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#$Date: 2021-02-18 12:20:21 +0200 (Thu, 18 Feb 2021) $
#$Revision: 262067 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560472.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_1560472
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     'Y3 Pd0.50 Si S7'
_chemical_formula_sum            'Pd0.5 S7 Si Y3'
_chemical_formula_weight         572.44
_chemical_name_common
'yttrium palladium silicon sulfide (3/0.5/1/7)'
_chemical_name_systematic
'yttrium palladium silicon 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                   9.7891(3)
_cell_length_b                   9.7891(3)
_cell_length_c                   5.6840(4)
_cell_measurement_reflns_used    2429
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.40
_cell_volume                     471.70(4)
_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 0.998
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6928
_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         33.131
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.824
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXL-2014/7 (Sheldrick, 2014)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.030
_exptl_crystal_description       irregular
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.954
_refine_diff_density_min         -1.845
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         1197
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0413
_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)+(0.0491P)²+0.7772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                989
_reflns_number_total             1197
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc22.cif
_cod_data_source_block           11
_cod_original_formula_sum        'Pd0.50 S7 Si Y3'
_cod_database_code               1560472
_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   0.405
_shelx_estimated_absorpt_t_max   0.429
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
Y Y 0.13099(9) 0.35711(9) 0.0286(2) 0.0256(2) Uani 1 1 d . . . . .
PdA Pd 0.0000 0.0000 0.2459(6) 0.0269(6) Uani 0.443(3) 3 d S T P . .
PdB Pd 0.0000 0.0000 -0.063(5) 0.0269(6) Uani 0.057(3) 3 d S T P . .
Si Si 0.3333 0.6667 0.6140(7) 0.0202(8) Uani 1 3 d S T P . .
S1 S 0.2524(3) 0.1591(3) 0.0000(6) 0.0382(6) Uani 1 1 d . . . . .
S2 S 0.5233(3) 0.1048(3) 0.2631(4) 0.0226(4) Uani 1 1 d . . . . .
S3 S 0.3333 0.6667 0.2455(7) 0.0239(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
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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 Y S1 86.61(12) 2 .
S1 Y S2 104.62(9) 2 5_564
S1 Y S2 140.46(10) . 5_564
S1 Y S1 80.07(9) 2 6
S1 Y S1 79.84(9) . 6
S2 Y S1 138.95(8) 5_564 6
S1 Y S2 140.02(10) 2 6_554
S1 Y S2 73.80(8) . 6_554
S2 Y S2 73.68(9) 5_564 6_554
S1 Y S2 128.04(8) 6 6_554
S1 Y S3 148.06(9) 2 .
S1 Y S3 116.61(7) . .
S2 Y S3 72.16(7) 5_564 .
S1 Y S3 82.80(9) 6 .
S2 Y S3 70.86(7) 6_554 .
S1 Y S2 70.85(8) 2 2
S1 Y S2 145.53(9) . 2
S2 Y S2 72.32(4) 5_564 2
S1 Y S2 71.02(7) 6 2
S2 Y S2 139.44(6) 6_554 2
S3 Y S2 78.15(6) . 2
S1 Y PdB 43.57(8) 2 .
S1 Y PdB 43.50(8) . .
S2 Y PdB 130.4(4) 5_564 .
S1 Y PdB 81.1(5) 6 .
S2 Y PdB 106.6(3) 6_554 .
S3 Y PdB 156.6(3) . .
S2 Y PdB 112.1(2) 2 .
S1 Y S1 74.72(8) 2 6_554
S1 Y S1 74.54(8) . 6_554
S2 Y S1 72.32(8) 5_564 6_554
S1 Y S1 144.77(11) 6 6_554
S2 Y S1 66.67(7) 6_554 6_554
S3 Y S1 130.39(9) . 6_554
S2 Y S1 121.26(7) 2 6_554
PdB Y S1 63.7(5) . 6_554
S1 Y PdA 49.46(7) 2 .
S1 Y PdA 49.40(7) . .
S2 Y PdA 154.01(6) 5_564 .
S1 Y PdA 49.48(8) 6 .
S2 Y PdA 123.19(5) 6_554 .
S3 Y PdA 129.78(9) . .
S2 Y PdA 96.67(6) 2 .
PdB Y PdA 31.6(5) . .
S1 Y PdA 95.30(8) 6_554 .
S1 Y PdA 47.96(7) 2 4_554
S1 Y PdA 47.92(7) . 4_554
S2 Y PdA 114.36(7) 5_564 4_554
S1 Y PdA 99.12(8) 6 4_554
S2 Y PdA 95.24(6) 6_554 4_554
S3 Y PdA 162.91(3) . 4_554
S2 Y PdA 118.63(5) 2 4_554
PdB Y PdA 18.0(5) . 4_554
S1 Y PdA 45.65(7) 6_554 4_554
PdA Y PdA 49.643(13) . 4_554
PdB PdA PdB 180.0 4 .
