#------------------------------------------------------------------------------
#$Date: 2021-02-18 12:18:04 +0200 (Thu, 18 Feb 2021) $
#$Revision: 262066 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560471.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_1560471
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     'Sm3 Ni0.50 Ge S7'
_chemical_formula_sum            'Ge Ni0.5 S7 Sm3'
_chemical_formula_weight         777.42
_chemical_name_common
'samarium nickel germanium sulfide (3/0.5/1/7)'
_chemical_name_systematic
'samarium 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                   9.9642(8)
_cell_length_b                   9.9642(8)
_cell_length_c                   5.7436(5)
_cell_measurement_reflns_used    2179
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      4.26
_cell_volume                     493.86(7)
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0387
_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       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7111
_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         33.149
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.917
_exptl_absorpt_correction_T_max  0.572
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXL-2014/7 (Sheldrick, 2014)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    5.228
_exptl_crystal_description       irregular
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.037
_refine_diff_density_max         4.305
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.336
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         1263
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0223P)²+0.3401P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1128
_reflns_number_total             1263
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc21.cif
_cod_data_source_block           10
_cod_original_cell_volume        493.86(9)
_cod_original_formula_sum        'Ge Ni0.50 S7 Sm3'
_cod_database_code               1560471
_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   0.406
_shelx_estimated_absorpt_t_max   0.484
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
Sm Sm 0.12991(4) 0.35587(4) 0.02096(18) 0.01061(11) Uani 1 1 d . . . . .
NiA Ni 0.0000 0.0000 0.2483(12) 0.0109(10) Uani 0.475(5) 3 d S T P . .
NiB Ni 0.0000 0.0000 0.03(2) 0.0109(10) Uani 0.025(5) 3 d S T P . .
Ge Ge 0.3333 0.6667 0.6019(3) 0.0108(3) Uani 1 3 d S T P . .
S1 S 0.2442(2) 0.1544(2) 0.0000(6) 0.0151(4) Uani 1 1 d . . . . .
S2 S 0.5195(3) 0.1000(3) 0.2570(4) 0.0120(4) Uani 1 1 d . . . . .
S3 S 0.3333 0.6667 0.2248(7) 0.0115(7) 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'
Sm Sm -0.1638 3.4418 '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 Sm S1 84.13(9) 2 .
S1 Sm S2 105.84(8) 2 5_564
S1 Sm S2 142.51(9) . 5_564
S1 Sm S1 78.18(8) 2 6
S1 Sm S1 77.97(7) . 6
S2 Sm S1 139.06(7) 5_564 6
S1 Sm S2 140.13(9) 2 6_554
S1 Sm S2 74.49(7) . 6_554
S2 Sm S2 75.36(10) 5_564 6_554
S1 Sm S2 127.51(6) 6 6_554
S1 Sm S3 149.44(8) 2 .
S1 Sm S3 117.48(5) . .
S2 Sm S3 70.98(8) 5_564 .
S1 Sm S3 85.28(9) 6 .
S2 Sm S3 69.77(7) 6_554 .
S1 Sm S2 72.24(7) 2 2
S1 Sm S2 144.30(8) . 2
S2 Sm S2 71.42(4) 5_564 2
S1 Sm S2 71.36(7) 6 2
S2 Sm S2 139.69(6) 6_554 2
S3 Sm S2 78.21(6) . 2
S1 Sm NiB 42.3(2) 2 .
S1 Sm NiB 42.2(2) . .
S2 Sm NiB 139(2) 5_564 .
S1 Sm NiB 70(2) 6 .
S2 Sm NiB 112.0(14) 6_554 .
S3 Sm NiB 150(2) . .
S2 Sm NiB 108.0(12) 2 .
S1 Sm S1 74.34(7) 2 6_554
S1 Sm S1 74.16(7) . 6_554
S2 Sm S1 74.11(7) 5_564 6_554
S1 Sm S1 142.40(8) 6 6_554
S2 Sm S1 67.68(6) 6_554 6_554
S3 Sm S1 130.10(9) . 6_554
S2 Sm S1 122.06(6) 2 6_554
NiB Sm S1 73(2) . 6_554
S1 Sm NiA 48.25(7) 2 .
S1 Sm NiA 48.19(7) . .
S2 Sm NiA 154.08(7) 5_564 .
S1 Sm NiA 47.68(12) 6 .
S2 Sm NiA 122.64(6) 6_554 .
S3 Sm NiA 130.40(13) . .
S2 Sm NiA 96.64(8) 2 .
NiB Sm NiA 22(2) . .
S1 Sm NiA 94.72(12) 6_554 .
