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#$Date: 2021-02-18 12:09:13 +0200 (Thu, 18 Feb 2021) $
#$Revision: 262064 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560469.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_1560469
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     'Pr3 Ni0.50 Ge S7'
_chemical_formula_sum            'Ge Ni0.5 Pr3 S7'
_chemical_formula_weight         749.09
_chemical_name_common
'praseodymium nickel germanium sulfide (3/0.5/1/7)'
_chemical_name_systematic
'praseodymium 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                   10.1303(4)
_cell_length_b                   10.1303(4)
_cell_length_c                   5.7752(2)
_cell_measurement_reflns_used    4898
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.78
_cell_measurement_theta_min      4.22
_cell_volume                     513.27(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0234
_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            7378
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.093
_diffrn_reflns_theta_min         2.321
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    19.128
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXL-2014/7 (Sheldrick, 2014)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.847
_exptl_crystal_description       irregular
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.059
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.013
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.0035(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   1.088
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1303
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0195
_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)+(0.0146P)²+1.0705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0400
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1255
_reflns_number_total             1303
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc19.cif
_cod_data_source_block           8
_cod_original_cell_volume        513.27(4)
_cod_original_formula_sum        'Ge Ni0.50 Pr3 S7'
_cod_database_code               1560469
_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   0.398
_shelx_estimated_absorpt_t_max   0.500
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
Pr Pr 0.12804(3) 0.35566(3) 0.01598(11) 0.00962(8) Uani 1 1 d . . . . .
NiA Ni 0.0000 0.0000 0.2492(9) 0.0126(6) Uani 0.478(3) 3 d S T P . .
NiB Ni 0.0000 0.0000 -0.007(14) 0.0126(6) Uani 0.022(3) 3 d S T P . .
Ge Ge 0.3333 0.6667 0.59784(18) 0.0097(2) Uani 1 3 d S T P . .
S1 S 0.24272(15) 0.15521(14) 0.0000(4) 0.0143(3) Uani 1 1 d . . . . .
S2 S 0.52039(16) 0.10305(16) 0.2483(3) 0.0106(2) Uani 1 1 d . . . . .
S3 S 0.3333 0.6667 0.2217(4) 0.0114(4) 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'
Pr Pr -0.2180 2.8214 '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 Pr S1 83.73(5) 2 .
S1 Pr S2 107.46(5) 2 5_564
S1 Pr S2 142.55(6) . 5_564
S1 Pr S1 77.28(5) 2 6
S1 Pr S1 77.25(5) . 6
S2 Pr S1 139.55(4) 5_564 6
S1 Pr S2 140.44(5) 2 6_554
S1 Pr S2 74.96(4) . 6_554
S2 Pr S2 74.29(6) 5_564 6_554
S1 Pr S2 127.74(4) 6 6_554
S1 Pr S3 149.70(5) 2 .
S1 Pr S3 116.79(3) . .
S2 Pr S3 70.63(5) 5_564 .
S1 Pr S3 85.52(5) 6 .
S2 Pr S3 69.40(4) 6_554 .
S1 Pr S2 72.00(4) 2 2
S1 Pr S2 144.07(5) . 2
S2 Pr S2 71.78(3) 5_564 2
S1 Pr S2 71.92(4) 6 2
S2 Pr S2 139.59(4) 6_554 2
S3 Pr S2 79.05(3) . 2
S1 Pr S1 74.43(5) 2 6_554
S1 Pr S1 74.39(5) . 6_554
S2 Pr S1 74.61(4) 5_564 6_554
S1 Pr S1 141.63(5) 6 6_554
S2 Pr S1 67.97(4) 6_554 6_554
S3 Pr S1 130.49(5) . 6_554
S2 Pr S1 121.48(4) 2 6_554
S1 Pr NiB 41.87(3) 2 .
S1 Pr NiB 41.86(3) . .
S2 Pr NiB 137.4(12) 5_564 .
S1 Pr NiB 72.6(15) 6 .
S2 Pr NiB 110.2(8) 6_554 .
S3 Pr NiB 151.8(11) . .
S2 Pr NiB 109.6(7) 2 .
S1 Pr NiB 69.0(15) 6_554 .
S1 Pr NiA 47.82(5) 2 .
S1 Pr NiA 47.81(5) . .
S2 Pr NiA 155.27(5) 5_564 .
S1 Pr NiA 47.17(8) 6 .
S2 Pr NiA 122.74(4) 6_554 .
S3 Pr NiA 129.95(8) . .
S2 Pr NiA 96.75(5) 2 .
S1 Pr NiA 94.46(8) 6_554 .
NiB Pr NiA 25.5(15) . .