PdB PdA S1 122.87(9) 4 3
PdB PdA S1 57.13(9) . 3
PdB PdA S1 122.87(9) 4 2
PdB PdA S1 57.13(9) . 2
S1 PdA S1 93.34(13) 3 2
PdB PdA S1 122.87(9) 4 .
PdB PdA S1 57.13(9) . .
S1 PdA S1 93.34(13) 3 .
S1 PdA S1 93.34(13) 2 .
PdB PdA S1 56.28(9) 4 6
PdB PdA S1 123.72(9) . 6
S1 PdA S1 179.14(17) 3 6
S1 PdA S1 87.25(5) 2 6
S1 PdA S1 87.25(5) . 6
PdB PdA S1 56.28(9) 4 5
PdB PdA S1 123.72(9) . 5
S1 PdA S1 87.25(5) 3 5
S1 PdA S1 179.14(17) 2 5
S1 PdA S1 87.25(5) . 5
S1 PdA S1 92.16(13) 6 5
PdB PdA S1 56.28(9) 4 4
PdB PdA S1 123.72(9) . 4
S1 PdA S1 87.25(5) 3 4
S1 PdA S1 87.25(5) 2 4
S1 PdA S1 179.14(17) . 4
S1 PdA S1 92.16(13) 6 4
S1 PdA S1 92.16(13) 5 4
PdB PdA PdA 180.0 4 4_554
PdB PdA PdA 0.0 . 4_554
S1 PdA PdA 57.13(9) 3 4_554
S1 PdA PdA 57.13(9) 2 4_554
S1 PdA PdA 57.13(9) . 4_554
S1 PdA PdA 123.72(9) 6 4_554
S1 PdA PdA 123.72(9) 5 4_554
S1 PdA PdA 123.72(9) 4 4_554
PdB PdA PdA 0.000(4) 4 4
PdB PdA PdA 180.0 . 4
S1 PdA PdA 122.87(9) 3 4
S1 PdA PdA 122.87(9) 2 4
S1 PdA PdA 122.87(9) . 4
S1 PdA PdA 56.28(9) 6 4
S1 PdA PdA 56.28(9) 5 4
S1 PdA PdA 56.28(9) 4 4
PdA PdA PdA 180.0 4_554 4
PdB PdA Y 111.96(6) 4 .
PdB PdA Y 68.04(6) . .
S1 PdA Y 125.17(13) 3 .
S1 PdA Y 53.51(6) 2 .
S1 PdA Y 53.82(6) . .
S1 PdA Y 55.69(7) 6 .
S1 PdA Y 126.55(6) 5 .
S1 PdA Y 126.24(6) 4 .
PdA PdA Y 68.04(6) 4_554 .
PdA PdA Y 111.96(6) 4 .
PdB PdA Y 111.96(6) 4 2
PdB PdA Y 68.04(6) . 2
S1 PdA Y 53.51(6) 3 2
S1 PdA Y 53.82(6) 2 2
S1 PdA Y 125.17(13) . 2
S1 PdA Y 126.55(6) 6 2
S1 PdA Y 126.24(6) 5 2
S1 PdA Y 55.69(7) 4 2
PdA PdA Y 68.04(6) 4_554 2
PdA PdA Y 111.96(6) 4 2
Y PdA Y 106.87(6) . 2
PdA PdB PdA 180.0 4_554 .
PdA PdB S1 99.4(7) 4_554 3
PdA PdB S1 80.6(7) . 3
PdA PdB S1 99.4(7) 4_554 2
PdA PdB S1 80.6(7) . 2
S1 PdB S1 117.4(4) 3 2
PdA PdB S1 99.4(7) 4_554 .
PdA PdB S1 80.6(7) . .
S1 PdB S1 117.4(4) 3 .
S1 PdB S1 117.4(4) 2 .
PdA PdB PdB 0.0 4_554 4_554
PdA PdB PdB 180.0 . 4_554
S1 PdB PdB 99.4(7) 3 4_554
S1 PdB PdB 99.4(7) 2 4_554
S1 PdB PdB 99.4(7) . 4_554
PdA PdB PdB 180.0 4_554 4
PdA PdB PdB 0.0 . 4
S1 PdB PdB 80.6(7) 3 4
S1 PdB PdB 80.6(7) 2 4
S1 PdB PdB 80.6(7) . 4
PdB PdB PdB 180.0 4_554 4
PdA PdB Y 99.7(5) 4_554 .
PdA PdB Y 80.3(5) . .
S1 PdB Y 160.9(12) 3 .
S1 PdB Y 58.90(13) 2 .