S1 Sm NiA 47.06(7) 2 4_554
S1 Sm NiA 47.02(7) . 4_554
S2 Sm NiA 115.50(11) 5_564 4_554
S1 Sm NiA 97.21(11) 6 4_554
S2 Sm NiA 95.47(8) 6_554 4_554
S3 Sm NiA 162.47(3) . 4_554
S2 Sm NiA 119.08(6) 2 4_554
NiB Sm NiA 28(2) . 4_554
S1 Sm NiA 45.19(11) 6_554 4_554
NiA Sm NiA 49.532(10) . 4_554
NiB NiA NiB 180.000(18) . 4
NiB NiA S1 56.22(14) . 3
NiB NiA S1 123.78(15) 4 3
NiB NiA S1 56.22(14) . 2
NiB NiA S1 123.78(14) 4 2
S1 NiA S1 92.1(2) 3 2
NiB NiA S1 56.22(14) . .
NiB NiA S1 123.78(14) 4 .
S1 NiA S1 92.1(2) 3 .
S1 NiA S1 92.1(2) 2 .
NiB NiA S1 124.14(14) . 6
NiB NiA S1 55.86(14) 4 6
S1 NiA S1 179.6(3) 3 6
S1 NiA S1 88.17(4) 2 6
S1 NiA S1 88.17(4) . 6
NiB NiA S1 124.14(14) . 5
NiB NiA S1 55.86(14) 4 5
S1 NiA S1 88.17(4) 3 5
S1 NiA S1 179.6(3) 2 5
S1 NiA S1 88.17(4) . 5
S1 NiA S1 91.6(2) 6 5
NiB NiA S1 124.14(14) . 4
NiB NiA S1 55.86(14) 4 4
S1 NiA S1 88.17(4) 3 4
S1 NiA S1 88.17(4) 2 4
S1 NiA S1 179.6(3) . 4
S1 NiA S1 91.6(2) 6 4
S1 NiA S1 91.6(2) 5 4
NiB NiA NiA 180.0 . 4
NiB NiA NiA 0.000(18) 4 4
S1 NiA NiA 123.78(14) 3 4
S1 NiA NiA 123.78(14) 2 4
S1 NiA NiA 123.78(14) . 4
S1 NiA NiA 55.86(14) 6 4
S1 NiA NiA 55.86(14) 5 4
S1 NiA NiA 55.86(14) 4 4
NiB NiA NiA 0.000(1) . 4_554
NiB NiA NiA 180.000(18) 4 4_554
S1 NiA NiA 56.22(14) 3 4_554
S1 NiA NiA 56.22(14) 2 4_554
S1 NiA NiA 56.22(14) . 4_554
S1 NiA NiA 124.14(14) 6 4_554
S1 NiA NiA 124.14(14) 5 4_554
S1 NiA NiA 124.14(14) 4 4_554
NiA NiA NiA 180.0 4 4_554
NiB NiA Sm 67.21(11) . 2
NiB NiA Sm 112.79(11) 4 2
S1 NiA Sm 53.08(7) 3 2
S1 NiA Sm 53.39(8) 2 2
S1 NiA Sm 123.4(2) . 2
S1 NiA Sm 126.95(6) 6 2
S1 NiA Sm 126.64(6) 5 2
S1 NiA Sm 56.93(7) 4 2
NiA NiA Sm 112.79(11) 4 2
NiA NiA Sm 67.21(11) 4_554 2
NiB NiA Sm 67.21(11) . 3
NiB NiA Sm 112.79(11) 4 3
S1 NiA Sm 53.39(8) 3 3
S1 NiA Sm 123.4(2) 2 3
S1 NiA Sm 53.08(7) . 3
S1 NiA Sm 126.64(6) 6 3
S1 NiA Sm 56.93(7) 5 3
S1 NiA Sm 126.95(6) 4 3
NiA NiA Sm 112.79(11) 4 3
NiA NiA Sm 67.21(11) 4_554 3
Sm NiA Sm 105.96(12) 2 3
NiA NiB NiA 180.0 . 4_554
NiA NiB S1 94(4) . 3
NiA NiB S1 86(4) 4_554 3
NiA NiB S1 94(4) . 2
NiA NiB S1 86(4) 4_554 2
S1 NiB S1 119.4(10) 3 2
NiA NiB S1 94(4) . .
NiA NiB S1 86(4) 4_554 .
S1 NiB S1 119.4(10) 3 .
S1 NiB S1 119.4(10) 2 .
NiA NiB NiB 0.000(1) . 4
NiA NiB NiB 180.0 4_554 4
S1 NiB NiB 94(4) 3 4
S1 NiB NiB 94(4) 2 4
S1 NiB NiB 94(4) . 4
NiA NiB NiB 180.0 . 4_554
NiA NiB NiB 0.0 4_554 4_554
S1 NiB NiB 86(4) 3 4_554
S1 NiB NiB 86(4) 2 4_554
S1 NiB NiB 86(4) . 4_554
NiB NiB NiB 180.000(10) 4 4_554
NiA NiB Sm 91(2) . 2
NiA NiB Sm 89(2) 4_554 2
S1 NiB Sm 59.84(11) 3 2
S1 NiB Sm 60.22(11) 2 2
S1 NiB Sm 175(6) . 2
NiB NiB Sm 91(2) 4 2
NiB NiB Sm 89(2) 4_554 2
NiA NiB Sm 91(2) . 3
NiA NiB Sm 89(2) 4_554 3
S1 NiB Sm 60.22(11) 3 3
S1 NiB Sm 175(6) 2 3
S1 NiB Sm 59.84(11) . 3
NiB NiB Sm 91(2) 4 3
NiB NiB Sm 89(2) 4_554 3
Sm NiB Sm 119.98(12) 2 3
NiA NiB Sm 91(2) . .
