NiA 180.000(14) 4 4_554
S1 NiA NiA 56.38(10) 3 4_554
S1 NiA NiA 56.38(10) 2 4_554
S1 NiA NiA 56.38(10) . 4_554
S1 NiA NiA 123.86(10) 6 4_554
S1 NiA NiA 123.86(10) 5 4_554
S1 NiA NiA 123.86(10) 4 4_554
NiB NiA NiA 180.0 . 4
NiB NiA NiA 0.000(14) 4 4
S1 NiA NiA 123.62(10) 3 4
S1 NiA NiA 123.62(10) 2 4
S1 NiA NiA 123.62(10) . 4
S1 NiA NiA 56.14(10) 6 4
S1 NiA NiA 56.14(10) 5 4
S1 NiA NiA 56.14(10) 4 4
NiA NiA NiA 180.0 4_554 4
NiB NiA La 66.89(8) . .
NiB NiA La 113.11(8) 4 .
S1 NiA La 123.26(18) 3 .
S1 NiA La 53.14(5) 2 .
S1 NiA La 53.07(5) . .
S1 NiA La 56.97(5) 6 .
S1 NiA La 126.88(4) 5 .
S1 NiA La 126.95(4) 4 .
NiA NiA La 66.89(8) 4_554 .
NiA NiA La 113.11(8) 4 .
NiB NiA La 66.89(8) . 2
NiB NiA La 113.11(8) 4 2
S1 NiA La 53.14(5) 3 2
S1 NiA La 53.07(5) 2 2
S1 NiA La 123.27(18) . 2
S1 NiA La 126.88(4) 6 2
S1 NiA La 126.95(4) 5 2
S1 NiA La 56.97(5) 4 2
NiA NiA La 66.89(8) 4_554 2
NiA NiA La 113.11(8) 4 2
La NiA La 105.60(9) . 2
NiA NiB NiA 180.0 . 4_554
NiA NiB S1 93(3) . 3
NiA NiB S1 87(3) 4_554 3
NiA NiB S1 93(3) . 2
NiA NiB S1 87(3) 4_554 2
S1 NiB S1 119.7(5) 3 2
NiA NiB S1 93(3) . .
NiA NiB S1 87(3) 4_554 .
S1 NiB S1 119.7(5) 3 .
S1 NiB S1 119.7(5) 2 .
NiA NiB NiB 0.0 . 4
NiA NiB NiB 180.0 4_554 4
S1 NiB NiB 93(3) 3 4
S1 NiB NiB 93(3) 2 4
S1 NiB NiB 93(3) . 4
NiA NiB NiB 180.0 . 4_554
NiA NiB NiB 0.0 4_554 4_554
S1 NiB NiB 87(3) 3 4_554
S1 NiB NiB 87(3) 2 4_554
S1 NiB NiB 87(3) . 4_554
NiB NiB NiB 180.0 4 4_554
NiA NiB La 90.7(19) . .
NiA NiB La 89.3(19) 4_554 .
S1 NiB La 176(5) 3 .
S1 NiB La 60.05(7) 2 .
S1 NiB La 59.96(7) . .
NiB NiB La 90.7(19) 4 .
NiB NiB La 89.3(19) 4_554 .
NiA NiB La 90.7(19) . 2
NiA NiB La 89.3(19) 4_554 2
S1 NiB La 60.05(7) 3 2
S1 NiB La 59.96(7) 2 2
S1 NiB La 176(5) . 2
NiB NiB La 90.7(19) 4 2
NiB NiB La 89.3(19) 4_554 2
La NiB La 119.98(9) . 2
NiA NiB La 90.7(19) . 3
NiA NiB La 89.3(19) 4_554 3
S1 NiB La 59.96(7) 3 3
S1 NiB La 176(5) 2 3
S1 NiB La 60.05(7) . 3
NiB NiB La 90.7(19) 4 3
NiB NiB La 89.3(19) 4_554 3
La NiB La 119.98(9) . 3
La NiB La 119.98(9) 2 3
S3 Ge S2 112.58(5) . 6
S3 Ge S2 112.57(5) . 4_665
S2 Ge S2 106.20(5) 6 4_665
S3 Ge S2 112.57(5) . 5_565
S2 Ge S2 106.20(5) 6 5_565
S2 Ge S2 106.20(5) 4_665 5_565
NiB S1 NiA 31(3) . .
NiB S1 NiA 37(3) . 4_554
NiA S1 NiA 67.48(3) . 4_554
NiB S1 La 78.50(6) . .
NiA S1 La 79.68(4) . .
NiA S1 La 81.35(4) 4_554 .
NiB S1 La 78.43(6) . 3
NiA S1 La 79.62(4) . 3
NiA S1 La 81.29(4) 4_554 3
La S1 La 156.87(6) . 3
NiB S1 La 113(3) . 5_554
NiA S1 La 143.85(12) . 5_554
NiA S1 La 76.37(11) 4_554 5_554
La S1 La 95.35(6) . 5_554
La S1 La 95.29(6) 3 5_554
NiB S1 La 106(3) . 5
NiA S1 La 75.69(11) . 5
NiA S1 La 143.17(12) 4_554 5
La S1 La 92.42(6) . 5
La S1 La 92.36(6) 3 5
La S1 La 140.46(5) 5_554 5
Ge S2 La 91.55(5) 4_664 6_655
Ge S2 La 89.03(5) 4_664 5
La S2 La 110.26(5) 6_655 5
Ge S2 La 122.64(6) 4_664 3
La S2 La 140.67(5) 6_655 3
La S2 La 90.79(4) 5 3
Ge S3 La 113.14(5) . 3_565
Ge S3 La 113.14(5) . 2_665
La S3 La 105.56(5) 3_565 2_665
Ge S3 La 113.14(5) . .
La S3 La 105.56(5) 3_565 .
La S3 La 105.56(5) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La S1 2.8420(13) .
La S1 2.8452(13) 2
La S2 2.9300(15) 5_564
La S1 3.017(3) 6
La S2 3.0273(16) 6_554
La S2 3.0594(15) 2
La S3 3.0690(11) .
La S1 3.154(3) 6_554
La NiB 3.2172(15) .
La NiA 3.498(2) .
La NiA 3.563(2) 4_554
NiA NiB 1.33(11) .
NiA NiB 1.57(11) 4
NiA S1 2.611(3) 3
NiA S1 2.611(3) 2
NiA S1 2.611(3) .
NiA S1 2.618(3) 6
NiA S1 2.618(3) 5
NiA S1 2.618(3) 4
NiA NiA 2.90389(10) 4_554
NiA NiA 2.90391(10) 4
NiA La 3.498(2) 2
NiB NiA 1.57(11) 4_554
NiB S1 2.177(6) 3
NiB S1 2.177(6) 2
NiB S1 2.177(6) .
NiB NiB 2.90388(10) 4
NiB NiB 2.90392(10) 4_554
NiB La 3.2172(14) 2
NiB La 3.2172(14) 3
Ge S3 2.171(3) .
Ge S2 2.2213(16) 6
Ge S2 2.2214(16) 4_665
Ge S2 2.2214(16) 5_565
S1 NiA 2.618(3) 4_554
S1 La 2.8452(13) 3
S1 La 3.017(3) 5_554
S1 La 3.154(3) 5
S2 Ge 2.2213(16) 4_664
S2 La 2.9299(15) 6_655
S2 La 3.0273(16) 5
S2 La 3.0595(15) 3
S3 La 3.0690(11) 3_565
S3 La 3.0690(11) 2_665