S1 PdB Y 59.27(13) . .
PdB PdB Y 99.7(5) 4_554 .
PdB PdB Y 80.3(5) 4 .
PdA PdB Y 99.7(5) 4_554 2
PdA PdB Y 80.3(5) . 2
S1 PdB Y 58.90(13) 3 2
S1 PdB Y 59.26(13) 2 2
S1 PdB Y 160.9(12) . 2
PdB PdB Y 99.7(5) 4_554 2
PdB PdB Y 80.3(5) 4 2
Y PdB Y 117.2(3) . 2
PdA PdB Y 99.7(5) 4_554 3
PdA PdB Y 80.3(5) . 3
S1 PdB Y 59.26(13) 3 3
S1 PdB Y 160.9(12) 2 3
S1 PdB Y 58.90(13) . 3
PdB PdB Y 99.7(5) 4_554 3
PdB PdB Y 80.3(5) 4 3
Y PdB Y 117.2(3) . 3
Y PdB Y 117.2(3) 2 3
S3 Si S2 113.41(12) . 6
S3 Si S2 113.41(12) . 4_665
S2 Si S2 105.26(13) 6 4_665
S3 Si S2 113.41(12) . 5_565
S2 Si S2 105.26(13) 6 5_565
S2 Si S2 105.26(13) 4_665 5_565
PdB S1 PdA 42.3(7) . .
PdB S1 PdA 24.3(7) . 4_554
PdA S1 PdA 66.59(7) . 4_554
PdB S1 Y 77.53(11) . 3
PdA S1 Y 77.03(8) . 3
PdA S1 Y 80.96(8) 4_554 3
PdB S1 Y 77.23(11) . .
PdA S1 Y 76.78(8) . .
PdA S1 Y 80.70(8) 4_554 .
Y S1 Y 152.36(12) 3 .
PdB S1 Y 99.1(7) . 5_554
PdA S1 Y 141.42(14) . 5_554
PdA S1 Y 74.83(10) 4_554 5_554
Y S1 Y 97.63(10) 3 5_554
Y S1 Y 97.31(9) . 5_554
PdB S1 Y 116.1(7) . 5
PdA S1 Y 73.80(10) . 5
PdA S1 Y 140.39(13) 4_554 5
Y S1 Y 90.66(9) 3 5
Y S1 Y 90.41(9) . 5
Y S1 Y 144.77(11) 5_554 5
Si S2 Y 91.79(10) 4_664 6_655
Si S2 Y 89.26(9) 4_664 5
Y S2 Y 109.42(9) 6_655 5
Si S2 Y 120.72(13) 4_664 3
Y S2 Y 142.18(8) 6_655 3
Y S2 Y 91.15(7) 5 3
Si S3 Y 114.82(7) . 3_565
Si S3 Y 114.82(7) . .
Y S3 Y 103.63(8) 3_565 .
Si S3 Y 114.82(7) . 2_665
Y S3 Y 103.63(8) 3_565 2_665
Y S3 Y 103.63(8) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y S1 2.725(3) 2
Y S1 2.739(3) .
Y S2 2.781(2) 5_564
Y S1 2.827(3) 6
Y S2 2.875(2) 6_554
Y S3 2.9366(18) .
Y S2 2.975(2) 2
Y PdB 3.107(5) .
Y S1 3.136(4) 6_554
Y PdA 3.3027(15) .
Y PdA 3.4588(18) 4_554
PdA PdB 1.08(3) 4
PdA PdB 1.76(3) .
PdA S1 2.576(3) 3
PdA S1 2.576(3) 2
PdA S1 2.576(3) .
PdA S1 2.601(4) 6
PdA S1 2.601(4) 5
PdA S1 2.601(4) 4
PdA PdA 2.8420(2) 4_554
PdA PdA 2.8420(2) 4
PdA Y 3.3027(15) 2
PdB PdA 1.08(3) 4_554
PdB S1 2.193(5) 3
PdB S1 2.193(5) 2
PdB S1 2.193(5) .
PdB PdB 2.8420(2) 4_554
PdB PdB 2.8420(2) 4
PdB Y 3.107(5) 2
PdB Y 3.107(5) 3
Si S3 2.094(5) .
Si S2 2.134(3) 6
Si S2 2.134(3) 4_665
Si S2 2.134(3) 5_565
S1 PdA 2.601(4) 4_554
S1 Y 2.725(3) 3
S1 Y 2.827(3) 5_554
S1 Y 3.136(4) 5
S2 Si 2.134(3) 4_664
S2 Y 2.781(2) 6_655
S2 Y 2.875(2) 5
S2 Y 2.975(2) 3
S3 Y 2.9366(18) 3_565
S3 Y 2.9366(18) 2_665