NiA NiB Sm 89(2) 4_554 .
S1 NiB Sm 175(6) 3 .
S1 NiB Sm 59.84(11) 2 .
S1 NiB Sm 60.22(11) . .
NiB NiB Sm 91(2) 4 .
NiB NiB Sm 89(2) 4_554 .
Sm NiB Sm 119.98(12) 2 .
Sm NiB Sm 119.98(13) 3 .
S3 Ge S2 113.62(8) . 4_665
S3 Ge S2 113.62(8) . 5_565
S2 Ge S2 105.02(9) 4_665 5_565
S3 Ge S2 113.62(8) . 6
S2 Ge S2 105.02(9) 4_665 6
S2 Ge S2 105.02(9) 5_565 6
NiB S1 NiA 29(4) . .
NiB S1 NiA 39(4) . 4_554
NiA S1 NiA 67.93(5) . 4_554
NiB S1 Sm 77.89(12) . 3
NiA S1 Sm 78.67(6) . 3
NiA S1 Sm 81.56(7) 4_554 3
NiB S1 Sm 77.58(12) . .
NiA S1 Sm 78.42(7) . .
NiA S1 Sm 81.30(7) 4_554 .
Sm S1 Sm 155.26(9) 3 .
NiB S1 Sm 114(4) . 5_554
NiA S1 Sm 143.32(16) . 5_554
NiA S1 Sm 75.39(15) 4_554 5_554
Sm S1 Sm 96.54(9) 3 5_554
Sm S1 Sm 96.24(8) . 5_554
NiB S1 Sm 104(4) . 5
NiA S1 Sm 74.28(15) . 5
NiA S1 Sm 142.21(16) 4_554 5
Sm S1 Sm 91.47(8) 3 5
Sm S1 Sm 91.22(8) . 5
Sm S1 Sm 142.40(8) 5_554 5
Ge S2 Sm 90.96(8) 4_664 6_655
Ge S2 Sm 88.65(8) 4_664 5
Sm S2 Sm 109.75(9) 6_655 5
Ge S2 Sm 120.05(10) 4_664 3
Sm S2 Sm 143.39(9) 6_655 3
Sm S2 Sm 91.26(7) 5 3
Ge S3 Sm 113.26(8) . .
Ge S3 Sm 113.26(8) . 3_565
Sm S3 Sm 105.44(9) . 3_565
Ge S3 Sm 113.26(8) . 2_665
Sm S3 Sm 105.44(9) . 2_665
Sm S3 Sm 105.44(9) 3_565 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm S1 2.749(2) 2
Sm S1 2.762(2) .
Sm S2 2.840(2) 5_564
Sm S1 2.919(3) 6
Sm S2 2.929(2) 6_554
Sm S3 2.9652(18) .
Sm S2 2.990(2) 2
Sm NiB 3.108(2) .
Sm S1 3.147(3) 6_554
Sm NiA 3.371(3) .
Sm NiA 3.480(3) 4_554
NiA NiB 1.26(13) .
NiA NiB 1.61(13) 4
NiA S1 2.565(5) 3
NiA S1 2.565(5) 2
NiA S1 2.565(5) .
NiA S1 2.576(5) 6
NiA S1 2.576(5) 5
NiA S1 2.576(5) 4
NiA NiA 2.8718(3) 4
NiA NiA 2.8718(3) 4_554
NiA Sm 3.371(3) 2
NiA Sm 3.371(3) 3
NiB NiA 1.61(13) 4_554
NiB S1 2.138(11) 3
NiB S1 2.138(11) 2
NiB S1 2.138(11) .
NiB NiB 2.8718(3) 4
NiB NiB 2.8718(3) 4_554
NiB Sm 3.108(2) 2
NiB Sm 3.108(2) 3
Ge S3 2.166(4) .
Ge S2 2.222(3) 4_665
Ge S2 2.222(3) 5_565
Ge S2 2.222(2) 6
S1 NiA 2.576(5) 4_554
S1 Sm 2.749(2) 3
S1 Sm 2.919(3) 5_554
S1 Sm 3.147(3) 5
S2 Ge 2.222(2) 4_664
S2 Sm 2.840(2) 6_655
S2 Sm 2.929(2) 5
S2 Sm 2.990(2) 3
S3 Sm 2.9653(18) 3_565
S3 Sm 2.9653(18) 2_665
