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#$Date: 2025-07-06 19:43:28 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/83/7718309.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_7718309
loop_
_publ_author_name
'Panigrahi, Gopabandhu'
'Kashem, Habiba Binte'
'Morrison, Gregory'
'zur Loye, Hans-Conrad'
_publ_section_title
;
 Synthesis of a series of rare-earth-based multi-anion chalcogenide
 iodides RE3Si2SexS8−xI (RE = La, Ce, Pr, and Nd) using the
 flux-assisted boron--chalcogen mixture method
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              6252
_journal_page_last               6260
_journal_paper_doi               10.1039/D4DT03506B
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'I Pr3 S6.78 Se1.22 Si2'
_chemical_formula_weight         919.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-10-02 deposited with the CCDC.	2025-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9823(4)
_cell_length_b                   7.84960(10)
_cell_length_c                   10.8814(2)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      32.60
_cell_measurement_theta_min      2.57
_cell_volume                     1352.82(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35512
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.572
_diffrn_source                   'fine-focus seald tube'
_exptl_absorpt_coefficient_mu    17.384
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.3422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan (SADABS" Sheldrick, 2016/2)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    4.515
_exptl_crystal_description       rod
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0083
_refine_ls_R_factor_gt           0.0081
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+2.0797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0191
_refine_ls_wR_factor_ref         0.0191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2030
_reflns_number_total             2055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03506b2.cif
_cod_data_source_block           GP1077A3_OSC1
_cod_depositor_comments
'Adding full bibliography for 7718307--7718310.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7718309
_shelx_shelxl_version_number     2018/3
_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   0.780
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Pr1 Pr 0.30176(2) 0.12067(2) 0.31796(2) 0.01162(3) Uani 1 1 d . . . . .
Pr2 Pr 0.000000 0.09729(2) 0.250000 0.01363(3) Uani 1 2 d S T P . .
I1 I 0.000000 0.51425(2) 0.250000 0.02398(4) Uani 1 2 d S T P A .
S2 S 0.14413(2) 0.24725(4) 0.14619(3) 0.01359(10) Uani 0.8938(15) 1 d . . P A 10
S3 S 0.21678(2) 0.43113(4) 0.41511(3) 0.01250(10) Uani 0.8926(15) 1 d . . P A 12
S4 S 0.35047(2) 0.39981(4) 0.16192(3) 0.01238(11) Uani 0.9557(15) 1 d . . P A 14
Si1 Si 0.16002(2) 0.03757(5) 0.02851(4) 0.01051(7) Uani 1 1 d . . . . .
S1 S 0.06540(2) 0.16046(3) 0.54230(2) 0.01401(8) Uani 0.6471(15) 1 d . . P A 8
Se1 Se 0.06540(2) 0.16046(3) 0.54230(2) 0.01401(8) Uani 0.3529(15) 1 d . . P A 9
Se2 Se 0.14413(2) 0.24725(4) 0.14619(3) 0.01359(10) Uani 0.1062(15) 1 d . . P A
11
Se3 Se 0.21678(2) 0.43113(4) 0.41511(3) 0.01250(10) Uani 0.1074(15) 1 d . . P A
13
Se4 Se 0.35047(2) 0.39981(4) 0.16192(3) 0.01238(11) Uani 0.0443(15) 1 d . . P A
15
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
_geom_angle_publ_flag
S3 Pr1 S3 135.272(6) 4_545 . ?
S3 Pr1 S3 70.404(10) 7_556 . ?
S2 Pr1 S2 125.241(9) 4_545 . ?
S2 Pr2 S2 132.858(13) 2 . ?
S1 Pr2 S1 162.449(10) 2 . ?
S4 Pr2 I1 122.293(7) 3_445 . ?
S4 Pr2 I1 122.292(7) 4_545 . ?
S2 Pr2 I1 66.429(7) 2 . ?
S2 Pr2 I1 66.429(7) . . ?
Se2 Pr2 I1 66.429(7) . . ?
S1 Pr2 I1 81.225(5) 2 . ?
S1 Pr2 I1 81.225(5) . . ?
Se1 Pr2 I1 81.225(5) . . ?
S4 Pr2 S1 76.646(8) 3_445 6 ?
S4 Pr2 S1 64.976(8) 4_545 6 ?
S2 Pr2 S1 147.405(8) 2 6 ?
S2 Pr2 S1 69.330(8) . 6 ?
Se2 Pr2 S1 69.330(8) . 6 ?
S1 Pr2 S1 60.921(7) 2 6 ?
S1 Pr2 S1 132.280(7) . 6 ?
Se1 Pr2 S1 132.280(7) . 6 ?
I1 Pr2 S1 127.738(5) . 6 ?
I1 Pr2 S1 127.738(5) . 5_556 ?
Pr2 I1 Pr1 104.007(3) . 4 ?
Pr2 I1 Pr1 104.007(3) . 3_455 ?
Pr1 I1 Pr1 151.987(6) 4 3_455 ?