S1 Pr NiA 46.91(4) 2 4_554
S1 Pr NiA 46.90(4) . 4_554
S2 Pr NiA 116.58(7) 5_564 4_554
S1 Pr NiA 96.23(8) 6 4_554
S2 Pr NiA 95.86(5) 6_554 4_554
S3 Pr NiA 161.926(16) . 4_554
S2 Pr NiA 118.64(4) 2 4_554
S1 Pr NiA 45.39(8) 6_554 4_554
NiB Pr NiA 23.6(15) . 4_554
NiA Pr NiA 49.067(5) . 4_554
NiB NiA NiB 180.00(2) 4 .
NiB NiA S1 123.71(10) 4 3
NiB NiA S1 56.29(10) . 3
NiB NiA S1 123.71(10) 4 2
NiB NiA S1 56.29(10) . 2
S1 NiA S1 92.17(14) 3 2
NiB NiA S1 123.71(10) 4 .
NiB NiA S1 56.29(10) . .
S1 NiA S1 92.17(14) 3 .
S1 NiA S1 92.17(14) 2 .
NiB NiA S1 56.12(10) 4 6
NiB NiA S1 123.88(10) . 6
S1 NiA S1 179.8(2) 3 6
S1 NiA S1 87.95(2) 2 6
S1 NiA S1 87.95(2) . 6
NiB NiA S1 56.12(10) 4 5
NiB NiA S1 123.88(10) . 5
S1 NiA S1 87.95(2) 3 5
S1 NiA S1 179.8(2) 2 5
S1 NiA S1 87.95(2) . 5
S1 NiA S1 91.93(14) 6 5
NiB NiA S1 56.12(10) 4 4
NiB NiA S1 123.88(10) . 4
S1 NiA S1 87.95(2) 3 4
S1 NiA S1 87.95(2) 2 4
S1 NiA S1 179.8(2) . 4
S1 NiA S1 91.93(14) 6 4
S1 NiA S1 91.93(14) 5 4
NiB NiA NiA 0.000(11) 4 4
NiB NiA NiA 180.0 . 4
S1 NiA NiA 123.71(10) 3 4
S1 NiA NiA 123.71(10) 2 4
S1 NiA NiA 123.71(10) . 4
S1 NiA NiA 56.12(10) 6 4
S1 NiA NiA 56.12(10) 5 4
S1 NiA NiA 56.12(10) 4 4
NiB NiA NiA 180.000(12) 4 4_554
NiB NiA NiA 0.0 . 4_554
S1 NiA NiA 56.29(10) 3 4_554
S1 NiA NiA 56.29(10) 2 4_554
S1 NiA NiA 56.29(10) . 4_554
S1 NiA NiA 123.88(10) 6 4_554
S1 NiA NiA 123.88(10) 5 4_554
S1 NiA NiA 123.88(10) 4 4_554
NiA NiA NiA 180.0 4 4_554
NiB NiA Pr 113.08(8) 4 2
NiB NiA Pr 66.92(8) . 2
S1 NiA Pr 53.09(5) 3 2
S1 NiA Pr 53.14(5) 2 2
S1 NiA Pr 123.21(17) . 2
S1 NiA Pr 126.93(4) 6 2
S1 NiA Pr 126.87(4) 5 2
S1 NiA Pr 56.96(5) 4 2
NiA NiA Pr 113.08(8) 4 2
NiA NiA Pr 66.92(8) 4_554 2
NiB NiA Pr 113.08(8) 4 .
NiB NiA Pr 66.92(8) . .
S1 NiA Pr 123.21(17) 3 .
S1 NiA Pr 53.09(5) 2 .
S1 NiA Pr 53.14(5) . .
S1 NiA Pr 56.96(5) 6 .
S1 NiA Pr 126.93(4) 5 .
S1 NiA Pr 126.87(4) 4 .
NiA NiA Pr 113.08(8) 4 .
NiA NiA Pr 66.92(8) 4_554 .
Pr NiA Pr 105.64(9) 2 .
NiA NiB NiA 180.0 4_554 .
NiA NiB S1 91(2) 4_554 3
NiA NiB S1 89(2) . 3
NiA NiB S1 91(2) 4_554 2
NiA NiB S1 89(2) . 2
S1 NiB S1 119.97(14) 3 2
NiA NiB S1 91(2) 4_554 .
NiA NiB S1 89(2) . .
S1 NiB S1 119.97(14) 3 .
S1 NiB S1 119.97(14) 2 .
NiA NiB NiB 0.0 4_554 4_554
NiA NiB NiB 180.0 . 4_554
S1 NiB NiB 91(2) 3 4_554
S1 NiB NiB 91(2) 2 4_554
S1 NiB NiB 91(2) . 4_554
NiA NiB NiB 180.0 4_554 4
NiA NiB NiB 0.0 . 4
S1 NiB NiB 89(2) 3 4
S1 NiB NiB 89(2) 2 4
S1 NiB NiB 89(2) . 4
NiB NiB NiB 180.0 4_554 4
NiA NiB Pr 92.4(15) 4_554 2
NiA NiB Pr 87.6(15) . 2
S1 NiB Pr 59.95(8) 3 2
S1 NiB Pr 60.02(8) 2 2
S1 NiB Pr 177(4) . 2
NiB NiB Pr 92.4(15) 4_554 2
NiB NiB Pr 87.6(15) 4 2
NiA NiB Pr 92.4(15) 4_554 .