Si1 S2 Pr2 94.845(16) . . ?
Si1 S2 Pr1 139.815(17) . 4 ?
Pr2 S2 Pr1 123.734(11) . 4 ?
Si1 S2 Pr1 87.817(15) . . ?
Pr2 S2 Pr1 104.807(10) . . ?
Pr1 S2 Pr1 92.133(9) 4 . ?
Si1 S3 Pr1 91.852(15) 4 4 ?
Si1 S3 Pr1 88.954(14) 4 7_556 ?
Pr1 S3 Pr1 154.421(12) 4 7_556 ?
Si1 S3 Pr1 88.629(15) 4 . ?
Pr1 S3 Pr1 95.983(9) 4 . ?
Pr1 S3 Pr1 109.595(10) 7_556 . ?
Si1 S4 Pr2 98.810(16) 7 3 ?
Si1 S4 Pr1 138.324(19) 7 . ?
Pr2 S4 Pr1 118.519(12) 3 . ?
Si1 S4 Pr1 88.779(16) 7 4 ?
Pr2 S4 Pr1 107.777(11) 3 4 ?
Pr1 S4 Pr1 96.188(10) . 4 ?
S4 Si1 S1 105.52(2) 7 6 ?
S2 Si1 S1 111.73(2) . 6 ?
Se2 Si1 S1 111.73(2) . 6 ?
S3 Si1 S1 108.61(2) 4_545 6 ?
Si1 S1 Pr1 89.592(13) 6_556 7_556 ?
Si1 S1 Pr2 87.658(13) 6_556 . ?
Pr1 S1 Pr2 134.426(9) 7_556 . ?
Si1 S1 Pr2 84.076(13) 6_556 5_556 ?
Pr1 S1 Pr2 105.815(8) 7_556 5_556 ?
Pr2 S1 Pr2 119.078(8) . 5_556 ?
Si1 Se1 Pr1 89.592(13) 6_556 7_556 ?
Si1 Se1 Pr2 87.658(13) 6_556 . ?
Pr1 Se1 Pr2 134.426(9) 7_556 . ?
Si1 Se1 Pr2 84.076(13) 6_556 5_556 ?
Pr1 Se1 Pr2 105.815(8) 7_556 5_556 ?
Pr2 Se1 Pr2 119.078(8) . 5_556 ?
Si1 Se2 Pr2 94.845(16) . . ?
Si1 Se2 Pr1 139.815(17) . 4 ?
Pr2 Se2 Pr1 123.734(11) . 4 ?
Si1 Se2 Pr1 87.817(15) . . ?
Pr2 Se2 Pr1 104.807(10) . . ?
Pr1 Se2 Pr1 92.133(9) 4 . ?
Si1 Se3 Pr1 91.852(15) 4 4 ?
Si1 Se3 Pr1 88.954(14) 4 7_556 ?
Pr1 Se3 Pr1 154.421(12) 4 7_556 ?
Si1 Se3 Pr1 88.629(15) 4 . ?
Pr1 Se3 Pr1 95.983(9) 4 . ?
Pr1 Se3 Pr1 109.595(10) 7_556 . ?
Si1 Se4 Pr2 98.810(16) 7 3 ?
Si1 Se4 Pr1 138.324(19) 7 . ?
Pr2 Se4 Pr1 118.519(12) 3 . ?
Si1 Se4 Pr1 88.779(16) 7 4 ?
Pr2 Se4 Pr1 107.777(11) 3 4 ?
Pr1 Se4 Pr1 96.188(10) . 4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 S3 2.9209(3) 4_545 ?
Pr1 Se4 2.9401(3) . ?
Pr1 S4 2.9401(3) . ?
Pr1 S1 2.9844(3) 7_556 ?
Pr1 S3 2.9867(3) 7_556 ?
Pr1 S4 3.0192(4) 4_545 ?
Pr1 S3 3.0472(3) . ?
Pr1 Se3 3.0472(3) . ?
Pr1 S2 3.0662(3) 4_545 ?
Pr1 Se2 3.0929(3) . ?
Pr1 S2 3.0929(3) . ?
Pr1 I1 3.45120(12) 3_545 ?
Pr2 S4 2.9016(3) 3_445 ?
Pr2 S4 2.9016(3) 4_545 ?
Pr2 S2 2.9437(3) 2 ?
Pr2 S2 2.9437(3) . ?
Pr2 Se2 2.9437(3) . ?
Pr2 S1 3.2502(3) 2 ?
Pr2 S1 3.2502(2) . ?
Pr2 Se1 3.2502(2) . ?
Pr2 I1 3.2730(2) . ?
Pr2 S1 3.3056(3) 6 ?
Pr2 S1 3.3056(3) 5_556 ?
S2 Si1 2.1214(5) . ?
S3 Si1 2.1513(5) 4 ?
S4 Si1 2.1143(5) 7 ?
Si1 Se2 2.1214(5) . ?
Si1 S1 2.1878(5) 6 ?