NiA NiB Pr 87.6(15) . .
S1 NiB Pr 177(4) 3 .
S1 NiB Pr 59.95(8) 2 .
S1 NiB Pr 60.02(8) . .
NiB NiB Pr 92.4(15) 4_554 .
NiB NiB Pr 87.6(15) 4 .
Pr NiB Pr 119.8(2) 2 .
NiA NiB Pr 92.4(15) 4_554 3
NiA NiB Pr 87.6(15) . 3
S1 NiB Pr 60.02(9) 3 3
S1 NiB Pr 177(4) 2 3
S1 NiB Pr 59.95(8) . 3
NiB NiB Pr 92.4(15) 4_554 3
NiB NiB Pr 87.6(15) 4 3
Pr NiB Pr 119.8(2) 2 3
Pr NiB Pr 119.8(2) . 3
S3 Ge S2 113.02(5) . 6
S3 Ge S2 113.02(5) . 4_665
S2 Ge S2 105.70(5) 6 4_665
S3 Ge S2 113.02(5) . 5_565
S2 Ge S2 105.70(5) 6 5_565
S2 Ge S2 105.70(5) 4_665 5_565
NiB S1 NiA 35(2) . .
NiB S1 NiA 33(2) . 4_554
NiA S1 NiA 67.60(3) . 4_554
NiB S1 Pr 78.18(9) . 3
NiA S1 Pr 79.09(4) . 3
NiA S1 Pr 81.25(4) 4_554 3
NiB S1 Pr 78.12(9) . .
NiA S1 Pr 79.05(4) . .
NiA S1 Pr 81.20(4) 4_554 .
Pr S1 Pr 155.92(5) 3 .
NiB S1 Pr 109(2) . 5_554
NiA S1 Pr 143.47(11) . 5_554
NiA S1 Pr 75.87(11) 4_554 5_554
Pr S1 Pr 95.80(6) 3 5_554
Pr S1 Pr 95.75(5) . 5_554
NiB S1 Pr 110(2) . 5
NiA S1 Pr 74.91(11) . 5
NiA S1 Pr 142.50(11) 4_554 5
Pr S1 Pr 92.00(5) 3 5
Pr S1 Pr 91.95(5) . 5
Pr S1 Pr 141.63(5) 5_554 5
Ge S2 Pr 91.21(5) 4_664 6_655
Ge S2 Pr 88.79(5) 4_664 5
Pr S2 Pr 110.07(5) 6_655 5
Ge S2 Pr 121.38(6) 4_664 3
Pr S2 Pr 142.03(5) 6_655 3
Pr S2 Pr 91.03(4) 5 3
Ge S3 Pr 113.19(5) . 3_565
Ge S3 Pr 113.18(5) . .
Pr S3 Pr 105.52(5) 3_565 .
Ge S3 Pr 113.18(5) . 2_665
Pr S3 Pr 105.52(5) 3_565 2_665
Pr S3 Pr 105.52(5) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr S1 2.7976(13) 2
Pr S1 2.8001(13) .
Pr S2 2.8852(14) 5_564
Pr S1 2.970(2) 6
Pr S2 2.9788(15) 6_554
Pr S3 3.0185(11) .
Pr S2 3.0221(14) 2
Pr S1 3.144(2) 6_554
Pr NiB 3.164(3) .
Pr NiA 3.436(2) .
Pr NiA 3.516(2) 4_554
NiA NiB 1.41(8) 4
NiA NiB 1.48(8) .
NiA S1 2.593(3) 3
NiA S1 2.593(3) 2
NiA S1 2.593(3) .
NiA S1 2.598(3) 6
NiA S1 2.598(3) 5
NiA S1 2.598(3) 4
NiA NiA 2.88760(9) 4
NiA NiA 2.88760(10) 4_554
NiA Pr 3.436(2) 2
NiB NiA 1.41(8) 4_554
NiB S1 2.157(2) 3
NiB S1 2.157(2) 2
NiB S1 2.157(2) .
NiB NiB 2.88758(10) 4_554
NiB NiB 2.88762(10) 4
NiB Pr 3.164(3) 2
NiB Pr 3.164(3) 3
Ge S3 2.172(3) .
Ge S2 2.2216(15) 6
Ge S2 2.2217(15) 4_665
Ge S2 2.2217(15) 5_565
S1 NiA 2.598(3) 4_554
S1 Pr 2.7977(13) 3
S1 Pr 2.970(2) 5_554
S1 Pr 3.144(2) 5
S2 Ge 2.2217(15) 4_664
S2 Pr 2.8852(14) 6_655
S2 Pr 2.9788(15) 5
S2 Pr 3.0221(14) 3
S3 Pr 3.0184(11) 3_565
S3 Pr 3.0185(11) 2_665
